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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a technique for controlling the operation of a pump, including providing a method of controlling the operation of a pump at a constant pressure using motor current as a sensing parameter and motor voltage as a controlling parameter.
[0003] More particularly, the present invention relates to a method and apparatus using a pump control to keep an outlet pressure constant based at least partly on sensing motor current and a unique algorithm of tracking the V-I characteristics of a pump.
[0004] 2. Brief Description of Related Art
[0005] Many pumps known in the art include a mechanical pressure switch, or semiconductor hall sensors, or load cells, or any other type of electronic pressure sensing device, that shuts off the pump when certain pressure (i.e., the shut-off pressure) is exceeded. The pressure switch, hall sensor or load cell is typically positioned in physical communication with the fluid in the pump. When the pressure of the fluid exceeds the shut-off pressure, the force of the fluid moves the mechanical switch to open the pump's power circuit or generates corresponding electrical signal to trace the set pressure. Mechanical switches have several limitations. For example, during the repeated opening and closing of the pump's power circuit, arcing and scorching often occurs between the contacts of the switch. The pressure cannot remain constant because of the non-repetitive and/or non-linear behavior. So relying totally on the pressure switch or sensor will always give an inconsistence control loop.
[0006] In view of this, there is a need in the art for an improved pump controller that solves the problems related to the mechanical pressure switches or sensors in the known pump designs.
SUMMARY OF THE INVENTION
[0007] To overcome the aforementioned problems with the mechanical pressure switch and pressure sensor, a new technique is provided using current sensing to control the pressure at a constant level without the direct sensing of the pressure. This new technique will help to reduce the dependency solely on the pressure switch or sensor and their non linearity and other associated problems such as the non-repetitive behavior, as well as other known problems associated with being affected by electromagnetic interference (EMI), etc.
[0008] According to some embodiments, the present invention may take the form of apparatus, such as a pump controller, featuring one or more modules configured to respond to one or more input signals containing information about current provided from a pump; and also configured to provide one or more output signals containing information to control the pump to operate at a substantially constant pressure without the direct sensing of pump pressure.
[0009] Embodiments of the present invention may also include one or more of the following features:
[0010] For example, the one or more modules may be configured to control the operation of the pump based at least partly on a table of characteristics related to voltage and current that is calibrated for each pump, where the characteristics may be determined with the following equation:
[0000]
I=Vm+C,
[0000] where
[0000] m =( I 1 −I 2)/( V 1 −V 2),
[0000] C =( V 1 *I 2 −V 2 *I 1)/( V 1 −V 2), (V1, I1): Low point of curve, and (V2, I2): High point of curve.
The one or more input signals may contain information about a sensed actual motor current to operate the pump, and the one or more output signals may contain information about a voltage read from the table that corresponds to the sensed actual motor current. The one or more input signals may also contain information about a comparison of the sensed actual motor current with a set current. The one or more modules may also be configured to provide a correction term to control the pump to operate at the substantially constant pressure.
[0013] Either the one or more modules or the apparatus as a whole may be configured as a PID controller for controlling the operation of the pump.
[0014] The apparatus may also take the form of a controller featuring one or more signal processing modules configured to respond to one or more input signals containing information about current provided from a pump; and configured to provide one or more output signals containing information to control the pump to operate at a substantially constant pressure without the direct sensing of pump pressure. Embodiments of the controller may include one or more of the features described herein. The controller may also form part of a pumping system or arrangement that includes the pump.
[0015] The present invention may also take the form of a method featuring steps for controlling the pump, including responding to one or more input signals containing information about current provided from a pump; and providing one or more output signals containing information to control the pump to operate at a substantially constant pressure without the direct sensing of pump pressure. Embodiments of the method may include steps for implementing one or more of the features described herein.
[0016] The present invention may also take the form of a computer program product having a computer readable medium with a computer executable code embedded therein for implementing the steps of the method when run on a signaling processing device that forms part of such a pump controller like element 10 . By way of example, the computer program product may take the form of a CD, a floppy disk, a memory stick, a memory card, as well as other types or kind of memory devices that may store such a computer executable code on such a computer readable medium either now known or later developed in the future.
BRIEF DESCRIPTION OF THE DRAWING
[0017] The drawing includes the following Figures, not drawn to scale:
[0018] FIG. 1 includes FIGS. 1 a and 1 b , where FIG. 1 a is a block diagram of apparatus, including a pump controller, according to some embodiments of the present invention; and where FIG. 1 b is a block diagram of flowchart of a method for implementing the apparatus of FIG. 1 a according to some embodiments of the present invention.
[0019] FIG. 2 is a graph of head-flow characteristics for a diaphragm pump.
[0020] FIG. 3 is a graph of current in relation to voltage showing V-I characteristics at a constant pressure of, e.g., 30 pounds per square inch (PSI) for a diaphragm pump.
[0021] FIG. 4 is a block diagram of apparatus, including a pump system having a controller, according to some embodiments of the present invention.
[0022] FIG. 5 shows a graph of current in relation to voltage having V-I characteristics for desired current and achieved current at a constant pressure for a diaphragm pump according to some embodiments of the present invention.
[0023] FIG. 6 , which includes FIGS. 6 a through 6 h , shows a functional flow chart showing steps for implementing the apparatus according to some embodiments of the present invention.
[0024] FIG. 7 shows a graph having a flow curve/operating envelope that forms part of PSI in relation to gallon per minute (GPM) according to some embodiments of the present invention.
[0025] FIG. 8 shows flow chart showing light emitting diode (LED) indicator codes according to some embodiments of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0026] FIGS. 1 a shows apparatus in the form of a pump controller generally indicated as 10 featuring one or more modules 12 and 14 . The one or more modules 12 is configured to respond to one or more input signals containing information about current provided from a pump (see element 30 ( FIG. 4 ); and also configured to provide one or more output signals containing information to control the pump 30 ( FIG. 4 ) to operate at a substantially constant pressure without the direct sensing of pump pressure.
[0027] According to some embodiments of the present invention, the one or more modules 12 may be configured to control the operation of the pump 30 ( FIG. 4 ) based at least partly on a table of characteristics related to voltage and current that is calibrated for each pump, where the characteristics may be determined with the following equation:
[0000]
I=Vm+C,
[0000] where
[0000] m =( I 1 −I 2)/( V 1− V 2),
[0000] C =( V 1 *I 2 −V 2 *I 1)/( V 1 −V 2), (V1, I1): Low point of curve, and (V2, I2): High point of curve.
The one or more input signals may contain information about a sensed actual motor current to operate the pump, and the one or more output signals may contain information about a voltage read from a calibration table that corresponds to the sensed actual motor current. The one or more input signals may also contain information about a comparison of the sensed actual motor current with a set current. The one or more modules 12 may also be configured to provide a correction term to control the pump to operate at the substantially constant pressure.
[0030] Either the one or more modules 12 or the apparatus 10 as a whole may be configured as, or form part of, a module (see element 40 ( FIG. 4 )) having a PID controller 41 along with other components or modules 42 , 44 , 46 , 48 described below for controlling the operation of the pump 30 . As shown, the module 40 includes, e.g., one or more signal processing modules configured to perform the signal processing for implementing the functionality of the present invention. The PID controller 40 may also form part of a pumping system or arrangement generally indicated as 50 in FIG. 4 for controlling the operation of the pump 30 .
[0031] The one or more modules 14 may include other modules that may form part of the pump controller to implement other controller functionality that does not form part of the underlying invention, e.g., including input/output functionality for processing signaling to and from a pump/motor, a sensing device, etc., as well as functionality associated with other devices or components, e.g., including a random access memory (RAM) type device, a read only memory (ROM) type device, control and data bus type devices, etc.
[0032] The calibration table may form part of, e.g., a memory storage device. The memory storage device itself may form part of the one or more modules 12 , the one or more other modules 14 , or some combination thereof. Memory storage devices are known in the art, and the scope of the invention is not intended to be limitation to any particular type or kind thereof either now known or later developed in the future.
[0033] The present invention may also take the form of a method shown in FIG. 1 b having steps 22 , 24 that form part of a flowchart generally indicated as 20 for controlling the pump 30 ( FIG. 4 ), including responding to one or more input signals containing information about current provided from the pump 30 , e.g. along signal path 42 a ( FIG. 4 ); and providing one or more output signals, e.g. along signal path 41 a ( FIG. 4 ), containing information to control the pump 30 to operate at a substantially constant pressure without the direct sensing of pump pressure.
Basic Pump Principle and the Building of the Table
[0034] The above indirect relationship between current and pressure according to the present invention is based at least partly on the built-up and working principle of general diaphragm pumps consistent with the following:
[0035] As a person skilled in the art would appreciate, in a typical diaphragm pump voltage is applied to a motor which in turn will rotate a rotor. The rotational motion will be transferred to a piston by a cam. The piston will in turn convert the rotational motion into linear motion. The linear motion of the piston to a diaphragm will force fluid from the pump's inlet to its outlet. This force in the outlet area will generate the pressure in fluid flowing out of the outlet.
[0036] In operation, if the demand at the pump's outlet is decreased, then the pressure at the outlet will increase. However, the pump is still rotating at the same speed as before. Because of this, the current will start increasing at the motor in response to the increased pressure. In the same way, if the pressure at the pump's outlet is decreased for the desired pressure, then the current flowing from the motor will decrease as the demand of torque to generate more pressure decreases.
[0037] By way of example, FIG. 2 is provided to show the general head-flow characteristics for a typical diaphragm pump. From the characteristics, the current and voltage are understood to be substantially unique for the head-flow desired. Another important outcome is that the pressure at the two different flow rates is understood not to substantially have the same voltage and current at any given time.
[0038] To support the understanding of the aforementioned principle, FIG. 3 is provided to show a V-I characteristic at a constant pressure for a typical diaphragm pump, which forms the basis for the table or table look-up technique according to the present invention.
[0039] The V-I characteristics can be determined by varying the voltages applied to the pump for its entire operating range (e.g. from 8.5 V to 14.8V for +12V motor and without any control electronics, i.e. a variable speed drive (VSD)) and plotting the current by keeping the pressure constant which is the desired constant pressure at which the pump needs to be maintained when it is in its intended normal operation (e.g., 30 PSI).
[0040] It is understood that the respective V-I characteristics in FIG. 3 that determine the table for a given pump are unique for that given pump since V-I characteristics substantially depend on the motor characteristics of that given pump, which typically vary from one motor when compared to another motor. In other words, according to the present invention respective V-I characteristics will be sensed and determined for each pump and a respective table will be formulated for each pump that are unique for each pump, and used to control each pump.
[0041] Once the V-I characteristics for the given pump are determined, any controller or control system may be implemented to control the pump at the constant pressure by looking up and following the above obtained trend line (V-I characteristics) using the table loop-up technique according to the present invention.
[0042] By way of example, FIG. 4 shows a diagram of a control block for a pump system 50 having a simple yet effective approaches according to some embodiments of the present invention. As shown, the control block or module 40 includes devices, components or modules such as the PI(D) controller module 41 , along with other components or modules 42 , 44 , 46 , 48 for controlling the operation of the pump 30 . The module 42 senses current from the motor along signal path 42 a , and provides a current sensing signal along signal path 42 b containing information about the sensed motor current. The module 44 is configured to respond to the current sensing signal along signal path 42 b , to measure current at a motor voltage, and provide a measured current signal along signal path 44 a containing information about the measured current at that motor voltage. The one or more input signals containing information about current provided from the pump 30 ( FIG. 4 ) includes the current sensing signal along signal path 42 b . The module 46 is configured to respond to a voltage output signal E along signal path 41 a provided from the PI(D) controller module 41 to the pump 30 along signal path 41 a for controlling the operation of the pump 30 , to set current at a particular voltage (calibration), and provide a signal along signal path 46 a containing information about the set current at the particular voltage (calibration). The node module 48 is configured to response to the signal along signal path 44 a containing information about the measured current at the motor voltage and the signal along signal path 46 a containing information about the set current at the particular voltage (calibration), and provide a signal e along signal path 48 a to the PI(D) module 41 containing information about the two signals. Consistent with that described in further detail below, the signal e provided from the node module 48 to the PI(D) module 41 along signal path 48 a contains information about an error between the set current and sensed actual motor current that will be used as input parameter for the PID controller 41 . The PI(D) module 41 is configured to respond to one or more input signals, including the signal e along signal path 48 a that contains information about current provided from the pump 30 , as well as voltage output signal E along signal path 41 a provided from the PI(D) controller module 41 to the pump 30 along signal path 41 a for controlling the operation of the pump 30 the voltage signal E along signal path 41 a to the pump 30 along signal path 41 a for controlling the operation of the pump 30 . Consistent with that described in further detail below, the voltage signal E from the PI(D) module 41 to the pump 30 along signal path 41 a will contain the correction term to the motor voltage to get the desire pressure. The one or more output signals containing information to control the pump 30 ( FIG. 4 ) to operate at the substantially constant pressure without the direct sensing of pump pressure includes the voltage output signal E along signal path 41 a . In operation, the voltage output signal E along signal path 41 a for controlling the operation of the pump 30 is effectively corrected or modified based at least partly on the control feedback system shown in FIG. 4 that depends on a relationship between the sensed motor current and the information contained in the table calibrated for the respective pump 30 so as to operate the respective pump 30 at the substantially constant pressure without the direct sensing of pump pressure.
[0043] The scope of the invention is not intended to be limited to the type or kind of signal path being used to exchange signal between the components or modules shown and described herein. Embodiments are envisioned using signal paths that are hard wired between the components or modules shown and described herein, or wireless communication couplings between the components or modules shown and described herein, or some combination thereof, as well as other types or kinds of signal paths either now known or later developed in the future.
[0044] FIG. 5 shows a graph of current in relation to voltage having V-I characteristics for desired current indicated as D (shown as having a lighter colored function) and achieved current indicated as A (shown as having a darker colored function) at a constant pressure without the direct sensing of pump pressure for controlling the operation of a diaphragm pump according to some embodiments of the present invention. In operation, the one or more modules 12 ( FIG. 1 ) or 41 ( FIG. 4 ) is configured to provide a correction term, e.g., in the form a modified voltage signal along signal path 41 a , to control the pump so as to operate at the substantially constant pressure, such that the desired current D and achieved current A have similar values at a similar motor voltage as shown in the graph FIG. 5 for controlling the operation of a diaphragm pump without the direct sensing of pump pressure, according to some embodiments of the present invention.
[0045] This control implementation according to the present invention as described herein provides a highly accurate, seamless yet easy to implement control algorithm, which provides a piece-wise linear approach that is easy to calibrate (obtain the V-I characteristics) and has less computational burden on the controller.
[0046] The reproduction of the V-I curve is done using the piece-wise linear method. According to the piece-wise linear method, the curve is divided in number (ideally infinite) small linear lines. Here one take two points (calibration point) and the relation between those two consecutive points will have the linear relation. This relation may be defined with following equation.
[0000]
I=Vm+C
[0000] m =( I 1 −I 2)/( V 1 −V 2)
[0000] C =( V 1 *I 2 −V 2 *I 1)/( V 1 −V 2) (V1, I1): Low point of curve; (V2, I2): High point of curve;
[0049] In normal condition, the pump will sense the actual motor current and apply the voltage to the motor. The same voltage will be sent to the set current prediction logic to get the set current for the desired pressure at the present motor voltage. The sensed actual motor current will be compared with the set current (desired current at that voltage for desired pressure—from the calibration table). The error between the set current and sensed actual motor current will be used as input parameter for the PID controller. The PID controller will generate the correction term to the motor voltage (controller by duty cycle) to get the desire pressure. Next time the above steps are repeated at a constant and very fast rate.
[0050] Once the algorithm is implemented consistent with that set forth herein, through electronics and signaling processing, the one or more output signals along signal path 41 a may be provided to get the output that gives the constant desired pressure at the pump's output through the predictive algorithm approach according to the present invention.
V-I Curve Equation
[0051] The following is a description regarding the V-I curve equation:
[0052] From a general linear equation:
[0000]
I=mV+C,
[0000] where: (V 1 , I 1 ): Low point of curve, and
(V 2 , I 2 ): High point of curve,
one has:
[0000]
I
-
I
2
I
1
-
I
2
=
V
-
V
2
V
1
-
V
2
I
-
I
2
=
(
V
-
V
2
)
(
I
1
-
I
2
)
(
V
1
-
V
2
)
I
=
(
I
1
-
I
2
)
V
V
1
-
V
2
-
V
2
(
I
1
-
I
2
)
V
1
-
V
2
+
I
2
Thus:
[0054]
m
=
(
I
1
-
I
2
)
V
1
-
V
2
C
=
V
2
(
I
2
-
I
1
)
V
1
-
V
2
+
I
2
C
=
V
2
(
I
2
-
I
1
)
+
I
2
(
V
1
-
V
2
)
V
1
-
V
2
Or
C
=
V
1
I
2
-
V
2
I
1
V
1
-
V
2
[0000] Based at least partly on this, the V-I Curve is:
[0000]
I
=
(
I
1
-
I
2
)
V
1
-
V
2
V
+
V
1
I
2
-
V
2
I
1
V
1
-
V
2
The Modules 12 , 41 , 42 , 44 , 46 or 48
[0055] By way of example, the functionality of the modules 12 , 41 , 42 , 44 , 46 or 48 may be implemented using hardware, software, firmware, or a combination thereof. In a typical software implementation, the modules 12 , 41 , 42 , 44 , 46 or 48 would include one or more microprocessor-based architectures having a microprocessor, a random access memory (RAM), a read only memory (ROM), input/output devices and control, data and address buses connecting the same. A person skilled in the art would be able to program such a microcontroller (or microprocessor)-based implementation to perform the functionality described herein without undue experimentation. The scope of the invention is not intended to be limited to any particular implementation using technology either now known or later developed in the future.
Possible Applications
[0056] Possible applications for the present invention include an implementation having some combination of the following features:
I. General Overview Description:
[0057] By way of example, the specification below is for the design and development of a variable speed drive pump controller (VSD) for a five chamber pump. By way of example, the applications for this specification may range from a water system to general industrial spraying, although the scope of the invention is not intended to be limited to the type of kind of application either now known or later developed in the future.
II. Functional requirements
1. Application Ratings
[0000]
1.1. Work in salt and fresh water environments.
1.2. Voltage 1.2.1. Direct Current Unit—9.5 VDC-28.0 VDC 1.2.2. Alternating Current Unit—85 VAC-250 VAC—Phase two of the project to be completed after completion of the DC version.
2. Abbreviations & Definitions
[0000]
2.1. Abbreviations
2.1.1. #F—Number of outlets/valves/faucets 2.1.2. C#—Flow curve at various voltages 2.1.3. P#—Point of Rating at various pressures and flow 2.1.4. GPM—Gallons Per Minutes 2.1.5. VDC—Voltage Direct Current 2.1.6. VAC—Voltage Alternating Current 2.1.7. MTBF—Mean time between failure 2.1.8. PSI—Pounds per square inch
2.2. Definitions
2.2.1. Outlet—Any flow output of the system 2.2.2. Run Dry—Occurs when the liquid supplied to the pump is either removed or the supply is exhausted. 2.2.3. Prime—The amount of time it takes for the pump to draw water and begin pumping.
3. Performance/Life Expectancy
[0000]
3.1. Performance
3.1.1 Functional Operations (See FIGS. 6-8 )
3.1.1.1 With a VSD pump installed on a vessel/RV and appropriate power source connected, the pump controller, e.g. controller 10 ( FIG. 1 ) or module 40 ( FIG. 4 ), may also run a diagnostic test as set forth and described in FIG. 6 every time the pump experiences an On/Off power cycle. Under a normal operation mode, the water system should be pressurized and maintained at the designed value until a demand is required (outlet opened.) 3.1.1.2 When there is a demand (P 1 ), (P 2 ), or (P 3 ), the pump controller turns the pump on at full speed/voltage, the pump will presumably run outside the operating envelope (high amp/volt), the pump controller may detect this condition and slow down the pump until a preset value of amp/volt is achieved. It may maintain the operation of pump at this value until new condition arises and the pump controller may react to the new condition. All these actions typically happen in a very short time span, e.g., a fraction of a second. 3.1.1.3 As more demand (P 2 ) or (P 3 ) or (P 4 ) arises, the water system drops in pressure and the pump experiences a drop in load/amp draw. The pump controller may detect this new condition and slowly speed up the pump until a preset value (amp/volt) is achieved, and it may maintain the operation of the pump at this value until a new condition arises and the controller shall react to the new condition. This technique may be applied to all the operating points defined as the operating envelope depicted in FIG. 7 . 3.1.1.4 If a high demand (P 4 ) is required, the pump controller may maintain full speed/voltage to keep up with the demand until this condition is changed. 3.1.1.5 When a demand is no longer present (outlet closed), the pump experiences a high pressure above the operating pressure, a pressure switch may disconnect the power to the pump. 3.1.1.6 Run-Dry Protection—If there is no fluid in the tank/inlet of pump, the pump controller may detect this condition and shut pump off after some predetermine time, e.g. X minutes. The controller may also turn on pump from time to time to test the empty/leakage condition for some predetermined number of times and send error signal to LED. 3.1.1.7 Learning—During all modes of operation, the pump controller may “Learn” the operating range of voltage/amperage for future reference. The learning may allow the unit to transition in the variation smoothly with less time lost. 3.1.1.8 Over Current/Under Current—Controller may monitor for extremes in amperage outside the learned range, and it shall shut off and blink the LED 1 Blink when this condition happens. See FIGS. 6 and 8 . 3.1.1.9 Leak Detection—The unit may monitor for slow leaks over time, when the pump controller detects a slow leak over a period of time with no normal operation, the unit may shut the pump off. A slow leak typically manifests itself as a slow loss of pressure then the pump ramps up to pressure and shuts off. This occurs may occur constantly over time in a leaking situation. This feature can allow for some predetermined period of cycling then shut off and blink the LED 2 blinks. See FIGS. 6 and 8 3.1.1.10 Data Storage
The pump controller may also be configured to store data in on-board's memory, e.g. that may form part of the one or more other modules 14 , including the following incidents: a. Run Dry/Under Current—Record the number of run dry incidents b. Over Current/Motor stalling—Record the number of incidents c. On-Hours for normal operation d. On hours at the time of each incident e. Under voltage/Over voltage—Record the number of incidents f. Leak detection—Record the number of incidents g. Time out—Record the number of incidents
3.2 Life Expectancy—Recommended functional life (MTBF)>500 hours of the box to include operation and water ingress.
4 Physical Features and Dimensions
[0000]
4.1 VSD housing shall be defined to mount as a base of the motor.
4.2 Power connections may be 12 ″ pigtails of sufficient gauge to handle the 28 amperes and to allow for sufficient wiring from harness to be reliably connected.
4.3 Connections
4.3.1 Pump connections may be based upon the 8 pin Molex MX150 connector or equivalent to be molded into the
4.3.1.2: 2 pins for power in+1 earth pin connection 4.3.1.3: 2 pins for power to motor 4.3.1.4: 2 pins for pressure switch input 4.3.1.5: 2 pins for LED indicator and ON/OFF switch option.
These pins plugged unless needed.
5 Some additional Features
[0000]
5.1 Thermal overload protection
5.2 Unit shall also, in addition to the software over current protection, utilize hardware redundancy for over current protection.
5.3 Shall have hardware over current protection in the event that the software over current fails.
5.4 Shall conform to PCB outline(s) provided by ITT Flow Control
5.5 SMT/THT construction
5.6 Operating temperature range −10° F. to 150° F.
5.7 Protection from Amperage/Voltage Spikes
[0106] The advantages of above implementations are numerous, and by way of example, may include some of that which follows.
Universal equation Extends and fits any diaphragm pump characteristics and ratings (same software for 30 PSI, 60 PSI, 80 PSI etc pump) Software tunes to the particular motor characteristics Functionality primarily depends on the calibration Easy calibration Easy portability to AC operations also Greater number of self diagnostics features can be given (as most of the errors can be a function of current) Uses ecumenical advance algorithm The algorithm uses predication logic Common software may be fit in relation to any diaphragm pump characteristics and ratings (same software for 1 PSI to 250 PSI) once the current handling capabilities are met by the hardware Software could be self-calibrated or externally calibrated Software does not use any pressure “sensors” for its main computational algorithm and does all the calculation based on motor current; so “sensorless.” Software establishes a relationship between motor current and output pressure with its highly advanced algorithm its output pressure control requirements. Smooth and placid flow at the output. Discharge pressure remains constant for extended range flow requirements (approximately about 85% of total flow range). Minimal outlet flow variation with change in input voltages Rapid and swift response software algorithm with advanced and sophisticated on-board electronics control. Extended pump life as advanced software assimilate and absorbs all the voltages higher than rated voltages going to the motor. Subjugated heat generation in motor as a result of no voltages higher than rated one applied to pump. An array of indicative self diagnostics features provided with the help of superior combination of hardware and software; diagnostics features such as run dry, lock rotor, leak detection, timeout, over voltage, under voltage, over current, etc. Run-dry of the pump, leak detection in the system, timeout, over voltage, under voltage. These are categorized as system issues. Over current, no-current (under current), over heating of an enclosure are categorized as pump issues. These diagnostics are visual indication by blinking the LED at the output. LED output codes are broadly accumulated as “System” or “Pump” issues/errors LED output may also be given for each diagnostic feature individually by changing the error code module in the software On-board over temperature cut-off enhances the life of electronics and safe guards the product. Conserves water by having advanced leak detection feature.
The Scope of the Invention
[0134] It should be understood that, unless stated otherwise herein, any of the features, characteristics, alternatives or modifications described regarding a particular embodiment herein may also be applied, used, or incorporated with any other embodiment described herein. Also, the drawings herein are not drawn to scale.
[0135] Although the present invention is described by way of example in relation to a diaphragm pump, the scope of the invention is intended to include using the same in relation to other types or kinds of pumps either now known or later developed in the future.
[0136] Although the invention has been described and illustrated with respect to exemplary embodiments thereof, the foregoing and various other additions and omissions may be made therein and thereto without departing from the spirit and scope of the present invention.
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The present invention provides a technique using current sensing to control the pressure at constant level without the direct sensing of the pressure. This technique will help to reduce dependency solely on switch or sensor and their non linearity and other associated problems such as the non-repetitive behavior, being affected by EMI etc. The technique includes using a pump controller featuring one or more modules configured to respond to one or more input signals containing information about current provided from a pump; and configured to provide one or more output signals containing information to control the pump to operate at a substantially constant pressure without the direct sensing of pump pressure. The one or more modules control the operation of the pump based at least partly on a table of characteristics related to voltage and current that is calibrated for each pump.
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CROSS REFERENCE TO RELATED APPLICATION
Priority of U.S. Provisional Patent Application Ser. No. 61/223,457 for “Ion Gyroscope,” filed Jul. 7, 2009, is claimed.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
N/A
BACKGROUND OF THE INVENTION
A gyroscope is a sensing device that detects rotational motion, i.e., angular velocity. Typical applications include, for example, navigation devices, camera image stabilization mechanisms and gaming equipment. There are different types of gyroscopes including optical (fiber gyro), flying wheel and MEMS (micro-electrical-mechanical-system).
In the consumer electronics market for mobile phones, GPS devices, etc., small size, low cost and robustness are critical to mass deployment. Currently, the MEMS-based gyroscope is gradually finding its way to this market. These gyroscopes are based on the Coriolis acceleration which is proportional to the velocity of a vibrating structure and the external rotation rate such that the Coriolis acceleration =2 × .
A known MEMS-based vibration-mode gyroscope uses a beam structure and a capacitive sensing mechanism. This approach, however, is subject to inaccuracy induced by mechanical shock and suffers from other reliability issues. In addition, such sensors require a complicated MEMS manufacturing process and a relatively large sensing area. As would be expected, therefore, the manufacturing costs are higher when compared to other MEMS-based devices, such as an accelerometer, a microphone, etc. These issues have prevented a MEMS-based gyroscope from being widely deployed in consumer electronics.
A convective gyroscope is known and its design involves a micro pump that generates a hot fluid jet stream. This hot jet stream will change its direction in the presence of rotational motion. The micro pump is typically actuated by a piezoelectric lead zirconate titanate (PZT) diaphragm but is difficult to manufacture in a MEMS process.
What is needed is a MEMS-based gyroscope that is accurate, has high reliability and that is economical to manufacture.
BRIEF SUMMARY OF THE INVENTION
An ion discharge gyroscope provides accurate measurement of rotational motion and linear acceleration by generating symmetrical ion jet streams and measuring respective amounts of the jet streams impinging on detectors located to intercept the respective ion jet streams. The ion jet streams will be diverted by operation of the Coriolis effect and the differences in the amount of each ion jet stream impinging on the detectors is an indication of rotational motion and linear acceleration. In one embodiment, the ion jet streams are heated and the respective temperatures of the detectors are measured. In another embodiment, the amounts of current flowing through each detector, as contributed by the ion jet stream, are measured and used to determine rotation and acceleration.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
Various aspects of at least one embodiment of the present invention are discussed below with reference to the accompanying figures. It will be appreciated that for simplicity and clarity of illustration, elements shown in the drawings have not necessarily been drawn accurately or to scale. For example, the dimensions of some of the elements may be exaggerated relative to other elements for clarity or several physical components may be included in one functional block or element. Further, where considered appropriate, reference numerals may be repeated among the drawings to indicate corresponding or analogous elements. For purposes of clarity, however, not every component may be labeled in every drawing. These figures are provided for the purposes of illustration and explanation and are not intended as a definition of the limits of the invention. In the figures:
FIG. 1 is a representation of an orientation and general shape of the sensors described herein;
FIGS. 2A-2C are schematic representations of an ion gyroscope according to one embodiment of the present invention;
FIGS. 3A-3D are schematic representations of an ion gyroscope according to a second embodiment of the present invention;
FIG. 4 is a measurement circuit for use with either of the first and second embodiments of the present invention shown in FIGS. 2 and 3 ;
FIGS. 5A-5D are schematic representations of an ion gyroscope according to a third embodiment of the present invention;
FIG. 6 is a measurement circuit for use in conjunction with the third embodiment of the present invention;
FIG. 7 is an alternate version of the third embodiment of the present invention;
FIG. 8 is another alternate version of the third embodiment of the present invention;
FIG. 9 is an alternate implementation of the first embodiment of the present invention; and
FIG. 10 is a flowchart of methods in accordance with embodiments of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
U.S. Provisional Patent Application Ser. No. 61/223,457 for “Ion Gyroscope,” filed Jul. 7, 2009, is incorporated by reference herein in its entirety and for all purposes.
One or more embodiments of the present invention are directed to an ion discharge gyroscope that provides accurate measurement of rotational motion in addition to being robust enough to withstand the forces of most consumer product implementations and in a structure that is relatively easy to manufacture.
As an overview, and referring now to FIG. 1 , a sensor 100 , embodiments of which will be described in more detail below, is generally formed on a rectangular substrate 102 fabricated out of silicon or other similar material. Typically, the substrate is on the order of 1-2 mm on a side. A cavity 104 is etched in the substrate 102 in order to provide a working space for the gyroscope movement. Generally, a longitudinal direction L will be defined and referenced throughout the present specification with the longitudinal direction L aligned with an X axis that is co-planar and perpendicular to a Y axis. For ease of explanation below, a Z axis is defined as being orthogonal to the plane defined by the X, Y axes.
In one embodiment of an ion gyroscope 200 , as shown in FIGS. 2A-2C , a substrate 102 is provided with a cavity 104 within which is disposed an anode 202 having a sharp anode tip 203 . Alternatively, there may be more than one sharp anode tip provided on the anode, however, a single anode tip makes it easier to ionize a gas as will be discussed below. A cathode 204 is disposed in the cavity 104 and opposite the sharp tip 203 . A first set 207 - 1 of thermocouples including a positive thermocouple (TCP) 208 and a negative thermocouple (TCM) 210 are provided within the cavity 104 and arranged such that, generally, the cathode 204 is disposed between the anode 202 and the positive and negative thermocouples 208 , 210 . A heater 206 is provided in the cavity 104 between the anode and cathode. The positive thermocouple 208 has a corresponding output TCP 1 and the negative thermocouple 210 has a corresponding output TCM 1 that are, respectively, coupled to the inputs of a differentiated amplified 402 - 1 , as shown in FIG. 4 .
A gas, for example, Nitrogen, Neon or Argon, is provided in the cavity 104 which is sealed to keep the gas in place. The provisioning of the gas and the sealing of the cavity 104 are done in accordance with practices known to those of ordinary skill in the art.
Referring now to FIG. 2B , in operation, a high DC voltage source 220 is coupled to the anode 202 and the cathode 204 . The voltage level of the DC voltage source 220 depends on the gas is used in the cavity 104 . For Neon and Argon, the voltage is in the range of 10-20 volts, however, Nitrogen requires around 300 volts. The voltage requirement increases as the distance from the anode to either the cathode or ground, as discussed below, increases. There are advantages to using a gas, therefore, that has a lower ionization voltage. When turned on, the gas in the cavity 104 is ionized by the high DC voltage source 220 to create an ion cloud 222 at the sharp anode tip 203 . An electric field created between the anode 202 and the cathode 204 drives the ion cloud 222 towards the cathode 204 thereby forming an ion jet stream 224 .
The heater 206 is placed in the path of the ion jet stream 224 , so as to heat the ion jet stream 224 before it reaches the temperature sensing positive and negative thermocouples 208 , 210 . The heater 206 is heated by passing current through its structure and, in one embodiment, is heated to about 100° K above ambient temperature. It should be noted that the heater 206 is positioned so as to heat the ion jet stream 224 without blocking the ion jet stream 224 from reaching the thermocouples 208 , 210 . A respective temperature of the ion jet stream 224 impinging on each of the thermocouples 208 , 210 is represented by the sensed values TCP 1 , TCM 1 .
The heater 206 is fabricated using standard CMOS layers, such as Polysilicon or metal. A release etch will remove silicon underneath the heater 206 and the release etch can be the same process step that is used to make the cavity 104 . The suspended structure of the heater 206 , discharge tip 203 and thermocouples 207 are thin in nature, generally a few microns (μm). The heater 206 will not block the ion jet stream 224 flow in the lateral direction.
At rest, i.e., when the device 200 is neither spinning nor linearly moving, the positive and negative thermocouples 208 , 210 should sense a same temperature. Thus, a difference between their respective signals TCP 1 , TCM 1 is zero as the ion jet stream 224 is traveling in a straight direction, in this case, along the X axis, and impinging equally on the thermocouples. Thus, the output signal ROTATIONØ, shown in FIG. 4 , would be zero.
In a situation where the device 200 is rotating, as shown in FIG. 2C , i.e., rotating about the Z axis which, in FIG. 2C , is coming up out of the drawing, the ion jet stream 224 will be skewed toward either the positive thermocouple 208 or the negative thermocouple 210 . As a result, there will be a temperature difference between the positive and negative thermocouples 208 , 210 resulting in a difference between the respective output signals TCP 1 , TCM 1 and the value ROTATIONØ will be greater or less than zero, depending upon the direction of spin.
The gyroscope 200 shown in FIGS. 2A-2C , however, is subject to interference in the output signal ROTATIONØ due to linear acceleration. That is, when the device 200 is accelerating along a direction that is, for example, perpendicular to the gas stream direction, the ion jet stream 224 will be skewed in the opposite direction. Such a skewing, however, will create an error in the reading that will be difficult to distinguish from the effects of rotation.
A symmetric ion gyroscope 300 , as shown in FIGS. 3A-3D , provides compensation for linear acceleration.
Referring now to FIG. 3A , the symmetric gyroscope 300 comprises a substrate 102 with a cavity 104 similar to the embodiment described above. A symmetric anode 302 is positioned in the cavity 104 and includes sharp tips 203 - 1 , 203 - 2 disposed on each side of the symmetric anode 302 . First and second cathodes 204 - 1 , 204 - 2 are disposed within the cavity 104 along with first and second heaters 206 - 1 , 206 - 2 positioned between the symmetric anode 302 and the first and second cathodes 204 - 1 , 204 - 2 , respectively. A first pair 207 - 1 of positive and negative thermocouples 208 - 1 , 210 - 1 that provide outputs TCP 1 and TCM 1 along with a second pair 207 - 2 of positive and negative thermocouples 208 - 2 , 210 - 2 that provide signals TCP 2 , TCM 1 are disposed in the cavity 104 . One of ordinary skill in the art will understand that the symmetric gyroscope 300 represents “mirror image” versions of the gyroscope 200 described above.
Referring now to FIG. 4 , a measurement circuit 400 consists of first and second differential amplifiers 402 - 1 , 402 - 2 , that receive, respectively, (TCP 1 , TCM 1 ) and (TCP 2 , TCM 2 ) the outputs of which are respectively coupled to the non-inverting and inverting inputs of a third differential amplifier 402 - 3 to output a difference therebetween as a ROTATION1 signal. In addition, the respective outputs of the first and second differential amplifiers 402 - 1 , 402 - 2 are input to a summer circuit 404 that adds the signals together to provide an indication of linear acceleration.
In operation, referring now to FIG. 3B , first and second high DC voltage power sources 220 - 1 , 220 - 2 , are coupled to the symmetric anode 302 and the first and second cathodes 204 - 1 , 204 - 2 , respectively.
When the first and second voltage sources 220 - 1 , 220 - 2 , and the heaters 206 - 1 , 206 - 2 , are turned on, and the symmetric gyroscope 300 , is at rest, the ion jet streams 224 - 1 , 224 - 2 resulting from the ion clouds 222 - 1 , 222 - 2 , respectively, strike the pairs 207 - 1 , 207 - 2 of positive and negative thermocouples 208 - 1 , 208 - 2 , 210 - 1 , 210 - 2 equally and the differences between all outputs TCP 1 , TCM 1 , and TCP 2 , TCM 2 are zero.
When the symmetric gyroscope 300 is rotated, as shown in FIG. 3C , the first and second ion jet streams 224 - 1 , 224 - 2 will be deflected in opposite directions. Accordingly, there will be a difference between the first and second pairs of thermocouples 207 - 1 , 207 - 2 output signals TCP 1 , TCM 1 and TCP 2 , TCM 2 . Such a difference, as will be calculated as described below, can be used to identify an amount of rotational motion.
As show in FIG. 3D , when the symmetric gyroscope 300 is linearly accelerated in, for example, the Y direction, the first and second jet streams 224 - 1 , 224 - 2 will be deflected in the opposite direction. An imbalance in the temperature sensed as between the pairs of positive and negative thermocouples 207 - 1 , 207 - 2 will indicate an amount of linear acceleration.
Thus, when the symmetric gyroscope 300 is rotating, the signals from the first and second pairs 207 - 1 , 207 - 2 of positive and negative thermocouples will have opposite polarities. The ROTATION1 signal output from the differential amplifier 402 - 3 will indicate a magnitude of rotation in addition to a direction.
The amount of linear acceleration is provided by the summer 404 which sums, i.e., averages, the differences between the pairs 207 - 1 , 207 - 2 , of positive and negative thermocouples 208 , 210 , while also indicating a direction of acceleration.
In a third embodiment of the present invention, an ion gyroscope 500 , as shown in FIGS. 5A-5D , uses current mode sensing rather than thermo sensing. Accordingly, as shown in FIG. 5A , the current mode gyroscope 500 includes a substrate 102 with a cavity 104 as described above. In addition, a symmetric anode 302 is positioned within the cavity 104 . A first ground electrode 501 - 1 is provided within the cavity 104 and consists of a first upper portion 502 - 1 and a first lower portion 504 - 1 . A second ground electrode 501 - 2 is split into respective upper and lower portions 502 - 2 , 504 - 2 , respectively. One will understand that these ground electrodes can also be considered as being cathodes.
As shown in FIG. 5B , a first DC voltage sources 220 - 1 and a first current meter 506 - 1 are coupled between the anode 302 and the first lower portion 504 - 1 . The first current meter 506 - 1 provides a signal Im 1 indicating the amount of current flowing in that leg of the circuit. A second DC voltage source 220 - 2 and a second current meter 506 - 2 are coupled between the anode 302 and the second lower portion 504 - 2 . The second current meter 506 - 2 provides a signal Im 2 indicating the amount of current flowing in that leg of the circuit. A third DC voltage source 220 - 3 and a third current meter 506 - 3 are coupled between the anode 302 and the first upper portion 502 - 1 of the first ground electrode. The third current meter 506 - 3 provides a signal Ip 1 indicating the amount of current flowing in that leg of the circuit. A fourth DC voltage source 220 - 4 and a fourth current meter 506 - 4 are coupled between the anode 302 and the second upper portion 502 - 2 of the second ground electrode 502 - 2 . The fourth current meter 506 - 4 provides a signal Ip 2 indicating the amount of current flowing in that leg of the circuit.
Similar to the first and second embodiments, when the power supplies are turned on, an ion cloud and ion jet stream will be formed and will flow from the anode toward the ground electrodes. As the ion jet streams 224 - 1 , 224 - 2 actually carry current, in the case of zero deflection, i.e., at a standstill, the currents will be equally split between the upper and lower ground electrodes in each of the first and second pairs 501 - 1 , 501 - 2 and reflected in the current measurements Ip 1 , Im 1 and Ip 2 , Im 2 . In the presence of deflection, either due to linear acceleration or rotation, the current will not be equal. The indication of motion and its magnitude will be reflected in the output signals.
A measurement circuit 600 , as shown in FIG. 6 , determines the amount of rotation or linear acceleration and includes first and second current difference devices 602 - 1 , 602 - 2 . The first current difference device 602 - 1 receives the current measurement signals Im 1 , Ip 1 from the first and third current meters 506 - 1 , 506 - 3 , respectively, and the second current difference device 602 - 2 receives the current measurements Im 2 and Ip 2 from the second and fourth current meters 506 - 2 , 506 - 4 . The outputs of the current difference devices 602 - 1 , 602 - 2 are amplified, respectively, by amplifiers 604 - 1 , 604 - 2 .
A differential amplifier 402 receives, at its inputs, the respective outputs from the amplifiers 604 - 1 , 604 - 2 and provides a ROTATION1 signal indicative of a direction and magnitude of rotation.
A summer 404 adds the outputs of the first and second amplifiers 604 - 1 , 604 - 2 to arrive at a linear acceleration signal LINEARACCEL indicating the direction and magnitude of linear acceleration, in the example shown in FIGS. 5A-5D , along the Y axis.
Referring to FIGS. 5C and 5D , when the current mode gyroscope 500 is spinning, or linearly accelerating, respectively, the jet streams 224 - 1 , 224 - 2 will be deflected, as has been described above.
Advantageously, the current mode sensing gyroscope 500 is a relatively simple device as compared to the prior embodiments described above. It not only removes some structure, for example, the heaters, it also removes the need for the power that would drive the heaters.
The above-described embodiments of the present invention may be modified in various ways. Referring now to FIG. 7 , the current mode gyroscope 500 described in FIGS. 5A-5D may be configured such that one DC voltage supply 220 - 1 , 220 - 2 is used, respectively, for the two sides of the device and the current sensing devices 506 then measure the currents found on respective “legs” of the circuits as shown.
Further, the circuit configuration shown in FIG. 7 may be modified, referring now to FIG. 8 , such that a first current difference device 802 - 1 is used to measure the currents Im 1 , Ip 1 and calculate a difference value therebetween and a second current difference device 802 - 2 provides the difference value between Im 2 and Ip 2 . This would reduce the number of discrete components necessary to support the current mode gyroscope 500 . One of ordinary skill in the art will understand that there are combinations of these alternate devices that may be used.
It should be appreciated that the circuit diagrams shown in the figures also represent some functional blocks and should not be used to limit the claims to any specific structure unless explicitly recited in a claim. Thus, while an inline current meter is shown above, any one of a number of other known current measuring devices may be used including, but not limited to, Hall effect sensors, magnetoresistive sensors, current clamps and current transformers.
In another implementation, as shown in FIG. 9 , two of the ion gyroscopes 200 - 1 , 200 - 2 may be oriented in opposition to one another. Essentially, as shown in FIG. 9 , two of these devices may be used to function as the symmetric gyroscope shown in FIGS. 3A-3D . Of course, one of ordinary skill in the art would understand that the necessary DC power sources and output circuitry would need to be connected although not shown in FIG. 9 in order to facilitate explanation. Still further, one of ordinary skill in the art would understand that the two devices 200 - 1 , 200 - 2 would have to be fixedly oriented, i.e., permanently mounted on a structure 902 , with respect to each other such that the linearity of the system is maintained. Accordingly, it may be necessary to calibrate or establish a zero point prior to operation. It is expected, however, that one of ordinary skill in the art would understand how to accomplish this.
Referring now to FIG. 10 , a flowchart 950 represents methods in accordance with embodiments of the present invention as described herein. Initially, step 952 , symmetric ion streams are generated. Subsequently, if implementing the heated ion gyroscope, control passes to step 954 where the ion streams are heated. The temperatures are measured on the first and second pairs of thermocouples, step 956 , and those temperatures on the first and second pairs of thermocouples are compared to one another, step 958 . Output signals indicative of rotation and/or linear acceleration as functions of the compared temperatures are then provided, step 960 .
If the current mode gyroscope is implemented then, step 962 , the currents flowing in the first and second pairs of electrodes are measured. These currents are then compared to one another, step 964 , and subsequently output signals indicative of rotation and linear acceleration are provided as a function of the compared current measurements, step 966 .
Further, the discrete devices in the measurement circuits 400 , 600 may be replaced by analog devices, digital devices, hybrid devices, and devices under the control of a microprocessor, e.g., Analog-Digital converters and Digital-Analog converters. These would all be understood by one of ordinary skill in the art.
Still further, the gyroscope, DC voltage sources, current meters, measurement circuits, etc. may all be combined in a single device having only a power input and output signals to offer a “system on a chip” operability.
Having thus described several features of at least one embodiment of the present invention, it is to be appreciated that various other alterations, modifications, and improvements will readily occur to those skilled in the art. Such alterations, modifications, and improvements are intended to be part of this disclosure and are intended to be within the scope of the invention. Accordingly, the foregoing description and drawings are by way of example only, and the scope of the invention should be determined from proper construction of the appended claims, and their equivalents.
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An ion discharge gyroscope measures rotational motion and linear acceleration by generating symmetrical ion jet streams and measuring respective amounts of the jet streams impinging on detectors located so as to intercept the ion jet streams. The ion jet streams will be diverted by operation of the Coriolis effect and the differences in the amount of each ion jet stream impinging on the detectors is an indication of rotational motion and linear acceleration. In one embodiment, the ion jet streams are heated and the respective temperatures of the detectors are measured. In another embodiment, the amounts of current flowing through each detector, as contributed by the ion jet streams, are measured and used to determine rotation and acceleration.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is based upon and claims the benefit of priority from prior Japanese Patent Application No. 2005-138668, filed May 11, 2005, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a portable electronic device and a list display method.
[0004] 2. Description of the Related Art
[0005] In many portable electronic devices such as portable phone, since a display area is limited, various types of information are displayed on a screen in a liquid crystal display device (LCD) in the form of list (hereinafter, simply referred to as “list”). Here, two methods are known in order to display list information for displaying a list on the screen.
[0006] A first method is to read information for displaying all lists registered in a database or the like (hereinafter, referred to as “display information”) on a work memory for display and to display only necessary part for display on the screen. Specifically, as shown in FIG. 1A and FIG. 1B , if it is assumed that five lists are displayed on the screen when there are 10 list elements (each list in the lists is referred to as “list element” in order to distinguish from the lists), all of the ten lists are first read. Then desired lists (list 3 to list 7 in FIG. 1B ) therefrom are displayed ( FIG. 1A ). When one desires to display other lists, a next item of the lists is displayed by, for example, scrolling down ( FIG. 1B ). In this manner, all the display information is read on the work memory in the first method so that the lists can be fast displayed. However, on the contrary,
[0007] (1) when a large amount of display information is present, the amount of consumption of memory accordingly increases. Further, there is a problem that decrease in a response speed is caused along with the increase in the amount of consumption of memory.
[0008] (2) When the number of list elements dynamically changes, or in the case of address book or received e-mail box, since the necessary amount of consumption of memory cannot be calculated previously, it is necessary to calculate the necessary amount of consumption of memory according to the number of items.
[0009] Thus, there is proposed a second method in which only part to be displayed on the screen is read on the work memory and is displayed (see FIG. 2A , FIG. 2B and Jpn. Pat. Appln. KOKOKU Publication No. 6-77231, for example). In this method, as shown in FIG. 2A similarly as in the first method, if one wants to display list 4 to list 8 by scrolling down the screen when list 3 to list 7 are displayed, a storage area for list 3 is released on the work memory to save a storage area for list 8 as shown in FIG. 2B . According to this method, since the display range is determined in designing the screen, the memory capacity for displaying list elements can be calculated (that is, only the memory capacity for displaying five lists has to be saved in FIG. 2A and FIG. 2B ). Further, since the portable electronic device is limited in the capacity for the work memory or database and its addition is impossible in many apparatuses, it is preferable to reduce the amount of consumption of memory.
[0010] As described above, although the list elements not displayed on the screen are displayed by user's scrolling the screen in the second method similarly as in the first method, the area used by the item of the list element which cannot be seen by scrolling is released and an area to be used by the list element to be newly displayed is saved instead. Specifically, the amount of consumption of memory along with user's scrolling of the screen does not change, and the amount of consumption of memory does not increase even when the number of list elements is several hundreds (or many). As described above, since the number of list elements to be displayed does not increase in the second method even if the number of list elements registered in the database or the like increases, the amount of consumption of memory to be used for the display processing or the processing time does not change as in the case where the number of items is small. Thus, when the number of list elements registered in the database or the like is small, a processing of changing list items along with the screen scrolling in the second method is later than a processing of scrolling the screen without changing the list items in the first method.
[0011] Since the second method is different from a list method previously mounted, there is a problem that the program requires to be corrected, which requires more cost or time.
BRIEF SUMMARY OF THE INVENTION
[0012] The present invention provides a portable electronic device and a list display method having the advantages of the above first and second methods.
[0013] A portable electronic device according to one aspect of the present invention is characterized by comprising a database configured to store therein a plurality of lists each including at least one list element; a display configured to display the list elements; and a controller configured to read the list elements to be displayed from the database and to display the list elements on the display, wherein the controller reads the list elements into a work memory for display from the database based on a identification data as to whether to read all the list elements into a work memory for display.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0014] FIGS. 1A and 1B are diagrams for explaining a conventional first display method;
[0015] FIGS. 2A and 2B are diagrams for explaining a conventional second display method;
[0016] FIG. 3 is a perspective view of an appearance of a portable electronic device to which a list display method according to an embodiment of the present invention is applied;
[0017] FIG. 4 is a block diagram of essential parts for displaying;
[0018] FIG. 5 is a flowchart showing an operation in creating a list; and
[0019] FIG. 6 is a flowchart of a display method based on the created list form.
DETAILED DESCRIPTION OF THE INVENTION
[0020] An embodiment according to the present invention will be described below with reference to the drawings. FIG. 3 is a perspective view of an appearance of a portable electronic device to which a list display method according to the embodiment of the present invention is applied. This portable electronic device is a so-called foldable portable communication terminal in which an upper portion 1 and a lower portion 2 are rotatably connected through a hinge mechanism 3 , and FIG. 3 shows a state where each portion 1 , 2 is opened.
[0021] The upper portion 1 is arranged with a main LCD (Liquid Crystal Display) 4 at its front and a sub-LCD (Liquid Crystal Display) at its back. On the other hand, the lower portion 2 incorporates therein a main printed wiring board (not shown), a key input device 5 and the like.
[0022] FIG. 4 is a block diagram of essential parts for displaying in the portable electronic device as constructed above. FIG. 4 shows a database 10 made of a nonvolatile memory (for example, EEPROM) or the like, a work memory 20 made of fast-accessible memory (for example, DRAM) or the like, a display API 30 for displaying a list read by the work memory 20 on a LCD 40 , and the LCD 40 for performing list displaying. The database 10 , the work memory 20 and the display API 30 are controlled by an application 50 operating on a CPU (not shown), respectively. Although the actual control is performed by a computing device such as the CPU through an application, the following description is made assuming that the display control is performed by the application 50 .
[0023] In FIG. 4 , the database 10 stores therein various types of list data used by the application 50 . When the application 50 accesses the database 10 , the application 50 saves an area for list data storage in the work memory 20 , and then reads predetermined list data from the database 10 to write it on the work memory 20 . Next, the display API 30 reads the list data from the work memory 20 , and the application 50 adds a list element to the display API 30 as needed. Then, the display API 30 sends the list to the LCD 40 , and the LCD 40 displays the received list thereon.
[0024] An operation according to the present invention with respect to the portable electronic device according to the embodiment of the present invention as constructed above will be described with reference to FIGS. 5 and 6 . FIG. 5 is a flowchart showing an operation in creating a list, and FIG. 6 is a flowchart of a display method based on the created list form.
[0025] At first, the operation in creating a list will be described with reference to FIG. 5 .
[0026] The display API 30 makes three determinations in creating a list. Based on the determination, it determines whether to take a list according to the first method (hereinafter, referred to as “first list”) or to take a list according to the second method (hereinafter, referred to as “second list”), and returns the number of list elements to be written into the work memory by the application 50 to the application 50 . Specifically, it is first checked whether the number of lists is small (step A 1 ), it is next checked whether the work memory 20 is sufficient (step A 2 ), and it is finally checked whether access to the database 10 (that is, time after accessing the database 10 until reading data and displaying it on the LCD 40 ) is fast (step A 3 ).
[0027] As a result of checking in steps A 1 to A 3 , when the number of list elements is small (Yes in step A 1 ), the work memory 20 is sufficient (Yes in step A 2 ), and access to the database 10 is fast (Yes in step A 3 ), it is determined to create the first list, that is, a list for reading all the lists on the work memory 20 (step A 4 ). As a result of checking from steps A 1 to A 3 , if any one check is “No”, it is determined to create the second list, that is, a list for reading only lists for displaying (step A 5 ). Discrimination between the first list and the second list may be performed by setting a flag on the header. For example, the first and second lists may be discriminated by adding a dedicated field (1-bit data will suffice) to the header of the list and based on a value of data of the field (for example, 1 or 0). Furthermore, the number of all list elements (total number) is set in the dedicated field in the header of the list when the application 50 creates a list, and the display API 30 may discriminate the first list from the second list based on a value of the data of the field (for example, less than 20, 20 or more).
[0028] The number of list elements determined in step A 4 or step A 5 is returned to the application 50 (step A 6 ), the application 50 reads the list from the database 10 according to the value returned by the display API 30 and writes it into the work memory 20 .
[0029] In the above processing, the number of lists depends on the size of the LCD to be displayed. For example, when the portable electronic device is a portable phone, the first list is preferable if the number of lists is 20 or less. This is because the use amount of memory is reduced when all the lists are assumed as the second list, but the display speed is rather reduced when the number of lists is small. Furthermore, since the capacity of the mounted work memory is actually different for each apparatus, it is preferably determined whether free capacity in creating a list is sufficient with respect to the free capacity for the work memory.
[0030] Next, a flow of the display method according to the present embodiment will be described with reference to FIG. 6 .
[0031] For example, when the user operates a scroll key (not shown) to scroll down (step B 1 ), it is checked whether the list form is the first list or the second list (step B 2 ). Here, when the list form is the first list, all the lists have been already read and it is not necessary to newly access the database 10 , and the display range is shifted downward (step B 3 ). In step B 2 , when the list form is the second list, a list element which the application 50 needs to scroll and display is requested to the database 10 and the required list element is read (step B 4 ). Then, the added list element is added to the lowermost stage of the displayed list elements to display the new list element (step B 5 ). At this time, the area for the work memory 20 saved for the list element, which does not require to be displayed, is released before newly adding a list element.
[0032] As described above, according to the embodiment of the present invention, the list form can be dynamically changed depending on the number of list elements such that the first list is employed when the number of list elements is small and the second list is employed when the number thereof is large. This function can be achieved only by adding a program (or module) for the added function without changing an existing application program.
[0033] Therefore, as compared with the fixed list form, the present embodiment can improve performance for displaying and restrict the amount of consumption of memory.
[0034] The present invention is not limited to the above embodiment and can accomplish various modifications without departing from the spirit thereof in implementation.
[0035] For example, although the first or second list is created depending on the number of list elements in the above embodiment, there may be employed the second list for a list whose list elements would dynamically change and increase in the future, such as address book or the number of received e-mail, even when the number of list elements is small.
[0036] According to the present invention, it is possible to provide a portable electronic device and a list display method having the advantages of the first and second methods without changing an existing application program.
[0037] Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details, representative devices, and illustrated examples shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents.
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A portable electronic device includes a database configured to store therein a plurality of lists each including at least one list element, a display configured to display the list elements, and controller configured to read list elements to be displayed from the database and to display the list elements on the display. The controller reads the list elements into a work memory for display from the database based on a identification data as to whether to read all the list elements into a work memory for display.
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RELATED APPLICATIONS
[0001] This application claims priority to European Patent Application No. EP06126475.0 filed on Dec. 19, 2006, and claims the benefit under 35 USC 119(e) of U.S. Provisional Application No. 60/870,870, filed on Dec. 20, 2006, both of which are incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] Various types of radiation detectors are used, including powder phosphor screens or needle image plates (needle IP), direct radiography detectors (amorphous silicon, amorphous selenium, Cmos, phosphor detector arranged for direct radiography etc.) or the like.
[0003] A radiation image is recorded on such a detector (also called ‘plate’) by exposing it to an x-ray field. The radiation image that is temporarily stored by the detector is read out in a read out system (also called ‘digitizer’) where the exposed detector is scanned with light of an appropriate wavelength and where the image-wise modulated light emitted by the detector upon stimulation is detected and converted into a digital image signal representative of the radiation image.
[0004] An embodiment of a digitizer is described in Ref. 1 (U.S. Pat. No. 6,369,402 B1).
[0005] The scanning technique in the digitizer could be flying-spot or one line at a time. See Ref. 5 (R. Schaetzing, R. Fasbender, P. Kersten, “New high-speed scanning technique for Computed Radiography”, Proc. SPIE 4682, pp. 511-520).
[0006] A phosphor screen or needle image plate is commonly conveyed in a cassette and is not part of the read out system.
[0007] The signal to noise ratio (SNR) or normalized noise power spectrum ((N)NPS) of the image data must be analyzed in order to evaluate the diagnostic capacity of the radiographic system. This implies that for each detector the uniformity of the detector needs to be evaluated, and corrected for. The techniques to do so are known in the state of the art.
[0008] The SNR or (N)NPS of the digitizer must be determined for different uniform dose levels to be able to study its behavior over the dynamic range.
[0009] Instead of using different detectors for each dose setting, a phantom target is used that contains a number of sub-targets each with a known absorption level for x-ray exposure. See Ref. 2 to 4 (EP 02 100 669.7, EP 02 100 792.7, EP 05 106 112.5).
[0010] Exposure of the detector then gives an image that contains the raw data needed for SNR or (N)NPS calculation. Every sub-target contains a region of interest (roi) with a known and constant attenuation and is exposed to a uniform radiation field.
SUMMARY OF THE INVENTION
[0011] The present invention relates to quality assurance of digital radiography systems.
[0012] More specifically the invention relates to the neutralization of the impact of artifacts in the system during quality control testing of the SNR and/or the (N)NPS of the digitizer. Determination of SNR or (N)NPS is important as it is an indicator for the capability of the system to detect low signal values.
[0013] The prescribed procedure relates to exposure of the detector whereby the detector is centered relative to the axis of an incident x-ray beam. The signal read out of the detector by a calibrated read out system is then evaluated relative to a pre-defined acceptance level.
[0014] The present invention starts with dose-linear roi data. This means that, dependent on the read out system, the signal read out has to be mathematically transformed into data that are proportional to the imposed x-ray dose. Such transformation are known in the art, and is not part of the current invention.
[0015] It is an object of the present invention to provide a method to preprocess the dose-linear roi data such that non-noise related multiplicative artifacts caused by exposure, detection or digitizer read-out are optimally suppressed prior to SNR or (N)NPS determination.
[0016] These artifacts are called multiplicative because the signal distortion is relative to the uniform dose level of the X-ray source. They are non-noise related because they do not have a statistical nature, but are caused by actual (but unavoidable) errors in the physical realization of the radiography system.
[0017] A problem with the determination of the SNR or (N)NPS of a digitizer based on raw, dose-linear image-data is that multiplicative artifacts in the overall imaging chain inevitably lead to a lower perceived performance, a subestimation of the system's real performance. The above mentioned method calls for a preprocessing of the image-data in such a way that the impact of these artifacts is maximally suppressed to safeguard the intrinsic value of the SNR or (N)NPS results calculated during quality control (QC) testing.
[0018] In general, according to one aspect, the invention features a method for statistically correcting the raw digital data output of a digitizer in a radiography system, prior to Signal-to-Noise Ratio or Noise Power Spectrum calculation, by use of a phantom target having sub-targets which form regions of interest (roi) in the x-ray of the image of the phantom target. The method comprises the steps of: identifying the sub-targets (rois) which have known absorption profiles, said profiles being constant or having a constant gradient; capturing the radiation image of said rois on a detector; converting each pixel of each roi on the digital detector image to dose-linear digital data; and correcting each pixel value for non-noise correlated multiplicative artifacts.
[0019] In embodiments, the correction is performed by multiplying the signal value of a pixel in the roi with the ratio of the roi median value to the row median value. In other cases, the correction is performed by multiplying the signal value of a pixel in the roi with the ratio of the roi median value to the column median value. In still other cases, the correction is performed by multiplying the signal value of a pixel in the roi with the ratio of the roi median value to the row median value AND with the ratio of the roi median value to the column median value.
[0020] In some implementations, the correction is performed by first splitting the signal value of a pixel in the roi in an effective signal part and a noise part; the effective signal part is then corrected by multiplying with the ratio of the roi median value to the row median value, the noise part is corrected by multiplying with the square root of said ratio. The ratio can be calculated as the ratio of the roi median value to the column median value.
[0021] In other embodiments, the correction is performed by first splitting the signal value of a pixel in the roi in an effective signal part and a noise part; the signal part is then corrected by multiplying with the ratio of the roi median value to the row median value and the ratio of the roi median value to the column median value, the noise part is corrected by multiplying with the square root of the product of said ratios.
[0022] In general, according to another aspect, the invention features a system used in radiography for statistically correcting the raw digital data output of a digitizer, prior to Signal-to-Noise Ratio or Noise Power Spectrum calculation, by use of a phantom target having sub-targets which form regions of interest (roi) in the x-ray of the image of the phantom target. The system comprises a memory for storing the raw digital data output of a digitizer and a processor coupled to the memory for identifying the sub-targets (rois) which have known absorption profiles, said profiles being constant or having a constant gradient; capturing the radiation image of said rois on a detector; converting each pixel of each roi on the digital detector image to dose-linear digital data; and correcting each pixel value for non-noise correlated multiplicative artifacts.
[0023] In general, according to another aspect, the invention features a computer-readable medium upon which a plurality of instructions are stored, the instructions for performing the steps of the method as described above.
[0024] The above and other features of the invention including various novel details of construction and combinations of parts, and other advantages, will now be more particularly described with reference to the accompanying drawings and pointed out in the claims. It will be understood that the particular method and device embodying the invention are shown by way of illustration and not as a limitation of the invention. The principles and features of this invention may be employed in various and numerous embodiments without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In the accompanying drawings, reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale; emphasis has instead been placed upon illustrating the principles of the invention. Of the drawings:
[0026] FIG. 1 is a general set up in digital radiography.
[0027] FIG. 2 is a schematic representation of the single pass multiplicative artifact affected image reconstruction.
[0028] FIG. 3 is a schematic representation of the dual pass multiplicative artifact affected image reconstruction, rows followed by columns.
[0029] FIG. 4 is a schematic representation of the dual pass multiplicative artifact affected image reconstruction, columns followed by rows.
[0030] FIG. 5 is the graphical representation of the single pass multiplicative artifact affected image reconstruction at the level of the image signals.
[0031] FIG. 6 is an image representation of the algorithm, with on the left the uncorrected signal, and on the right the corrected signal. Also the histogram of uncorrected (roi) and corrected (roi**) is shown in the low middle.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0032] SNR: Signal to Noise Ratio.
[0033] (N)NPS: (Normalized) Noise Power Spectrum.
[0034] image: Any digital image, acquired by means of a scanner (X-ray, document scanning, . . . ) using a photonintegrating detector (photo-multiplier tubes, photo-diode arrays, charge coupled devices (CCD's)) to convert the spatially distributed impinging exposure into image-signals.
[0035] image mn : The image with m rows and n columns.
[0036] roi: Any region of interest within such an image, representing a substantially constant exposure (flat-field, white balance, . . . ), defined to calculate the SNR or (N)NPS.
[0037] roi kl : The roi with k rows and l columns.
[0038] p: Any image pixel within a roi.
[0039] p ij : The pixel in roi kl at row i and column j.
[0040] V ij : The exposure-linear (original or after conversion) digital value associated with pixel P ij .
[0041] V ij *: The unidirectionally (along the image rows) multiplicative artifact corrected value of exposure-linear value V ij .
[0042] V ij *′: The unidirectionally (along the image columns) multiplicative artifact corrected value of exposure-linear value V ij .
[0043] V ij **: The bidirectionally (along the image rows and columns) multiplicative artifact corrected value of exposure-linear value V ij .
[0044] ROI kl : The median of all the values V ij over roi kl .
[0045] row i : The median of all the values V ij over the i-th row of roi kl , divided by ROI kl .
[0046] col j : The median of all the values V ij over the j-th column of roi kl , divided by ROI kl .
[0047] The image is acquired by x-ray exposing the phantom target and recording the transmitted x-ray flux with the detector. In the following it is assumed that the detector is a photostimulable phosphor screen, however other types of detectors may be used.
[0048] The phantom target contains a number of sub-targets that are constructed in such a way that each sub-target absorbs a larger part of the incoming x-rays, forming a known cascade of absorption levels. After converting the residual exposure signal coming from each sub-target (the region of interest, roi) into raw digital data the SNR and/or (N)NPS for each roi can be calculated with standard methods, known to those skilled in the art.
[0049] However, the roi might contain one or more artifacts that will make the calculated SNR and/or (N)NPS of the roi to behave atypically. This could render the calculated results useless as not being an accurate representation of the digitizer's real performance. Artifacts are detected in other quality control tests, and are not relevant in said calculations.
[0050] Artifacts introduced by the digitizer can be vertical, caused by non-uniformity in the fast (horizontal) scan direction, or horizontal, caused by non-uniformity in the slow (vertical) scan direction, and cannot be completely physically eliminated. They are caused e.g. by speed variations in the slow scan direction (banding), giving a horizontal artifact, or by a defect or pollution in a light guide component or a CCD, giving a vertical artifact. Also dust or scratches on the detector plate could cause an artifact, but since these can take any shape, the current invention, as will be seen, will not be able to completely eliminate the negative impact of these artifacts, but their impact will be minimized. In what follows we will focus on horizontal and vertical artifacts.
[0051] The digitizer converts the signal-with-noise from every roi to raw digital data, which can be presented, the roi being rectangular, in a table with k rows and l columns.
[0052] The median value of the signal-with-noise for the whole roi can now be calculated (ROI kl ), as well as for every row (row i ) and for every column (col j ) in the roi separately.
[0053] A vertical artifact (fast scan direction) will have the effect that the median value for one or more rows or columns is lower than the median value for the roi.
[0054] A horizontal artifact (slow scan direction) will result in a lower median value if the artifact was caused by the scanner speeding up, or in a higher median value if caused by the scanner slowing down.
[0055] Suppose that we have a horizontal artifact, resulting in a higher median value for the i-th row, and a vertical artifact, resulting in a lower median value for the j-th column. See FIG. 5 .
[0056] One way to correct the negative effect of a horizontal artifact in the i-th row is to multiply the values of all cells in the affected row with the ratio of ROI kl to the row median value. This effectively removes the artifact on the signal level.
[0057] The same goes, mutatis mutandis, for a vertical artifact.
[0058] This results in the dual pass algorithm:
[0000] V ij *=V ij /row i
[0000]
V
ij
**=V
ij
/col
j
[0059] Or, combined in a single pass algorithm:
[0000] V ij **=V ij /(row i ·col j )
[0060] A drawback is then, that the noise (inherently part of the signal) at the location of the artifact is over-corrected, resulting in a sub-optimal correction. The present invention gives a cure to this problem.
[0061] Since the noise in the signal is photon noise, the variance of the noise is proportional to the square root of the average number of photons.
[0062] For a horizontal artifact this means that the correction factor for V ij has to be replaced by its square root:
[0063] The same goes, mutatis mutandis, for a vertical artifact.
[0064] This results in the dual pass algorithm:
[0000] V ij *=ROI kl +( V ij −row i ·ROI kl )/(row i ) 1/2
[0000] ROI kl *=Median over roi kl after one pass of the algorithm
col j *=Median over j-th column after one pass of the algorithm
[0000] V ij **=ROI kl *+( V ij *−col j *·ROI kl *)/( col j *) 1/2
[0065] Or, combined in a single pass algorithm:
[0000] V ij **=ROI kl +( V ij −row i ·col j ·ROI kl )/(row i ·col j ) 1/2
[0066] The latter is a single pass algorithm, i.e. it is independent of the fact that first the rows are considered, and then the columns, or vice versa.
[0067] the current invention first calculates roi kl , and the values for every i and j for row i and col j . It then corrects the value of every point in the ROI (every cell in the spreadsheet) according to the algorithm, before delivering the corrected data to the SNR or (N)NPS calculation process, which is not part of the invention.
[0068] The result is that the impact of the multiplicative artifact is neutralized, meaning effectively that the artifact is eliminated.
[0069] Embodiments of the current invention will also eliminate the impact of misalignment of the roi on the sub-target. If one of the sides of the roi (top, bottom, left or right) is close to the corresponding side of the sub-target, the signal will drop because of partial loss of scatterexposure near the surrounding shields. This physical phenomenon will have the same impact on the calculation of the SNR or (N)NPS as a linear artifact would have, so it will be as effectively eliminated.
[0070] The current invention also works for sub-targets that show a continuous gradient in absorbed dose. If the sub-target is a wedge with a constant slope, the absorption changes continuously with distance. During the correction phase the parts with high absorption will be adjusted upwards, and the parts with low absorption will be adjusted downwards, so that all parts of the roi will be adjusted towards the median value of the dose-linear data.
[0071] It will be clear to those skilled in the art that, wherever the median value is used in this description, the average value could have been used also. The median value however is the superior embodiment, since single extreme values in the distribution affect the median less than the average.
[0072] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
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A method for neutralizing the non-noise correlated, multiplicative image-artifacts introduced by the X-ray exposure, the detector or the digitizer prior to the determination of the Signal-to-Noise Ratio or the (Normalized) Noise Power Spectrum in CR/DR radiography systems. This method uses statistical techniques and the photon-noise physical model to correct the raw, digital image-data obtained in the selected region of interest (roi) for evaluation during quality control (QC).
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FIELD OF THE INVENTION
The present invention relates to training devices used for practicing golf skills and more specifically to a pair of golf gloves worn playing golf that will aid a golfer in achieving and maintaining a preferred grip on a golf club.
PRIOR ART
Achieving and maintaining the consistency and feel of the preferred grip position on a golf club is somewhat difficult to learn, especially for beginner and intermediate golfers. A faulty grip position, whether too strong or too weak, directly affects the position of the club face at impact leading to shots that end up well right or well left of the target. In addition, many of these golfers, upon addressing a ball, tend to fidget around with their grip position and may inadvertently shift their hands on a golf club during their back swing and forward swing, adversely affecting their golf shot.
Most golf instructors tell their students that in order to execute a well coordinated, smooth flowing, swing of a golf club, the fundamentals of a neutral grip position must first be learned and repeatedly practiced. Many amateur golfers tend to grasp a golf club without careful consideration of their hand position on the club. They may also use one or two golf gloves. Such gloves do enhance the golfers grip on the club, but none have been produced that direct and secure a golfer's hands in the preferred neutral grip position.
Thus, there is a need in the art for an aid to help a golfer achieve and maintain a preferred neutral grip position on the golf club during the entire swing to realize a golf shot.
SUMMARY OF THE INVENTION
The foregoing need in the prior art is satisfied by the present invention. The present invention provides a pair of interlocking golf gloves which help a golfer achieve, secure and maintain the preferred neutral grip position on a golf club during the entire swing process and to achieve a good golf shot. These golf gloves are properly sized, easily worn and are not cumbersome on the golf course.
The golf gloves of the preferred embodiment of the invention utilize hook and pile fasteners of the type available commercially under the trademark VELCRO®. Segments of such hook and pile fasteners are permanently attached to each of the gloves. A golfer wearing a pair of these golf gloves is aided in how to properly grip a golf club in a preferred neutral grip so as not to have: (a) too weak a grip where the golf club handle slides into the lifeline of the golfer's upper hand instead of resting in the heel pad of the hand and results in slicing a golf shot; or (b) too strong a grip where there is pressure in the upper hand wrist socket and the outside of the lower arm forearm tighten up and results in a hook shot. With the preferred neutral grip a golfer will achieve and maintain the preferred grip on a golf club during an entire swing to achieve a good golf shot.
For a right handed golfer their upper hand is their left hand and their lower hand is their right hand. Conversely, for a left handed golfer their upper hand is their right hand and their lower hand is their left hand.
DESCRIPTION OF THE DRAWING
The invention will be better understood upon reading the following Detailed Description in conjunction with the drawings in which:
FIG. 1 is a palm up view of the left hand glove with the thumb extended;
FIG. 2 is a palm up view of the left hand glove with the thumb folded in;
FIG. 3 is a palm up view of the right hand glove with the thumb extended; and
FIG. 4 shows a top view of a golfer holding a golf club in a preferred manner using the golf gloves.
DETAILED DESCRIPTION
The pair of golf gloves described herein are for a right handed person. Therefore, the left hand glove 10 shown in FIGS. 1 and 2 are for the upper hand (furthest from the ground), and the right hand glove 9 shown in FIG. 3 is for the lower hand (closest to the ground). For a pair of golf gloves for a left handed person the position of the hook and pile fasteners on the left hand glove 10 and right hand glove 9 are reversed. For a left handed person the right hand is the upper hand and the hook and pile fasteners shown in FIGS. 1 and 2 would instead be oil the right hand glove 9 in a mirror image orientation. Similarly, for the left handed person the left hand is the lower hand and the hook and pile fasteners shown in FIG. 3 would instead be on the left hand glove 10 in a mirror image orientation.
In FIGS. 1 and 2, left hand glove 10 has fastener elements 11 and 13 that are hook type material and fastener element 12 that is a pile type material. On the right hand glove 9 shown in FIG. 3 fastener elements 27 and 29 are pile type material and fastener element 28 is hook type material. As is well-known in the fastener art, pile type material will not fasten to other pile type material, hook type material will not fastened to other hook type material, but hook type material will fasten firmly to pile type material. The orientation of hook type and pile type fastener material on the left hand glove 10 and right hand glove 9 is such that a golfer cannot inadvertently hold a golf club in a wrong matter and fasten the left hand glove 10 to the right hand glove 9 in an improper orientation.
Left golf glove 10 , shown in FIGS. 1 and 2, has a glove thumb 14 , index glove finger 15 , middle glove finger 16 , ring glove finger 17 , little glove finger 18 , and palm area 19 . Attached to glove finger 14 are three pieces of fastener material. An elongated piece of hook type fastener material 11 is attached to the side of glove thumb 14 on the side furthest from glove index finger 15 . A piece of pile type fastener material 12 is attached to the back side of glove thumb 14 adjacent to tip end of glove thumb 14 and adjacent to fastener material 11 as shown. A piece of hook type fastener material 13 is attached to the side of glove thumb 14 on the side nearest to glove index finger 15 , adjacent to the tip of glove thumb 14 , and adjacent to fastener material 12 as shown.
Fastener material 11 , 12 and 13 fasten to and cooperate with other faster elements attached to right hand glove 11 , shown in FIG. 3, and these other faster elements are described further in this Detailed Description with reference to FIG. 3 .
In FIG. 3, right golf glove 9 has a glove thumb 20 , index glove finger 21 , middle glove finger 22 , ring glove finger 23 , little glove finger 24 , and palm area 25 . Attached to right golf glove 9 are fastener elements 14 , 15 and 29 . Fasteners 14 and 29 are pile type material, and fastener 28 is hook type material.
Fastener 27 is elongated, is the same length as fastener 11 on left glove 10 , and is attached to the palm of the lower hand right glove 9 near, but spaced from, the base of glove thumb 20 . Fastener 28 is attached to the base of the glove thumb 20 . Fastener 29 is attached to the tip of glove ring finger 23 on the palm side of glove 11 .
When gloves 9 and 10 are worn by a golfer who is holding a golf club (not shown) to swing same, and the hook and loop fastener elements on both gloves 9 and 10 are all properly fastened to each other, they are fastened together as follows. Hook fastener 11 on left golf glove 10 is parallel to and fastened to loop fastener 27 on right golf glove 9 . Loop fastener 12 on left golf glove 10 is fastened to hook fastener 28 on right golf glove 9 . Loop fastener 29 on right golf glove 9 is fastened to hook fastener 13 on left golf glove 10 .
Across the base of fingers 16 , 17 and 18 of left golf glove 10 , and on the palm side of the glove, is a colored stripe 26 that guides the correct placement of a golf club (not shown) in the left hand of the golfer. Any color may be used. After laying the club head on the ground in one of the well known open, closed or squared positions, as selected by the golfer, the golfer wearing gloves 9 and 10 places the handle of the golf club (not shown) along the colored stripe 26 across the palm side of left golf glove 10 and closes the left hand over the club handle. Left golf glove 10 fingers 16 , 17 and 18 are firmly but softly closed around the golf club handle. Glove thumb 14 is placed parallel to and along the shaft of the golf club pointing toward the head of the club. Left glove 10 index finger 15 is not closed around the shaft of the golf club, but is curved slightly and lightly touches the handle of the golf club.
The golfer then places right golf glove 9 around the shaft of the golf club using fasteners 11 and 12 on left golf glove 10 as a guide to fasten its fastener 27 to fastener 11 on left golf glove 10 , and its fastener 28 to fastener 12 on left golf glove 10 . Fasteners 11 and 27 are elongated and are positioned parallel to and directly on top of each other when they are brought into contact to fasten them together. Right glove glove 9 thumb 20 is placed parallel to and along the shaft of the golf club (see FIG. 4) pointing toward the head of the club. Right golf glove 9 thumb 20 is then rolled leftward to fasten its fastener 28 to fastener 12 on left golf glove 10 . Right golf glove 9 fingers 22 , 23 and 24 are then firmly but softly closed around the golf club handle. As this is done fastener 29 on the tip of right golf glove 9 ring finger 23 is pushed into and fastens to fastener 13 on the end of left golf glove 10 thumb 14 . Right glove index finger 21 is not fully closed around the shaft of the golf club, but is curved and touches the shaft of the club in a well known manner. Gloves 9 and 10 are now fastened together in a preferred neutral hold around the golf club (see FIG. 4) and remain in that hold during a back swing and forward swing to hit a golf ball.
In FIG. 4 is shown a top view of a golfer holding a golf club in the preferred neutral manner described in the previous paragraph using gloves 10 and 11 .
While what has been described above is the preferred embodiment of the invention, it will be understood that changes may be made thereto without departing from the spirit and scope of the invention. For example, fastener means other than loop and pile fasteners may be utilized, or no fasteners at all need be utilized.
For more experienced golfers the previously described fasteners may be replaced with colored areas or interface elements, similar to colored stripe 26 , to direct the placement of the golfer's hands. Fasteners 11 and 27 would be replaced by colored interface elements of a first color that may or may not have the same shape and size as the fasteners, fasteners 12 and 28 would be replaced by colored interface elements of a second color that may or may not have the same shape and size as the fasteners, and fasteners 13 and 29 would be replaced by colored interface elements of a third color that may or may not have the same shape and size as the fasteners. A golfer wearing such gloves would align the like colored interfaces on each of the gloves, as described above for the fasteners, to achieve the preferred neutral grip on the golf club.
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A pair of golf gloves each having loop and pile interfaces at specific locations that fasten together as a golfer grasps a golf club, and they aid the golfer to properly grasp, hold and maintain a preferred neutral hold on a golf club during back swing and forward swing to achieve a good golf shot.
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CROSS REFERENCE TO A RELATED APPLICATION
The present application is a divisional of U.S. patent application Ser. No. 08/662,842 filed Jun. 12, 1996, which was a continuation-in-part of U.S. patent application Ser. No. 08/489,611, filed Jun. 12, 1995 abandoned.
BACKGROUND OF THE INVENTION
This invention relates to labels and, more particularly, to pressure sensitive labels of the kinds which may adhesively be secured to substrates, such as bottles or other containers, and which provide an integral brochure. In another of its aspects, this invention relates to a method of making such labels. In general, this invention relates to an improved label integrated with a printed brochure and a method of making such a label and an assembly of such labels carried on a flexible liner.
SUMMARY OF INVENTION
Labels which incorporate brochures or booklets have heretofore been proposed. Such labels, sometimes called “brochure labels,” are useful for applications in which (1) it is expedient or necessary to provide with a packaged product detailed directions for usage; (2) regulatory requirements, as in the case of pharmaceuticals, make it necessary to provide with the product a great deal of explanatory information; and (3) it is desired to provide promotional or game materials with the product. Other applications will occur to those skilled in the art.
It is particularly desirable, from both practical and aesthetic points of view, that a brochure label be made “resealable,” that is, so constructed and arranged that opening or use of the brochure associated with the label does not render impossible resealing of the brochure. A resealable brochure label may be restored to its initial appearance and condition after having been opened. It is also highly desirable that a brochure label be capable of neatly wrapping around the sharp or small radius corners of a square container. In such an application, the brochure must often be made to wrap around three or four corners, each of which provides a stress point for the brochure and an opportunity for highly undesirable local bunching or buckling. The present invention provides for a smooth and highly pleasing wrap.
Another desirable attribute in a brochure label is ease of opening and resealability. The present invention provides a simple and effective tab to facilitate opening, as well as capability of repeated resealing.
In some applications, it is necessary or desirable that the graphics and other aesthetic aspects of the brochure be integrated with those of the products labeled, so as to provide a uniform appearance and appeal. In prior art constructions, the label design has often been different from the brochure, imparting to the entire product the appearance of an “afterthought” rather than a well-integrated whole. In accordance with the present invention, the printing of the brochure component of a brochure label can be coordinated with that of the base label, using matched or coordinated materials or printing techniques, so that the base label and brochure provide the appearance of a unitary piece.
Finally, in some instances it is desirable that one or more leaves or pages of the brochure be made removable, or that provision be made for removability of the entire brochure at the user's option. As is explained below, suitable structural features may be provided within the purview of the present invention to achieve these desirable ends.
Labels in accordance with the present invention may be delivered to users in roll form and applied to packages in the same manner, using the same equipment, and at satisfactory production speeds (generally in excess of 200 bottles per minute) as standard pressure sensitive labels.
Accordingly, and in general, the present invention provides an adhesive label assembly which includes an integral brochure. The assembly comprises a pressure sensitive base label, adhesively and releasably supported by a flexible liner. A brochure is associated with the base label and is made up of a folded sheet providing panels, or pages, of the brochure. The brochure is positioned to overlie at least a portion of the base label, and the top panel of the brochure is made to project laterally beyond a lateral edge of the base label. The projecting portion of the top panel may provide a tab to facilitate opening of the brochure. A self-adhesive transparent overlayer is provided over the upper surface of the base label and also the top panel of the brochure. The overlayer is made to extend beyond an edge of the top panel, to facilitate sealing and resealing by adhesion of the overlayer to the container or other substrate to which the base label is applied or to a remote end portion of the base label. Alternatively, sealing and resealing of the overlayer may be accomplished by adhering the extended portion of the overlayer to a portion of the base label which extends beyond a bottom panel of the brochure. Regardless of the specific embodiment of the invention, the top panel may also provide a tab, which, in association with the projecting portion of the overlayer, provides both a means for sealing the brochure and a means for easily gripping the brochure to facilitate opening.
Optionally, perforations may be provided on one or more panels of the brochure, to facilitate ready removal of the page provided by that panel. Those skilled in the art will appreciate that the removed page may be or include a coupon, a premium, or a pre-printed request for additional information.
Optionally and alternatively, a line of perforations may be provided in the base label and overlayer, so that the consumer may remove the booklet without destroying the copy contained on the base label beneath it.
In still another of its aspects, the invention provides a method of making an adhesive label assembly of the kind having an integral brochure. The method comprises steps of: providing a pressure sensitive base label web comprising a base label sheet and a flexible liner releasably secured to the base label sheet; die cutting through the base label sheet but not the liner to form a blank for at least one and preferably two or more base labels; and stripping from the liner the material of the base label sheet other than the blank. Next, a brochure blank assembly, printed to provide multiple brochures, is mated to the base label web and so positioned that a top panel of the assembly projects laterally beyond what will be the lateral edge of the base label. Alternatively, at least a portion of the base label also extends beyond a bottom panel of the brochure. Next, there is applied over the liner, brochure blank assembly and base label an overlayer of self-adhesive material, the self-adhesive material serving to secure the brochure blank assembly to the base label blank and also adhering to the liner adjacent to the tab portion. Alternatively, where the base label extends beyond the bottom panel of the brochure, the overlayer self-adhesive material serves to secure the brochure blank assembly to the base label and also adhere to the extended portion of the base label.
Optionally, brochure blank assembly may be affixed to the base label by a suitable adhesive or by other affixation means. Die cutting through the overlayer and stripping of the waste yields the desired label assembly, with the individual labels releasably secured to the flexible liner.
BRIEF DESCRIPTION OF THE DRAWINGS
There are seen in the drawings forms of the invention which are presently preferred (and which constitute the best mode contemplated for carrying the invention into effect), but it should be understood that the invention is not limited to the precise arrangements and instrumentalities shown.
FIG. 1 is a pictorial view, in perspective, of a label assembly in accordance with the invention.
FIG. 2 is a cross-sectional view taken along the line 2 — 2 in FIG. 1 .
FIG. 3 is a cross-sectional view of a form of label in accordance with the invention.
FIG. 4 is a cross-sectional view of another form of label in accordance with the invention.
FIG. 5 is a top plan view, in cross-section, of an exemplary label in accordance with the invention, applied to a substrate in the form of a flat-sided container with small radius corners.
FIG. 5 a is a top plan view similar to FIG. 5, also in cross-section, of another exemplary label in accordance with the invention, applied to a substrate in the form of a container of round cross-section.
FIG. 6 is a plan view of a brochure blank for use in the invention.
FIG. 7 is a plan view of a brochure blank for use in an alternative form of the invention.
FIG. 8 depicts a portion of a base label web as used in the invention.
FIG. 9 depicts a base label web, die cut prior to stripping waste, to provide intermediate blanks for base labels in accordance with the invention.
FIG. 9 a depicts an alternative form of base label web.
FIG. 10 is a plan view illustrating a brochure blank assembly associated with a base label web in accordance with the invention.
FIG. 11 is a view similar to FIG. 10, illustrating the step of die cutting to produce finished labels.
FIG. 12 is a detail view of a portion of a label in accordance with the invention.
FIG. 13 is a cross-sectional view of yet another form of label in accordance with the invention.
FIG. 14 is a pictorial view, in perspective, of another form of the label assembly in accordance with the invention.
FIG. 15 is a cross-sectional view taken along the line 15 — 15 in FIG. 14 of a label of this invention in a closed position.
FIG. 16 is a cross-sectional view taken along the line 15 — 15 in FIG. 14 of a label of this invention in an open position.
FIG. 17 is a detail view of a portion of the label of FIG. 14 .
FIG. 18 is a plan view of a brochure blank for use with the label of FIG. 14 .
FIG. 19 depicts a base label web, die cut prior to stripping waste, to provide intermediate blanks for base labels in accordance with the invention.
FIG. 20 is a plan view illustrating the brochure blank assembly associated with the base label web in accordance with the label of FIG. 14 .
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring now to the drawings in detail, wherein like reference numerals indicate like elements, there is seen in FIG. 1 a label assembly designated generally by the reference numeral 10 . The label assembly 10 includes plural individual labels 12 , disposed on a flexible liner 14 . It should be understood that the thicknesses of the liner 14 and labels 12 , as well as the various components which are laminated to make up the label 12 , are exaggerated for clarity.
Referring to FIGS. 1 and 2, an individual label 12 will be described in detail. The label 12 includes a base label 16 , a brochure 18 and a transparent overlayer 20 . Seen in FIG. 2 is an adhesive layer 22 by which the overlayer 20 is secured to the base label and the brochure 18 (and which, in turn, secures the brochure 18 to the base label 16 ), and an adhesive layer 24 which releasably secures the base label 16 to the liner 14 .
The brochure 18 in FIGS. 1 and 2 is a leaflet which has two leaves 26 and 28 , separated by a fold line 30 . The top leaf 26 , it will be seen, is wider than the bottom leaf 28 , and thus extends further from the fold line 30 than does the bottom leaf 28 . A portion of the top leaf 26 extends beyond the lateral edge 31 of the base label 16 . As is perhaps best seen in FIG. 1 (and also in FIG. 12 ), a portion of the top leaf 26 is shaped to provide a tab 32 , the purpose of which will be described shortly. As is also apparent in FIG. 1, a portion 34 of the overlayer 20 projects beyond a lateral edge 36 of the top leaf 26 in the vicinity of the tab 32 , and is thus adhesively joined directly to the liner 14 .
Referring now to FIG. 5, the manner in which a label such as the label 12 may be affixed to a substrate in the form of a container 38 is seen. In the example shown in FIG. 5, the container 38 is a round cornered square container. The label 12 wraps completely around the circumference of the container 38 , without any bunching or buckling of the brochure 18 at the corners. This desirable result is achieved because, as described above, the top leaf 26 of the brochure 18 and the portion 34 of the overlayer 20 extend beyond the lateral edge 31 of the base label 16 . In such an arrangement, the top leaf 26 , with its associated overlayer 20 can be drawn tightly and smoothly during application of the label 12 to the container 38 , thus enabling the adhesive 22 of the portion 34 to self-adhere (in the illustrated example) to a terminal portion 13 of the label 12 . In other applications, such as the one shown in FIG. 5 a (in which elements corresponding to those already described are designated by like, primed (′), reference numerals), the adhesive 22 ′ of a portion 34 ′ may adhere directly to a container 38 ′.
The tab 32 facilitates opening of the brochure, because it is interposed between the adhesive 22 , 22 ′ and, as the case may be, the terminal portion 13 of the label 12 or the container 38 ′. The tab 32 thus provides a convenient “handle” and an aid to opening of the brochure. On the other hand, the adhesive 22 , 22 ′ on the portions 34 , 34 ′ facilitates repeated resealing of the brochure as the contents of the containers 38 , 38 ′ are used.
It should be understood that the embodiments seen in FIGS. 5 and 5 a are illustrative, and that a label applied as shown in FIG. 5 may be used to advantage on a round or otherwise shaped container or substrate, such as the round container 38 shown in FIG. 5 a . Similarly, a label may be applied as shown in FIG. 5 a to a square or rectangular container, such as the container 38 of FIG. 5 .
The stock from which the base labels 16 are made is commercially available and familiar to those skilled in the art. It generally comprises a layer of paper, peelably joined by pressure sensitive adhesive to a liner of flexible plastic polymeric film.
The material for the overlayer 20 is also commercially available, and comprises a flexible clear plastic polymeric film, coated on one face with a clear pressure sensitive adhesive (which provides the adhesive 22 , 22 ′). The top surface of the overlayer 20 may be treated in a known manner (as by having on it a release agent) to facilitate release and to avoid co-adhesion failure.
Referring now to FIGS. 1 and 6 through 11 , a method of making an adhesive label assembly in accordance with the invention will be described.
In general, the method involves the following steps, each of which will be described in somewhat greater detail below: A brochure blank assembly 40 is created by printing, cutting and folding. The brochure blank assembly is prepared in full web width. A base label is printed, also in full web width. Next, the base label is die cut from a base label web 42 and, excess is stripped to base label blanks, each blank ultimately providing, in the presently preferred form of the method, two base labels. Next, the brochure blank assembly 40 is brought together with the die cut and stripped base label web, and a pressure sensitive overlayer 20 is applied over the exposed liner 14 , the base label and brochure blank assembly, joining in the process the base label and brochure. No glue is required to assemble the base label and brochure, although glue may optionally be used in some embodiments. Finally, the assembled base label, brochure and overlayer are die cut to the final outline of the label, and waste is stripped to yield the final label assembly.
Referring now to FIG. 6, the brochure blank assembly 40 may be created as follows: The brochure is printed by any suitable process, in the presently preferred process by sheet-fed offset printing in full web width (typically about twelve inches). Each sheet may contain multiple repetitions width wise. One presently preferred form of the process prints four wide. The portions of the blank assembly 40 which, with further trimming, will ultimately form the above-mentioned tabs 32 , are preferably die cut, although other techniques may occur to those skilled in the art. The sheet is then trimmed to size and folded as desired, as at fold line 30 in FIG. 6 .
Referring now to FIG. 8, a base label web, designated generally by the reference numeral 42 , a portion of which is seen in the Figure, is provided. The base label web is comprised of a base label sheet 44 , of paper or other suitable material and liner 14 releasably adhered to the base label sheet 42 . The base label web 42 has respective lower 46 and upper 48 faces, and has on its lower face a continuous layer 24 of adhesive which provides the above-mentioned adhesive layer 24 in the finished product. Printed matter suitable to the intended finished product may be applied to the upper face 48 of the base label sheet 44 by any suitable printing process. Suitable eye and machine-readable positioning, “eye” and registration marks “M” may also be printed on the base label sheet 44 , to facilitate joining of the brochure blank assembly 40 with the base label web 42 (as described below) and other automated process steps. As is apparent in FIG. 8, printing of the base label sheet 44 is preferably done in full web width, providing multiple repetitions across the width of the web. The illustrated example provides four repetitions designated in the Figure as 50 a-d.
FIGS. 9 and 9 a depict alternative forms of the base label web 42 after die cutting through the base label sheet 44 (but not the liner 14 ) to form base label blanks 52 . In FIG. 9, the die cutting operation provides two base label blanks 52 , the width of each blank 52 enabling it to provide a base label 16 (FIG. 1) for two labels 12 . In the alternative arrangement shown in FIG. 9 a , a single base label blank 52 ′ is provided, of a width enabling it to provide a base label 16 for four labels 12 . Other equivalent arrangements will occur to those skilled in the art. After die cutting, waste material “W” around the base label blanks may be stripped from the base label web 42 .
Referring now to FIGS. 10 and 11, the step of joining the brochure blank assembly 40 with the base label web 42 is illustrated. As is best seen in FIG. 10, the brochure blank assembly 40 is brought into juxtaposition with the base label web 42 in such a way that the fold 30 extends transversely with respect to the base label sheet 44 . It will be recognized that this operation may be automated in ways familiar to those skilled in the art, drawing brochure blank assemblies 40 , for example, from a hopper (not seen) and synchronizing the application of brochure blank assemblies 40 to a moving base label web 42 . Folding of the brochure blank 40 is done in such a way as to provide an assembly having a top panel 54 , which ultimately forms the abovementioned top leaves 26 of the brochures 18 , and a bottom panel 56 , which ultimately forms the bottom leaves 28 of the brochure 18 . Associated with the top panel 54 are projections 58 which, after further cutting described below, form the tabs 32 associated with the top leaves 26 . The top panel 54 , it should be understood, extends from the fold line 30 a distance greater than the width of the bottom panel 56 , so that when the brochure blank assembly 40 is positioned with respect to the base label web 42 , the panel 54 projects beyond a lateral edge 60 of what will become the base label 16 .
A continuous transparent overlayer 20 is next applied, by conventional laminating techniques, over the joined brochure blank assembly 40 and base label web 42 , covering and adhering to the portions of the base label blanks 52 not covered by the brochure blank assembly 40 , to the top panel 54 of the brochure blank 40 , and to the remainder of the base label web 42 .
Referring now to FIG. 11, the final die cutting step will now be described. In this step, the individual labels 12 are cut to their final external dimensions by cutting through the overlayer 20 , the brochure blank assembly 40 and the base label blanks 52 , but not the liner 14 . This die cutting step establishes the final outline of the tabs 32 as well. Stripping from the liner 14 of the excess material (i.e., material outside the outline of the label as defined by the die) yields the label assembly 10 depicted in FIG. 1 .
The overlayer 20 may also be perforated, as at 62 in FIG. 11, adjacent to the fold line 30 of the brochure blank assembly 40 . Such a perforation facilitates selective ready removal of the entire brochure 18 from a label 12 , by grasping of the brochure and tearing of the overlayer 20 along the perforation 62 . The perforation 62 may be made as part of the final die cutting step described above, by die cutting through the overlayer 20 .
FIGS. 3 and 4 illustrate particular features of various forms of labels in accordance with the invention. In FIG. 3, there is shown in dotted line the manner in which one of the leaves of the brochure may be removed, for use as a return coupon or a source of information. For this purpose, a line of perforations 63 may be provided across the leaf 28 in a direction transverse to the leaf, to facilitate removal of the leaf. The perforation 63 may be made during printing or die cutting of the brochure blank assembly from which the brochure 18 is made.
FIGS. 4 and 7 illustrate aspects of an alternative form of the invention, which provides a potential for eight pages of text within a brochure made up of four leaves. In this embodiment a brochure blank 64 , as seen in FIG. 7, is so folded as to provide respective panels 66 , 68 , 70 and 72 . The panels 70 and 72 , it will be understood, may be folded behind the panels 66 and 68 , and the thus-folded blank 64 thereafter used in the manner described above in connection with the brochure blank assembly 40 . Final die cutting in the manner described above yields from the panels 66 - 72 a total of 4 leaves.
It will be appreciated that in folding the brochure blank 64 , a line of glue 74 may be applied to the blank 64 , as illustrated in FIG. 7, to maintain the leaves provided by the panels 70 and 72 in position relative to the other panels after the final die cutting step. The glue 74 may be applied in a conventional manner before the folding step. As is apparent from FIG. 4, with this embodiment, one pair of leaves may, if desired, be extracted from the brochure as a return coupon or informational piece.
Those skilled in the art will appreciate that although the above-described embodiments of the brochure are “book-like” in the sense that they have leaves joined at a spine (defined by a fold line), it is within the purview of the invention to provide a brochure whose panels are joined by spaced parallel fold lines. Such an embodiment of the invention is seen in FIG. 13 and designated generally by reference numeral 76 .
FIGS. 14 through 20 depict yet another embodiment of this invention. Referring to FIGS. 14 and 15, label 12 comprises base label 16 , brochure 18 and overlayer 20 . Brochure 18 may comprise any number of panels as exemplified by the seven panel construction depicted in FIGS. 14, 15 , 16 and 17 . Seen in FIG. 15 is adhesive layer 22 by which overlayer 20 is secured to top leaf 26 of brochure 18 and base label 16 , an adhesive layer 80 which secures bottom leaf 28 of brochure 18 to base label 16 , and adhesive layer 24 which releasably secures base label 16 to liner 14 .
Although brochure 18 in FIGS. 14, 15 , 16 , and 17 is a leaflet which is formed or folded to provide seven printed surfaces or “panels,” it will be apparent to those skilled in the art that label 12 may accommodate numerous configurations of brochure 18 . In the embodiment of FIGS. 14, 15 , 16 and 17 , fold line 30 separates leaves 26 and 28 . Fold line 30 also forms an area in which the additional panels of brochure 18 may be folded (for example along fold lines 30 ′ and 30 ″ as shown in FIGS. 15 and 16) and inserted between leaves 26 and 28 when label 12 is in the closed position.
Top leaf 26 is wider than bottom leaf 28 , and thus extends further from fold line 30 than does bottom leaf 28 . Additionally, a portion of top leaf 26 designated as area 32 in FIGS. 14, 15 and 17 extend beyond lateral edge 31 of base label 16 shown in FIG. 14 .
As will be apparent to those skilled in the art, label 12 as depicted in FIGS. 14, 15 , 16 and 17 may be affixed to containers with various cross-sections including, but not limited to, containers 38 shown in FIGS. 5 and 5 a . Generally, label 12 may take numerous shapes and may be adhered to the entire surface area of container 38 , such as container 38 shown in FIG. 5 a . For example, label 12 of FIG. 14 could be adhered to any one of the four sides of container 38 shown in FIG. 5 . Alternatively, label 12 could be adhered to any two sides and any corner of container 38 .
Tab 32 of label 12 depicted in FIGS. 14, 15 , and 17 (shown with a corner turned upward in order to demonstrate the flexibility of tab 32 ) facilitates the opening of the brochure because it is interposed between leaf 26 of brochure 18 and container 38 , and further, because of notched opening 82 in base label 16 . When applied to container 38 , relief notch 82 creates a space between leaf 26 and the substrate (such as container 38 ) to which label 12 is affixed. Tab 32 thus provides a convenient “handle” and an aid to gaining access to brochure 18 . On the other hand, as best shown in FIG. 17, adhesive 22 present on portion 34 of overlayer 20 facilitates repeated unsealing and resealing of brochure 18 as container 38 is used.
The materials used in the construction of this embodiment of the invention depicted in FIGS. 14, 15 , 16 and 17 may be the same as used in the construction of other embodiments of this invention. In addition, adhesive 80 may be any material suitable for adhering brochure 18 to base label 16 and preferably is a cold glue.
Referring now to FIGS. 14 and 18 through 20 , a method of making an adhesive label assembly in accordance with the instant embodiment of label 12 will be described.
In general, the method involves the following steps, each of which will be described in greater detail below: brochure blank assembly 40 is created by printing, cutting and folding. Brochure blank assembly 40 is prepared in full web width. Base label 16 is printed, also in full web width. Next, base label 16 is die cut from base label web 42 (which, in part, forms relief notch 82 ) and excess waste (depicted in the accompanying figures as “W”) is stripped from base label blanks 52 , each blank ultimately providing, in the presently preferred form of the method, three base labels 16 . Next, brochure blank assembly 40 is affixed to base label blank 52 by applying adhesive 80 to base label blank 52 and joining brochure blank assembly 40 to adhesive 80 . Although in this embodiment adhesive 80 is generally necessary if brochure 18 is to remain affixed to base base label 16 , it is not necessary to use adhesive 80 if brochure 18 is to be completely removed from label 12 . Overlayer 20 is then applied over exposed liner 14 , base label blank 52 , and brochure blank assembly 40 . Finally, base label blank 52 , brochure assembly 40 and overlayer 20 are die cut to final outline 86 of label 12 , and waste “W” is stripped to yield the final label assembly.
Referring now to FIG. 18, brochure blank assembly 40 may be created as follows: brochure blanks are printed by any suitable process. In the presently preferred process, brochure blank 40 is printed by sheetfed offset printing in full sheets (typically about twenty-four inches wide) and which are cut in half to form a full web width (typically about approximately twelve inches). Each full web width may contain multiple repetitions of printed matter. One presently preferred form of the process prints on each full web width three brochures 18 . Optionally, brochures may be printed on one or both sides of brochure blank assembly 40 . The portions of brochure blank assembly 40 which, with further trimming, will ultimately form tabs 32 of the embodiment of FIGS. 14, 15 , 16 and 17 , are preferably die cut, although other techniques may occur to those skilled in the art. The full web width is then trimmed to size and folded as desired, such as at fold lines 30 , 30 ′ and 30 ″ depicted in FIG. 18 .
Turning now to FIG. 19, base label web 42 of this embodiment is preferably printed as disclosed above except that three rather than four repetitions are preferably printed across base label web 24 , although other repetitions are possible.
FIG. 19 depicts a form of base label web 42 after die cutting through base label sheet 44 (but not liner 14 ) to form three attached base label blanks 52 . The die cutting operation of FIG. 19 provides three attached base label blanks 52 , which blanks 52 are to be separated in a later step in the process. The width of each blank 52 enables it to provide a base label 16 for three labels 12 . Other equivalent arrangements will occur in those skilled in the art. After die cutting, the waste material “W” around base label blanks 52 may be stripped from base label web 42 .
Referring now to FIG. 20, the step of joining the brochure blank assembly 40 with base label web 42 is illustrated. First, adhesive 80 is applied to a section of each label blank 52 at which section brochure blank assembly 40 will be applied to label blank 52 . Adhesive 80 may be applied by any means shown in the art but preferably adhesive 80 will be applied to base label blanks 52 in a continuous area approximately the size and shape of brochure blank assembly 40 . Alternatively, adhesive 80 may be applied to the underside of brochure leaf 28 .
After application of adhesive 80 , brochure blank assembly 40 is brought into juxtaposition with base label web 42 in such a way that fold 30 extends transversely with respect to base label sheet 44 . It will be recognized that this operation may be automated in ways described above with respect to the embodiment of the invention described herein. Folding of brochure label 40 is done in such a way as to provide an assembly having a top panel 54 , which ultimately forms the above-mentioned top leaves 26 of brochures 18 , and bottom panels 56 (not shown in FIG. 20 ), which ultimately forms bottom leaves 28 of brochure 18 . Associated with top panel 54 are projections 58 which, after further cutting described below, form tabs 32 associated with top leaves 26 . Top panel 54 , it should be understood, extends from fold line 30 a distance greater than the width of bottom panel 56 , so that when brochure blank assembly 40 is positioned with respect to base label web 42 , panel 54 projects beyond lateral edge 60 of what is fold 30 ′ such that top panel 54 may contact at least a portion of label blank 52 .
A continuous transparent overlayer 20 is next applied, by conventional laminating techniques, over joined brochure blank assembly 40 and base label web 42 , covering and adhering to the portions of base label blanks 52 not covered by brochure blank assembly 40 , to top panel 54 of brochure blank 40 , and the remainder of the base label web 42 .
The final die cutting step is substantially as described with respect to other embodiments of this invention. In this step, individual labels 12 are cut to the final external dimensions. This die cutting step establishes a final label outline 86 of label 12 (including tab 32 ) as depicted in FIG. 20 . Stripping from liner 14 of excess material (i.e., material outside final label outline 86 ) yields label assembly 10 depicted in FIG. 14 .
The present invention may be embodied in other specific forms without departing from its spirit or essential attributes. Accordingly, reference should be made to the appended claims rather than the foregoing specification as indicating the scope of the invention.
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A pressure sensitive brochure label is both resealable and readily applicable to containers with sharp or small radius corners. The label comprises a pressure sensitive base label, a specially die cut brochure and a pressure sensitive overlayer, the overlayer serving to join the brochure to the base label, the base label and the brochure providing areas capable of carrying printing. The top leaf of the brochure projects beyond an edge of the base label and a portion of the overlayer projecting beyond the top leaf provides for sealing and resealing of the brochure in conjunction with a die cut tab on the brochure. In another embodiment, a relief notch in the base label in conjunction with the tab and portion of the overlayer which projects beyond the top leaf provides for sealing and resealing of the brochure. A method of making an adhesive brochure label assembly involves die cutting base label blanks from a base label web, applying a web-width brochure assembly over the base label blanks, applying an overlayer to the base label web and brochure assembly, and cutting the overlayer, brochure assembly and base label blanks to define the final outline of the brochure labels of the assembly.
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FEDERAL RESEARCH STATEMENT
[0001] This invention was made with government support under contract number DE-EE0003955 awarded by the Department of Energy. The government has certain rights in the invention.
BACKGROUND OF THE INVENTION
[0002] The present disclosure relates to refrigeration systems. More specifically, the present disclosure relates to refrigeration systems with multiple heat transfer fluid circulation loops.
[0003] Refrigerant systems are known in the HVAC&R (heating, ventilation, air conditioning and refrigeration) art, and operate to compress and circulate a heat transfer fluid throughout a closed-loop heat transfer fluid circuit connecting a plurality of components, to transfer heat away from a secondary fluid to be delivered to a climate-controlled space. In a basic refrigerant system, heat transfer fluid is compressed in a compressor from a lower to a higher pressure and delivered to a downstream heat rejection heat exchanger, commonly referred to as a condenser for applications where the fluid is sub-critical and the heat rejection heat exchanger also serves to condense heat transfer fluid from a gas state to a liquid state. From the heat rejection heat exchanger, where heat is typically transferred from the heat transfer fluid to ambient environment, high-pressure heat transfer fluid flows to an expansion device where it is expanded to a lower pressure and temperature and then is routed to an evaporator, where heat transfer fluid cools a secondary heat transfer fluid to be delivered to the conditioned environment. From the evaporator, heat transfer fluid is returned to the compressor. One common example of refrigerant systems is an air conditioning system, which operates to condition (cool and often dehumidify) air to be delivered into a climate-controlled zone or space. Other examples may include refrigeration systems for various applications requiring refrigerated environments.
[0004] However, many proposed systems having two-phase CO 2 as a secondary heat transfer fluid require the CO 2 to be maintained in a supercritical fluid state, which can add to equipment and operating complexity and cost. Further, conventional operation, especially startup, of such a system can result in operational inefficiency and pump cavitation in the secondary heat transfer loop.
BRIEF DESCRIPTION OF THE INVENTION
[0005] In one embodiment, a method of operating a heat transfer system includes starting operation of a first heat transfer fluid vapor/compression circulation loop including a fluid pumping mechanism, a heat exchanger for rejecting thermal energy from a first heat transfer fluid, and a heat absorption side of an internal heat exchanger. A first conduit in a closed fluid circulation loop circulates the first heat transfer fluid therethrough. Operation of a second two-phase heat transfer fluid circulation loop is started after starting operation of the first heat transfer fluid circulation loop. The second heat transfer fluid circulation loop transfers heat to the first heat transfer fluid circulation loop through the internal heat exchanger and includes a heat rejection side of the internal heat exchanger, a liquid pump, and a heat exchanger evaporator. A second conduit in a closed fluid circulation loop circulates a second heat transfer fluid therethrough.
[0006] In another embodiment, a heat transfer system includes a first two-phase heat transfer fluid vapor/compression circulation loop including a compressor, a heat exchanger condenser, an expansion device, and a heat absorption side of a heat exchanger evaporator/condenser. A first conduit in a closed fluid circulation loop circulates a first heat transfer fluid therethrough. A second two-phase heat transfer fluid circulation loop that transfers heat to the first heat transfer fluid circulation loop through the heat exchanger evaporator/condenser and includes a heat rejection side of the heat exchanger evaporator/condenser, a liquid pump disposed vertically lower than the heat exchanger evaporator/condenser, and a heat exchanger evaporator. A second conduit in a closed fluid circulation loop circulates a second heat transfer fluid therethrough.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] The subject matter which is regarded as the invention is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other features, and advantages of the invention are apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
[0008] FIG. 1 is a block schematic diagram depicting an embodiment of a heat transfer system having first and second heat transfer fluid circulation loops;
[0009] FIG. 2 is an elevation view of an embodiment of a heat transfer system having first and second heat transfer fluid circulation loops; and
[0010] FIG. 3 is a schematic plot illustrating an embodiment of a startup sequence for a heat transfer system having first and second heat transfer fluid circulation loops.
DETAILED DESCRIPTION OF THE INVENTION
[0011] An exemplary heat transfer system with first and second heat transfer fluid circulation loop is shown in block diagram form in FIG. 1 . As shown in FIG. 1 , a compressor 110 or other pumping device in first fluid circulation loop 100 pressurizes a first heat transfer fluid in its gaseous state, which both heats the fluid and provides pressure to circulate it throughout the system. The hot pressurized gaseous heat transfer fluid exiting from the compressor 110 flows through conduit 115 to heat exchanger condenser 120 , which functions as a heat exchanger to transfer heat from the heat transfer fluid to the surrounding environment, such as to air blown by fan 122 through conduit 124 across the heat exchanger condenser 120 . The hot heat transfer fluid condenses in the condenser 120 to a pressurized moderate temperature liquid. The liquid heat transfer fluid exiting from the condenser 120 flows through conduit 125 to expansion device 130 , where the pressure is reduced. The reduced pressure liquid heat transfer fluid exiting the expansion device 130 flows through conduit 135 to the heat absorption side of heat exchanger evaporator/condenser 140 , which functions as a heat exchanger to absorb heat from a second heat transfer fluid in secondary fluid circulation loop 200 , and vaporize the first heat transfer fluid to produce heat transfer fluid in its gas state to feed the compressor 110 through conduit 105 , thus completing the first fluid circulation loop.
[0012] A second heat transfer fluid in second fluid circulation loop 200 transfers heat from the heat rejection side of heat exchanger evaporator/condenser 140 to the first heat transfer fluid on the heat absorption side of the heat exchanger 140 , and the second heat transfer fluid vapor is condensed in the process to form second heat transfer fluid in its liquid state. The liquid second heat transfer fluid exits the heat exchanger evaporator/condenser 140 and flows through conduit 205 as a feed stream for liquid pump 210 . The liquid second heat transfer fluid exits pump 210 at a higher pressure than the pump inlet pressure and flows through conduit 215 to heat exchanger evaporator 220 , where heat is transferred to air blown by fan 225 through conduit 230 . Liquid second heat transfer fluid vaporizes in heat exchanger evaporator 220 , and gaseous second heat transfer fluid exits the heat exchanger evaporator 220 and flows through conduit 235 to the heat rejection side of heat exchanger evaporator/condenser 140 , where it condenses and transfers heat to the first heat transfer fluid in the primary fluid circulation loop 100 , thus completing the second fluid circulation loop 200 .
[0013] In an additional exemplary embodiment, the second fluid circulation loop 200 may include multiple heat exchanger evaporators (and accompanying fans) disposed in parallel in the fluid circulation loop. This may be accomplished by including a header (not shown) in conduit 215 to distribute the second heat transfer fluid output from pump 210 in parallel to a plurality of conduits, each leading to a different heat exchanger evaporator (not shown). The output of each heat exchanger evaporator would feed into another header (not shown), which would feed into conduit 235 . Such a system with multiple parallel heat exchanger evaporators can provide heat transfer from a number of locations throughout an indoor environment without requiring a separate outdoor fluid distribution loop for each indoor unit, which cannot be readily achieved using indoor loops based on conventional 2-phase variable refrigerant flow systems that require an expansion device for each evaporator. A similar configuration can optionally be employed in the first fluid circulation loop 100 to include multiple heat exchanger condensers (and accompanying fans and expansion devices) disposed in parallel in the fluid circulation loop, with a header (not shown) in conduit 115 distributing the first heat transfer fluid in parallel to a plurality of conduits each leading to a different heat exchanger condenser and expansion device (not shown), and a header (not shown) in conduit 135 to recombine the parallel fluid flow paths. When multiple heat exchanger condensers are used, the number of heat exchanger condensers and expansion devices would generally be fewer than the number of heat exchanger evaporators.
[0014] The first heat transfer fluid circulation loop utilizes heat transfer fluids that are not restricted in terms of flammability and/or toxicity, and this loop is a substantially outdoor loop. The second heat transfer fluid circulation loop utilizes heat transfer fluids that meet certain flammability and toxicity requirements, and this loop is substantially an indoor loop. By substantially outdoor, it is understood that a majority if not the entire loop is outdoors, but that portions of the substantially outdoor first loop may be indoors and that portions of the substantially indoor second loop may be outdoors. In an exemplary embodiment, any indoor portion of the outdoor loop is isolated in a sealed fashion from other protected portions of the indoors so that any leak of the first heat transfer fluid will not escape to protected portions of the indoor structure. In another exemplary embodiment, all of the substantially outdoor loop and components thereof is located outdoors. By at least partially indoor, it is understood that at least a portion of the loop and components thereof is indoors, although some components such as the liquid pump 210 and/or the heat exchanger evaporator condenser 140 may be located outdoors. The at least partially indoor loop can be used to transfer heat from an indoor location that is remote from exterior walls of a building and has more stringent requirements for flammability and toxicity of the heat transfer fluid. The substantially outdoor loop can be used to transfer heat from the indoor loop to the outside environment, and can utilize a heat transfer fluid chosen to provide the outdoor loop with thermodynamic that work efficiently while meeting targets for global warming potential and ozone depleting potential. The placement of portions of the substantially outdoor loop indoors, or portions of the indoor loop outdoors will depend in part on the placement and configuration of the heat exchanger evaporator/condenser, where the two loops come into thermal contact. In an exemplary embodiment where the heat exchanger evaporator/condenser is outdoors, then portions of conduits 205 and/or 235 of the second loop will extend through an exterior building wall to connect with the outdoor heat exchanger evaporator/condenser 140 . In an exemplary embodiment where the heat exchanger evaporator/condenser 140 is indoors, then portions of conduits 105 and/or 135 of the first substantially outdoor loop will extend through an exterior building wall to connect with the indoor heat exchanger evaporator/condenser 140 . In such an embodiment where portions of the first loop extend indoors, then an enclosure vented to the outside may be provided for the heat exchanger evaporator/condenser 140 and the indoor-extending portions of conduits 105 and/or 135 . In another exemplary embodiment, the heat exchanger evaporator/condenser 140 may be integrated with an exterior wall so that neither of the fluid circulation loops will cross outside of their primary (indoor or outdoor) areas.
[0015] Referring now to FIG. 2 , in some embodiments, the liquid pump 210 is located at a position vertically lower than the heat exchanger evaporator/condenser 140 , with conduit 205 extending downwardly from the heat exchanger evaporator/condenser 140 to ensure sufficient column height of the second heat transfer fluid at the inlet of the liquid pump 210 to avoid cavitation of the liquid pump 210 . Further, internal volumes of the heat exchanger evaporator/condenser 140 and the heat exchanger evaporator 220 are matched to ensure charge balance of the system during a wide range of expected operating conditions. Still further, in some embodiments, the amount of liquid charge in the system, as a percentage of total heat exchanger volume in the system, is about 50% liquid to ensure proper startup of the system, especially the second fluid circulation loop 200 .
[0016] Starting operation of the first fluid circulation loop 100 and the second fluid circulation loop 200 requires coordination of various components in the first fluid circulation loop 100 and the second fluid circulation loop 200 via a plurality of actuators controlling components thereof. Initializing operation of the entire loops 100 and 200 simultaneously reduces system efficiency and may result in system stoppage or breakdown. To maximize system efficiency at startup, the first fluid circulation loop 100 is initialized before startup of the second fluid circulation loop 200 , typically in a range between 0.1 second and 10 minutes prior to second fluid circulation loop 200 startup. In other embodiments, startup of the second fluid circulation loop 200 is started between 0.1 second and 5 minutes or between 0.1 second and 1 minute after startup of the first fluid circulation loop 100 . This ensures a flow of cooled first heat transfer fluid through the heat exchanger evaporator/condenser 140 for thermal exchange with the second heat transfer fluid.
[0017] More particularly, as shown in FIG. 3 , startup of the system begins with opening of the expansion device 130 , followed by startup of the fan 122 to flow air across the condenser 120 . The compressor 110 is then started. After compressor 110 startup and flow of the first heat transfer fluid through the heat exchanger evaporator/condenser 140 begins, after a delay of between 0.1 second and 10 minutes, the liquid pump 210 is then started to draw the second heat transfer fluid through the heat exchanger evaporator/condenser 140 and toward the heat exchanger evaporator 220 . Once flow of cooled second heat transfer fluid through the heat exchanger evaporator 220 is achieved, fan 225 is started to flow air across the heat exchanger evaporator 220 .
[0018] Similarly, when stopping operation of the system, operation of the first fluid circulation loop 100 is stopped before operation of the second fluid circulation loop 200 is stopped. The time delay between shutdown of the first fluid circulation loop 100 and shutdown of the second fluid transfer loop 200 is in a range of between 0.1 second and 10 minutes. In other embodiments, the time delay is between 0.1 second and 5 minutes or between 0.1 second and 1 minute.
[0019] The heat transfer fluid used in the first fluid circulation loop has a critical temperature of greater than or equal to 31.2° C., more specifically greater than or equal to 35° C., which helps enable it to maintain two phases under normal operating conditions. Exemplary heat transfer fluids for use in the first fluid circulation loop include but are not limited to saturated hydrocarbons (e.g., propane, isobutane), unsaturated hydrocarbons (e.g., propene), R32, R152a, ammonia, an R1234 isomer (e.g., R1234yf, R1234ze, R1234zf), R410a, and mixtures comprising one or more of the foregoing.
[0020] The heat transfer fluid used in the second fluid circulation loop has an ASHRAE Class A toxicity rating and an ASHRAE Class 1 or 2L flammability rating. Exemplary heat transfer fluids for use in the second fluid circulation loop include but are not limited to sub-critical fluid CO 2 , a mixture comprising an R1234 isomer (e.g., R1234yf, R1234ze) and an R134 isomer (e.g., R134a, R134) or R32, 2-phase water, or mixtures comprising one or more of the foregoing. In another exemplary embodiment, the second heat transfer fluid comprises at least 25 wt %, and more specifically at least 50 wt % sub-critical fluid CO 2 . In yet another exemplary embodiment, the second heat transfer fluid comprises nanoparticles to provide enhanced thermal conductivity. Exemplary nanoparticles include, but are not limited to, particles having a particle size less than 500 nm (more specifically less than 200 nm). In an exemplary embodiment, the nanoparticles have a specific heat greater than that of the second fluid. In yet another exemplary embodiment, the nanoparticles have a thermal conductivity greater than that of the second fluid. In further exemplary embodiments, the nanoparticles have a specific heat greater than at least 5 J/mol·K (more specifically at least 20 J/mol·K), and/or a thermal conductivity of at least 0.5 W/m·K (more specifically at least 1 W/m·K). In another exemplary embodiment, the second heat transfer fluid comprises greater than 0 wt % and less than or equal to 10 wt % nanoparticles, more specifically from 0.01 to 5 wt % nanoparticles. Exemplary nanoparticles include but are not limited to carbon nanotubes and metal or metalloid oxides such as Si 2 O 3 , CuO, or Al 2 O 3 .
[0021] The expansion device used in the first heat transfer fluid circulation loop may be any sort of known thermal expansion device, including a simple orifice or a thermal expansion valve (TXV) or an electronically controllable expansion valve (EXV). Expansion valves can be controlled to control superheating at the outlet of the heat absorption side of the heat exchanger evaporator/condenser and optimize system performance. Such devices and their operation are well-known in the art and do not require additional detailed explanation herein.
[0022] In another exemplary embodiment, one or more of the compressor 110 , fan 122 , fan 225 , and/or pump 210 utilizes a variable speed drive (VSD). Control of VSD's can be implemented utilizing known power control technologies, such as an integrated power electronic system incorporating an input power factor correction (PFC) rectifier and one or more inverters (e.g., an inverter for each separate VSD). The input PFC rectifier converts single-phase AC input voltage into a regulated DC common bus voltage in order to provide a near unity power factor with low harmonic current from the AC supply. The motor inverters can be connected in parallel with input drawn from the common DC bus. Motors with higher power requirements (e.g., >1 kW such as for compressors) can use insulated gate bipolar transistors (IGBT's) as power switches whereas motors with lower power requirements (e.g., <1 kW such as for fan blowers) can use lower-cost metal oxide semiconductor field effect transistors (MOSFET's). Any type of electric motor can be used in the VSD's, including induction motors or permanent magnet (PM) motors. In an exemplary embodiment, the compressor 110 utilizes a PM motor, optionally in conjunction with electronic circuitry and/or a microprocessor that adaptively estimates the rotor magnet position using only the winding current signals, thus eliminating the need for expensive Hall effect sensors typically used in PM motors. The precise speed settings of the VSD's will vary depending on the demands placed on the system, but can be set by system control algorithms to maximize system operating efficiency and/or meet system demand as is known in the art. Typically, compressor and pump speed can be varied to control system capacity based on user demand, while the speed of the indoor and outdoor fan blowers can be controlled to optimize system efficiency.
[0023] While the invention has been described in detail in connection with only a limited number of embodiments, it should be readily understood that the invention is not limited to such disclosed embodiments. Rather, the invention can be modified to incorporate any number of variations, alterations, substitutions or equivalent arrangements not heretofore described, but which are commensurate with the spirit and scope of the invention. Additionally, while various embodiments of the invention have been described, it is to be understood that aspects of the invention may include only some of the described embodiments. Accordingly, the invention is not to be seen as limited by the foregoing description, but is only limited by the scope of the appended claims.
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A method of operating a heat transfer system includes starting operation of a first heat transfer fluid vapor/compression circulation loop including a fluid pumping mechanism, a heat exchanger for rejecting thermal energy from a first heat transfer fluid, and a heat absorption side of an internal heat exchanger. A first conduit in a closed fluid circulation loop circulates the first heat transfer fluid therethrough. Operation of a second two-phase heat transfer fluid circulation loop is started after starting operation of the first heat transfer fluid circulation loop. The second heat transfer fluid circulation loop transfers heat to the first heat transfer fluid circulation loop through the internal heat exchanger and includes a heat rejection side of the internal heat exchanger, a liquid pump, and a heat exchanger evaporator. A second conduit in a closed fluid circulation loop circulates a second heat transfer fluid therethrough.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to liquid crystal alignment, and more particularly to an apparatus and method for preparing surfaces to provide tilted and vertical alignment of liquid crystal material.
2. Description of the Related Art
Liquid crystal (LC) material employed in liquid crystal displays typically relies on alignment layers to establish a stable pretilt angle for the liquid crystal material. Typically, the alignment of the liquid crystals for flat panel liquid crystal displays (LCD) is accomplished by placing a thin film of LC material on a mechanically rubbed polyimide film coated on a suitable substrate. Limitations imposed by the mechanical rubbing method (e.g., creating multiple domains for improving the viewing angle) in conjunction with the difficulty of optimizing polymer materials (e.g., polymers that avoid image sticking) make it highly desirable to use alternative materials and a non-contact LC alignment method.
There are a number of different methods/materials which have been shown to create LC alignment besides rubbing. For example, these methods/materials may include a stretched polymer, a Langmuir Blodgett film, a grating structure produced by microlithography, oblique angle deposition of silicon oxide, and polarized ultraviolet (UV) irradiation of a polymer film.
Non-contact methods to replace rubbing are described in commonly assigned U.S. Pat. No. 5,770,826, incorporated herein by reference, which describes a particularly attractive and versatile LC alignment process based on ion beam irradiation of a polyimide surface. The method places the LCs on a polyimide surface which has been bombarded with low energy (about 100 eV) Ar + ions. This process has many characteristics which make it suitable for the manufacture of LC displays. This method has been extended to include diamond-like carbon (DLC), amorphous hydrogenated silicon, SiC, SiO 2 , glass, Si 3 N 4 , Al 2 O 3 , CeO 2 , SnO 2 , and ZnTiO 2 films as described in commonly assigned U.S. Pat. No. 6,020,946, incorporated herein by reference. Another method for creating an LC alignment layer in a single deposition process has been described in commonly assigned U.S. Pat. No. 6,061,114, incorporated herein by reference.
Ion-beam treatment on DLC films (IB/DLC) for the alignment of liquid crystals has many advantages over conventional rubbed polyimide alignment, such as, non-contact processing, alignment uniformity, etc. Usually, DLC films of about 50 angstroms thick are deposited by plasma enhanced chemical vapor deposition (PECVD), and followed by Ar ion beam irradiation. It is believed that the Ar ion beam destroys the amorphous-carbon rings which have a large collision cross section to the ion beam. The amorphous-carbon rings which have a small or zero collision cross section to the ion beam are preserved. The average direction of the remaining carbon rings align the liquid crystal and generate a pretilt angle. The pretilt angle of IB/DLC alignment is not stable. The pretilt angle tends to decrease when the IB/DLC substrates are in contact with moisture or other components in air. The pretilt angle decreases as a function of storage time in vacuum-sealed LC cells with IB/DLC alignment. In addition, the pretilt angle is not stable under ultra-violet (UV) or violet irradiation.
After ion-beam treatment, the surface of the DLC films are very active due to the ion-beam induced free radicals on the DLC surface. These free radicals tend to react with many chemical species in contact with them. This reaction may change the surface chemistry of the DLC film or change the orientation the carbon rings. As a result, the pretilt angle will degrade.
Vertical alignment liquid crystal displays (LCD) have become one of the top candidates for LCD monitor applications. This is due, in part, to the wide viewing angle and fast response time provided by vertical alignment LCDs. To control declination in the vertical alignment LCD, a certain pretilt angle is needed. However, good vertical alignment, especially with a pretilt angle, is very difficult to obtain.
Conventional alignment methods include surfactance attachments on oblique evaporated silicon oxide surfaces and rubbed side chain polyimides, as described above. The surfactance attachments approach requires double evaporation processing plus a surfactance attachment. This approach is very complicated and the charge holding ratio of the resultant surface is often excessive. The rubbed side chain polyimides approach uses rubbing to generate pretilt angle. This process is difficult to control and leaves rubbing traces on the display.
Using single oblique evaporation of silicon dioxide to obtain vertical and tilted vertical alignment, high quality vertical alignment may be provided. Van der Waals interaction has been used to explain this phenomena. However, the deposition may be slow and may include unconventional semiconductor processes. The vertical alignment of negative dielectric anisotropic liquid crystal (LC) on silicon dioxide is dominated by the van der Waals interaction and not due to the surface morphology. The thin film deposition method is therefore not limited to oblique evaporation. Other thin film deposition methods, such as sputtering, chemical vapor deposition (CVD) and plasma enhanced chemical vapor deposition (PECVD), can be used to produce zero tilt vertical alignment, as well.
However, since the directionality of sputtering, CVD and PECVD are not as good as oblique evaporation, it is difficult to obtain a suitable pretilt angle. For example, sputtered silicon dioxide from a tilted target can give a pretilt angle of 0.4 degrees. This may be enough to control the domain formation, but the response time is slow.
Therefore, a need exists for a reliable generalized method to produce vertical and tilted vertical alignment by a thin film deposition process and ion beam treatment.
SUMMARY OF THE INVENTION
A liquid crystal display device includes an alignment layer with constituent materials. The constituent materials have a stoichiometric relationship configured to provide a given pretilt angle. Liquid crystal material is provided in contact with the alignment layer. A method for forming an alignment layer for liquid crystal displays includes forming the alignment layer on a substrate by introducing an amount of material to adjust a stoichiometric ratio of constituent materials wherein the amount is determined to provide a given pretilt angle to the alignment layer. Ions are directed at the alignment layer to provide the pretilt angle.
These and other objects, features and advantages of the present invention will become apparent from the following detailed description of illustrative embodiments thereof, which is to be read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF DRAWINGS
The invention will be described in detail in the following description of preferred embodiments with reference to the following figures wherein:
FIG. 1 is a cross-sectional view of a plate having a conductive layer formed thereon in accordance with the present invention;
FIG. 2 is a cross-sectional view of the conductive layer of FIG. 1 showing an alignment base layer formed with a predetermined composition to promote pretilt angle in accordance with the present invention;
FIG. 3 is a cross-sectional view showing the alignment layer of FIG. 2 being treated by an ion beam treatment in accordance with the present invention;
FIG. 4 is a cross-sectional view of an alternate embodiment which shows a quenching step after the ion beam treatment in accordance with the present invention;
FIG. 5 is a cross-sectional view showing a liquid crystal display in accordance with the present invention; and
FIGS. 6A and 6B show pretilt angle (from the vertical direction) against ion beam direction for different materials, and FIG. 6B is a magnified view of FIG. 6 A.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The present invention solves the problems of film deposition by oblique evaporation. The present invention provides a tilted vertical alignment surface for liquid crystal materials and can adjust the pretilt by providing an inorganic film with a particular material composition. Advantageously, tilted vertical alignment can be achieved by employing ion beam irradiation without rubbing. The pretilt angle can be tuned by the composition of the thin film. The present invention generalizes the use of inorganic film vertical alignment to make the process easier for manufacturing.
Negative dielectric liquid crystal (LC) will align vertically when van der Waals interactions are the dominate force. Since the van der Waals force is a short-range interaction, the existence of any other interactions, such as, influences due to grooves, steric hindrance and/or Pi-electron coupling will override the van der Waals forces resulting in non-vertical alignment.
Diamond-like-carbon (DLC) films are used for homogeneous alignment with ion beam treatment. For DLC films, Pi-electrons (π-electrons) from carbon rings are responsible for the alignment of LC. Since the Pi—Pi interactions of the carbon rings are stronger than the van der Waals interaction, the LC tends be parallel to the DLC substrate or gives planar alignment.
In amorphous silicon (a-Si) films, such a Pi-electron loop will not form, and LC will align perpendicularly. Similar alignment was observed on SiOx and SiNx surfaces.
Referring now in detail to the figures in which like numerals represent the same or similar elements and initially to FIG. 1, a cross-section of a portion of a display device 10 is shown for the formation of an alignment layer for liquid crystal. A plate 100 may include a glass substrate or other transparent substrate, such as a plastic substrate. Plate 100 may include a conductive layer 102 formed thereon. Conductive layer 102 may be continuous across the surface of plate 100 (e.g., to form a common electrode for the display) or patterned to form a plurality of pixels or sub-pixels for the display. Conductive layer 102 preferably includes a transparent conductor, such as for example, indium tin oxide (ITO), indium zinc oxide (IZO) or any other suitable conductive material, such as opaque conductive materials for display circuitry.
Conductive layer 102 may include a plurality of different arrangements or patterns. For example, conductive layer 102 may be adapted for use with twisted nematic (TN), in plane switching (IPS) or any other display mode. Conductive layer 102 may not be employed, for example, when an in-plane switching (IPS) device is employed.
Referring to FIG. 2, an alignment layer 104 is formed on conductive layer 102 and on substrate layer 100 in areas not covered by layer 102 . It is to be understood that the structure on which alignment base layer 104 is formed is described for illustrative purposes and should not be construed as limiting the present invention. Alignment layer 104 preferably includes an inorganic layer. In one embodiment, layer 104 begins with a material with homeotropic alignment tendencies, such as, for example, Si, SiO x , Si x N y , etc. In an alternate embodiment, layer 104 may begin with a material with homogeneous alignment tendencies, such as, for example, carbon or silicon carbide.
During the formation of alignment layer 104 , the composition of layer 104 is adjusted to provide a predetermined pre-tilt angle associated with alignment layer 104 . A source 105 is employed to set the composition of alignment layer. The composition of the alignment layer creates a propensity for the layer to provide a stable pretilt angle as a function of the composition alignment layer 104 .
Where layer 104 began as a material with homeotropic alignment tendencies, a material with homogenous alignment tendencies may be added. Where layer 104 began as a material with homogenous alignment tendencies, a material with homeotropic alignment tendencies may be added. This results in stoichiometric relationships which provide a given pretilt angle.
When liquid crystal is in contact with alignment layer 104 , the Pi—Pi interaction due to carbon atoms will compete with van der Waals interaction which arises from atoms such as Si, O, N, etc. which do not form Pi bonds. Depending on the relative composition of the Carbon atoms to the other atoms, the alignment varies from homogeneous (amorphous carbon (a-C) to homeotropic (a-Si, SiO x , etc.). Silicon carbide (SiC x ) provides a system which can be employed to demonstrate the present invention.
Referring to FIGS. 6A and 6B, pretilt angle from homeotropic is plotted against ion beam direction from the substrate normal for different materials. The materials includes amorphous silicon (a-Si), amorphous carbon (a-C:H or diamond-like-carbon (DLC)), glass (SiO x ) and SiC. In accordance with experiments carried out by the inventors, thin films of a-Si, SiC and a-C:H were subjected to ion beam irradiation. Pretilt angles were measured by the crystal rotation method. Pretilt (from homeotropic) for the a-C (DLC) film was very high (e.g., greater than 20 degrees), which means that a-C:H tends to have a homogeneous alignment. For the a-Si film, however, the pretilt angle is very small (e.g., less than 1.0 degrees). Liquid crystal tends to align homeotropically for a-Si. By adding C into the a-Si, the pretilt angle of SiC increases. In accordance with the present invention, by varying the concentration of carbon in the film, the pretilt angle can be adjusted within a wide range of angles.
FIG. 6B is a magnified view of FIG. 6 A. FIGS. 6A and 6B show the pretilt angle (from the vertical direction) against ion beam direction. The pretilt angle of a-C:H is over 15 degrees and not stable. The pretilt angle for a-Si is less than 0.5 degrees and the alignment is stable. By adding carbon to a-Si, the pre-tilt angle increases to 1.5 degrees, which is suitable for display applications.
Referring again to FIG. 2, in one example, a silicon carbide layer ( 104 ) may be formed to provide a given pretilt angle. During formation of a silicon carbide (SiC) alignment layer 104 , a sputtering process may be employed, although other processes may be employed. In accordance with the present invention, the sputtering process employs a larger target area (e.g., source 115 ) for carbon to provide a predetermined amount of carbon in the SiC alignment layer. This results in a SiC x alignment layer where x is greater than zero is set in accordance with an amount of pretilt angle needed for a particular display device. x can by any positive integer depending on the pretilt needed. in other embodiments, a silicon layer is formed first followed by treatment of the silicon with carbon to obtain the desired stoichiometric relationship to provide a given pretilt angle.
Illustratively, a pretilt angle provided by SiC x , where x is about 2, may provide about 4-5 degrees of pretilt, while a pretilt angle provided by SiC x , where x is about 1.5, is between about 0.5 degrees and 1 degree.
For a silicon oxide or a silicon nitride alignment layer or film 104 , N 2 or O 2 , respectively, may be introduced to form a SiO y N z layer, where y and z are adjusted to provide a pretilt angle between about 0 to one degree. y and z are preferably adjusted according to the deposition process for alignment layer 104 . A pretilt angle about 0.4 degrees can be obtained by ion beam treated SiO 2 . Si 2 N 3 surfaces provide a more planar pretilt angle as compared to SiO 2 . Therefore, SiO y N z can be used to tune the pretilt angle for liquid crystal by adjusting the stoichiometric ratio (e.g., adjusting y and z).
Alignment layer 104 may be formed by a plurality of different processes, for example, chemical vapor deposition (CVD), plasma enhanced CVD, sputtering, etc. These processes are modified to provide a desired composition of the deposited alignment layer 104 .
Referring to FIG. 3, alignment layer 104 is treated with an ion beam 110 to create a surface alignment layer 112 . It is noted that ion bombardment may be performed simultaneously with the formation of layer 104 . Surface 112 interacts with the LC (after a display cell is made) and acts as an alignment layer. Advantageously, ion beam 110 is employed to treat alignment layer 104 to provide a pretilt angle to the surface. Ion beam treatment provides unidirectional and controllable pretilt. Pretilt may be generated directly when only oblique deposition is used. For large areas, it is difficult to obtain sufficient and uniform pretilt due to divergence in deposition angle.
In alternate embodiments, ion beam 110 may include Ar or a mixture of Ar and a reactive gas for saturating dangling bonds, and ion bombardment may be followed by immersing surface 112 in a gas or liquid to saturate dangling bonds.
An additional treatment to surface layer 112 may be carried out subsequent to ion bombardment. Such treatments, called “quenching”, may include subjecting surface layer 112 to an ambient chemistry 114 (FIG. 4 ), which may include a gas, plasma, atoms or liquid.
Referring to FIG. 4, a chemically modified surface 117 is formed as a result of quenching and/or ion beam treatment in accordance with the present invention. Layer 117 is now substantially free from dangling bonds and free radicals which could degrade properties of a liquid crystal display. A substrate 101 is now formed for use in a liquid crystal display device.
Referring to FIG. 5, a portion of a liquid crystal display device 10 is illustratively shown in accordance with the present invention. A liquid crystal material 115 is disposed in a gap 120 between substrates 101 . Molecules of liquid crystal material 115 assume a pretilted orientation (angle A) in accordance with the composition of layer 104 as modified by ion beam bombardment (layer 112 ) and/or quenching (layer 117 ).
It is to be understood that the present invention may be employed in twisted nematic (TN), in plane switching (IPS) or any other display mode, for example, multiple domain IPS mode structures, etc. Other display structures or layers may be employed in accordance with the present invention in addition to or instead of the layers shown in the FIGS.
The present invention solves the problems associated with film deposition by oblique evaporation. The tilted vertical alignment on inorganic films can be achieved by non-rubbing ion beam irradiation. The pretilt angle can be tuned by the composition of the thin film.
Having described preferred embodiments of tilted vertical alignment of liquid crystals employing inorganic thin film composition and ion beam treatment (which are intended to be illustrative and not limiting), it is noted that modifications and variations can be made by persons skilled in the art in light of the above teachings. It is therefore to be understood that changes may be made in the particular embodiments of the invention disclosed which are within the scope and spirit of the invention as outlined by the appended claims. Having thus described the invention with the details and particularity required by the patent laws, what is claimed and desired protected by Letters Patent is set forth in the appended claims.
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A liquid crystal display device includes an alignment layer with constituent materials. The constituent materials have a stoichiometric relationship configured to provide a given pretilt angle. Liquid crystal material is provided in contact with the alignment layer. A method for forming an alignment layer for liquid crystal displays includes forming the alignment layer on a substrate by introducing an amount of material to adjust a stoichiometric ratio of constituent materials wherein the amount is determined to provide a given pretilt angle to the alignment layer. Ions are directed at the alignment layer to provide uniformity of the pretilt angle.
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RELATED APPLICATIONS
[0001] The patents entitled ELECTROSTATIC FLUID ACCELERATOR, Ser. No. 09/419,720, filed Oct. 14, 1999; METHOD OF AND APPARATUS FOR ELECTROSTATIC FLUID ACCELERATION CONTROL OF A FLUID FLOW, Ser. No. ______, filed Jun. 21, 2002, (attorney docket no. 432.004); and AN ELECTROSTATIC FLUID ACCELERATOR FOR AND A METHOD OF CONTROLLING FLUID FLOW, Ser. No. ______ filed ______ (attorney docket no. 432.005), all of which are incorporated herein in their entireties by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to a method and device for the corona discharge generation and, especially, to spark and arc prevention and management.
[0004] 2. Description of the Prior Art
[0005] A number of patents (see, e.g., U.S. Pat. No. 4,210,847 of Shannon et al. and U.S. Pat. No. 4,231,766 of Spurgin) have recognized the fact that corona discharge may be used for generating ions and charging particles. Such techniques are widely used in electrostatic precipitators. Therein a corona discharge is generated by application of a high voltage power source to pairs of electrodes. The electrodes are configured and arranged to generate a non-uniform electric field proxite one of the electrodes (called a corona discharge electrode) so as to generate a corona and a resultant corona current toward a nearby complementary electrode (called a collector or attractor electrode). The requisite corona discharge electrode geometry typically requires a sharp point or edge directed toward the direction of corona current flow, i.e., facing the collector or attractor electrode.
[0006] Thus at least the corona discharge electrode should be small or include sharp points or edges to generate the required electric field gradient in the vicinity of the electrode. The corona discharge takes place in the comparatively narrow voltage range between a lower corona onset voltage and a higher breakdown (or spark) voltage. Below the corona onset voltage, no ions are emitted from the corona discharge electrodes and, therefore, no air acceleration is generated. If, on the other hand, the applied voltage approaches a dielectric breakdown or spark level, sparks and electric arcs may result that interrupt the corona discharge process and create unpleasant electrical arcing sounds. Thus, it is generally advantageous to maintain high voltage between these values and, more especially, near but slightly below the spark level where fluid acceleration is most efficient.
[0007] There are a number of patents that address the problem of sparking in electrostatic devices. For instance, U.S. Pat. No. 4,061,961 of Baker describes a circuit for controlling the duty cycle of a two-stage electrostatic precipitator power supply. The circuit includes a switching device connected in series with the primary winding of the power supply transformer and a circuit operable for controlling the switching device. A capacitive network, adapted to monitor the current in the primary winding of the power supply transformer, is provided for operating the control circuit. Under normal operating conditions, i.e., when the current in the primary winding of the power supply transformer is within nominal limits, the capacitive network operates the control circuit to allow current to flow through the power supply transformer primary winding. However, upon sensing an increased primary current level associated with a high voltage transient generated by arcing between components of the precipitator and reflected from the secondary winding of the power supply transformer to the primary winding thereof, the capacitive network operates the control circuit. In response, the control circuit causes the switching device to inhibit current flow through the primary winding of the transformer until the arcing condition associated with the high voltage transient is extinguished or otherwise suppressed. Following some time interval after termination of the high voltage transient, the switching device automatically re-establishes power supply to the primary winding thereby resuming normal operation of the electrostatic precipitator power supply.
[0008] U.S. Pat. No. 4,156,885 of Baker et al., describes an automatic current overload protection circuit for electrostatic precipitator power supplies operable after a sustained overload is detected.
[0009] U.S. Pat. No. 4,335,414 of Weber describes an automatic electronic reset current cut-off for an electrostatic precipitator air cleaner power supply. A protection circuit protects power supplies utilizing a ferroresonant transformer having a primary power winding, a secondary winding providing relatively high voltage and a tertiary winding providing a relatively low voltage. The protection circuit operates to inhibit power supply operation in the event of an overload in an ionizer or collector cell by sensing a voltage derived from the high voltage and comparing the sense voltage with a fixed reference. When the sense voltage falls below a predetermined value, current flow through the transformer primary is inhibited for a predetermined time period. Current flow is automatically reinstated and the circuit will cyclically cause the power supply to shut down until the fault has cleared. The reference voltage is derived from the tertiary winding voltage resulting in increased sensitivity of the circuit to short duration overload conditions.
[0010] As recognized by the prior art, any high voltage application assumes a risk of electrical discharge. For some applications a discharge is desirable. For many other high voltage applications a spark is an undesirable event that should be avoided or prevented. This is especially true for the applications where high voltage is maintained at close to a spark level i.e., dielectric breakdown voltage. Electrostatic precipitators, for instance, operate with the highest voltage level possible so that sparks are inevitably generated. Electrostatic precipitators typically maintain a spark-rate of 50-100 sparks per minute. When a spark occurs, the power supply output usually drops to zero volts and only resumes operation after lapse of a predetermined period of time called the “deionization time” during which the air discharges and a pre-spark resistance is reestablished. Each spark event decreases the overall efficiency of the high voltage device and is one of the leading reasons for electrode deterioration and aging. Spark generation also produces an unpleasant sound that is not acceptable in many environments and associated applications, like home-use electrostatic air accelerators, filters and appliances.
[0011] Accordingly, a need exists for a system for and method of handling and managing, and reducing or preventing spark generation in high voltage devices such as for corona discharge devices.
SUMMARY OF THE INVENTION
[0012] It has been found that spark onset voltage levels do not have a constant value even for the same set of the electrodes. A spark is a sudden event that cannot be predicted with great certainty. Electrical spark generation is often an unpredictable event that may be caused my multiple reasons, many if not most of them being transitory conditions. Spark onset tends to vary with fluid (i.e., dielectric) conditions like humidity, temperature, contamination and others. For the same set of electrodes, a spark voltage may have an onset margin variation as large as 10% or greater.
[0013] High voltage applications and apparatus known to the art typically deal with sparks only after spark creation. If all sparks are to be avoided, an operational voltage must be maintained at a comparatively low level. The necessarily reduced voltage level decreases air flow rate and device performance in associated devices such as electrostatic fluid accelerators and precipitators.
[0014] As noted, prior techniques and devices only deal with a spark event after spark onset; there has been no known technical solution to prevent sparks from occurring. Providing a dynamic mechanism to avoid sparking (rather than merely extinguish an existing arc) while maintaining voltage levels within a range likely to produce sparks would result in more efficient device operation while avoiding electrical arcing sound accompanying sparking.
[0015] The present invention generates high voltage for devices such as, but not limited to, corona discharge systems. The invention provides the capability to detect spark onset some time prior to complete dielectric breakdown and spark discharge. Employing an “inertialess” high voltage power supply, an embodiment of the invention makes it possible to manage electrical discharge associated with sparks. Thus, it becomes practical to employ a high voltage level that is substantially closer to a spark onset level while preventing spark creation.
[0016] Embodiments of the invention are also directed to spark management such as where absolute spark suppression is not required or may not even be desirable.
[0017] According to one aspect of the invention, a spark management device includes a high voltage power source and a detector configured to monitor a parameter of an electric current provided to a load device. In response to the parameter, a pre-spark condition is identified. A switching circuit is responsive to identification of the pre-spark condition for controlling the electric current provided to the load device.
[0018] According to a feature of the invention, the high voltage power source may include a high voltage power supply configured to transform a primary power source to a high voltage electric power feed for supplying the electric current.
[0019] According to another feature of the invention, the high voltage power source may include a step-up power transformer and a high voltage power supply including an alternating current (a.c.) pulse generator having an output connected to a primary winding of the step-up power transformer. A rectifier circuit is connected to a secondary winding of the step-up power transformer for providing the electric current at a high voltage level.
[0020] According to another feature of the invention, the high voltage power source may include a high voltage power supply having a low inertia output circuit.
[0021] According to another feature of the invention, the high voltage power supply may include a control circuit operable to monitor a current of the electric current. In response to detecting a pre-spark condition, a voltage of the electric current is decreased to a level not conducive to spark generation (e.g., below a spark level).
[0022] According to another feature of the invention, a load circuit may be connected to the high voltage power source for selectively receiving a substantial portion of the electric current in response to the identification of the pre-spark condition. The load circuit may be, for example, an electrical device for dissipating electrical energy (e.g., a resistor converting electrical energy into heat energy) or an electrical device for storing electrical energy (e.g., a capacitor or an inductor). The load device may further include some operational device, such as a different stage of a corona discharge device including a plurality of electrodes configured to receive the electric current for creating a corona discharge. The corona discharge device may be in the form of an electrostatic air acceleration device, electrostatic air cleaner and/or an electrostatic precipitator.
[0023] According to another feature of the invention, the switching circuit may include circuitry for selectively powering an auxiliary device in addition to the primary load device supplied by the power supply. Thus, in the event an incipient spark is detected, at least a portion of the power regularly supplied to the primary device may be instead diverted to the auxiliary device in response to the identification of the pre-spark condition, thereby lowering the voltage at the primary device and avoiding sparking. One or both of the primary load and devices may be electrostatic air handling devices configured to accelerate a fluid under influence of an electrostatic force created by a corona discharge structure.
[0024] According to another feature of the invention, the detector may be sensitive to a phenomenon including a change in current level or waveform, change in voltage level or waveform, or magnetic, electrical, or optical events associated with a pre-spark condition.
[0025] According to another aspect of the invention, a method of spark management may include supplying a high voltage current to a device and monitoring the high voltage current to detect a pre-spark condition of the device. The high voltage current is controlled in response to the pre-spark condition to control an occurrence of a spark event associated with the pre-spark condition.
[0026] According to another feature of the invention, the step of monitoring may include sensing a current spike in the high voltage current.
[0027] According to a feature of the invention, the step of supplying a high voltage current may include transforming a source of electrical power from a primary voltage level to a secondary voltage level higher than the primary voltage level. The electrical power at the secondary voltage level may then be rectified to supply the high voltage current to the device. This may include reducing the output voltage or the voltage at the device, e.g., the voltage level on the corona discharge electrodes of a corona discharge air accelerator. The voltage may be reduced to a level this is not conducive to spark generation. Control may also be accomplished by routing at least a portion of the high voltage current to an auxiliary loading device. Routing may be performed by switching a resistor into an output circuit of a high voltage power supply supplying the high voltage current.
[0028] According to another feature of the invention, additional steps may include introducing a fluid to a corona discharge electrode, electrifying the corona discharge electrode with the high voltage current, generating a corona discharge into the fluid, and accelerating the fluid under influence of the corona discharge.
[0029] According to another aspect of the invention, an electrostatic fluid accelerator may include an array of corona discharge and collector electrodes and a high voltage power source electrically connected to the array for supplying a high voltage current to the corona discharge electrodes. A detector may be configured to monitor a current level of the high voltage current and, in response, identify a pre-spark condition. A switching circuit may respond to identification of the pre-spark condition to control the high voltage current.
[0030] According to a feature of the invention, the switching circuit may be configured to inhibit supply of the high voltage current to the corona discharge electrodes by the high voltage power supply in response to the pre-spark condition.
[0031] According to another feature of the invention, the switching circuit may include a dump resistor configured to receive at least a portion of the high voltage current in response to the identification of the pre-spark condition.
[0032] It has been found that a corona discharge spark is preceded by certain observable electrical events that telegraph the imminent occurrence of a spark event and may be monitored to predict when a dielectric breakdown is about to occur. The indicator of a spark may be an electrical current increase, or change or variation in a magnetic field in the vicinity of the corona discharge (e.g., an increase) or other monitorable conditions within the circuit or in the environment of the electrodes. It has been experimentally determined, in particular, that a spark event is typically preceded by a corona current increase. This increase in current takes place a short time (i.e., 0.1-1.0 milliseconds) before the spark event. The increase in current may be in the form of a short duration current spike appearing some 0.1-1.0 milliseconds (msec) before the associated electrical discharge. This increase is substantially independent of the voltage change. To prevent the spark event, it is necessary to detect the incipient current spike event and sharply decrease the voltage level applied to and/or at the corona discharge electrode below the spark level.
[0033] Two conditions should be satisfied to enable such spark management. First, the high voltage power supply should be capable of rapidly decreasing the output voltage before the spark event occurs, i.e., within the time period from event detection until spark event start. Second, the corona discharge device should be able to discharge and stored electrical energy, i.e., discharge prior to a spark.
[0034] The time between the corona current increase and the spark is on the order of 0.1-1.0 msec. Therefore, the electrical energy that is stored in the corona discharge device (including the power supply and corona discharge electrode array being powered) should be able to dissipate the stored energy in a shorter time period of, i.e., in a sub-millisecond range. Moreover, the high voltage power supply should have a “low inertia” property (i.e., be capable of rapidly changing a voltage level at its output) and circuitry to interrupt voltage generation, preferably in the sub-millisecond or microsecond range. Such a rapid voltage decrease is practical using a high frequency switching high voltage power supply operating in the range of 100 kHz to 1 MHz that has low stored energy and circuitry to decrease or shut down output voltage rapidly. In order to provide such capability, the power supply should operate at a high switching frequency with a “shut down” period (i.e., time required to discontinue a high power output) smaller than the time between corona current spike detection and any resultant spark event. Since state-of-the-art power supplies may work at the switching frequencies up to 1 MHz, specially an appropriately designed (e.g., inertialess) power supply may be capable of interrupting power generation with the requisite sub-millisecond range. That is, it is possible to shut down the power supply and significantly decrease output voltage to a safe level, i.e., to a level well below the onset of an electrical discharge in the form of a spark.
[0035] There are different techniques to detect the electrical event preceding an electrical spark. An electrical current sensor may be used to measure peak, or average, or RMS or any other output current magnitude or value as well as the current rate of change, i.e., dI/dt. Alternatively, a voltage sensor may be used to detect a voltage level of the voltage supply or a voltage level of an AC component. Another parameter that may be monitored to identify an imminent spark event is an output voltage drop or, a first derivative with respect to time of the voltage, (i.e., dV/dt) of an AC component of the output voltage. It is further possible to detect an electrical or magnetic field strength or other changes in the corona discharge that precede an electrical discharge in the form of a spark. A common feature of these techniques is that the corona current spike increase is not accompanied by output voltage increase or by any substantial power surge.
[0036] Different techniques may be employed to rapidly decrease the output voltage generated by the power supply. A preferred method is to shut down power transistors, or SCRs, or any other switching components of the power supply that create the pulsed high frequency a.c. power provided to the primary of a step-up transformer to interrupt the power generation process. In this case the switching components are rendered non-operational and no power is generated or supplied to the load. A disadvantage of this approach is that residual energy accumulated in the power supply components, particularly in output filtering stages such as capacitors and inductors (including stray capacitances and leakage inductances) must be released to somewhere, i.e., discharged to an appropriate energy sink, typically “ground.” Absent some rapid discharge mechanism, it is likely that the residual energy stored by the power supply would be released into the load, thus slowing-down the rate at which the output voltage decreases (i.e., “falls”). Alternatively, a preferred configuration and method electrically “shorts” the primary winding (i.e., interconnects the terminals of the winding) of the magnetic component(s) (transformer and/or multi-winding inductor) to dissipate any stored energy by collapsing the magnetic field and thereby ensure that no energy is transmitted to the load. Another, more radical approach, shorts the output of the power supply to a comparatively low value resistance. This resistance should be, however, much higher than the spark resistance and at the same time should be less than an operational resistance of the corona discharge device being powered as it would appear at the moment immediately preceding a spark event. For example, if a high voltage corona device (e.g., an electrostatic fluid accelerator) consumes 1 mA of current immediately prior to spark detection and an output current from the power supply is limited to 1 A by a current limiting device (e.g., series current limiting resistor) during a spark event (or other short-circuit condition), a “dumping” resistance applied across the load (i.e., between the corona discharge and attractor electrodes of a corona discharge device) should develop more than 1 mA (i.e., provide a lower resistance and thereby conduct more current than a normal operating load current) but less than 1 A (i.e., less than the current limited maximum shorted current). This additional dumping resistor may be connected to the power supply output by a high voltage reed-type relay or other high voltage high speed relay or switching component (e.g., SCR, transistor, etc.). The common and paramount feature of the inertialess high voltage power supply is that it can interrupt power generation in less time than the time from the electrical event preceding and indicative of an incipient spark event and the moment in time when the spark actually would have occurred absent some intervention, i.e., typically in a sub-millisecond or microsecond range.
[0037] Another important feature of such an inertialess power supply is that any residual energy that is accumulated and stored in the power supply components should not substantially slow down or otherwise impede discharge processes in the load, e.g., corona discharge device. If, for example, the corona discharge device discharges its own electrical energy in 50 microseconds and the minimum expected time to a spark event is 100 microseconds, then the power supply should not add more than 50 microseconds to the discharge time, so the actual discharge time would not exceed 100 microseconds. Therefore, the high voltage power supply should not use any energy storing components like capacitors or inductors that may discharge their energy into the corona discharge device after active components, such as power transistors, are switched off. To provide this capability and functionality, any high voltage transformer should have a relatively small leakage inductance and either small or no output filter capacitive. It has been found that conventional high voltage power supply topologies including voltage multipliers and fly-back inductors are not generally suitable for such spark management or prevention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0038] FIG. 1 is a schematic circuit diagram of a high voltage power supply (HVPS) with a low inertia output circuit controllable to rapidly decrease a voltage output level to a level some margin below a dielectric breakdown initiation level;
[0039] FIG. 2 is a schematic circuit diagram of another high voltage power supply configured to prevent a spark event in high voltage device such as a corona discharge apparatus;
[0040] FIG. 3 is a schematic circuit diagram of another high voltage power supply configured to prevent a spark event occurrence in a high voltage device;
[0041] FIG. 4 is a schematic circuit diagram of a high voltage power supply configured to prevent a spark event occurrence in a high voltage device;
[0042] FIG. 5 is an oscilloscope trace of an output corona current and output voltage at a corona discharge electrode of an electrostatic fluid accelerator receiving power from a HVPS configured to anticipate and avoid spark events; and
[0043] FIG. 6 is a diagram of a HVPS connected to supply HV power to an electrostatic device.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0044] FIG. 1 is a schematic circuit diagram of high voltage power supply (HVPS) 100 configured to prevent a spark event occurrence in a high voltage device such as electrostatic fluid accelerator. HVPS 100 includes a high voltage set-up transformer 106 with primary winding 107 and the secondary winding 108 . Primary winding 107 is connected to an a.c. voltage provided by DC voltage source 101 through half-bridge inverter (power transistors 104 , 113 and capacitors 105 , 114 ). Gate signal controller 111 produces control pulses at the gates of the transistors 104 , 113 , the frequency of which is determined by the values of resistor 110 and capacitor 116 forming an RC timing circuit. Secondary winding 108 is connected to voltage rectifier 109 including four high voltage (HV), high frequency diodes configured as a full-wave bridge rectifier circuit. HVPS 100 generates a high voltage between terminal 120 and ground that are connected to a HV device or electrodes (e.g., corona discharge device). An AC component of the voltage applied to the HV device, e.g., across an array of corona discharge electrodes, is sensed by high voltage capacitor 119 and the sensed voltage is limited by zener diode 122 . When the output voltage exhibits a characteristic voltage fluctuation preceding a spark, the characteristic AC component of the fluctuation leads to a comparatively large signal level across resistor 121 , turning on transistor 115 . Transistor 115 grounds pin 3 of the signal controller 111 and interrupts a voltage across the gates of power transistors 104 and 113 . With transistors 104 and 113 rendered nonconductive, an almost instant voltage interruption is affected across the primary winding 107 and, therefore, transmitted to the tightly coupled secondary winding 108 . Since a similar rapid voltage drop results at the corona discharge device below a spark onset level, any imminent arcing or dielectrical breakdown is avoided.
[0045] The spark prevention technique includes two steps or stages. First, energy stored in the stray capacitance of the corona discharge device is discharged through the corona current down to the corona onset voltage. This voltage is always well below spark onset voltage. If this discharge happens in time period that is shorter than about 0.1 msec (i.e., less than 100 mksec), the voltage drop will efficiently prevent a spark event from occurring. It has been experimentally determined that voltage drops from the higher spark onset voltage level to the corona onset level may preferably be accomplished in about 50 mksec.
[0046] After the power supply voltage reaches the corona onset level and cessation of the corona current, the discharge process is much slower and voltage drops to zero over a period of several milliseconds. Power supply 100 resumes voltage generation after same predetermined time period defined by resistor 121 and the self-capacitance of the gate-source of transistor 115 . The predetermined time, usually on the order of several milliseconds, has been found to be sufficient for the deionization process and normal operation restoration. In response to re-application of primary power to transformer 106 , voltage provided to the corona discharge device rises from approximately the corona onset level to the normal operating level in a matter of several microseconds. With such an arrangement no spark events occur even when output voltage exceeds a value that otherwise causes frequent sparking across the same corona discharge arrangement and configuration. Power supply 100 may be built using available electronic components; no special components are required.
[0047] FIG. 2 is a schematic circuit diagram of an alternative power supply 200 with reed contact 222 and an additional load 223 . Power supply 200 includes high voltage two winding inductor 209 with primary winding 210 and secondary winding 211 . Primary winding 210 is connected to ground through power transistor 208 and to a d.c. power source provided at terminal 201 . PWM controller 205 (e.g., a UC3843 current mode PWM controller) produces control pulses at the gate of the transistor 208 , an operating frequency of which is determined by an RC circuit including resistor 202 and capacitor 204 . Typical frequencies may be 100 kHz or higher. Secondary winding 211 is connected to a voltage doubler circuit including HV capacitors 215 and 218 , and high frequency HV diodes 216 and 217 . Power supply 200 generates a HV d.c. power of between 10 and 25 kV and typically 18 kV between output terminals 219 and 220 that are connected to a HV device or electrodes (i.e., a load). Control transistor 203 turns ON when current through shunt resistor 212 exceeds a preset level and allows a current to flow through control coil 221 of a reed type relay including reed contacts 222 . When current flows through coil 221 , the reed contact 222 close, shunting the HV output to HV dumping resistor 223 , loading the output and decreasing a level of the output voltage for some time period determined by resistor 207 and capacitor 206 . Using this spark management circuitry in combination with various EFA components and/or device results in a virtual elimination of all sparks during normal operation. Reed relay 203 / 222 may be a ZP-3 of Ge-Ding Information Inc., Taiwan.
[0048] FIG. 3 is a schematic circuit diagram of another HVPS arrangement similar to that shown in FIG. 2 . However, in this case HVPS 300 includes reed contact 322 and an additional load 323 connected directly to the output terminals of the HVPS. HVPS 300 includes high voltage transformer 309 with primary winding 310 and secondary winding 311 . Primary winding 310 is connected to ground through power transistor 308 and to a DC source connected to power input terminal 301 . PWM controller 305 (e.g., a UC3843) produces control pulses at the gate of the transistor 308 . An operating frequency of these control pulses is determined by resistor 302 and the capacitor 304 . Secondary winding 311 is connected to a voltage doubler circuit that includes HV capacitors 315 and 318 and high frequency HV diodes 316 and 317 . HVPS 300 generates a high voltage output of approximately 18 kV at output terminals 319 and 320 that are connected to the HV device or electrodes (the load). Spark control transistor 303 turns ON when current through the shunt resistor 312 exceeds some predetermined preset level and allows current to flow through control coil 321 . When current flows through coil 321 , reed contact 322 closes to shunt the HV output of the HVPS to HV dumping resistor 323 , thereby reducing a level of the output voltage for a time period determined by resistor 307 and capacitor 306 . Use of this incipient spark detection and mitigation arrangement results in virtually no spark production for extended periods of operation.
[0049] FIG. 4 shows a power supply configuration similar to that depicted in FIG. 2 , HVPS 400 further including relay including normally open contacts 422 and coil 421 , and power dumping load 423 . HVPS 400 includes power transformer 409 with primary winding 410 and the secondary winding 411 . Primary winding 410 is connected to ground through power transistor 408 and to a d.c. power source at terminal 401 . PWM controller 405 (e.g., a UC3843) produces a train of control pulses at the gate of the transistor 408 . An operating frequency of these pulses is set by the resistor 402 and capacitor 404 . Secondary winding 411 is connected to supply a high voltage (e.g., 9 kV) to a voltage doubler circuit that includes HV capacitors 415 and 418 , and high frequency HV diodes 416 and 417 . Power supply 400 generates a high voltage output at terminals 419 and 420 that are connected to the HV device or corona electrodes (load). Control transistor 403 turns ON when current through shunt resistor 412 exceeds some preset level predetermined to be characteristic of an incipient spark event, allowing current to flow through coil 421 . When current flows through the coil 421 , relay contact 422 closes, shortening primary winding 410 through dumping resistor 423 . The additional load provided by dumping resistor 423 rapidly decreases the output voltage level over some period of time determined by resistor 407 and capacitor 406 .
[0050] FIG. 5 is an oscilloscope display including two traces of a power supply output in terms of a corona current 501 and output voltage 502 . As it can be seen corona current has a characteristic narrow spike 503 indicative of an incipient spark event within a time period of about 0.1 to 1.0 msec, herein shown at about 2.2 msec after the current spike. Detection of current spike 503 in corona discharge or similar HV apparatus triggers a control circuit, turns the HVPS OFF and preferably dumps any stored energy necessary to lower an electrode potential to or below a dielectric breakdown safety level. Thus, in addition to interrupting primary power to the HVPS by, for example, inhibiting an operation of a high frequency pulse generator (e.g., PWM controller 205 ), other steps may be taken to rapidly lower voltage applied to the HV apparatus to a level below a spark initiation or dielectric breakdown potential. These steps and supportive circuitry may include “dumping” any stored charge into an appropriate “sink”, such as a resistor, capacitor, inductor, or some combination thereof. The sink may be located within the physical confines of the HVPS and/or at the device being powered, i.e., the HV apparatus or load. If located at the load, the sink may be able to more quickly receive a charge stored within the load, while a sink located at the HVPS may be directed to lower a voltage level of the HVPS output. Note that the sink may dissipate power to lower the voltage level supplied to or at the load using, for example, a HV resistor. Alternatively, the energy may be stored and reapplied after the spark event has been addressed to rapidly bring the apparatus back up to an optimal operating. Further, it is not necessary to lower the voltage to a zero potential level in all cases, but it may be satisfactory to reduce the voltage level to some value known or predicted to avoid a spark event. According to one embodiment, the HVPS includes processing and memory capabilities to associate characteristics of particular pre-spark indicators (e.g., current spike intensity, waveform, duration, etc.) with appropriate responses to avoid or minimize, to some preset level, the chance of a spark event. For example, the HVPS may be responsive to an absolute amplitude or an area under a current spike (i.e.,
( i . e . , ∫ t1 t2 ( i t - i average ) ⅆ t )
for selectively inserting a number of loads previously determined to provide a desired amount of spark event control, e.g., avoid a spark event, delay or reduce an intensity of a spark event, provide a desired number or rate of spark events, etc.
[0051] Referring again to FIG. 5 , if an output of the HVPS is totally interrupted, with no current flowing to the corona discharge apparatus, the voltage across the corona discharge device rapidly drops as shown in the FIG. 5 and described above. After some short period, a current spike 504 may be observed that indicates the moment when actual spark event would have occurred had no action been taken to reduce the voltage level applied to the HV device. Fortunately, since the output voltage is well below the spark level, no spark or arc is produced. Instead, only a moderate current spike is seen which is sufficiently small as to not cause any disturbances or undesirable electrical arcing sound. After a certain period on the order of 2-10 msec after detection of current spike 504 or 1-9 msec after current spike 503 , the HVPS turns ON and resumes normal operation.
[0052] FIG. 6 is a diagram of HVPS 601 according to an embodiment of the invention connected to supply HV power to an electrostatic device 602 , e.g., a corona discharge fluid accelerator. Electrostatic device 602 may include a plurality of corona discharge electrodes 603 connected to HVPS 601 by common connection 604 . Attractor or collector electrodes 605 are connected to the complementary HV output of HVPS 601 by connection 606 . Upon application of a HV potential to corona discharge electrodes 603 , respective corona discharge electron clouds are formed in the vicinity of the electrodes, charging the intervening fluid (e.g., air) molecules acting as a dielectric between corona discharge electrodes 603 and the oppositely charged attractor or collector electrodes 605 . The ionized fluid molecules are accelerated toward the opposite charge of collector/attractor electrodes 605 , resulting in a desired fluid movement. However, due to various environmental and other disturbances, the dielectric properties of the fluid may vary. This variation may be sufficient such that the dielectric breakdown voltage may be lowered to a point where electrical arcing may occur between sets of corona discharge and attractor electrodes 603 , 605 . For example, dust, moisture, and/or fluid density changes may lower the dielectric breakdown level to a point below the operating voltage being applied to the device. By monitoring the electrical characteristics of the power signal for a pre-spark signature event (e.g., a current spike or pulse, etc.), appropriate steps are implemented to manage the event, such as lowering the operating voltage in those situations wherein it is desirable to avoid a spark.
[0053] While the embodiment described above is directed to eliminating or reducing a number and/or intensity of spark events, other embodiments may provide other spark management facilities capabilities and functionalities. For example, a method according to an embodiment of the invention may manage spark events by rapidly changing voltage levels (for example, by changing duty cycle of PWM controller) to make spark discharge more uniform, provide a desired spark intensity and/or rate, or for any other purpose. Thus, additional applications and implementations of embodiments of the current invention include pre-park detection and rapid voltage change to a particular level so as to achieve a desired result.
[0054] According to embodiments of the invention, three features provide for the efficient management of spark events. First, the power supply should be inertialess. That means that the power supply should be capable of rapidly varying an output voltage in less time than a time period between a pre-spark indicator and occurrence of a spark event. That time is usually in a matter of one millisecond or less. Secondly, an efficient and rapid method of pre-spark detection should be incorporated into power supply shut-down circuitry. Third, the load device, e.g., corona discharge device, should have low self-capacitance capable of being discharged in a time period that is shorter than time period between a pre-spark signature and actual spark events.
[0055] It should be noted and understood that all publications, patents and patent applications mentioned in this specification are indicative of the level of skill in the art to which the invention pertains. All publications, patents and patent applications are herein incorporated by reference to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated by reference in its entirety.
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A spark management device includes a high voltage power source and a detector configured to monitor a parameter of an electric current provided to a load device. In response to the parameter, a pre-spark condition is identified. A switching circuit is responsive to identification of the pre-spark condition for controlling the electric current provided to the load device so as to manage sparking including, but not limited to, reducing, eliminating, regulating, timing, and/or controlling any intensity of arcs generated.
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BACKGROUND OF THE INVENTION
[0001] 1. The Technical Field
[0002] The present invention is directed to twist drills for use, primarily by non-professionals, for multiple material applications (wood, drywall, plastic, rubber, non-ferrous metals and thin ferrous plate or sheets).
[0003] 2. The Prior Art
[0004] For each type of material (wood, drywall, plastic, rubber, non-ferrous metals, ferrous metals, ceramics, glass), there exists a specific twist drill design which can be optimized for use with that particular material. However, such highly specialized twist drills can be expensive in and of themselves, and having a complete suite of twist drills for each material can present an expense that only a professional machine shop can afford. For individual persons or small businesses, such highly specialized twist drills can be an unjustifiable expense.
[0005] In addition, twist drills that are made for “home” or non-professional use, that is, for drilling in typical materials as wood, drywall, plastic, rubber, non-ferrous metals (e.g., aluminum, copper), and thin ferrous plate (sheet steel), are typically configured to produce relatively long spiral or coiled chips, which can be bothersome as they tend to collect around the drilling site, and can interfere with the actual operation of the twist drill.
[0006] Therefore, it would be desirable to provide an improved twist drill design that is capable of performing well when used with a wide variety of materials.
[0007] It would be desirable to provide a twist drill design, particularly for multiple materials, that is capable of providing smooth, clean drilling.
[0008] It would also be desirable to provide a twist drill design that has improved material removal characteristics.
[0009] It would also be desirable to provide a twist drill design particularly suited for non-professional or home use, which is configured to produce small chips that are readily removed from the interface between the work material and the twist drill, for improved performance.
[0010] These and other desirable characteristics of the present invention will become apparent in view of the present specification, including claims, and drawings.
SUMMARY OF THE INVENTION
[0011] The present invention comprises in part a twist drill for forming holes in or through a workpiece, having a longitudinal axis around which the twist drill is rotated and in the direction of which the twist drill is advanced into the workpiece, and two transverse axes disposed perpendicular to each other and to the longitudinal axis.
[0012] The twist drill comprises a shank, for enabling the twist drill to be mounted to a driving device. A body emanates from, and is coaxial with the shank. The body has a radius. At least one flute extends helically along the body. At least one land is disposed adjacent to the at least one flute. A point structure is formed on an end of the body distal to the shank. The point structure is generally in the form of a brad point having an extreme tip through which the longitudinal axis of the drill passes. The point structure further has two spur structures on opposite sides thereof. A cutting lip is disposed on a leading edge of each of the spur structures. The drill further includes planar axial relief surfaces on trailing surfaces of the lands which intersect the cutting lips.
[0013] The point preferably comprises a first radially outwardly disposed portion of the at least one land angling inwardly and axially toward the shank, to a position between a peripheral portion of the body, and the longitudinal axis and a second, radially inwardly disposed portion of the at least one land, angling inwardly and axially away from the shank and toward the central point structure.
[0014] The first radially outwardly disposed portion of the at least one land is preferably defined at least in part by a leading edge angle β 1 and a trailing edge angle β 2 , wherein β 1 =15°±10° and β 2 =12°±70°.
[0015] The second, radially inwardly disposed portion of the at least one land is preferably defined at least in part by a point angle α 1 , and an angle α 2 which represents an axial separation between the central point structure and radially outer portions of the at least one land, wherein α 1 =80°-100°, inclusive; and α 2 =140°-170°, inclusive.
[0016] The twist drill further comprises the at least one flute terminating in a cutting lip disposed proximate the point. The at least one flute has a sectional configuration, in a plane perpendicular to the longitudinal axis, incorporating a leading edge and a trailing edge. A straight surface extends inwardly from the leading edge, at least to a position coplanar with a plane passing perpendicularly through the straight surface to the longitudinal axis. A first concave curved portion extends from an inward end of the straight surface and may have at least one radius of curvature less than one-half the radius of the twist drill body. A second concave curved portion extends inwardly from the trailing toward an outer edge region of the first concave curved portion. A ridge is formed by the intersection of the outer edge region of the first concave curved portion and an inner edge region of the second concave curved portion.
[0017] The ridge may be in the form of a pointed spike. Alternatively, the ridge may be in the form of a rounded bump.
[0018] The present invention is also directed to a twist drill for forming holes in or through a workpiece, having a longitudinal axis around which the twist drill is rotated and in the direction of which the twist drill is advanced into the workpiece, and two transverse axes disposed perpendicular to each other and to the longitudinal axis. The twist drill comprises a shank, for enabling the twist drill to be mounted to a driving device. A body emanates from, and is coaxial with the shank, the body having a radius. At least one flute extends helically along the body. At least one land is disposed adjacent to the at least one flute. A point structure is formed on an end of the body distal to the shank. The point structure is generally in the form of a brad point having an extreme tip through which the longitudinal axis of the drill passes. The point structure further has two spur structures on opposite sides thereof. A cutting lip is disposed on a leading edge of each of the spur structures.
[0019] The drill further includes planar axial relief surfaces on trailing surfaces of the lands which intersect the cutting lips.
[0020] The at least one flute includes a leading edge. A flat surface extends parallel to one of the transverse axes inwardly a distance at least equal to a radius of the drill from the leading edge to a position proximate the second of the transverse axes. At least a first convex curved portion emanates from an inner end of the flat surface, for prompting rapid breakup of chips formed by the point and guided into the at least one flute by rotation of the drill. The at least first convex curved portion terminates in a ridge disposed between the longitudinal axis of the drill and a trailing edge of the at least one flute.
[0021] The twist drill further comprises a second convex curved portion, disposed in the at least one flute, between the ridge and the trailing edge of the at least one flute. The ridge may be in the form of a sharp spike extending along the at least one flute. Alternatively, the ridge may be in the form of a rounded bump extending along the at least one flute.
[0022] The invention also comprises, in part, a method for making a twist drill comprising the steps of:
forming a cylindrical blank, having a longitudinal axis and two transverse axes extending perpendicular to one another and to the longitudinal axis; forming at least one flute in the cylindrical blank, the at least one flute including a ridge disposed therein for prompting breakage of chips formed during use of the drill, the at least one flute extending from a point region of the cylindrical blank to a shank region of the cylindrical blank; forming at least one land in the cylindrical blank, the at least one land extending along the blank adjacent to the at least one land; grinding the point region of the cylindrical blank to a contact angle; grinding a brad and spur configuration onto the point region; forming an axial relief surface on the at least one land, by aligning the blank along a first axis of an three coordinate axis system, inclining the blank a selected angle away from the first axis while maintaining the blank within a plane defined by the first axis and another axis of the three coordinate system, and then inclining the blank a selected angle away from the plane defined by the first axis and another axis of the three coordinate system; and presenting the blank to a planar grinding surface disposed perpendicular to the first axis of a three coordinate system.
[0030] The step of grinding the point region of the cylindrical blank to a contact angle, preferably comprises grinding the contact angle α 2 to be 140°-170°, inclusive.
[0031] The step of grinding a brad and spur configuration onto the point region preferably comprises grinding the point region such that α 1 =80°-100°, inclusive; β 1 =15°±10° and β 2 =12°±7°.
[0032] The step of forming an axial relief surface on the at least one land preferably comprises the steps of:
aligning the blank along the z axis of an x-y-z coordinate system; inclining the blank, in the y-z plane, a distance of 60°±20° away from the z axis; inclining the blank, away from the y-z plane, a distance of 20°±10°; and presenting the so inclined blank to a planar grinding surface disposed perpendicular to the z axis.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] FIG. 1 is a side elevation of a prior art general purpose twist drill.
[0038] FIG. 2 is a tip end view of the prior art general purpose twist drill of FIG. 1 .
[0039] FIG. 3 is a side elevation of a prior art twist drill configured principally for wood drilling.
[0040] FIG. 4 is a side elevation of the prior art wood twist drill of FIG. 3 , rotated approximately 90°.
[0041] FIG. 5 is a tip end view of the prior art wood twist drill of FIGS. 3 and 4 .
[0042] FIG. 6 is a sectional view which may be applicable to the twist drill of FIGS. 1-2 , as well as of FIGS. 3-5 .
[0043] FIG. 7 is a sectional view of a body portion of a twist drill according to an embodiment of the present invention.
[0044] FIG. 8 is a fragmentary side elevation of the point of a twist drill according to an embodiment of the invention, shown in a preliminary stage of formation.
[0045] FIG. 9 is a fragmentary side elevation of the point of the partially completed twist drill according to the embodiment of FIG. 8 , rotated relative to the view of FIG. 8 .
[0046] FIG. 10 is a top view of the point of the partially completed twist drill of FIGS. 8 and 9 .
[0047] FIG. 11 is a fragmentary side elevation of a completed drill point according to a preferred embodiment of the present invention.
[0048] FIG. 11A is a fragmentary side elevation of the completed drill point according to the preferred embodiment FIG. 11 , shown rotated approximately 90° from the view of FIG. 11 .
[0049] FIG. 12 is a top view of the point of the drill of FIGS. 11 and 11 A.
[0050] FIG. 13 is a fragmentary side elevation of the drill point of FIG. 12 .
[0051] FIG. 14 is a further fragmentary side elevation of the drill point of FIGS. 12 and 13 .
[0052] FIG. 15 is a schematic illustration of the geometry for axial relief for the drill point of FIGS. 12-14 .
[0053] FIG. 16 is a sectional view of a prior art drill.
[0054] FIG. 17 is a sectional view of a prior art drill.
[0055] FIG. 18 is a sectional view of a prior art three-flute drill.
[0056] FIG. 19 is a sectional view of a prior art four-flute drill.
[0057] FIG. 20 illustrates side elevations of different styles of drills that may employ point constructions, as that shown in the embodiment of FIGS. 11-15 .
DETAILED DESCRIPTION OF THE INVENTION
[0058] While this invention is susceptible of embodiment in many different forms, there is shown in the drawings and will be described in detail several specific embodiments, with the understanding that the present disclosure is to be considered an exemplification of the principles of the invention and is not intended to limit the invention to the embodiments illustrated.
[0059] FIGS. 1-2 illustrate a prior art general purpose twist drill 10 , which may be formed from any suitable material, such as M50 steel, although other materials may be used. Twist drill 10 is shown, not only to provide an illustration of a representative general purpose bit, but also to provide visual reference for certain terms to be used herein, with reference to the twist drill construction of the present invention. Twist drill 10 may be used typically on materials such as brass, bronze, as well as hard plastics, drywall, fiberboard and the like, and such bits are often used by non-professional do-it-yourselfers.
[0060] Twist drill 10 (like any twist drill) includes a shank 12 (the end which is gripped by a drill chuck or other mounting structure, a body 14 (the portion of the drill extending from the shank 12 or a neck—not shown—to the outer corners of the cutting lips 16 ), and a point 17 , all of which are centered about the longitudinal axis of the drill, about which the drill rotates, and in the direction of which, the drill is advanced toward and into the workpiece. Only a portion of shank 12 is shown in FIG. 1 , and none in FIG. 2 . Shank 12 is shown as being cylindrical (the typical home user configuration), but may be tapered (when viewed from the side) and/or polygonal (when viewed in section or from the end), as desired. Twist drill 10 has two flutes 18 , separated by two lands 20 . Web 22 (generally indicated by the broken line) is the central portion of the body that joins the lands. The extreme end of the web forms the chisel edge 24 of a two-flute drill.
[0061] While a drill bit such as bit 10 of FIGS. 1-2 is useful for a relatively wide variety of materials, such drills are less effective for softer materials, such as wood, very soft non-ferrous materials (e.g., lead), rubber and leather, because the shape of the point may tend to merely rub against, heat up and burn the surface of the soft material, rather than digging in, and actually cutting and removing material.
[0062] Accordingly, twist drills for soft materials are fabricated having a brad and spur configuration such as that shown in FIGS. 3-5 . The brad is the center part, and the spurs are the forward angling radially outward portions of the lands (often referred to as a “fish-tail”), particularly the leading edge (relative to the direction of rotation) portions of the lands/flutes. Twist drill 40 includes a body 42 and a point 47 . The shank is not shown, but is understood to be present. Point 47 includes two cutting lips 46 . Twist drill 40 has two flutes 48 , separated by two lands 50 . Web 52 (generally indicated by the broken line) is the central portion of the body that joins the lands. The extreme end of the web 50 forms the sharp-pointed pyramidal tip of the brad and spur two-flute drill 40 .
[0063] FIG. 6 is a sectional view, which may be applicable to either twist drill 10 or twist drill 40 . Distance C represents the clearance, that is the material removed from lands 18 , 48 , to reduce the amount of undesired rubbing of the lands against the inside surface of the hole being formed by the drill. The margin M is the cylindrical portion of the land which is not cut away to provide clearance. Note that in a conventional section of a twist drill body, there is an elongated straight portion S which ends in a smoothly and continuously curved, often semicircular or elliptical portion SC. During use of the drill, this typically results in the formation of an elongated coiled chip. If the radius of curvature of portion SC decreases toward the radially outer portion of the section, then there will be a tendency for the chip to be more tightly coiled.
[0064] FIG. 16 is a sectional view of a prior art drill. FIG. 17 is a sectional view of another prior art drill. In the drill of FIG. 16 , while the flutes are somewhat divided by a ridge, in view of the presence of the long, continuously curving surface leading from the opposite outer (leading) edge of the flute to the ridge, this design is provided for making tightly curved chips, and not for producing small, quickly broken chips. The short curved surface on the other side of the ridge is not believed to make significant contact with the chip, due to the lack of breakage of the chips. In view of the similarity of the drill of FIG. 16 to that of FIG. 17 , it is possible that the short curved section of the flute is for removing material from the drill, for weight saving purposes.
[0065] FIG. 18 is a sectional view of a prior art three-flute drill. FIG. 19 is a sectional view of a prior art four-flute drill. These multi-flute drills are not for originating holes, as is well known in the art. Instead, drills having three or more flutes are for enlarging holes that have already been initiated by a one- or two-flute drill, or have been previously cored or punched.
[0066] FIG. 7 is a representative section of a twist drill according to the present invention, which is independent of the architecture of the point. In section 80 , flutes 82 are provided with leading edges 83 , straight portions 84 , trailing edges 85 , and two curved portions 86 , 88 , which are separated by ridge 90 . Straight portions 84 extend from the leading edges of the flutes inwardly, up to and/or past a position coplanar with the axis A of drill section 80 . That is, straight section 84 extends up to or past axis X of FIG. 7 . Curved portions 86 , 88 may be circular, elliptical, or of variable curvature. In FIG. 7 , curved portions 86 in particular are of radially outwardly decreasing curvature (which promotes breakage of the chips into small, short pieces), while curved portions 88 are of radially outwardly increasing curvature (which may promote movement of the chip pieces radially outwardly, and along the length of the body portion of the drill, and out of the hole being drilled). The radius curvature of curved portion 86 may be, in at least one location (or in the case of a semi-circle), half or less of the radius of section 80 . While ridge 90 ideally is in the form of a sharp spike, as shown in solid lines in FIG. 7 , such a configuration requires more intensive manufacturing steps, and increases the cost of each individual drill. Thus, manufacturability and cost considerations mean that in practical commercial versions, ridge 90 will likely be in the form of a broader, blunter spike, or of a rounded or flattened bump, as shown in broken lines in FIG. 10 , or of some combination of rounded and/or curved shapes, such as combined convex, concave and/or straight surfaces. The specific form of the ridge 90 itself is not believed to significantly affect the desired result of causing the breakage of the forming chips into short pieces, rather than permitting the chip to form as an elongated spiral. Instead, it is the believed to be the presence of the long straight portion 84 , which extends a distance up to and preferably slightly beyond the radius of the drill 80 , combined with and followed by the sharp turn created by curved portion 86 , which promotes the chip breakage into small pieces.
[0067] By providing a twist drill with a flute construction in which the leading section of the flute is straight, and leads to a ridge with a tight radius of curvature, so that chips are broken in to small short lengths, the common problem of melting and clumping (at the drill hole opening) of chips caused by the heat generated by the drilling (typical of plastic, rubber, non-ferrous metals) can be reduced or avoided, because the smaller chip pieces can be expelled more readily through the operation of the drill than elongated chip pieces.
[0068] While the flute structure is shown in the environment of a twist drill having a helical flute, the flute structure can also be employed in drills having flutes with less of a spiral nature, such as a spade drill.
[0069] FIGS. 8-10 illustrate the first stage for the point construction for a twist drill according to a preferred embodiment of the present invention. Drill 100 includes a body having lands 102 , and flutes 104 . Flutes 104 will incorporate two curved portions, 86 , 88 (shown in FIG. 10 , not shown in FIGS. 8 and 9 ), as described with respect to the body section of FIG. 7 . To form the drill, first a raw cylindrical metal blank, often referred to as a “black” is provided with the flutes (including ridges 90 ), through a roll forging process, the particular details of which would be readily understood by one of ordinary skill in the art, having the present disclosure before them, and so are omitted herein as being not necessary for a complete understanding of the invention. After the flutes are formed, the drill tip is preliminarily formed through a succession of grinding steps. Drill 100 initially is formed with a chisel point 110 , which is defined by the following values, making reference to FIGS. 8 and 9 :
α 1 =80°-100°, inclusive (this angle may be called the “sharp” or “brad” angle; α 2 =140°-170°, inclusive (this angle may be referred to as the “contact” angle, and which is the angle formed by the first grinding operation; β 1 =15°±10°; and β 2 =12°±7° (this angle may be referred to as a “relief” angle).
[0074] Once these parameters have been selected, in combination with the understanding that in a rotationally symmetrical two-flute drill bit, the leading edges of the cutting lips are 180° opposed from one another, one of ordinary skill in the art having the disclosure before them will be aware of or can readily calculate using known algorithms, all of the contours of the partially fabricated drill of FIGS. 8-10 .
[0075] The selection of angles β 1 and β 2 is dependent, in part, on the diameter of the particular drill. That is, within the given ranges, β 1 varies in inverse proportion to the diameter of the drill, while β 2 varies proportionally to the diameter of the drill. After the tip is formed through grinding, according to these initial parameters, the final tip configuration is shown in FIGS. 11-14 . After the second stage of grinding is performed, chisel point 110 is re-shaped into its final form, as shown and described herein.
[0076] In the final configuration of drill 100 , lands 102 are provided with surfaces 154 , which slope away from the central point 110 , and surfaces 158 , which angle upwardly and outwardly from the intersection 160 of surfaces 154 and 158 . In addition, as described hereinbelow, drill 100 is also provided with axial relief surfaces 162 , on lands 102 . The positions of surfaces 154 and 158 result from the configuration of drill 100 as shown in FIGS. 8-10 , as subsequently modified by the formation of the axial relief surfaces, as described with respect to FIGS. 12-15 .
[0077] The radially outer edges of surfaces 158 are, preferably either perpendicular to the longitudinal axis of the drill, or preferably at the very shallow angle β 1 , as defined hereinabove.
[0078] While intersection 160 is shown in the form of a sharp intersection, this is somewhat idealized, in that in preferred embodiments of the invention, intersection will be a rounded transition, having a relatively small radius of curvature, as an intersection in the form of a sharp line may be less effective in enabling chip removal.
[0079] In addition, the lands 102 of drill 150 are provided with axial relief, as shown in FIG. 14 . As indicated, the angle of the axial relief is between β 2 (15°±7°, as defined in the previous embodiment) and 60°, maximum. This axial relief is provided at a steeper angle than in prior art drills, particular multi-material drills, in order to provide for rapid chip removal, which is particularly useful when drilling wood. In traditional wood drills, the angle of the cutting lip is the same as the angle of the chip removal surface, that is, the relatively shallow angle β 1 (relative to a perpendicular to the longitudinal axis of the drill).
[0080] FIG. 15 is an illustration, which would be readily understood, by one of ordinary skill in the art of making drills, and having the present disclosure before them, of the geometry and process for forming the axial relief. The process begins with a partially completed drill 100 , as represented by FIGS. 8-10 . Making reference to FIG. 15 , a drill 100 will be placed in a workpiece holder in a position that is the end result of the following orientation steps. First, visualize, for the purposes of explanation, axes x (horizontal and parallel to the plane of observation of FIG. 15 ), y (vertical and parallel to the plane of observation of FIG. 15 ) and z (perpendicular to axes x and y, but shown in perspective). A drill 100 is initially arranged with its shank end at the origin, and the longitudinal axis L extending along and concentric to axis z. Drill 100 would have the rotational orientation shown in FIG. 8 , in that axis I (of drill 100 in FIG. 8 ) would be parallel to axis y, while axis II (of drill 100 in FIG. 8 ) would be parallel to axis x. The first orientation would be to pivot the drill upwardly from axis z an angle q an amount of 60°±20° in the y-z plane (see the projection line up from axis z). The second orientation would be to pivot the drill an angle w an amount of 20°±10° away from the y-z plane. Once the drill is so oriented (this orientation being performed in a workpiece holder), the drill is then presented (moved along the z axis) to a grinding surface which is parallel to the x-y axis and perpendicular to the z axis. It is this orientation that defines lines A, B and C, of FIG. 12 . That is, the further the drill is moved into the grinding surface, the further lines A, B and C are moved “up” the tip of the drill, or in other words, toward axis II, as shown in FIG. 12 . It is believed that for drills according to the present invention that are intended for harder materials, it is desired that line A, in particular, is moved farther up the tip of the drill, toward axis II.
[0081] A notable difference between the axial relief feature (surface 162 ) of the present, and such tip structures as a “split point” is that the plane of the axial relief feature of the present invention intersects the cutting lip, along axis II (see FIG. 12 ), where, in “split point” drills the plane of the cut is well moved off of the cutting lip and intersects and passes through the longitudinal axis of the drill, instead of extending tangentially through it.
[0082] The angle q is directly proportional to the diameter of the drill, so that q is progressively greater in larger diameter drills and progressively less in smaller diameter drills. The angle w is inversely proportional to the diameter of the drill. Hardness is also a factor, in that for drills of the same diameter, for a relatively harder material to be drilled, angle q goes down, while angle w goes up.
[0083] Once this final axial relief forming step is complete, then the drill is given any final surface finishing steps as may be desired, as are customary in the art of making drill bits.
[0084] While axial relief has been employed on end mills, such axial relief which is below 40°, and cannot exceed such a degree of sharpness, as it tends to weaken a tool (end mill) the principal direction of movement of which is perpendicular to the axis of rotation. That is, if the axial relief is too great, it removes from the tip area, the cutting surfaces that are needed for effective end milling material removal, and likewise makes it more likely that the tip will break during such lateral movements.
[0085] The steep axial relief employed in the present invention provides less heat created by the drilling process, due to less surface contact. In addition, it is believed that faster drilling can be achieved, in that the axial relief splits the chisel point of the drill to provide easier drilling starts, and because there is less contacting surface, each rotation of the drill can dig deeper into the workpiece. It is also believed that the provision of axial relief in the manner described results in improved self-centering of the drill, which is important to non-professional or non-industrial applications.
[0086] The drill of FIGS. 11-14 incorporates a brad and spur point construction which renders the drill usable for both wood, as well as other soft materials, and plastics and metals as well. Its use in non-ferrous materials, such as aluminum or copper, is advantageous because the axial relief provides less surface contact area, which means less heat generated by the drilling, and less sticking of the chips to the bit, through the melting described hereinabove.
[0087] FIG. 20 illustrates side elevations of different styles of drills that may employ point constructions, as that shown in the twist embodiment of FIGS. 11-15 . FIG. 20 -A illustrates for example, a short-flute drill, for which FIG. 20 -A-I is a section through the drill body. FIG. 20 -B is a straight flute drill, for which FIG. 20 -B-II is a section through the body. FIG. 20 -C-III is a spade drill, for which FIG. 20 -C-III is a section through the body. Each of these is shown, in the sections, as incorporating the axial relief surfaces as shown and described with respect to the twist drill configuration.
[0088] In preferred embodiments of the invention, the twist drills are formed from single materials, such as High Speed Steel, M50 steel, M2-M12 steel, carbon steel or any other suitable material.
[0089] The foregoing description and drawings merely explain and illustrate the invention, and the invention is not limited thereto, except as those skilled in the art who have the present disclosure before them will be able to make modifications and variations therein without departing from the scope of the invention.
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A twist drill for use, predominantly by non-professional do-it-yourself workers incorporates a flute architecture with an internal ridge for promoting the break up of chips into short length components. The tip of the twist drill includes an axial relief construction for improved performance across a wide variety of materials, and a highly sloped face for prompting transport of chips away from the drill tip.
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BACKGROUND OF THE INVENTION
The field of the present invention is oil well completion tools and techniques.
Wells are conventionally drilled through production zones with casings installed to adjacent the production zones. Such casings may extend through certain production zones where multiple zones exist. In such cases, the casings may be strategically placed or later perforated to provide access to additional zones. Typically a casing does not extend to the bottom of unconsolidated sand in the production zone of the well as drilled. In sandy conditions, the bottom of the well may fill in before completion. Under many circumstances, a liner is to be placed in the well with perforations at the productive zones. Additionally, gravel packing about the liner is common.
Upon the completion of such wells, sand control adapters are frequently employed to seal the joints between the upper ends of the liners and the casings. Such devices prevent sand from being entrained into the production. One such adapter is illustrated in U.S. Pat. No. 5,052,483, the disclosure of which is incorporated herein by reference.
For well completion, it is frequently necessary to clear out the bottom of the hole, insert an appropriate liner, gravel pack the production zone or zones and seal the liner off at the casing. Multiple trips down a well are frequently required to accomplish each of these tasks. The pulling of tools is, of course, expensive. Mechanisms have been designed for accomplishing a variety of tasks with one trip down the well. U.S. Pat. No. 5,425,423, the disclosure of which is incorporated herein by reference, illustrates a well tool which can drill, under ream and gravel pack with one trip down the well. U.S. Pat. No. 5,497,840, the disclosure of which is incorporated herein by reference, discloses another completion system for drilling in, placing and hanging a liner, cementing portions of the well and providing a seal between the casing and the liner. This may be accomplished with one trip down the well. Of course all systems allow for retraction of the drill string. Some equipment may be sacrificed in the well.
SUMMARY OF THE INVENTION
The present invention is directed to a landing adapter which may be associated with a liner positionable within a well for well completion. The adapter provides a seal between the liner and the casing. It also keeps the liner from being inadvertently pulled upwardly and yet can provide for shear-out.
Accordingly, it is an object of the present invention to provide improved well completion equipment. Other and further objects and advantages will appear hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a slotted liner and landing adapter shown partially installed with the formation and casing in cross section.
FIG. 2 is a partially cross-sectioned side view of a landing fixture.
FIG. 3 is a partially cross-sectioned side view of an adapter body with an actuator and a shear ring.
FIG. 4 is a detail of the device of FIG. 3 with the actuator in a second position.
FIG. 5 is a side view partially in cross section of a by-pass tool.
FIG. 6 is a side view of the center portion of the bypass tool of FIG. 5 rotated 90° from that of FIG. 5.
FIG. 7 is a cross-sectional view taken along line 7--7 of FIG. 6.
FIG. 8 is a side view of the by-pass tool in partial cross section with the tool configured for flow fully therethrough.
FIG. 9 is a side view of the by-pass tool in partial cross section with the tool configured for gravel pack flow.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning in detail to the drawings, FIG. 1 illustrates a landing adapter, generally designated 10, coupled with a conventional expansion joint 12 which is in turn coupled with a liner assembly, generally designated 14. The entire string is positioned with a casing 16 shown to be in multiple sections. This string may be run into a well and positioned through production zones all in one trip with a by-pass tool used to complete each zone.
The liner assembly 14 has multiple perforated sections 18 and multiple gravel pack port collars 20 most conveniently adjacent the perforated sections 18, respectively. The gravel pack port collars 20 are conventional with a rotatable sleeve within each gravel pack port collar having slots to receive dogs for rotation of the sleeve. The sleeve is rotated 90° one way to open and 90° back to close. A wash-in shoe 22 with stab-in blades 24 is attached at the end of the liner assembly 14. This shoe has ports 26 at the bottom thereof and an annular seal 28 inside of the hollow shoe 22.
Looking to FIG. 2, a landing fixture 30 is illustrated which may be rigidly held in place on a casing pin. The landing fixture 30 is essentially a pipe section with a threaded socket end 32 and a threaded pin end 34. The socket end 32 may be associated with the pin of a casing section to locate the fixture 30 within the well. Additional casing may be added to the threaded pin end 34.
The inside profile of the landing fixture 30 is of specific interest. A landing ring 36 extends inwardly to define a hole 38 extending axially through the fixture 30. At the upper end of the landing ring 36 is an upward landing shoulder 40 which is in the shape of a circular, truncated conical section. At the lower end of the landing ring 36 is a downward landing shoulder 42. The downward landing shoulder 42 lies within a plane normal to the axis of the landing fixture 30. A shallow inwardly facing annular channel 44 is located adjacent to the downward landing shoulder 42. The lower wall of the channel 44 is shown to be tapered.
Turning to FIG. 3, an adaptor body, generally designated 46, is constructed principally as a pipe assembly. The adaptor body 46 includes a two-thread box 48 having square threads 50 for attachment to the lower end of a drill string and the body portion 52 threaded and permanently fixed to the two-thread box 48. The body portion 52 has a pin 54 which may be configured for attachment by conventional means to a liner assembly.
The body portion 52 extends to a pin 56 which is associated with the two-thread box 48. Adjacent to that pin 56 is a thin cylindrical section 58 defining the bottom of a cavity which is an outwardly facing annular channel 60. The channel 60 is bounded on one end by the lower terminal shoulder of the two-thread box 48. At the other end, a thicker cylindrical section 61 defines the lower extent of the annular channel 60. The thicker cylindrical section 61 is beveled at the lower end 62 so as to ensure passage down the well and includes a shoulder 63 at its other end which is normal to the axis of the adaptor body 46. Between the bevel 62 and the shoulder 63, a second cavity which is an outwardly facing annular channel 64 is cut into the cylindrical section 61. Between the shoulder 63 and the annular channel 64, an outwardly facing annular recess 65 provides relief in the outer surface.
An actuator sleeve, generally designated 66, is positioned within the outwardly facing annular channel 60. The sleeve 66 is positionable on the thinner cylindrical section 61 prior to assembly of the two-thread box 48 with the body portion 52. The sleeve 66 has an annular body 67 which specifically fits on the thinner cylindrical section 61 to slide along the surface thereof. The body 67 is shorter in axial length than the annular channel 60 in order that it might take either of two extreme positions, either against the shoulder 63 or against the terminal shoulder of the two-thread box 48.
The actuator sleeve 66 further includes an engagement shoulder 68. The engagement shoulder 68 is shown to be a circular, truncated conical shoulder defined by a thicker cylindrical portion 69 at one end of the actuator sleeve 66.
At the other end of the actuator sleeve 66, an extension in the form of annular skirt 70 extends from one end of the annular body 67. The skirt 70 is sized to extend over the outwardly facing annular recess 65 and is of sufficient length to further extend over the annular channel 64 when the actuator sleeve 66 is positioned against the shoulder 63.
A shear ring 71 is located within the annular channel 64. This shear ring 71 may be of brass, metal or even plastic, depending upon its dimensions and the amount of force at which it is to be sheared. In the current embodiment, the shear strength of the ring may be on the order of 80,000-100,000 pounds. The shear ring 71 is also split and arranged in a relaxed state to have a gap in order that the ring may be compressed. The dimensions of the shear ring 71 are such that a first position is achieved with the shear ring 71 extending outwardly of the annular channel 64 in the relaxed state. In a compressed state, the shear ring 71 assumes a second position which has an outside diameter allowing the ring 71 to be placed within the skirt 70.
Before entry into a well, the adaptor is arranged with the actuator sleeve in the extreme lower position. In this position, the shear ring 71 is compressed and arranged beneath the skirt 70. Shear pins 72 are arranged about the adaptor and extend between the adaptor body and the actuator sleeve. The skirt 70 further fits within the outwardly facing annular recess 65 so that the entire adaptor below the engagement shoulder 68 fits within the hole 38 in the landing ring 36.
In the second extreme position, the annular body 67 is against the lower terminal shoulder of the two-thread box 48. The shear pins 72 are sheared and the skirt 70 has fully disengaged the shear ring 71 so that it may obtain its relaxed state. The axial difference between the annular channel 60 and the annular body 67 is such that the annular skirt 70 is fully displaced from the shear ring 71. The engagement shoulder 68 with the annular body in the upper extreme position is to be distanced from the near side of the shear ring 71 such that the landing ring 36 fits within that space.
In operation, the adaptor is placed down the well with the landing fixture 30 already in place and attached to the well casing. The adaptor body 46 is arranged with the actuator sleeve 66 with the shear pins 72 unbroken and the skirt 70 extending over the shear ring 71. Once the adaptor meets the landing ring 36, the engagement shoulder 68 engages the upward landing shoulder 40. This shears the pins 72 and causes the sleeve 66 to move to its second extreme position. At this time, the actuator sleeve is seated. The shear ring 71 is released so as to extend into the shallow channel 44 below the downward landing shoulder 42. In this way, the landing ring 36 is captured between the engagement shoulder 68 and the shear ring 71. Once positioned, extraction requires a shearing of the shear ring 71. By requiring a shear strength of 80,000-100,000 pounds, the shear ring 71 is only likely to be sheared under intentional upward force applied through the drill string.
Delivered to the well with the liner assembly 14 and landing adapter 10 is a by-pass tool, generally designated 74. Associated with the lower end of the by-pass tool 74 is a stinger 76 (FIG. 1). The stinger fits within and is sealed by the annular seal 28 within the wash-in shoe 22. The stinger is thus in communication with the ports 26.
The by-pass tool 74 includes a main barrel 78. The barrel 78 is substantially cylindrical except for the lower portion which includes a cross section as seen in FIG. 7. A pin 80 is at one end and an interiorly threaded socket 82 is at the other. A barrel extension 84 includes a pin 86 associated with the socket 82. The barrel extension 84 is also generally cylindrical and extends to a pin 88 to which may be attached the stinger 76. A central bore 90 extends through the barrel 78 and the barrel extension 84. Gravel pack cups 92 and 94 are conventionally arranged and accommodated on the exterior of the barrel 78. Similarly gravel pack cups 96 and 98 are associated with the exterior of the barrel extension 84. The cups, 92, 94, 96 and 98 are arranged to either side of a gravel packing section of the barrel 78. A collar 100 is associated with the pin 80 of the barrel 78 for attachment to the drill string.
Diametrically opposed gravel ports 102 extend radially through the barrel 78 at a position between the upwardly sealing pack cups 92 and 94 and the downwardly sealing gravel pack cups 96 and 98. These ports 102 are sized and arranged such that they may be aligned with the ports located in the gravel pack port collars 20 when indexed axially in the bore. Also extending radially through the barrel 76 are upper ports 104 located above the gravel pack cup 92 for communication with the annular space between the liner assembly 14 and the barrel 78. The barrel also includes spring loaded radially outwardly biased dogs 106 which are conventionally employed with the gravel pack port collars 20. With the dogs 106 engaged with a specific port collar 20, the gravel ports 102 are then aligned with the gravel pack port collar 20. Rotation of the string 90° then causes the port collar 20 to open. Rotation in the opposite direction then closes the port collar 20.
Turning to inwardly of the barrel 78, an annular sleeve 108 is positioned concentrically within and displaced inwardly from the barrel 78. The sleeve extends through a first length of the barrel defining a substantially annular side passage 110. At the upper end, a ring 112 closes the side passage 110. This ring 112 is above the upper ports 104 such that the annular side passage 110 is in communication with those upper ports 104. At the lower end of the annular sleeve 108, an annular seat 114 is defined which defines the annular space forming the annular side passage 110 below the annular sleeve 108. The annular seat 114, however, divides the annular side passage 110 into two by-pass passages 116 and 118 extending lengthwise through a portion of the bore of the barrel 78. The annular seat 114 thus defines a portion of the gravel ports 102 by outwardly extending walls 120 as can best be seen in FIG. 7 which form oblong passages from the center of the annular seat to the gravel ports 102. In this way, the annular seat 114 defines by-pass passages 116 and 118 which communicate with the annular side passage 110 to extend communication downwardly around the gravel ports 102 in a manner such that the by-pass passages 116 and 118 are not in communication with the gravel ports 102 extending through both the annular seat 114 and the wall of the barrel 78.
The annular seat 114 has a central bore 122 as can best be seen in FIG. 7. A valve sleeve 124 is positioned within the central bore 122 of the annular seat 114. The valve sleeve 124 itself includes a bore 126 in part defining the central bore 90.
The valve sleeve 124 includes return ports 128 extending radially through the sidewall. Below the return ports, a retainer 130 extends across the bore 126. A one-way valve including a valve seat 132 and a valve ball 134 are provided within the bore 126 of the valve sleeve 124. The retainer 130 keeps the valve ball 134 near the valve seat 132. The one-way valve controls flow through the bore 126. Above the valve ball 134 when positioned on the valve seat 132 are wash-in ports 136.
The valve sleeve 124 moves from a first, closed position as illustrated in FIG. 8 to an open position as illustrated in FIG. 9. Shear pins retain the valve sleeve 124 in the closed position through initial operations. In the closed position, the valve sleeve 124 extends over the gravel ports 102. The return ports 128 are also positioned on the valve sleeve 124 such that they are closed with the valve sleeve 124 in the closed position. The valve sleeve 124 extends downwardly below the annular seat 114 such that the wash-in ports 136 are open with the valve sleeve 124 in the closed position. Also in the closed position, the lower end of the valve sleeve 124 is displaced from the pin 86 of the barrel extension 84 so that communication may flow from the central bore 90 through the central bore 122, out the wash-in ports 138, around the lower end of the closed valve sleeve 124 and again down through the central bore 90 in the barrel extension 84.
The valve sleeve 124 has a second valve seat 138 above the one-way valve. The placement of a valve ball 140 on the valve seat 138 causes pressure to increase in drilling fluid above the ball valve 140. The shear pins fail and the valve sleeve 124 moves to the open position as seen in FIG. 9. In the open position, the valve sleeve 124 is displaced from the gravel ports 102 such that they are in communication with the central bore 90. The return ports 128 also pass downwardly below the bottom of the annular seat 114 and are open to communicate with the by-pass passages 116 and 118. The lower portion of the valve sleeve 124 seats into the pin 86 of the barrel extension 84. Thus, any communication along the central bore 90 across the one-way valve is controlled by the valve ball 134.
In operation, the by-pass tool is assembled with the liner assembly 14 before lowering into the well. The stinger 76 extends through the annular seal 28 to be in communication with the ports 26 of the wash-in shoe 22. The valve sleeve 124 is in the closed position. The condition of the by-pass tool is as seen in FIG. 8 at this time. The well was first drilled, a casing positioned and portions under reamed. Consequently, accumulation of debris is expected to have accumulated at the bottom of the well.
As the combination of the liner assembly 14 and the by-pass tool is lowered to encounter the debris, the fluid is pumped down the drill pipe and through the central bore 90. When the fluid encounters the one-way valve at the bottom of the valve sleeve 124, it is able to flow through the wash-in ports 136, around the bottom end of the valve sleeve 124 and back to the central bore 90 as it extends through the barrel extension 84. The flow continues to the stinger 76 and out through the ports 26 of the wash-in shoe 22. Because of the annular seal 28, the drilling fluid exits through the ports 28 to outwardly of the liner assembly 14. The fluid along with entrained debris flows upwardly in the annular space between the liner assembly 14 and either the well bore or the casing 16. This flow washes out debris and allows the liner assembly 14 to be washed into position at the bottom of the well.
When appropriately positioned, the landing adapter 10 associated with the liner assembly 14 approaches and captures the landing ring 30. The flow of fluid and debris had been proceeding about the landing adapter and up the annulus within the casing 16. However, when the landing adapter 10 seats on the landing ring 30, this circulation is interrupted. The ball valve 140 is then placed in the drill pipe bore where it is conveyed to the valve seat 138. The pressure of the fluid behind the seated valve ball 140 shears the pins associated with the valve sleeve 124 and the valve sleeve 124 assumes the second, open position.
Once the valve ball 140 is in place and the valve sleeve 124 opened, flow can proceed through the pipe bore downwardly through the central bore 90 and out the gravel ports 102. The lowermost zone may then be gravel packed in a conventional manner.
The fluid return during gravel packing may be through the perforated liner sections 18 and up through the stinger 76. The valve ball 134 of the one-way valve allows flow upwardly into the valve sleeve 124. Return fluid may then pass through the return ports 128 to the by-pass passages 116 and 118 and the annular side passage 110. The returning flow then exits through the upper ports 104 to the annulus within the casing 16 to return to surface.
Once the gravel pack has been complete in an under reamed zone, it may be advantageous to clear the liner between the gravel pack cups 94 and 96 and the central bore 90 as well as the drill string. Flow of the drilling fluid can be reversed, delivered down the annulus of the well, past the cups 92 and 94 to the gravel ports 102. The fluid can then return through the central bore 90.
Once this operation has been completed, the by-pass tool can be lifted upwardly to the next gravel pack port collar 20 and the tool positioning, gravel packing and cleaning may be repeated. This process can be repeated for each zone. Once this is accomplished, the tool may be pulled from the well. Manipulation of by-pass tools have tended to lift the liner assembly 14 out of position. Use of the landing adapter 10 prevents such unwanted extraction of the liner assembly 14. With the removal of the by-pass tool, the well is complete.
Accordingly, improved completion equipment and methods have been disclosed. While embodiments and applications of this invention have been shown and described, it would be apparent to those skilled in the art that many more modifications are possible without departing from the inventive concepts herein. The invention, therefore is not to be restricted except in the spirit of the appended claims.
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A well completion system and method including a landing adapter which can be interlocked with a landing ring. A split ring is retained within a groove in the landing adapter which operates to lock the landing adapter with the landing ring. The groove into which the shear ring is positioned has two effective diameters. A first diameter allows the shear ring to compress and pass within the landing ring. The second diameter prevents extraction without shearing of the ring. A by-pass tool is positioned with a liner assembly 14 having a landing adapter. The by-pass tool includes a valve sleeve having a first position allowing flow down the center bore into a stinger extending to a wash-in shoe. Once the liner assembly has been washed in, the valve sleeve assumes a second, open position. Gravel packing may then occur through the central bore with return through a by-pass passage through the tool. Cleaning of the liner and tool can also occur through reverse flow to the gravel packed area.
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RELATED PATENT APPLICATION
This application claims priority to commonly owned U.S. Provisional Patent Application Ser. No. 61/249,745; filed Oct. 8, 2009; entitled “Slow Speed Operation of Brushless Direct Current Motors by Gating Pulse Width Modulation Drive,” by Ward R. Brown; and is related to commonly owned U.S. patent application Ser. No. 12/767,101; filed Apr. 26, 2010; entitled “Variable Pulse Width Modulation for Reduced Zero-Crossing Granularity in Sensorless Brushless Direct Current Motors,” by Ward R. Brown; and U.S. patent application Ser. No. 12/767,052; filed Apr. 26, 2010; entitled “Synchronized Minimum Frequency Pulse Width Modulation Drive for Sensorless Brushless Direct Current Motor,” by Ward R. Brown; wherein all are hereby incorporated by reference herein for all purposes.
TECHNICAL FIELD
The present disclosure relates to brushless direct current (BLDC) motors, and more particularly, to slow speed operation of BLDC motors by gating pulse width modulation (PWM) drive.
BACKGROUND
Brushless direct current (BLDC) motors are used in industries such as appliances, automotive, aerospace, consumer, medical, industrial automation equipment and instrumentation. BLDC motors do not use brushes for commutation, instead, electronic commutation is used. BLDC motors have advantages over brushed DC motors and induction motors such as: better speed versus torque characteristics, high dynamic response, high efficiency, long operating life, longer time intervals between service, substantially noiseless operation, and higher speed ranges. More detailed information on BLDC motors may be found in Microchip Application Notes: AN857, entitled “Brushless DC Motor Control Made Easy,” (2002); AN885, entitled “Brushless DC (BLDC) Motor Fundamentals,” (2003); AN894, entitled “Motor Control Sensor Feedback Circuits,” (2003); AN901, entitled “Using the dsPIC30 F for Sensorless BLDC Control,” (2004); and AN970, entitled “Using the PIC18F2431 for Sensorless BLDC Motor Control,” (2005); all are hereby incorporated by reference herein for all purposes.
A three-phase BLDC motor completes an electrical cycle, i.e., 360 electrical degrees of rotation, in six steps at 60 electrical degrees per step. Synchronously at every 60 electrical degrees, phase current switching is updated (commutation). However, one electrical cycle may not correspond to one mechanical revolution (360 mechanical degrees) of the motor rotor. The number of electrical cycles to be repeated to complete one mechanical revolution depends upon the number of rotor pole pairs. For example, a four-pole BLDC motor will require two electrical cycles to complete one mechanical revolution of the motor rotor (see FIG. 5 ).
Drive commutation for a BLDC motor may be determined by position sensors that monitor the rotational position of the motor rotor shaft. Such position sensors may be, for example but are not limited to, Hall Effect position sensors embedded into the stator on the non-driving end of the motor.
Drive commutation for a sensorless BLDC motor may also be determined by monitoring the back electromotive force (EMF) voltages at each phase (A-B-C) of the motor. The drive commutation is synchronized with the motor when the back EMF of the un-driven phase crosses one-half of the motor supply voltage during a commutation period. This is referred to as “zero-crossing” where the back EMF is equal to one-half of the motor supply voltage, over each electrical cycle. Zero-crossing is detected on the un-driven phase when the drive voltage is being applied to the driven phases. A voltage polarity change about the zero-crossing voltage of the back EMF on the un-driven phase may also be used in detecting a zero-crossing event, e.g., from positive to negative or negative to positive during application of the drive voltage to the driven phases within certain limits.
The rotational speed of a BLDC motor is dependent upon the amplitude of the average DC voltages applied to the stator windings of the motor. The higher the average DC voltage applied the faster will the BLDC motor rotate. Generally, DC voltages are generated using pulse width modulation (PWM) to control the voltage amplitudes applied to the stator windings. The PWM maximum frequency is limited by the switching losses of the drive transistors. The PWM minimum frequency is limited by the undesirable audio emissions at frequencies in the audio range. An acceptable compromise is in the 15 KHz to 20 KHz range. PWM duty cycle can only be reduced to the point where the drive pulse width can still propagate through the drive power field effect transistors (FETs) and low-pass filter characteristics inherent in all motor designs. Reducing the PWM frequency would allow longer drive periods but this would also introduce audible noise from the motor.
SUMMARY
The aforementioned problem is solved, and other and further benefits achieved by driving the brushless DC motor during a partial commutation period. The average drive voltage to the motor can be reduced further than available from the minimum pulse width and still maintain an inaudible PWM frequency by reducing the number of pulses in each commutation period. Therefore, average drive voltage to a BLDC motor can be further reduced by limiting the number of PWM pulses in each commutation period while maintaining an inaudible PWM signal period and duty cycle.
According to a specific example embodiment of this disclosure, a method for controlling low speed operation of a brushless direct current motor comprises the steps of: generating a plurality of pulse width modulation (PWM) pulses at a certain duty cycle; determining electrical timing centers for each of a plurality of commutation periods of a brushless direct current motor; gating off some of the plurality of PWM pulses in each of the plurality of commutation periods, wherein the plurality of PWM pulses not gated off are grouped toward the electrical timing centers of the plurality of commutation periods; and driving power switching transistors with the plurality of PWM pulses not gated off during the plurality of commutation periods, wherein the power switching transistors are connected between the stator coils of the brushless direct current motor and a direct current power source.
According to another specific example embodiment of this disclosure, a method for controlling low speed operation of a sensorless brushless direct current motor, said method comprising the steps of: generating a plurality of pulse width modulation (PWM) pulses at a certain duty cycle; determining electrical timing centers for each of a plurality of commutation periods of a brushless direct current motor by measuring back electromotive force voltages at each stator coil of the sensorless brushless direct current motor, and determining from the measured back electromotive force voltages when each of the measured back electromotive force voltages is at substantially a zero-crossing voltage value, wherein the zero-crossing voltage value is about one-half of a voltage value of a direct current power source; gating off some of the plurality of PWM pulses in each of the plurality of commutation periods, wherein the plurality of PWM pulses not gated off are grouped toward the electrical timing centers of the plurality commutation periods; and driving power switching transistors with the plurality of PWM pulses not gated off during the plurality commutation periods, wherein the power switching transistors are connected between the stator coils of the sensorless brushless direct current motor and the direct current power source.
BRIEF DESCRIPTION OF THE DRAWINGS
A more complete understanding of the present disclosure thereof may be acquired by referring to the following description taken in conjunction with the accompanying drawings wherein:
FIG. 1 illustrates a schematic diagram of a three-phase brushless direct current motor, Hall Effect position sensors and electronically commutating motor controller, according to a specific example embodiment of this disclosure;
FIG. 2 illustrates a schematic diagram of a three-phase sensorless brushless direct current motor and electronically commutating motor controller, according to another specific example embodiment of this disclosure;
FIG. 3 illustrates schematic diagrams showing current flows in each of the three stator windings of a three-phase brushless direct current motor during each 60 degree commutation period;
FIG. 4 illustrates a more detailed schematic diagram of the back EMF zero-cross detectors shown in FIG. 2 ;
FIG. 5 illustrates schematic timing and amplitude graphs of a four-pole motor showing back electromotive force (EMF) voltages at each of the three stator windings during each 60 degree commutation period; and
FIG. 6 illustrates schematic amplitude and timing graphs of voltages at one phase of the BLDC motor during each commutation period for different PWM duty cycles, according to the teachings of this disclosure.
While the present disclosure is susceptible to various modifications and alternative forms, specific example embodiments thereof have been shown in the drawings and are herein described in detail. It should be understood, however, that the description herein of specific example embodiments is not intended to limit the disclosure to the particular forms disclosed herein, but on the contrary, this disclosure is to cover all modifications and equivalents as defined by the appended claims.
DETAILED DESCRIPTION
Referring now to the drawing, the details of specific example embodiments are schematically illustrated. Like elements in the drawings will be represented by like numbers, and similar elements will be represented by like numbers with a different lower case letter suffix.
Referring to FIG. 1 , depicted is a schematic diagram of a three-phase brushless direct current motor, Hall Effect position sensors and electronically commutating motor controller, according to a specific example embodiment of this disclosure. A three-phase brushless direct current motor, generally represented by the numeral 100 , comprises a plurality of stator coils 102 and a rotor (not shown) having magnets arranged in a three-phase configuration. For discussion purposes the motor 100 described herein will be in a two pole three-phase configuration requiring 360 degrees of electrical rotation to produce one mechanical revolution of 360 degrees. The motor 100 is electronically commutated with power switching transistors 108 and 110 connected to the three-phase brushless direct current motor 100 and a direct current (DC) power source. The Hall Effect position sensors 104 supply rotor position information to a digital device 106 that may comprise a microcontroller (not shown), PWM generators having outputs coupled to power transistor drivers providing pulse width modulation (PWM) control outputs (PWM 0 -PWM 5 ) that are used to control turn-on and turn-off of the power switching transistors 108 and 110 . Based upon the combination of the three signals from the Hall Effect sensors 104 , the exact sequence of commutation can be determined. Use of Hall Effect position sensors 104 for rotor position indication is preferable and may even be required in low speed motor applications.
The motor 100 is electronically commutated from a direct current (DC) source (not shown) through the power switching power transistors 108 and 110 , e.g., power field effect transistors (one pair per phase for a three-phase motor). The power transistors 108 and 110 are controlled by the digital device 106 , e.g., a microcontroller, that is coupled to the power transistors 108 and 110 through drivers for the power transistors (not shown). The digital device 106 provides six pulse width modulation (PWM) outputs, PWM 0 -PWM 5 , that control both the motor rotation direction and speed by turning on and off selected phase pairs of the power transistors 108 and 110 according to PWM signals appropriately sequenced and timed.
Referring to FIG. 2 , depicted is a schematic diagram of a three-phase sensorless brushless direct current motor and electronically commutating motor controller, according to another specific example embodiment of this disclosure. A three-phase sensorless brushless direct current motor, generally represented by the numeral 200 , comprises a plurality of stator coils 102 and a rotor (not shown) having magnets arranged in a three-phase configuration. For discussion purposes the motor 200 described herein will be in a two pole three-phase configuration requiring 360 degrees of electrical rotation to produce one mechanical revolution of 360 degrees. The motor 200 is electronically commutated with power switching transistors 108 and 110 connected to the three-phase sensorless brushless direct current motor 200 and a direct current (DC) power source. Back electromotive force (EMF) zero-cross detectors 204 , a digital device 206 , e.g., a microcontroller, having PWM generators that provide pulse width modulation (PWM) outputs coupled to power transistor drivers. The power transistor drivers (PWM 0 -PWM 5 ) control turn-on and turn-off of the power switching transistors 108 and 110 .
Each stator coil 102 is connected to the positive of the DC power source for two commutation periods, the negative of the DC power source for two commutation periods, and is disconnected from both the positive and negative of the DC power source for two commutation periods. The motor phase position is determined by back electromotive force (EMF) voltages measured at a stator coil 102 when not connected to the DC power source at the time of measurement while the other two stator coils 102 are connected to the DC power source. The back EMF voltages at each of the stator coils 102 are monitored by the back EMF zero-cross detectors 204 (one per phase). However, the back EMF voltage to be measured requires connection to the positive of the DC power source of one of the stator coils 102 so as to enable current flow therethrough, thereby biasing the motor generated voltage to a level centered around the detection reference level (“zero-crossing” event), e.g., one-half the supply voltage. The other stator coil 102 of the pair of coils having current flow therethrough is connected to the negative of the DC power source.
Referring to FIG. 3 , depicted are schematic diagrams showing current flows in each of the three stator windings (coils 102 ) of a three-phase brushless direct current motor during each 60 degree commutation period. Rotation of the motor 100 is divided into six commutation periods (1) through (6), and current flows through different combinations of two of the three coils 102 during each of the six commutation periods. While combinations of two of the coils 102 are connected to the DC power source, a third coil 102 (three-phase motor) is not connected to the power source. However the unconnected coil 102 is monitored by the back EMF zero-cross detectors 204 such that upon detection of a “zero crossing” event, i.e., back EMF voltage on the unconnected coil 102 changes polarity while going through a substantially zero voltage (“zero voltage” is defined herein as one-half of the DC supply voltage). At approximately the zero voltage point detected by a respective one of the back EMF zero-cross detectors 204 , a synchronization relationship of the motor 200 stator coils 102 is ascertained, as more fully described hereinbelow. When Hall Effect position sensors 104 are used, back EMF zero-cross detection is not necessary as the Hall Effect position sensors 104 directly transmit the rotor position to the digital device 106 .
Referring to FIG. 4 , depicted is a more detailed schematic block diagram of the back EMF zero-cross detectors shown in FIG. 2 . The back EMF zero-cross detectors 204 may comprise three-phase voltage divider resistors 418 and 420 , phase low-pass filters 422 , reference low-pass filter 430 , reference voltage divider resistors 426 and 428 , and voltage comparators 424 . The reference voltage divider resistors 426 and 428 are used to derive a “virtual” neutral reference voltage for use by the comparators 424 and/or the digital device 206 having analog inputs. The three-phase voltage divider resistors 418 and 420 reduce the stator coils 102 voltages to much lower voltages for use by the low-pass filters 422 and comparators 424 . Preferred resistance relationships for the resistors 418 , 420 , 426 and 428 are as follows:
Raa=Rbb=Rcc=Rrr
Ra=Rb=Rc= 2 *Rr
Ra /( Raa+Ra )=Vcomparator_maximum_input/DC+)−(DC−))
The low pass filters 422 may be used to substantially reduce unwanted noise from the inputs to the comparators 424 . The comparators 424 are used in determining when a back EMF voltage on an unconnected coil 102 is greater than the neutral reference voltage, or less than or equal to the neutral reference voltage. The outputs of the comparators 424 when at a logic high (“1”) may represent that the back EMF voltage is greater than the neutral reference voltage, and when at a logic low (“0”) may represent that the back EMF voltage is less than or equal to the neutral reference voltage, or visa-versa (designer's choice). The outputs of each of the comparators 424 may thereby be used to indicate when the back EMF voltage is at its “zero” transition point or when a back EMF polarity transition occurs, and indicate same to the digital device 206 . If the digital device has analog inputs and analog-to-digital (ADC) conversion capabilities and/or voltage comparators, the external comparators may not be required. When this is the case, the outputs from the low pass filters and the neutral reference voltage from the resistors 426 and 428 may be connected directly to the analog inputs (not shown) of the digital device 206 (e.g., mixed signal device).
Referring to FIG. 5 , depicted are schematic timing and amplitude graphs of a four-pole motor showing back electromotive force (EMF) voltages at each of the three stator windings during each 60 degree commutation period. When a phase coil is not connected to the DC power source no current flows therethrough. When a phase coil is connected to the positive (DC+) power source, current flows in a positive direction for two commutation periods (120 electrical degrees), then no current flows (coil is unconnected from the DC power source) for a subsequent commutation period (60 electrical degrees), and after the unconnected commutation period the very same coil has current flow in a negative direction for two commutation periods (120 electrical degrees) when connected to the negative (DC−) power source, and then no current flows in a next commutation period (60 electrical degrees) before the aforementioned electrical cycle repeats, i.e., for another 360 degree electrical cycle.
When using a sensorless BLDC motor, the back EMF voltage on the unconnected coil is transitioning from the positively driven polarity to the negatively driven polarity and does so throughout the 60 degree period when not being connected. If current is initially going into the coil when the connection is broken then the current will continue to flow thereby forward biasing a diode in parallel with the low-side drive transistor 110 presenting a voltage on the motor coil terminal equal to the negative (DC−) power source voltage plus the forward bias voltage of the diode. This negative spike persists until the energy in the coil is dissipated.
A “zero crossing” is where the measured voltage at each phase coil 102 goes to substantially one-half of the DC supply voltage (in the graphs normalized to “zero”), and is illustrated by the small circles of the back EMF graphs. When the PWM duty cycle is 100% in a commutation period, the measured back EMF varies between the full positive (DC+) rail voltage and the full negative (DC−) rail voltage of the power source. When the PWM duty cycle is 50% in a commutation period, the measured back EMF varies between 50% (one-half) of the full positive (DC+) rail voltage and 50% (one-half) of the full negative (DC−) rail voltage of the power source. When the PWM duty cycle is 25% in a commutation period, the measured back EMF varies between 25% (one-half) of the full positive (DC+) rail voltage and 25% (one-half) of the full negative (DC−) rail voltage of the power source. Therefore there is a direct correlation between the PWM duty cycle applied to the two current carrying coils 102 and the measured back EMF on the unconnected coil 102 . However, the back EMF always passes through the “zero crossing” point at substantially the center (e.g., middle, half-way point) of a commutation period when the other two coils are excited (current flowing therethrough). Just at lower PWM duty cycles, there is less variation of the back EMF voltage in the commutation period. This is not problematic since the “zero crossing” point is what is of interest.
It is important to remember that back EMF on the unconnected coil 102 is biased properly for detection only when the other two coils 102 are connected to the positive (DC+) and negative (DC−) power source rails and current flows through them. If there is no current flow in the two connected coils 102 at the time when a “zero crossing” should occur then the back EMF voltage at the unconnected coil 102 will not be centered relative to the reference voltage, and detection of the exact “zero crossing” will not be possible. However, missing detection of the exact “zero crossing” point in time because power drive is off (no current flow) at the instant of exact zero crossing may not be fatal so long as a change in polarity, e.g., positive to negative or visa versa, of the back EMF is determined when the power drive returns soon after zero crossing, and that this occurs close enough in time (electrical degrees) so as not to cause too great of a commutation timing error in normal operation. Instability problems do result when low duty cycle PWM signals cause significant commutation timing errors. As illustrated in the back EMF graphs shown in FIG. 5 , “zero crossing” points occur at approximately 30 electrical degrees from a commutation period change, i.e., substantially in the center (middle) of a commutation period. Use of Hall Effect position sensors 104 ( FIG. 1 ) are preferable when low duty cycle PWM signals are used for low speed motor applications.
Referring to FIG. 6 , depicted are schematic amplitude and timing graphs of voltages at one phase of the sensorless BLDC motor during each commutation period for different PWM duty cycles, according to the teachings of this disclosure. The BLDC motor operates at rotational speeds that are dependent upon the average voltages on each stator coil 102 during appropriate 60 degree commutation periods. Direction of rotation of the motor 100 ( 200 ) is dependent upon the commutation connection order of the coils 102 to the DC power source over each (360 degree) electrical cycle.
Graph 530 represents a 100 percent PWM drive duty cycle over one electrical cycle at one phase of the motor 100 . The 100 percent duty cycle will result in maximum voltages resulting in maximum rotational speed of the motor 100 .
Graph 532 represents approximately a five (5) percent PWM drive duty cycle over one electrical cycle at one phase of the motor 100 or 200 . At low PWM duty cycles, less average voltages will be created and thus slower rotational speeds will result since motor speed is directly proportional to the applied voltage. The ratio of rotational speed to applied voltage is much higher in high speed motors than that of low speed motors. Therefore, relatively small applied voltages in high speed motors will still result in significantly fast speed. Reducing the voltage by PWM is limited by the drive transistors 108 and 110 and the electrical characteristics of the motor since the PWM duty cycle can only be reduced to the point where the drive pulse widths can still propagate through the low pass frequency characteristics inherent in all motor designs. PWM signals whose pulse widths are too short are either attenuated by the low-pass characteristics of the motor and/or are shorter than the switching times of the drive power transistors 108 and 110 . Reducing the PWM frequency to enable use of longer pulse widths creates audible noise disturbances from the motor. Thus, the minimum inaudible PWM frequency determines the maximum pulse widths that can be used for slow speed operation of the motor 100 or 200 .
Graph 534 represents approximately a ten (10) percent PWM drive duty cycle over one electrical cycle at one phase of the motor 100 or 200 . At lower duty cycles of the PWM signal, less average voltages will be created and thus slower rotational speeds will result. However, the average drive voltage to the motor can be reduced further than is possible with the minimum inaudible PWM frequency (shown in graph 532 ) by reducing the number of PWM pulses in each commutation period. This may be accomplished by gating off some of the PWM pulses that would normally be generated, as shown in graph 532 . This allows the average drive voltage to the BLDC motor 100 or 200 to be reduced by limiting the number of PWM pulses while maintaining the PWM period and duty cycle. The use of longer PWM pulse widths (e.g., 10%) are more compatible with the motor 100 or 200 and the driver transistors 108 and 110 characteristics. Use of fewer PWM pulses in a commutation period allows lower average drive voltages (slower rotational speeds). Preferably, the PWM drive pulses may be centered on the peak back EMF in the commutation periods to keep the current-resistance (I−R) losses at a minimum and to deliver maximum torque.
Note that since the PWM pulses are substantially centered within each of the commutation periods, e.g., at +/−, 30, 90, 150, 210, 270, 330 degrees (electrical timing centers). The exact electrical timing center for each of the commutation periods may be shifted slightly +/− from the +30 degree values depending upon inductive lag and motor characteristics. Commutation period timing relationships are preferably determined using the rotor position signals from the Hall Effect position sensors 104 to the digital device 106 when operating at low rotational speeds. However, since the PWM signal pulses during each commutation period are substantially centered therein, there will be back EMF excitation voltage in an unconnected coil 102 near a “zero-crossing” (e.g., near points 544 ). Therefore, even during low PWM drive duty cycles where the off times of the PWM pulses in each commutation period are significant, a “zero-crossing” (points 544 ) may be determined when the measured back EMF changes polarity (referenced to the neutral reference voltage shown in FIG. 4 ).
While embodiments of this disclosure have been depicted, described, and are defined by reference to example embodiments of the disclosure, such references do not imply a limitation on the disclosure, and no such limitation is to be inferred. The subject matter disclosed is capable of considerable modification, alteration, and equivalents in form and function, as will occur to those ordinarily skilled in the pertinent art and having the benefit of this disclosure. The depicted and described embodiments of this disclosure are examples only, and are not exhaustive of the scope of the disclosure.
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Slow speed operation of a brushless DC (BLDC) motor is enhanced by gating off some of the PWM pulses in each commutation period. By doing so, longer PWM pulse widths may be used at PWM signal frequencies that are inaudible while still allowing desired slow speed operation of the BLDC motor. Centering the non-gated PWM pulses in each commutation period where peak back EMF occurs, further reduces losses and improves delivery of maximum torque from the BLDC motor.
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BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION
This invention relates to a hollow housing including structure for supporting new, unused scalpel blades therefrom and also structure for removing used scalpel blades from a scalpel handle shank as well as a substantially fully closed storage chamber in which to contain used scalpel blades after they have been removed. The blade removable structure is in operative association with a used blade receiving opening formed in the top of the housing and a used blade to be removed from a scalpel handle shank is initially positioned within the opening in a manner such that when removal of a used blade is effected, the used blade is free to fall by gravity into the interior of the housing.
DESCRIPTION OF RELATED ART
Various different forms of surgical blade dispensers and disposal devices heretofore have been provided such as those disclosed in U.S. Pat. Nos. 3,002,607, 4,106,620, 4,120,397, 4,180,162, 4,395,807, 4,730,376, 4,746,016, 4,903,390, 5,088,173 and 5,361,902.
While these previously known apparatuses include some of the general structural and operational features of the instant invention, the specific blade removal structure of the instant invention enabling a one handed blade removal operation and the specific new blade support structure enabling a one handed new blade attachment operation are not disclosed by the above mentioned prior art references.
SUMMARY OF THE INVENTION
The surgical blade dispenser and disposal apparatus of the instant invention is in the form of a hollow housing including a top wall. The top wall includes blade support structure for supporting a plurality of new surgical blades therefrom in position to be operationally engaged by the shank of a scalpel handle through utilization of a one handed operation. The top wall further includes an opening formed therethrough for entrance of used blades by gravity into an interior used blade storage compartment within the housing and the top wall of the housing also includes blade removal structure, in operative association with the blade receiving opening, for effecting blade removal from a scalpel handle shank through utilization of a one handed operation.
By providing a surgical blade dispenser and disposal apparatus of this type a person conducting an autopsy may quickly and conveniently change surgical blades with his or her hand and fingers spaced at least one inch remote from the cutting edge of a used blade being discarded or a new blade being attached to the scalpel shank.
The main object of this invention is to provide a surgical blade dispenser and disposal apparatus defining a receptacle for used scalpel blades.
Another object of this invention is to provide a used blade receptacle including used blade removal structure.
Yet another object of this invention is to provide a used blade receptacle for containing used blades in a safe and fully enclosed manner.
A further object of this invention is to provide a receptacle for used blades including used blade removal structure and also provided with new blade support structure enabling a scalpel handle blade shank to be operatively engaged with a new blade and utilized to remove the new blade from the blade support structure through utilization of a one handed operation.
A still further object of this invention is to provide a receptacle for used blades operative to effectively remove a scalpel blade from a scalpel handle shank through utilization of a one hand operation.
A final object of this invention to be specifically enumerated herein is to provide a surgical blade dispenser and disposal apparatus in accordance with the preceding objects and which will conform to conventional forms of manufacture, be of simple construction and easy to use so as to provide a device that will be economically feasible, long lasting and relatively trouble free in operation.
These together with other objects and advantages which will become subsequentially apparent reside in the details of construction and operation as more fully hereinafter described and claimed, reference being had to the accompanying drawings forming a part hereof, wherein like numerals refer to like parts throughout.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the combined dispenser and disposal apparatus of the instant invention and illustrating one new blade magazine removably supported in one of the two magazine receiving recesses formed in the removable top of the apparatus and with a removable cover for the blade magazine illustrated in exploded position, a surgical knife handle and shank being illustrated in phantom lines in position for removable engagement with a new surgical blade;
FIG. 2 is a longitudinal vertical sectional view of the blade dispenser and disposal apparatus taken substantially upon a plane indicated by the section line 2--2 of FIG. 1 illustrating one new blade support structure of one of the new blade magazines shown in elevation and the cover of the second new blade magazine illustrated in exploded position;
FIG. 3 is a transverse vertical sectional view of the surgical blade dispenser and disposal apparatus taken substantially upon a plane indicated by the section line 3--3 of FIG. 1 and passing through the used blade receiving opening formed in the top wall of the blade dispenser and disposal apparatus;
FIG. 4 is an enlarged fragmentary vertical sectional view taken substantially upon a plane indicated by the section line 4--4 of FIG.1 illustrating the manner in which a used surgical blade is downwardly inserted into the used blade receiving opening at the beginning of a blade disposal operation;
FIG. 5 is an enlarged fragmentary vertical sectional view similar to FIG. 4 but illustrating the used blade in its initial clamped disposal position and with the surgical blade handle and support shank angularly displaced to a blade release position immediately prior to upward disengagement of the support shank from the used blade and counterclockwise angular displacement of the cam lever to a release position for gravity release of the used surgical blade down into the used blade compartment of the dispenser and disposal apparatus; and
FIG. 6 is an enlarged horizontal sectional view taken substantially upon a plane indicated by the section line 6--6 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now more specifically to the drawings the numeral 10 generally designates the surgical blade dispenser and disposal apparatus of the instant invention. The apparatus 10 includes a base 12 downwardly over which a downwardly opening cover or housing 14 is removably positionable, the base 12 including 90° angularly displaceable latches 16 for removably securing the cover or housing 14 to the base 12.
The combination of the base 12 and the housing 14 defines a hollow receptacle including a first wall 18 comprising the top wall of the housing 14 and defining a pair of upwardly opening recesses 20 in which surgical blade magazines 22 are receivable, the magazines 22 including yieldable latches 24 cooperating with extensions 26 of the recesses 20 for releasably securing the magazines 22 within the recesses 20.
The first or top wall 18 also has a vertical slot 28 formed therein defining a pair of opposite sides 30 and 31. The side 30 includes a vertical notch 32 defining a pair of laterally spaced abutments 34 extending outwardly of the outer side 36 of the first or top wall 18 with the spacing between the laterally spaced abutments 34 registered with the notch 32. The abutments 34 comprise horizontally laterally spaced vertical ridges defined on an abutment plate 38 projecting upwardly and outwardly of the outer side 36 of the first or top wall 18 and opposite side margins of the abutment plate 38 include horizontally directed and laterally spaced apart mounting flanges 40 between which a bifurcated cam lever 42 is pivotally mounted as at 44. The lever 42 is swingable between an inoperative substantially vertical position and the operative horizontal position thereof illustrated in FIGS. 2 and 5 abutted against an upwardly projecting stop pin 46 carried by and projecting upwardly from the first or top wall 18.
With attention now invited more specifically to FIGS. 1 and 3 of the drawings, it may be seen that a plurality of surgical blades 48 may be carried in each magazine 22, the blades 48 each being received in an individual upstanding and upwardly opening slot 50 defined by the corresponding magazine 22. Each surgical blade receiving slot 50 includes an enlarged portion 52 defining an area of greater width of the slot and the blade mounting shank 54 of a surgical blade handle 56 is downwardly receivable in each enlarged portion 52 along side the corresponding surgical blade 48. The surgical blades 48 are of conventional design and include a longitudinal slot 58 including greater and smaller dimension ends 60 and 62. The mounting shank 54 is conventional in design and includes narrow opposite side grooves 64, see FIG. 5, in which those portions of the corresponding blade 48 disposed on opposite sides of the small dimension end 62 of the slot 58 engage, this cooperating structure of the mounting shank 54 and blades 48 being old and well known.
Each of the magazines 22 includes a removable downwardly opening cover 68 therefor to protect the blades 48 and when a new blade 48 is required, the corresponding cover is lifted and the shank 54, supported from the handle 56, is downwardly inserted into the corresponding enlarged portion 52 with the shank 54 slightly inclined downwardly toward the blade 48 to be engaged. The free end of the shank 54 is then engaged with those portions of the blade defining the opposite sides of the small dimension end 62, which blade portions are received in the grooves 64. As downward movement of the shank 54 continues the blade 48 flexes until the upper end of the greater dimension end 60 registers with the upper end 70 of the laterally enlarged portion 72 of the shank 54 in which the grooves 64 are formed. At this point, the resiliency of the blade 48 snaps the upper end of the blade 48 into engagement with the upper side surface 76 of the mounting shank 54 above the enlarged portion 72 to thus lock the blade 48 to the mounting shank 54. Thereafter, the handle 56 is upwardly displaced to withdraw the mounting shank 54 and the attached new blade 48 from the associated slot 50 of the magazine 22.
When it is desired, on the other hand, to remove a used blade 48 from the mounting shank 54, the handle 56 is used to insert the mounting shank 54 and the used blade 48 down into the slot 28. The initial positioning of the shank 54 and blade 48 in the slot 28 is illustrated in FIG. 4 of the drawings with the lever 42 in the position thereof illustrated in FIG. 4 and the laterally enlarged portion 72 of the shank 54 received in the notch 32. Thereafter, the handle 56 is further displaced downwardly from the position thereof illustrated in FIG. 4 until the lower end of the handle 56 abuts the upper end of the abutment plate 38 and/or one of the flanges 40. Thereafter, the free end of the cam lever 42 is swung downwardly from the position thereof illustrated in FIG. 4 toward the position illustrated in FIG. 5 in order to tightly clamp the blade 48 against the abutments 34, the cam end of the lever 42 being bifurcated to include bifurcations 80 and 82, see FIG. 1, which bifurcations are registered with the abutments 34 with the spacing between the bifurcations 80 and 82 being registered with the notch 32.
The pivoted end of the lever 42 thus tightly clamps those portions of the blade 48 on opposite sides of the small dimension end 62 of the slot 58 against the abutments 34. At this point, the handle 56 is laterally displaced to the right as viewed in FIG. 4 to generally the position thereof illustrated in FIG. 5, whereupon the lower end of the blade 48 is flexed and the upper end of the enlarged portion 72 is laterally displaced outwardly of the greater dimension end 60 of the slot 58. Thereafter, an upward force is applied to the handle 56 in order to upwardly withdraw the latter and thus the lower end portion of the slotted enlarged portion 72 upwardly from engagement with the blade 48. This of course completely disengages the mounting shank 54 from the used blade 48. After upward withdrawal of the mounting shank 54 from the slot 28 has been completed, the free end of the lever 42 may be swung upwardly from the position thereof illustrated in FIG. 5 to the position illustrated in FIG. 4 whereupon the used blade 48 projecting through the slot 28 will be released for falling by gravity downwardly through the slot 28 and into the used blade receiving chamber 86 defined within the interior of the housing 14.
Of course, if a new blade 48 is desired on the shank 54, a new blade from the magazine 22 is selected and the mounting shank 54 is engaged therewith in the manner hereinabove set forth.
The underside of the base 12 is provided with resilient feet 88 for support from any suitable supporting surface and, if desired, such supporting surface may include suction cups (or suction cups may be provided on the bottom of the base 12) for releasably securely fastening the base 12 to a suitable support surface. In this case, the mounting of a new blade on the mounting shank 54 may be accomplished by a one hand operation and the removal of a used blade 48 from the mounting shank 54 also may be accomplished through utilization of a one handed operation. Such operation will of course be of great benefit to a single person conducting an autopsy.
The foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes readily will occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and, accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A hollow housing is provided including a top wall defining at least one upwardly opening new blade magazine receiving recess therein and a vertical slot therethrough. The housing top wall further includes a pivoted cam lever closely adjacent the slot and by which a surgical blade releasably mounted from a surgical blade support shank may be stationarily clamped relative to the top wall to enable one handed manipulation of the support shank in a manner to disengage the latter from the surgical blade.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation application of PCT Application No. PCT/CN2016/089992 filed on Jul. 14, 2016, the entire contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to fields of clinical application of nerve defect repair and the medical three-dimensional (3D) printing technology, and in particular provides an integrated visualization method for three-dimensional reconstruction of internal fascicular structure of human peripheral nerves.
BACKGROUND OF THE INVENTION
[0003] The primary function of peripheral nerves is to connect the central nervous system with target organs, and also play a role of conveying information. Peripheral nerves contain internal nerve fascicles, the internal nerve fascicles of peripheral nerves can be divided into sensory fascicles, motion fascicles and mixed fascicles. The primary functions of these nerve fascicles are to afferent and efferent information. It is well known that the most optimal repair methods in clinical is to achieve anastomosis between functional fascicles once an injury or defect of human peripheral nerves occurs. However, since the anatomical structure of human peripheral nerve fascicles is quite complicated, a precondition for clinicians is understanding of the anatomical structure law and morphology of fascicular type of human peripheral nerves in order to achieve a goal of anastomosis between functional fascicles. A visualization model of internal fascicular structure obtained for reconstruction of human peripheral nerve three-dimensional structure is expected to provide an effective method for improving the functional recovery after peripheral nerve defect.
[0004] On the other hand, three-dimensional reconstruction of human peripheral nerve fascicles also holds a more far-reaching significance, with the development of modern bio-manufacturing technology, biomimetic manufacture of many tissues and organs has already been achieved. But it is very difficult to achieve the biomimetic manufacture of peripheral nerves, the reasons are chiefly as follows: {circle around (1)} the internal structure of nerves is complicated and fine, the required precision cannot be achieved using the existing bio-manufacturing methods; {circle around (2)} each piece of, and even each segment of nerve fascicle has its own corresponding biological functions, which have not been fully understood for the present. The visualization model of three-dimensional reconstruction of peripheral nerve fascicles will solve the above problems being faced during bio-manufacturing of peripheral nerve biomaterials, namely to achieve a standard of precision medicine.
[0005] In terms of three-dimensional reconstruction of peripheral nerve fascicles, many scholars have done a lot of research, for example, understanding of three-dimensional anatomical structure of human nerve fascicles by Sunderland has undergone the following process: it was initially regarded as frequently crossing on the same plane, whereas at present it is observed that vascular network is formed at its proximal end, and at its distal end fascicles are frequently mixed or divided into several small fascicles. Jian Qi et al. reconstructed a three-dimensional structure of the median nerve using the histological section method on peripheral nerves, at the same time they also found the complexity in configuration of nerve fascicles. However, all these methods of reconstructing three-dimensional anatomical structure of peripheral nerve fascicles have their own disadvantages, such as inadequate precision in acquiring two-dimensional structure, bad matching in the course of reconstruction, image distortion and involvement of abundant anthropic factors. Therefore, it is quite necessary to seek a simple and effective technical method which is capable of capturing two-dimensional images with high resolution and simultaneously achieving a successive matching at the three-dimensional level.
[0006] With the development of modern technology, computed tomography (CT) and magnetic resonance imaging (MRI) have become the major imaging means for three-dimensional reconstruction. But because the internal structure of peripheral nerves are relative fine, such scanning precision cannot be achieved using the existing MRI. Therefore, it is urgent currently to find a method to construct a visualization model for internal fascicles structure of human peripheral nerves and to implement a three-dimensional reconstruction of human peripheral nerves.
SUMMARY OF THE INVENTION
[0007] In order to solve the above problems, and construct a visualization model for internal fascicular structure of human peripheral nerves, the present invention performs a scan on the pretreated specimens of human peripheral nerves using Micro CT to acquire the most excellent, biomimetic and lossless two-dimensional images, followed by automatic segmentation on nerve fascicles, and quickly executes the three-dimensional reconstruction using powerful computer processing systems.
[0008] The present invention provides a constructing method for visualization models of human peripheral nerve fascicles, comprising the following steps of:
[0009] obtaining human peripheral nerves, staining with an iodine preparation and combination with freeze-drying;
[0010] scanning the stained peripheral nerves by using Micro CT to acquire two-dimensional lossless images, and performing binarization processing of the two-dimensional images to acquire segmented images of nerve fascicles;
[0011] reconstructing the segmented images into visualization models.
[0012] The present invention also provides a method for three-dimensional reconstruction of human peripheral nerves, comprising the following steps of:
[0013] obtaining human peripheral nerves, staining with an iodine preparation in combination with freeze-drying;
[0014] scanning the stained peripheral nerves by using Micro CT to acquire two-dimensional lossless images, and performing binarization processing of the two-dimensional images to acquire segmented images of nerve fascicles;
[0015] reconstructing the segmented images into visualization models.
[0016] The present invention has the following beneficial effects: 1. The invention performs a scan on the pretreated specimens of human peripheral nerves using Micro CT, enabling the accuracy to meet the requirements of reconstructing nerve fascicles. The technology for pretreating specimens can also be used for other soft tissues to achieve two-dimensional lossless images with high resolution; 2. Three-dimensional visualization models of peripheral nerve fascicles are able to provide the stereoscopic anatomical atlas required for interfascicular nerve anastomosis in clinical practice; 3. The invention will lay the technical foundation for visualization processing of massive medical pictures by using a supercomputer; 4. The invention will create templates for bio-manufactured neurobiological materials to achieve a goal of precise repair; 5. Different from the prior art in which nerve specimens require section processing, the method provided in the present invention has no any damage to specimens, which can be used in living bodies; 6. In the prior art, the acquired images by using microscope photography have some disadvantages, such as image distortion, requirement of processing by human intervention, and involvement of abundant anthropic factors, whereas the method provided in the present invention is able to acquire lossless two-dimensional images with high resolution, and in the meanwhile achieves a successive matching at the three-dimensional level, it is easy to operate and the results are more accurate.
BRIEF DESCRIPTION OF DRAWINGS
[0017] FIG. 1 shows a flowchart of the preparation method for visualization models of internal fascicular type of human peripheral nerves according to an embodiment of the present invention;
[0018] FIGS. 2A to 2D show Micro CT scanned images of peripheral nerve structures acquired after different pretreatment ways, wherein FIG. 2A shows the image of a fresh nerve without any treatment, FIG. 2B shows the image of the fresh nerve after treatment with a freeze-drying method, FIG. 2C shows the image of a nerve specimen after treatment of just adding an iodine preparation, FIG. 2D shows the image of a nerve specimens after adding an iodine preparation followed by freeze-drying;
[0019] FIGS. 3A to 3C show Micro CT images of the specimens after staining by adding an iodine preparation followed by freeze-drying to remove moisture, wherein FIG. 3A shows the two-dimensional planar image of peripheral nerve, FIG. 3B shows the image of nerve fascicle, and FIG. 3C shows the image of endoneurium; FIGS. 4A-4C show generally morphological changes in the course of pretreatment on peripheral nerve specimens, wherein FIG. 4A shows the fresh nerve, FIG. 4B shows the nerve stained with the iodine preparation, and FIG. 4C shows the nerve stained with the iodine preparation and followed by freeze-drying;
[0020] FIGS. 5A-5D show automatic segmentation process of peripheral nerve fascicles, wherein FIG. 5A shows the original image, FIG. 5B shows the textural features of the extracted region of interest, FIG. 5C shows automatically extracted profile of nerve fascicles based on textural features, and FIG. 5D shows the extracted nerve fascicles after the region of interest is merged;
[0021] FIGS. 6A-6D show views after three-dimensional visualization reconstruction of peripheral nerve fascicles, wherein FIG. 6A shows the reconstruction performance after 1500 pictures are combined together, FIG. 6B shows the amplified reconstruction performance after 1500 pictures are combined together, FIG. 6C shows the reconstruction performance of endoneurium, and FIG. 6D shows the reconstruction performance after 7248 pictures are combined together.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0022] In order to make the technical problems to be solved, technical solutions and advantages of the present invention clearer, the content of the invention will now be described in more detail with reference to figures and embodiments below. It should be understood that the specific embodiments described herein are only for purpose of illustration and not to be construed as limitations of the present invention.
[0023] The embodiment of the present invention provides a method for internal fascicular structure visualization of human peripheral nerves used in the course of three-dimensional reconstruction of human peripheral nerves, refer to FIG. 1 which shows the main process flows of the method in the present invention. As shown in FIG. 1 , the method comprises the following steps:
[0024] A constructing method for visualization models of human peripheral nerve fascicles, comprising the following steps of:
[0025] obtaining human peripheral nerves, staining with an iodine preparation in combination with freeze-drying;
[0026] scanning the stained peripheral nerves by using Micro CT to acquire lossless two-dimensional images, and performing binarization processing of the two-dimensional images to acquire segmented images of nerve fascicles;
[0027] reconstructing the segmented images into visualization models.
[0028] In the prior art, it is general to perform a scan immediately after staining, and the obtained images in this way have a poor quality in performance. After freeze-drying to remove moisture, the contrast ratio of the scanned images is increased.
[0029] Specifically, the method of the present invention comprises the following specific steps:
[0030] (1) performing a pretreatment on the fresh isolated human peripheral nerves, making them satisfy the conditions of two-dimensional lossless images with high resolution by Micro CT scanning;
[0031] (2) obtaining the optimal parameters for scanning the pretreated specimens of peripheral nerves to achieve two-dimensional images with high resolution, by adjusting scanning parameters of Micro CT;
[0032] (3) conducting image segmentation based on diverse grayscale difference and internal structure features of nerve images acquired by scanning, and developing a mathematical algorithm suitable for segmentation on peripheral nerve fascicles using integrative classic mathematical formulas;
[0033] (4) with regard to the massive segmented pictures of nerve fascicles, performing three-dimensional reconstruction of visualization models of peripheral nerve fascicles by using supercomputers with powerful computing and processing capacities.
[0034] FIGS. 2A to 2D show different images of peripheral nerve structures acquired by Micro CT scanning after undergoing different pretreatment ways, wherein FIG. 2A refers to the image of fresh nerve, without any treatment (FN); FIG. 2B refers to the image of fresh nerve after treatment with a freeze-drying method (FDN); FIG. 2C refers to the image just adding an iodine preparation (IN); FIG. 2D refers to the image after adding an iodine preparation followed by freeze-drying (IFDN).
[0035] Preferably, human peripheral nerves are fixed with a fixing agent before staining with the iodine preparation, and preferably, the fixing agent is 3.5%-4.5% paraformaldehyde solution, or 9%-11% glutaraldehyde solution.
[0036] According to the specific embodiment, the iodine preparation is 40%-50% iodine solution, namely the aqueous solution of iodine, which can be self-prepared or purchased from the market.
[0037] Preferably, the specimens of human peripheral nerves are wrapped with tinfoil and placed in liquid nitrogen for quick-freezing before the freeze-drying process, in order to prevent specimen morphology from being changed and in turn to avoid affecting the subsequent scanning imaging treatment.
[0038] Specifically, the specimens of human peripheral nerves are wrapped with tinfoil, placed in liquid nitrogen and frozen for 0.5-2 minutes.
[0039] FIGS. 3A-3C show Micro CT images after the specimens being freeze-drying to remove moisture before which the specimens have been stained by adding the iodine preparation, wherein FIG. 3A refers to the two-dimensional planar image of peripheral nerve; FIG. 3B refers to the image of nerve fascicle; FIG. 3C refers to the image of endoneurium.
[0040] Specifically, the specimens of peripheral nerves are placed in the freeze-dryer at a temperature of −80° C. to remove moisture during freeze-drying. The removal of moisture is extremely important for the subsequent scanning. If the moisture is removed insufficiently, the scanning effect will decrease significantly.
[0041] FIGS. 4A-4C show the generally morphological changes of the peripheral nerve in the course of pretreatment, wherein FIG. 4A refers to the fresh nerve (FN); FIG. 4B refers to the nerve stained with the iodine preparation (IN); FIG. 4C refers to the nerve stained with the iodine preparation and followed by freeze-drying (IFDN).
[0042] In the present invention, the reconstruction of three-dimensional anatomical structure of peripheral nerve fascicles is realized by Micro CT. The advantages of Micro CT imaging is the resolution of imaging is pretty high, and the ultrastructure of tissues, namely within 10 μm, can be distinguished from the acquired images, which can even be used to analyze the mechanical properties of tissue scaffolds, thereby helping to improve the design and manufacture of ultrastructure of the scaffolds. According to reports from the existing literature, the disadvantages reside in the fact that the main principle of imaging is relied on attenuation ratio after X-rays penetrate different tissues, as a result, soft tissues with the same density cannot be differentiated. In theory, such properties are more suitable for reconstruction of hard tissues, accordingly it is quite convenient for Micro CT to be used in bone tissue imaging, whereas difficult in soft tissues, especially peripheral nerves, due to the almost same density in soft tissues and lack of contrast, resulting in a failure of imaging. In order to achieve an imaging goal in soft tissues using Micro CT, addition of contrast agent is the main solution, such as injection of contrast agents into knee joints and lungs, which have already been realized.
[0043] So far there has been no report on three-dimensional reconstruction of soft tissues using Micro CT, while in the present invention, staining with an iodine preparation is adopted to increase the contrast ratio when Micro CT scans peripheral nerve structures, achieving better effects.
[0044] On the other hand, in order to acquire peripheral nerve images with high resolution by using Micro CT, it is not enough to just use a method of adding staining agents. Inventors of the present invention also find that moisture has a huge impact on transmission of X-rays after analyzing the conditions of Micro CT scanning and making improvements to them, therefore, in order to acquire images with high resolution, we utilize the best method for keeping morphology, namely freeze-drying method, to remove the moisture of nerve specimens, and simultaneously in combination with an adjustment to Micro CT parameters. In the experiments, lossless two-dimensional images are first acquired by integrating the two techniques, from which the entire internal structures of peripheral nerves can be observed.
[0045] Specifically, in terms of parameter adjustment, the diameter of visual field, namely the inner diameter of scanning tube, is set to 9 mm, in the meanwhile the voxel size is set to 3 μm. If the voxel value is set too high, the scanning accuracy will be decreased, while the voxel value is less than 3 μm, which will result in overloaded operation of the scanner, it is quite possible that the scanning will not be completed in case of interference from other environmental factors.
[0046] In order to construct a set of entire three-dimensional visualization models of peripheral nerve fascicles, the acquirement of two-dimensional images with high resolution is regarded as a basis and the most important tache. To achieve the goal of biomimetic three-dimensional reconstruction, the smaller the distance between two-dimensional images is, the better, thus, such three-dimensional reconstruction becomes more accurate, and the matching between images gets better. For this purpose, in the experiments, the selected interlayer space between two-dimensional images is 3 μm, that is to say, the voxel size is 3 μm, which can meet the requirements of three-dimensional reconstruction, however, the resulted huge picture information cannot be managed by the existing software for three-dimensional reconstruction, and the segmentation between nerve fascicles and connective tissues cannot reach the perfect segmentation by using the existing software, for this purpose we have independently developed a set of mathematical algorithms used for automatic segmentation on peripheral nerve fascicles and reconstruction of them, which are compatible with the environments generated by supercomputers, thereby achieving a goal of automatic and rapid acquisition of visualization biomimetic three-dimensional models of peripheral nerve fascicles.
[0047] FIGS. 5A-5D show the automatic segmentation process of peripheral nerve fascicles, wherein FIG. 5A is the original image; FIG. 5B indicates the textural features of the extracted region of interest; FIG. 5C refers to automatically extracted profile of nerve fascicles based on textural features; FIG. 5D refers to the extracted nerve fascicles after the region of interest is merged.
[0048] FIGS. 6A-6D show views resulted from three-dimensional visualization reconstruction of peripheral nerve fascicles, wherein FIG. 6A refers to the reconstruction performance after 1500 pictures are combined together; FIG. 6B refers to the amplified reconstruction performance after 1500 pictures are combined together; FIG. 6C shows the reconstruction performance of endoneurium; FIG. 6D shows the reconstruction performance after 7248 pictures are combined together.
[0049] Under the circumstances of the preferred parameter settings, it needs a longer cycle to scan images by using Micro CT, from a dozen hours to dozens of hours, as a result, slight changes of environmental factors in the machine will influence the scanning outcome, especially moisture variation in the environment. In order to avoid the influence of moisture, peripheral nerve specimens can be placed in preservative films or preservation bags to insulate moisture during scanning, and meanwhile preservative films or preservation bags have not any adverse impact on scanning performance.
[0050] Specifically, during acquiring the segmented images of nerve fascicles, auto-adaptable topological variations are mainly utilized to acquire the profile of nerve fascicles, without a need to provide the initial profile and central point in advance, and the computation will be quickly completed by the system at the computing center.
[0051] According to an embodiment, the length of the peripheral nerve specimen is 2.1 cm, and the interlayer spacing space between two adjacent pictures is 3 μm, 3 μm*7000=2.1 cm, consequently the number of acquired pictures by scanning is 7000; DICOM (Digital Imaging and Communications in Medicine) files for so many such pictures occupy a capacity of 63 Gigabytes (G), and conventional workstations are not capable of managing such huge pictures. Supercomputers are used to accomplish the picture processing in the present invention. Performing a three-dimensional rendering will take 10 hours when using a conventional computer, while it takes only 10 min to perform a three-dimensional rendering when using a supercomputer. In the meanwhile, the constructing method of the invention can also be used in big data applications.
[0052] Furthermore, the present invention also provides a method for three-dimensional reconstruction of human peripheral nerves, which includes the above-mentioned constructing method for visualization models of human peripheral nerve fascicles.
[0053] The present invention will now be further illustrated by way of embodiments below.
Embodiment 1
[0054] Step 1: Obtaining Human Peripheral Nerves, and Performing a Corresponding Pretreatment on them.
[0055] Obtaining human peripheral nerves, removing fat and connective tissues around nerves under the microscope, followed by fixing in 4% paraformaldehyde solution for 4 days. Cutting them into small segments of about 2 cm length. At room temperature, soaking the dissected nerve tissues into 40%-50% iodine solution (aqueous solution of iodine, Lugol's iodine solution Sigma-Aldrich, St. Louis, USA) followed by oscillation treatment for 2 days, the staining is judged successful until the color changes from milky white to brown.
[0056] Wrapping the iodine preparation stained specimens of peripheral nerves with tinfoil and placing them into liquid nitrogen for quick-freezing, then taking the specimens out of liquid nitrogen and placing them in freeze-dryer for thermostatic drying at a temperature of −80° C. for 3 days to remove moisture, and putting them in the airtight and dry container to be stored for use later.
[0057] Step 2: Scanning the Pretreated Human Peripheral Nerves by Using Micro CT.
[0058] Scanning the above-mentioned peripheral nerve specimens obtained from Step 1 by using a Scanco μCT50 from Scanco Medical AG, Switzerland, and setting the scanner in accordance with the following scanning parameters:
[0059] Visual scanning field of Micro CT: 9 mm;
[0060] Energy/current intensity: 55 kVp, 72 μA, 6 W
[0061] Filtration: 0.1 mm Al
[0062] Calibration: 55 kVp, 0.1 mm Al, BH: organic glass (PMMA board)
[0063] Integration time: 1500 ms
[0064] Average data: 3
[0065] Diameter of visual field: 9 mm
[0066] Voxel size: 3 μm
[0067] Specimens: 3400
[0068] Projection/180°: 1500.
[0069] Step 3: Extracting Nerve Fascicles from the Original Image by Using Segmentation Formulas.
[0070] Drawing the gray histogram based on original two-dimensional images acquired by Micro CT scanning, obtaining the reasonable binarization threshold after computation and performing binarization processing of images. Acquiring the profile of nerve fascicles by extracting the information of textural features from binary images and differentiating between internal and external regions of nerve fascicles. Obtaining the segmented images of nerve fascicles by filtering out the information outside the profile on the binary images in view of the acquired the profile.
[0071] Step 4: Forming a Visualization Model of Nerve Fascicles Based on Three-Dimensional Reconstruction of the Segmented Two-Dimensional Images.
[0072] The method of the present invention performs volume rendering mainly by using VTK, and obtains three-dimensional visualization models of nerve fascicles by multi-node parallel computing under the Linux environment provided by a supercomputer, moreover, the method considerably shortens the duration required for volume rendering of big data.
[0073] The above descriptions are just preferred embodiments of the invention, not for the purpose of limiting the invention, and any modification, equivalent substitution or improvement within the spirit and principles of the invention, should be included in the scope of protection of the present invention.
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The present invention relates to fields of clinical application of nerve defect repair and the medical three-dimensional (3D) printing technology, and provides an integrated visualization method for three-dimensional (3D) reconstruction of internal structure of human peripheral nerves. The method comprises the following steps: obtaining human peripheral nerves, preparing nerve specimens ex vivo by staining with an iodine preparation in combination with a freeze-drying method; scanning the pretreated peripheral nerves using Micro CT to acquire lossless two-dimensional images, and performing binarization processing to the two-dimensional images, then conducting image segmentation based on textural features to acquire images of nerve fascicles; finally, reconstructing the segmented images into a visualization model by using a supercomputer.
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This is a continuation application from application Ser. No. 670,340 filed Nov. 9, 1984, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus for controlling the speed of an internal combustion engine vehicle, and more particularly to a vehicle speed control apparatus for an internal combustion engine vehicle in which switching between a manual vehicle speed controlling mode and an automatic vehicle speed controlling mode by means of an automatic vehicle speed controlling device can be smoothly carried out.
2. Description of the Prior Art
Automatic vehicle speed controlling devices have been widely used for the purpose of automatically maintaining the speed of vehicles driven by internal combustion engines, such as diesel engines, gasoline engines and the like at a desired speed. In the internal combustion engine vehicle equipped with such an automatic vehicle speed controlling device, the desired amount of fuel supply corresponding to the amount of depression of an accelerator pedal and the amount of fuel supply required for maintaining the vehicle speed at a desired speed are separately calculated. Then, the larger of the two amounts of fuel supply is selected aand the engine speed is controlled in accordance with control data showing the selected amount of fuel supply.
Therefore, in the conventional automatic vehicle speed controlling device when, for example, the accelerator pedal is deeply depressed at a time when the amount of fuel supply calculated in accordance with the degree of depression of the acceleration pedal is smaller than that calculated by the automatic vehicle speed controlling device because the accelerator pedal has been in the released condition up to that time, the amount of fuel supply calculated in accordance with the degree of the depression of the accelerator pedal increases beyond the amount of fuel supply calculated by the automatic vehicle speed controlling device, so that the vehicle speed is controlled in accordance with the degree of depression of the accelerator pedal.
In addition, in the conventional automatic vehicle speed controlling device, when the vehicle speed controlling state is switched to the mode of control by operation of the accelerator pedal, the amount of fuel supply calculated by the automatic vehicle speed controlling device becomes zero and control of vehicle speed by the automatic vehicle speed controlling device is discontinued until, for example, a predetermined switch is depressed. Such an automatic vehicle speed controlling device is disclosed in, for example, U.S. Pat. No. 4,337,511.
In such a device, the amount of the fuel supply calculated by the automatic vehicle speed controlling device returns to the previous value, when the predetermined switch is depressed after the vehicle speed control mode is changed from control by the automatic vehicle speed controlling device to that by the accelerator pedal, and the accelerator pedal is released. Therefore, especially when the accelerator pedal is released suddenly, there is the disadvantage that the vehicle rapidly decelerates for a moment just after changing to the automatic vehicle speed control mode so that the vehicle does not travel smoothly. This condition will occur in a vehicle driven by any kind of internal combustion engine.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved apparatus for controlling the speed of an internal combustion engine vehicle.
It is an object of the present invention to provide an apparatus for controlling the speed of an internal combustion engine vehicle, which can prevent a rapid change in the state of vehicle speed control at the time of switching over between vehicle speed control carried out by the operation of the accelerator pedal and that carried out by an automatic vehicle speed controlling device, thereby realizing smooth vehicle speed control.
According to the present invention, in a vehicle speed control apparatus for a vehicle powered by an internal combustion engine, the apparatus comprises a first detecting means for producing a vehicle speed signal indicating the actual vehicle speed at each instant, a first calculating means responsive to at least the vehicle speed signal for calculating a first data indicating a first amount of fuel supply required for maintaining the vehicle speed at a desired value, a second calculating means responsive to the operation of an accelerator pedal for calculating a second data indicating a second amount of fuel supply required for controlling the vehicle speed in accordance with the amount of operation of the accelerator pedal, a selecting means responsive to the first and second data for selecting the larger of the first and second data as control data, a comprising means responsive to the first and second data for comparing the first amount of fuel supply with the second amount of fuel supply, and a modifying means responsive to the result of the comparison by the comparing means for modifying the output data from the first calculating means to cause it to slowly change, taking into account the value of the second data just before the second amount of fuel supply becomes smaller than the first amount of the fuel supply, whereby the vehicle speed is prevented from being rapidly decelerated when the mode of vehicle speed control is changed from that by the second data to that by the first data.
With the arrangement described above, when the mode of vehicle speed control once switched over from that by the automatic vehicle speed controlling device to that in response to the operation of the accelerator pedal returns to the mode controlled by the automatic vehicle speed controlling device, and the accelerator pedal is thereafter released, the value of the firt data is gradually lowered from the value of the second data just before the accelerator pedal is released to the value showing the amount of fuel supply necessary for the keeping the desired constant speed of the vehicle.
As a result, a sudden change in the control data can be prevented and the vehicle speed can be prevented from suddenly changing at the time of changing over between vehicle speed control carried out by the accelerator pedal and that by the automatic vehicle speed controlling device, to obtain smooth control of the vehicle speed.
The invention will be better understood and the other objects and advantages thereof will be more apparent from the following detailed description of a preferred embodiment with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of an embodiment of a vehicle speed controlling system in accordance with the present invention for use in a vehicle driven by a diesel engine,
FIG. 2 is a graph showing the relationship among various signals over the course of time during the operation of the vehicle speed controlling system of FIG. 1,
FIG. 3 is a graph showing the change in vehicle speed corresponding to the operation of the vehicle speed controlling system of FIG. 1 as illustrated in FIG. 2,
FIG. 4 is a flow chart of a program to be executed by a microcomputer used as the data modifying circuit of the vehicle speed controlling system of FIG. 1,
FIG. 5 is a block diagram of a second embodiment of a vehicle speed controlling system in accordance with the present invention,
FIG. 6 is a flow chart of a program to be executed by the central processing unit of the vehicle speed controlling system of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a block diagram of an embodiment of a vehicle speed controlling system in accordance with the present invention as applied to a vehicle driven by a diesel engine. The vehicle speed controlling apparatus denoted by reference numeral 1 controls the speed of a vehicle (not shown) driven by a diesel engine 2 by regulating the position of a control rack 4 of a fuel injection pump 3 for supplying fuel to the diesel engine 2. The vehicle speed controlling apparatus 1 has a first calculating circuit 6 for calculating a first data DQ 1 showing a first amount of fuel supply Q 1 necessary for maintaining the vehicle speed at a desired target speed in response to vehicle speed data DV which is produced by a vehicle speed detector 5 and is indicative of the vehicle speed at each instant, and a second calculating circuit 8 for calculating a second data DQ 2 showing a second amount of fuel supply Q 2 necessary for controlling the vehicle speed in accordance with the amount of operation of an accelerator pedal 7 at each instant.
The accelerator pedal 7 is connected with an acceleration detector 9 which produces acceleration data DA showing the amount of depression of the accelerator pedal 7. Acceleration data DA and an engine speed signal DE produced by an engine speed detector 10 and indicative of the speed of the diesel engine 2 are applied to the second calculating circuit 8, in which the second amount of the fuel supply Q 2 required for controlling the vehicle speed in accordance with the amount of operation of the accelerator pedal 7 at each instant is calculated. Data showing the calculated result is produced as the second data DQ 2 and is applied to a data selector 11.
The first calculating circuit 6, in cooperation with a control signal generator 12, constitutes a so-called cruise control device which controls the vehicle speed to maintain it at the desired level. The first calculating circuit 6 has a normaly closed type switch 14 which is closed when a set switch 13 is ON and a memory 15 connected through the switch 14 with the vehicle speed detector 5. Vehicle speed data DV at the time the once closed switch 14 is opened is stored as target vehicle speed data DV 0 in the memory 15, and the target vehicle speed data DV 0 stored in the memory 15 is applied to a computing circuit 16 to which vehicle speed data DV is input. The first amount of fuel supply Q 1 necessary for maintaining the actual vehicle speed at the target vehicle speed indicated by target vehicle speed data DV 0 is calculated by the computing circuit 16 and data showing the calculated result is produced as the first data DQ 1 which is applied through a switch 17 to a data modifying circuit 18.
The switch 17 is arranged to close when the level of an output line 12a is high and to open when the level thereof is low. In addition to the set switch 13, a resume switch 19, a brake switch 20 which is turned ON when a brake pedal (not shown) is depressed, a clutch switch 21 which is turned ON when the vehicle clutch is disengaged and a neutral switch 22 which is turned ON when the vehicle transmission is shifted into neutral position are connected to the control signal generator 12. The control signal generator 12 changes the level of the output line 12a from low to high when the set switch 13 is turned ON and latches the high-level state. The control signal generator 12 releases the latched high-level state of the output line 12a when at least one of switches 20, 21 and 22 is turned ON and holds the low-level state of the output line 12a. Furthermore, the control signal generator 12 has a function of changing the level of the output line 12a from low to high and holding its high-level state when the switch 19 is closed after the high-level state of the output line 12a is released as described above. A control signal generator having such functions is known in the prior art.
As a result of this arrangement, the switch 17 is closed when the set switch 13 or the resume switch 19 has operated, and the first data DQ 1 is applied to the data modifying circuit 18. On the other hand, when any one of the switches 20 to 22 is turned ON to open the switch 17, the first data DQ 1 is prevented from being applied to the data modifying circuit 18.
The data modifying circuit 18 has a memory 25 to which the second data DQ 2 is applied through a normally open type switch 24 and clock pulses TP from a clock pulse generator 26 are applied as read-in timing pulses for the memory 25. Consequently, when the switch 24 is closed as described hereinafter, the second data DQ 2 is read into the memory 25 at predetermined intervals in response to the output of the clock pulses TP. Data DM read from the memory 25 is applied through a switch 27 to an input terminal 28b of a data processing circuit 28, to another input terminal 28a of which the first data DQ 1 is applied.
The data processing circuit 28 is a circuit for processing the data applied to the input terminal 28a in such a way that the value of output data DI is gradually changed at a predetermined rate from the value of the data applied to the input terminal 28b at that time to the value of the data applied to the input terminal 28a. This data processing may be carried out in the analog form or in the digital form, or be carried out by the use of a microcomputer.
FIG. 4 shows the flow chart of a program executed when a microcomputer is used for the data processing circuit 28. Execution of the program starts in response to the closing of the switch 27 to apply data MD to the input terminal 28b. Data DM is first read in in step 101, whereafter it is discriminated whether or not data DM is larger than first data DQ 1 in step 102. Step 103 is executed when the discriminated result in step 102 is NO, whereby the content of data DI is replaced by first data DQ 1 and data DI is output. Then, the execution of the program is terminated.
When the discriminated result in step 102 is YES, the computation for gradually changing data DM to data DQ 1 at that time is executed in the following steps. Namely, the content of data DM is replaced by the result obtained by subtracting a predetermined value ΔQ from data DM in step 104, and the replaced data DM is output as output data DI (steps 105 and 106). Then, it is discriminated whether or not output data DI is less than first data DQ 1 (step 107) and steps 104 to 106 are executed repetitively until data DI is less than first data DQ 1 . When data DI becomes less than DQ 1 , the content of output data DI is replaced by first data DQ 1 (step 103), and then the execution of the program is terminated.
As a result, after the switch 27 is closed, output data DI is gradually decreased from data DM at the time the switch 27 is closed until it reaches the value of first data DQ 1 .
Output data DI is provided to one fixed contact of the selecting switch 23, and first data DQ1 is provided to the other fixed contact as shown in FIG. 1, so that the first data DQ 1 is derived from the selecting switch 23 when the selecting switch 23 is switched over as shown by the solid line in FIG. 1 and is supplied to the data selector 11 and a comparator 29. On the other hand, when the selecting switch 23 is switched over as shown by the broken line of FIG. 1, output data DI is derived from the selecting switch 23 and is supplied to the data selector 11 and the comparator 29.
The data selector 11 is a circuit for selecting and outputting the larger of the two input data. The data selected by the data selector 11 is derived as output data DS and the output data DS is applied to a driving circuit 30, in which the position of the control rack 4 necessary for obtaining the amount of fuel injected shown by output data DS is computed and produces a driving signal SD to be supplied to an actuator 31 in order to position the control rack 4 at the computed position. The driving signal SD is applied to an actuator 31 which is connected to the control rack 4 for actuating the control rack 4.
On the other hand, the comparator 29 compares the magnitude of the two input data, and the level of the output line 29a of the comparator 29 is changed from low to high when the second data DQ 2 becomes more than the data from the data modifying circuit 18. When the second data DQ 2 becomes equal to or les than the data from the data modifying circuit 18, the level of the output line 29a is changed from high to low.
The output line 29a is connected to the switch 24, which is closed when the level of the output line 29a becomes high to provide the second data DQ 2 to the memory 25. The output line 29a is also connected to a timer 32 which is triggered to start operation when the level of the output line 29a is changed from high to low. Then, the level of the output line 32a becomes high during a predetermined time period T 0 . The output line 32a of the timer 32 is connected to the switches 23 and 27. The switch 23 is switched over as shown by the solid line of FIG. 1 when the level of the output line 32a is low, while the switch 23 is switched over as shown by the broken line of FIG. 1 when the level of the output line 32a is high. That is, the switch 23 is switched over to the state as shown by the broken line of FIG. 1 during the time period T 0 when the level of the output line 29 a is changed from high to low. The output line 32a is also connected to the clock pulse generator 26 which is arranged so as to stop the outputting of the clock pulses TP only when the level of the output line 32a is high.
The operation of the apparatus shown in FIG. 1 will now be described hereinafter with reference to FIGS. 2 and 3.
Description is made of the operation from before automatic vehicle speed control is initiated from time t 1 . Assume that the accelerator pedal 7 is released and the first data DQ 1 necessary for automatically controlling the vehicle speed is produced by the first calculating circuit 6 to automatically control the vehicle speed and maintain it at the target speed indicated by the target vehicle speed data DV 0 . In this case, the first data DQ 1 is larger than the second data DQ 2 since the amount Q 1 is larger than Q 2 , and the level of the output line 29a of the comparator 29 is low, so that the switch 24 is OFF. Since the output line 32a of the timer 32 is at low level at this time, the switch 27 is OFF and the switch 23 is switched over as shown by the solid line of FIG. 1. Therefore, the first data DQ 1 from the first calculating circuit 6 is derived through the switch 23 and is applied to the data selector 11 and the comparator 29.
Since the amount Q 1 is larger than the amount Q 2 as described above, the first data DQ 1 is selected as output data DS by the data selector 11 and output data DS is applied to the driving circuit 30. Consequently, the vehicle speed is controlled in accordance with the first data DQ 1 and the adjustment of the amount of fuel injected is performed in order to maintain the vehicle speed at the desired target speed.
When the accelerator pedal 7 is depressed at t 1 , the second amount of fuel supply Q 2 increases in proportion to the amount of depression of the accelerator pedal 7. As a result, the value of the second data DQ 2 increases and the second data DQ 2 is selected instead of the output of data modifying circuit 18 by the data selector 11 when the second data DQ 2 becomes more than the first data DQ 1 at time t 2 . As a result, the value of the first data DQ 1 decreases after time t 2 , while the value of the output data DS changes to the value of the second data DQ 2 .
When the second data DQ 2 becomes larger than the first data DQ 1 at time t 2 , since the comparator 29 also operates and the level of the output line 29a becomes high, the switch 24 is closed. The clock pulses TP are being output since the level of the output line 32a is low at this time, so that the second data DQ 2 at each instant is read and stored in the memory 25 at predetermined intervals in response to the clock pulses TP.
Therefore, when the vehicle speed control is changed from the automatic mode to the manual mode, the data stored in the memory 25 is up-dated at predetermined intervals to the value of the second data DQ 2 at that instant.
When the depressed accelerator pedal 7 is released at time t 4 , the second data DQ 2 rapidly decreases and becomes zero. As a result, the level of the output line 29a of the comparator 29 is changed from high to low when the first data DQ 1 exceeds the second data DQ 2 derived from the switch 23, so that the switch 24 is closed to stop the derivation of the clock pulses TP. Therefore, it follows that the value X of the second data DQ 2 stored in memory 25 just before the level of the output line 29a of the comparator 29 changed from high to low is maintained therein and the timer 32 is triggered at the same time. As a result, the switch 27 is closed by a predetermined time period T 0 and the switch 23 is switched over as shown by the broken line in FIG. 1 by the period T 0 . Since the first calculating circuit 6 calculates the amount of fuel supply necessary for carrying out the vehicle speed control in accordance with the target vehicle speed data stored in the memory and produces the first data DQ 1 indicating the calculated result at this time, the value of the first data DQ 1 rapidly increases after time t 4 and returns to the value Y which is the value before time t 2 . As a result, the first data DQ 1 , namely Y, and data DM, namely X, are input into the data processing circuit 28. The data DI derived from the data processing circuit 28 is decreased from value X to value Y at a predetermined rate after time t 4 .
That is, even when the second data DQ 2 becomes approximately zero at time t 4 and the first data DQ 1 returns from approximately zero to the previous value Y, the operation of the data processing circuit 28 assures that data DI, whose value gradually decreases from X toward Y, is supplied to the driving circuit 30. Consequently, sudden deceleration of the vehicle is effectively prevented even when the accelerator pedal 7 is suddenly released at time t 4 .
When the level of the output line 32a of the timer 32 changes from high to low at time t 6 after the data DS becomes coincident with the first data DQ 1 at time t 5 , the switch 27 is opened and the switch 23 is switched over as shown by the solid line of FIG. 1. Thus, the first data DQ 1 is applied through the data selector 11 the driving circuit 30.
As a result, the output data DS changes as shown in FIG. 2. Consequently, as shown in FIG. 3, the vehicle speed V is varied in accordance with the change in the output data DS shown in FIG. 2, so that the vehicle speed V is slowly decreased after time t 4 to reach the desired speed, without occurrence of sudden deceleration.
A vehicle speed control apparatus having functions equivalent to those of the embodiment shown in FIG. 1 can be realized by the use of a microcomputer, and another embodiment of the present invention using a microcomputer is shown in FIG. 5. In FIG. 5, portions the same as those shown in FIG. 1 are designated by the same reference numbers, and the explanation thereof will be omitted.
In a vehicle speed controlling apparatus 41, the computation for positioning the control rack 4 driven by the actuator 31 is executed in a central processing unit (CPU) 46 in accordance with a predetermined control program stored in a memory 45. This computation for positioning the control rack 4 is carried out on the basis of data produced by detectors which detect different aspects of the operation condition of the diesel engine 2. In the embodiment shown in FIG. 5, there are provided a coolant temperature detector 43 for generating coolant temperature data DW showing the temperature of the engine coolant and a fuel temperature detector 42 for generating fuel temperature data DF showing the fuel temperature, the vehicle speed detector 5, the acceleration detector 9 and the engine speed detector 10. The output data from these detectors are input though an input/output device (I/O) 44 to the CPU 46.
FIG. 6 shows a flow chart of the control program of the vehicle speed controlling apparatus 41, which is stored in the memory 45 and executed in the CPU 46. The control program will be explained. Initialization is made in step 50 after the start of execution of the program, and each of data DW, DF, DA and DE is read in in step 51 to carry out the computation of the second data DQ 2 showing the second amount of fuel supply Q 2 in accordance with the amount of operation of the accelerator pedal 7 in step 52. Then, vehicle speed data DV is read in in step 53 and the first data DQ 1 showing the first amount of fuel supply Q 1 is computed in step 54. After this, a comparison between the first data DQ 1 and the second data DQ 2 is made in step 55. Since the amount Q 1 is larger than the amount Q 2 when the vehicle speed is being automatically controlled the result of step 55 is YES, so that it is discriminated whether or not a flag F is "1" in step 56. As described hereinafter, the flag F is set when the result in step 55 becomes NO and is reset when the first data DQ 1 reaches at a stationary state after the first data DQ 1 becomes greater than the second data DQ 2 .
In this case, since the flag F maintains the state as reset in the initialization step 50, the result in step 56 becomes NO and the first data DQ 1 is substituted for the content of control data DQ for controlling the position of the control rack 4 (step 57). Then, after the flag F is reset (step 58), control data DQ is substituted for the content of output data DS and data DS is output (step 59). After this, the procedure returns to step 51. As a result, the actuator 31 is driven in accordance with data DS and the position of the control rack 4 is controlled so as to maintain the vehicle speed at a desired target vehicle speed. The operation for setting the target vehicle speed and the computation for maintaining the vehicle speed at a desired target vehicle speed are carried out in step 54.
When the amount of duel supply Q 2 becomes greater than or equal to the amount of fuel supply Q 1 , because of a large depression of the accelerator pedal 7 at the time the vehicle speed is being automatically controlled, the result in step 55 becomes NO. As a result, the step 60 is executed and the second data DQ 2 is substituted for the content of control data DQ. After this, step 61 is executed to substitute the second data DQ 2 for the content of data DQ M , the flag F is set (step 62), and then step 59 is executed to produce output data DS showing the control data DQ. Thus, the vehicle speed is controlled in accordance with the degree of depression of the accelerator pedal 7 when the second amount of fuel supply Q 2 is equal to or more than the first amount of fuel supply Q 1 .
The result in step 55 becomes YES when the accelerator pedal 7 is released during the state described above, and the result in step 56 also becomes YES. Consequently, it is discriminated whether or not the flag A is "0" in step 63. As described hereinafter in more detail, the flag A is set to "1" when the control data DQ is gradually decreased from data DQ M and data DQ m becomes equal to or less than the first data DQ 1 .
In this case, since the flag A is reset by the initialization, the result in step 63 becomes YES, and DQ M -ΔQ is substituted for the content of data DQ (step 64), where ΔQ is a predetermined value. In step 65, it is deiscriminated whether control data DQ is more than the first data DQ 1 at that time. When the result in step 65 is YES, step 66 is executed to substitute DQ M -ΔQ for the content of DQ M . Then, output data DS showing the value of Q obtained in step 64 is output (step 59) and the program procedure returns to step 51.
When control data DQ is gradually decreased by the repetitive execution of the program and control data DQ becomes equal to or less than the first data DQ 1 , the result in step 65 becomes NO and the flag A is set to become " 1". Therefore, in the following program cycle, the result in step 63 becomes NO and the first data DQ 1 is substituted for the content of the control data DQ. After this, the vehicle speed in controlled in accordance with the first data DQ 1 . In addition since the flag F is reset in step 58 after the execution of step 57, the result in step 56 becomes NO in the following program cycle, so that step 64 is not executed.
As a result, even if the acceleration pedal 7 is suddenly released for carrying out automatic vehicle speed control again, the amount Q is gradually changed from Q 2 just before the acceleration pedal 7 is released to Q 1 , which is the value required for automatically controlling the vehicle speed at the desired speed so that sudden deceleration of vehicle speed can be effectively prevented.
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In a vehicle speed control apparatus for an internal combustion engine vehicle, in which the first amount of fuel supply required for maintaining the vehicle speed at a desired speed and the second amount of fuel supply corresponding to the amount of depression of an accelerator pedal are separately calculated, the apparatus comprises a selector for selecting the larger of the first and second amount of fuel supply to control the fuel adjusting member, and a modifying circuit for modifying the output data showing the first amount of fuel supply to cause it to slowly change, taking into account the value of the second data showing the second amount of fuel supply just before the second amount of fuel supply becomes smaller than the first amount of fuel supply, whereby the vehicle speed is prevented from being rapidly decelerated when the mode of vehicle speed control is changed from that by the second data to that by the first data. With this arrangement, a sudden change in the control data can be prevented and the vehicle speed can be prevented from suddenly changing at the time of changing over between vehicle speed control carried out by the accelerator pedal and that by the automatic vehicle speed controlling device, to obtain smooth control of the vehicle speed.
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BACKGROUND OF THE INVENTION
[0001] Peroxisome Proliferator Activated Receptors (PPARs) are members of the nuclear hormone receptor superfamily, a large and diverse group of proteins that mediate ligand-dependent transcriptional activation and repression. Three subtypes of PPARs have been isolated: PPARα, PPARγ and PPARδ.
[0002] The expression profile of each isoform differs significantly from the others, whereby PPARα is expressed primarily, but not exclusively in liver; PPARγ is expressed primarily in adipose tissue; and PPARδ is expressed ubiquitously. Studies of the individual PPAR isoforms and ligands have revealed their regulation of processes involved in insulin resistance and diabetes, as well as lipid disorders, such as hyperlipidemia and dyslipidemia. PPARγ agonists, such as pioglitazone, can be useful in the treatment of non-insulin dependent diabetes mellitus. Such PPARγ agonists are associated with insulin sensitization.
[0003] PPARα agonists, such as fenofibrate, can be useful in the treatment of hyperlipidemia. Although clinical evidence is not available to reveal the utility of PPARδ agonists in humans, several preclinical studies suggest that PPARδ agonists can be useful in the treatment of diabetes and lipid disorders.
[0004] The prevalence of the conditions that comprise Metabolic Syndrome (obesity, insulin resistance, hyperlipidemia, hypertension and atherosclerosis) continues to increase. New pharmaceutical agents are needed to address the unmet clinical needs of patients.
[0005] PPARδ agonists have been suggested as a potential treatment for use in regulating many of the parameters associated with Metabolic Syndrome and Atherosclerosis. For example, in obese, non-diabetic rhesus monkeys, a PPARδ agonist reduced circulating triglycerides and LDL, decreased basal insulin levels and increased HDL (Oliver, W. R. et al. Proc Natl Acad Sci 98:5306-5311; 2001). The insulin sensitization observed with the use of a PPARδ agonist is thought to be in part due to decreased myocellular lipids (Dressel, U. et al. Mol Endocrinol 17:2477-2493; 2003).
[0006] Further, atherosclerosis is considered to be a disease consequence of dyslipidemia and may be associated with inflammatory disease. C-reactive protein (CRP) production is part of the acute-phase response to most forms of inflammation, infection and tissue damage. It is measured diagnostically as a marker of low-grade inflammation. Plasma CRP levels of greater than 3 mg/L have been considered predictive of high risk for coronary artery disease (J. Clin. Invest 111: 1085-1812, 2003).
[0007] PPARδ agonists are believed to mediate anti-inflammatory effects. Indeed, treatment of LPS-stimulated macrophages with a PPARδ agonist has been observed to reduce the expression of iNOS, IL12, and IL-6 (Welch, J. S. et al. Proc Natl Acad Sci 100:6712-67172003).
[0008] It may be especially desirable when the active pharmaceutical agent selectively modulates a PPAR receptor subtype to provide an especially desirable pharmacological profile. In some instances, it can be desirable when the active pharmacological agent selectively modulates more than one PPAR receptor subtype to provide a desired pharmacological profile.
SUMMARY OF THE INVENTION
[0009] The present invention is directed to compounds represented by the following structural Formula I′:
and stereoisomers, pharmaceutically acceptable salts, solvates and hydrates thereof, wherein:
(a) R1 is selected from the group consisting of hydrogen, C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and, wherein C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents independently selected from R1′; (b) R1′, R26, R27, R28 and R31 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12, C 1 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryloxy, aryl-C 0-4 -alkyl, heteroaryl, heterocycloalkyl, C(O)R13, COOR14, OC(O)R15, OS(O) 2 R16, N(R17) 2 , NR18C(O)R19, NR20SO 2 R21, SR22, S(O)R23, S(O) 2 R24, and S(O) 2 N(R25) 2 ; R12, R13, R14, R15, R16, R17, R18, R19, R20, R21, R22, R23, R24 and R25 are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (c) R2 is selected from the group consisting of C 0 -C 8 alkyl and C 1-4 -heteroalkyl; (d) X is selected from the group consisting of a single bond, O, S, S(O) 2 and N; (e) U is an aliphatic linker wherein one carbon atom of the aliphatic linker is optionally replaced with O, NH or S, and wherein such aliphatic linker is optionally substituted with from one to four substituents each independently selected from R30; (f) Y is selected from the group consisting of C, NH, and a single bond; (g) E is C(R3)(R4)A or A and wherein
(i) A is selected from the group consisting of carboxyl, tetrazole, C 1 -C 6 alkylnitrile, carboxamide, sulfonamide and acylsulfonamide; wherein sulfonamide, acylsulfonamide and tetrazole are each optionally substituted with from one to two groups independently selected from R 7 ; (ii) each R 7 is independently selected from the group consisting of hydrogen, C 1 -C 6 haloalkyl, aryl C 0 -C 4 alkyl and C 1 -C 6 alkyl; (iii) R3 is selected from the group consisting of hydrogen, C 1 -C 5 alkyl, and C 1 -C 5 alkoxy; and (iv) R4 is selected from the group consisting of H, C 1 -C 5 alkyl, C 1 -C 5 alkoxy, aryloxy, C 3 -C 6 cycloalkyl, and aryl C 0 -C 4 alkyl, and R3 and R4 are optionally combined to form a C 3 -C 4 cycloalkyl, and wherein alkyl, alkoxy, aryloxy, cycloalkyl and aryl-alkyl are each optionally substituted with from one to three substituents each independently selected from R26;
(h) Z1 and Z2 are each independently selected from the group consisting of N, O, and C with the proviso that at least one of Z1 and Z2 is N; (i) Z3 is selected from the group consisting of N, O, and C; (j) R8 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, and halo; (k) R9 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, halo, aryl-C 0 -C 4 alkyl, heteroaryl, C 1 -C 6 allyl, and OR29, and wherein aryl-C 0 -C 4 alkyl, heteroaryl are each optionally substituted with from one to three independently selected from R27; R29 is selected from the group consisting of hydrogen and C 1 -C 4 alkyl; (l) R10, R11 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12″, C 0 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl, aryloxy, C(O)R13′, COOR14′, OC(O)R15′, OS(O) 2 R16′, N(R17′) 2 , NR18′C(O)R19′, NR20′SO 2 R21′, SR22′, S(O)R23′, S(O) 2 R24′, and S(O) 2 N(R25′) 2 ; and wherein aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three independently selected from R28; (m) R12′, R12″, R13′, R14′, R15′, R16′, R17′, R18′, R19′, R20′, R21′, R22′, R23′, R24′, and R25′ are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (n) R30 is selected from the group consisting of C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and wherein C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents each independently selected from R31; (o) R32 is selected from the group consisting of a bond, hydrogen, halo, C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, and C 1 -C 6 alkyloxo; and (p) — is optionally a bond to form a double bond at the indicated position.
[0030] A further embodiement of the present invention is a compound of the Formula I″:
and stereoisomers, pharmaceutically acceptable salts, solvates and hydrates thereof, wherein:
(a) R1 is selected from the group consisting of hydrogen, C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and, wherein C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents independently selected from R1′; (b) R1′, R26, R27, R28 and R31 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12, C 1 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryloxy, aryl-C 0-4 -alkyl, heteroaryl, heterocycloalkyl, C(O)R13, COOR14, OC(O)R15, OS(O) 2 R16, N(R17) 2 , NR18C(O)R19, NR20SO 2 R21, SR22, S(O)R23, S(O) 2 R24, and S(O) 2 N(R25) 2 ; R12, R13, R14, R15, R16, R17, R18, R19, R20, R21, R22, R23, R24 and R25 are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (c) R2 is selected from the group consisting of C 0 -C 8 alkyl and C 1-4 -heteroalkyl; (d) X is selected from the group consisting of a single bond, O, S, S(O) 2 and N; (e) U is an aliphatic linker wherein one carbon atom of the aliphatic linker is optionally replaced with O, NH or S, and wherein such aliphatic linker is substituted with from one to four substituents each independently selected from R30; (f) Y is selected from the group consisting of C, O, S, NH and a single bond; (g) E is C(R3)(R4)A or A and wherein
(i) A is selected from the group consisting of carboxyl, tetrazole, C 1 -C 6 alkylnitrile, carboxamide, sulfonamide and acylsulfonamide; wherein sulfonamide, acylsulfonamide and tetrazole are each optionally substituted with from one to two groups independently selected from R 7 ; (ii) each R 7 is independently selected from the group consisting of hydrogen, C 1 -C 6 haloalkyl, aryl C 0 -C 4 alkyl and C 1 -C 6 alkyl; (iii) R3 is selected from the group consisting of hydrogen, C 1 -C 5 alkyl, and C 1 -C 5 alkoxy; and (iv) R4 is selected from the group consisting of H, C 1 -C 5 alkyl, C 1 -C 5 alkoxy, aryloxy, C 3 -C 6 cycloalkyl, and aryl C 0 -C 4 alkyl, and R3 and R4 are optionally combined to form a C 3 -C 4 cycloalkyl, and wherein alkyl, alkoxy, aryloxy, cycloalkyl and aryl-alkyl are each optionally substituted with from one to three substituents each independently selected from R26;
(h) Z1 and Z2 are each independently selected from the group consisting of N, O, and C with the proviso that at least one of Z1 and Z2 is N; (i) Z3 is selected from the group consisting of N, O, and C; (j) R8 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, and halo; (k) R9 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, halo, aryl-C 0 -C 4 alkyl, heteroaryl, C 1 -C 6 allyl, and OR29, and wherein aryl-C 0 -C 4 alkyl, heteroaryl are each optionally substituted with from one to three independently selected from R27; R29 is selected from the group consisting of hydrogen and C 1 -C 4 alkyl; (l) R10, R11 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12″, C 0 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl, aryloxy, C(O)R13′, COOR14′, OC(O)R15′, OS(O) 2 R16′, N(R17′) 2 , NR18′C(O)R19′, NR20′SO 2 R21′, SR22′, S(O)R23′, S(O) 2 R24′, and S(O) 2 N(R25′) 2 ; and wherein aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three independently selected from R28; (m) R12′, R12″, R13′, R14′, R15′, R16′, R17′, R18′, R19′, R20′, R21′, R22′, R23′, R24′, and R25′ are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (n) R30 is selected from the group consisting of C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and wherein C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents each independently selected from R31; (o) R32 is selected from the group consisting of a bond, hydrogen, halo, C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, and C 1 -C 6 alkyloxo; and (p) — is optionally a bond to form a double bond at the indicated position.
[0051] Another embodiment of the present invention is a compound of the Formula I′″:
and stereoisomers, pharmaceutically acceptable salts, solvates and hydrates thereof, wherein:
(a) R1 is selected from the group consisting of hydrogen, C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and, wherein C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents independently selected from R1′; (b) R1′, R26, R27, R28 and R31 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12, C 1 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryloxy, aryl-C 0-4 -alkyl, heteroaryl, heterocycloalkyl, C(O)R13, COOR14, OC(O)R15, OS(O) 2 R16, N(R17) 2 , NR18C(O)R19, NR20SO 2 R21, SR22, S(O)R23, S(O) 2 R24, and S(O) 2 N(R25) 2 ; R12, R13, R14, R15, R16, R17, R18, R19, R20, R21, R22, R23, R24 and R25 are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (c) R2 is selected from the group consisting of C 0 -C 8 alkyl and C 1-4 -heteroalkyl; (d) X is selected from the group consisting of a single bond, O, S, S(O) 2 and N; (e) U is an aliphatic linker wherein one carbon atom of the aliphatic linker is optionally replaced with O, NH or S, and wherein such aliphatic linker is optionally substituted with from one to four substituents each independently selected from R30; (f) Y is selected from the group consisting of O, S, NH, C, and a single bond; (g) E is C(R3)(R4)A; wherein
(i) A is selected from the group consisting of carboxyl, tetrazole, C 1 -C 6 alkylnitrile, carboxamide, sulfonamide and acylsulfonamide; wherein sulfonamide, acylsulfonamide and tetrazole are each optionally substituted with from one to two groups independently selected from R 7 ; (ii) each R 7 is independently selected from the group consisting of hydrogen, C 1 -C 6 haloalkyl, aryl C 0 -C 4 alkyl and C 1 -C 6 alkyl; (iii) R3 is selected from the group consisting of C 1 -C 5 alkyl, and C 1 -C 5 alkoxy; and (iv) R4 is selected from the group consisting of H, C 1 -C 5 alkyl, C 1 -C 5 alkoxy, aryloxy, C 3 -C 6 cycloalkyl, and aryl C 0 -C 4 alkyl, and R3 and R4 are optionally combined to form a C 3 -C 4 cycloalkyl, and wherein alkyl, alkoxy, aryloxy, cycloalkyl and aryl-alkyl are each optionally substituted with from one to three substituents each independently selected from R26; with the proviso that when Y is C then R4 is selected from the group consisting of C 1 -C 5 alkyl, C 1 -C 5 alkoxy, aryloxy, C 3 -C 6 cycloalkyl, and aryl C 0 -C 4 alkyl, and R3 and R4 are optionally combined to form a C 3 -C 4 cycloalkyl, and wherein alkyl, alkoxy, cycloalkyl and aryl-alkyl are each optionally substituted with one to three each independently selected from R26;
(h) Z1 and Z2 are each independently selected from the group consisting of N, O, and C with the proviso that at least one of Z1 and Z2 is N; (i) Z3 is selected from the group consisting of N, O, and C; (j) R8 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, and halo; (k) R9 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, halo, aryl-C 0 -C 4 alkyl, heteroaryl, C 1 -C 6 allyl, and OR29, and wherein aryl-C 0 -C 4 alkyl, heteroaryl are each optionally substituted with from one to three independently selected from R27; R29 is selected from the group consisting of hydrogen and C 1 -C 4 alkyl; (l) R10, R11 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12″, C 0 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl, aryloxy, C(O)R13′, COOR14′, OC(O)R15′, OS(O) 2 R16′, N(R17′) 2 , NR18′C(O)R19′, NR20′SO 2 R21′, SR22′, S(O)R23′, S(O) 2 R24′, and S(O) 2 N(R25′) 2 ; and wherein aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three independently selected from R28; (m) R12′, R12″, R13′, R14′, R15′, R16′, R17′, R18′, R19′, R20′, R21′, R22′, R23′, R24′, and R25′ are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (n) R30 is selected from the group consisting of C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and wherein C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents each independently selected from R31; (o) R32 is selected from the group consisting of a bond, hydrogen, halo, C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, and C 1 -C 6 alkyloxo; and (p) — is optionally a bond to form a double bond at the indicated position.
[0073] Another embodiment claimed herein is a compound of the Formula I:
and stereoisomers, pharmaceutically acceptable salts, solvates and hydrates thereof, wherein:
(a) R1 is selected from the group consisting of hydrogen, C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and, wherein C 1 -C 8 alkyl, C 1 -C 8 alkenyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents independently selected from R1′; (b) R1′, R26, R27, R28 and R31 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12, C 1 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryloxy, aryl-C 0-4 -alkyl, heteroaryl, heterocycloalkyl, C(O)R13, COOR14, OC(O)R15, OS(O) 2 R16, N(R17) 2 , NR18C(O)R19, NR20SO 2 R21, SR22, S(O)R23, S(O) 2 R24, and S(O) 2 N(R25) 2 ; R12, R13, R14, R15, R16, R17, R18, R19, R20, R21, R22, R23, R24 and R25 are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (c) R2 is selected from the group consisting of C 0 -C 8 alkyl and C 1-4 -heteroalkyl; (d) X is selected from the group consisting of a single bond, O, S, S(O) 2 and N; (e) U is an aliphatic linker wherein one carbon atom of the aliphatic linker may be replaced with O, NH or S, and wherein such aliphatic linker is optionally substituted with R30; (f) Y is selected from the group consisting of C, O, S, NH and a single bond; (g) E is C(R3)(R4)A or A and wherein
(i) A is selected from the group consisting of carboxyl, tetrazole, C 1 -C 6 alkylnitrile, carboxamide, sulfonamide and acylsulfonamide; wherein sulfonamide, acylsulfonamide and tetrazole are each optionally substituted with from one to two groups independently selected from R 7 ; (ii) each R 7 is independently selected from the group consisting of hydrogen, C 1 -C 6 haloalkyl, aryl C 0 -C 4 alkyl and C 1 -C 6 alkyl; (iii) R3 is selected from the group consisting of hydrogen, C 1 -C 5 alkyl, and C 1 -C 5 alkoxy; and (iv) R4 is selected from the group consisting of H, C 1 -C 5 alkyl, C 1 -C 5 alkoxy, aryloxy, C 3 -C 6 cycloalkyl, and aryl C 0 -C 4 alkyl, and R3 and R4 are optionally combined to form a C 3 -C 4 cycloalkyl, and wherein alkyl, alkoxy, aryloxy, cycloalkyl and aryl-alkyl are each optionally substituted with from one to three substituents each independently selected from R26;
(h) Z1 and Z2 are each independently selected from the group consisting of N, O, and C with the proviso that at least one of Z1 and Z2 is N; (i) Z3 is selected from the group consisting of N, O, and C; (j) R8 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, and halo; (k) R9 is selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 alkylenyl, halo, aryl-C 0 -C 4 alkyl, heteroaryl, C 1 -C 6 allyl, and OR29, and wherein aryl-C 0 -C 4 alkyl, heteroaryl are each optionally substituted with from one to three independently selected from R27; R29 is selected from the group consisting of hydrogen and C 1 -C 4 alkyl; (l) R10, R11 are each independently selected from the group consisting of hydrogen, hydroxy, cyano, nitro, halo, oxo, C 1 -C 6 alkyl, C 1 -C 6 alkyl-COOR12″, C 0 -C 6 alkoxy, C 1 -C 6 haloalkyl, C 1 -C 6 haloalkyloxy, C 3 -C 7 cycloalkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, C3-C6 cycloalkylaryl-C 0-2 -alkyl, aryloxy, C(O)R13′, COOR14′, OC(O)R15′, OS(O) 2 R16′, N(R17′) 2 , NR18′C(O)R19′, NR20′SO 2 R21′, SR22′, S(O)R23′, S(O) 2 R24′, and S(O) 2 N(R25′) 2 ; and wherein aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three independently selected from R28; (m) R12′, R12″, R13′, R14′, R15′, R16′, R17′, R18′, R19′, R20′, R21′, R22′, R23′, R24′, and R25′ are each independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl and aryl; (n) R30 is selected from the group consisting of C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl, and wherein C 1 -C 6 alkyl, aryl-C 0-4 -alkyl, aryl-C 1-4 -heteroalkyl, heteroaryl-C 0-4 -alkyl, and C3-C6 cycloalkylaryl-C 0-2 -alkyl are each optionally substituted with from one to three substituents each independently selected from R31; (o) R32 is selected from the group consisting of a bond, hydrogen, halo, C 1 -C 6 alkyl, C 1 -C 6 haloalkyl, and C 1 -C 6 alkyloxo; and (p) — is optionally a bond to form a double bond at the indicated position.
[0094] In one embodiment, the present invention also relates to pharmaceutical compositions comprising at least one compound of the present invention, or a pharmaceutically acceptable salt, solvate, hydrate, or stereioisomer thereof, and a pharmaceutically acceptable carrier.
[0095] In another embodiment, the present invention relates to a method of selectively modulating a PPAR delta receptor by contacting the receptor with at least one compound represented by Structural Formula I, or a pharmaceutically acceptable salt, solvate, hydrate, or stereioisomer thereof.
[0096] In another embodiment, the present invention relates to a method of modulating one or more of the PPAR alpha, beta, gamma, and/or delta receptors.
[0097] In a further embodiment, the present invention relates to a method of making a compound represented by Structural Formula I.
[0098] The compounds of the present invention are believed to be effective in treating and preventing Metabolic Disorder, Type II diabetes, hyperglycemia, hyperlipidemia, obesity, coagaulopathy, hypertension, atherosclerosis, and other disorders related to Metabolic Disorder and cardiovascular diseases. Further, compounds of this invention can be useful for lowering fibrinogen, increasing HDL levels, treating renal disease, controlling desirable weight, treating demyelinating diseases, treating certain viral infections, and treating liver disease. In addition, the compounds can be associated with fewer clinical side effects than compounds currently used to treat such conditions.
DETAILED DESCRIPTION OF THE INVENTION
[0099] The terms used to describe the instant invention have the following meanings.
[0100] As used herein, the term “aliphatic linker” or “aliphatic group” is a non-aromatic, consisting solely of carbon and hydrogen and may optionally contain one or more units of unsaturation, e.g., double and/or triple bonds (also refer herein as “alkenyl” and “alkynyl”). An aliphatic or aliphatic group may be straight chained, branched (also refer herein as “alkyl”) or cyclic (also refer herein as “cycloalkyl). When straight chained or branched, an aliphatic group typically contains between about 1 and about 10 carbon atoms, more typically between about 1 and about 6 carbon atoms. When cyclic, an aliphatic typically contains between about 3 and about 10 carbon atoms, more typically between about 3 and about 7 carbon atoms. Aliphatics are preferably C 1 -C 10 straight chained or branched alkyl groups (i.e. completely saturated aliphatic groups), more preferably C 1 -C 6 straight chained or branched alkyl groups. Examples include, but are not limited to methyl, ethyl, propyl, n-propyl, iso-propyl, n-butyl, sec-butyl, and tert-butyl. Additional examples include, but are not limited to, cyclopropyl, cyclopentyl, cyclohexyl, cyclopentyl, cyclohexylyl and the like. Such aliphatic linker is optionally substituted with from one to four substituents each independently selected from R30. It can be preferred that aliphatic linker is substituted with from zero to two substituents each independently selected from R30. Further, it may be preferred that one carbon of the alphatic linker is replaced with an O, NH, or S.
[0101] The term “alkyl,” unless otherwise indicated, refers to those alkyl groups of a designated number of carbon atoms of either a straight or branched saturated configuration. As used herein, “C 0 alkyl” means that there is no carbon and therefore represents a bond. Examples of “alkyl” include, but are not limited to, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl and tert-butyl, pentyl, hexyl, isopentyl and the like. Alkyl as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above. As used herein, the term “alkyloxo” means an alkyl group of the designated number of carbon atoms with a “═O” substituent.
[0102] The term “alkenyl” or “alkylenyl” means hydrocarbon chain of a specified number of carbon atoms of either a straight or branched configuration and having at least one carbon-carbon double bond, which may occur at any point along the chain, such as ethenyl, propenyl, butenyl, pentenyl, vinyl, alkyl, 2-butenyl and the like. Alkenyl as defined above may be optionally substituted with designated number of substituents as set forth in the embodiment recited above.
[0103] The term “alkynyl” means hydrocarbon chain of a specified number of carbon atoms of either a straight or branched configuration and having at least one carbon-carbon triple bond, which may occur at any point along the chain. Example of alkynyl is acetylene. Alkynyl as defined above may be optionally substituted with designated number of substituents as set forth in the embodiment recited above.
[0104] The term “heteroalkyl” refers to a means hydrocarbon chain of a specified number of carbon atoms wherein at least one carbon is replaced by a heteroatom selected from the group consisting of O, N and S.
[0105] The term “cycloalkyl” refers to a saturated or partially saturated carbocycle containing one or more rings of from 3 to 12 carbon atoms, typically 3 to 7 carbon atoms. Examples of cycloalkyl includes, but are not limited to cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and cycloheptyl, and the like. “Cycloalkyaryl” means that an aryl is fused with a cycloalkyl, and “Cycloalkylaryl-alkyl” means that the cycloalkylaryl is linked to the parent molecule through the alkyl. Cycloalkyl as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above.
[0106] The term “halo” refers to fluoro, chloro, bromo and iodo.
[0107] The term “haloalkyl” is a C 1 -C 6 alkyl group, which is substituted with one or more halo atoms selected from F, Br, Cl and I. An example of a haloalkyl group is trifluoromethyl (CF 3 ).
[0108] The term “alkoxy” represents an alkyl group of indicated number of carbon atoms attached through an oxygen bridge, such as methoxy, ethoxy, propoxy, isopropoxy, butoxy, tert-butoxy, pentoxy, and the like. Alkoxy as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above.
[0109] The term “haloalkyloxy” represents a C 1 -C 6 haloalkyl group attached through an oxygen bridge, such as OCF 3 . The “haloalkyloxy” as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above.
[0110] The term “aryl” includes carbocyclic aromatic ring systems (e.g. phenyl), fused polycyclic aromatic ring systems (e.g. naphthyl and anthracenyl) and aromatic ring systems fused to carbocyclic non-aromatic ring systems (e.g., 1,2,3,4-tetrahydronaphthyl). “Aryl” as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above.
[0111] The term “arylalkyl” refers to an aryl alkyl group which is linked to the parent molecule through the alkyl group, which may be further optionally substituted with a designated number of substituents as set forth in the embodiment recited above. When arylalkyl is arylC 0 alkyl, then the aryl group is bonded directly to the parent molecule. Likewise, arylheteroalkyl means an aryl group linked to the parent molecule through the heteroalkyl group.
[0112] The term “acyl” refers to alkylcarbonyl species.
[0113] The term “heteroaryl” group, as used herein, is an aromatic ring system having at least one heteroatom such as nitrogen, sulfur or oxygen and includes monocyclic, bicyclic or tricyclic aromatic ring of 5- to 14-carbon atoms containing one or more heteroatoms selected from the group consisting of O, N, and S. The “heteroaryl” as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above. Examples of heteroaryl are, but are not limited to, furanyl, indolyl, thienyl (also referred to herein as “thiophenyl”) thiazolyl, imidazolyl, isoxazoyl, oxazoyl, pyrazoyl, pyrrolyl, pyrazinyl, pyridyl, pyrimidyl, pyrimidinyl and purinyl, cinnolinyl, benzofuranyl, benzothienyl, benzotriazolyl, benzoxazolyl, quinoline, isoxazolyl, isoquinoline and the like. The term “heteroarylalkyl” means that the heteroaryl group is linked to the parent molecule through the alkyl portion of the heteroarylalkyl.
[0114] The term “heterocycloalkyl” refers to a non-aromatic ring which contains one or more oxygen, nitrogen or sulfur and includes a monocyclic, bicyclic or tricyclic non-aromatic ring of 5 to 14 carbon atoms containing one or more heteroatoms selected from O, N or S. The “heterocycloalkyl” as defined above may be optionally substituted with a designated number of substituents as set forth in the embodiment recited above. Examples of heterocycloalkyl include, but are not limited to, morpholine, piperidine, piperazine, pyrrolidine, and thiomorpholine. As used herein, alkyl groups include straight chained and branched hydrocarbons, which are completely saturated.
[0115] As used herein, the phrase “selectively modulate” means a compound whose EC50 for the stated PPAR receptor is at least ten fold lower than its EC50 for the other PPAR receptor subtypes.
[0116] PPARδ has been proposed to associate with and dissociate from selective co-repressors (BCL-6) that control basal and stimulated anti-inflammatory activities (Lee, C-H. et al. Science 302:453-4572003). PPARδ agonists are thought to be useful to attenuate other inflammatory conditions such as inflammation of the joints and connective tissue as occurs in rheumatoid arthritis, related autoimmune diseases, osteroarthritis, as well as myriad other inflammatory diseases, Crohne's disease, and psoriasis.
[0117] When a compound represented by Structural Formula I has more than one chiral substituent it may exist in diastereoisomeric forms. The diastereoisomeric pairs may be separated by methods known to those skilled in the art, for example chromatography or crystallization and the individual enantiomers within each pair may be separated using methods familiar to the skilled artisan. The present invention includes each diastereoisomer of compounds of Structural Formula I and mixtures thereof.
[0118] Certain compounds of Structural Formula I may exist in different stable conformational forms which may be separable. Torsional asymmetry due to restricted rotation about an asymmetric single bond, for example because of steric hindrance or ring strain, may permit separation of different conformers. The present invention includes each conformational isomer of compounds of Structural Formula I and mixtures thereof.
[0119] Certain compounds of Structural Formula I may exist in zwitterionic form and the present invention includes each zwitterionic form of compounds of Structural Formula I and mixtures thereof.
[0120] “Pharmaceutically-acceptable salt” refers to salts of the compounds of the Structural Formula I which are considered to be acceptable for clinical and/or veterinary use. Typical pharmaceutically-acceptable salts include those salts prepared by reaction of the compounds of the present invention with a mineral or organic acid or an organic or inorganic base. Such salts are known as acid additiona salts and base addition salts, respectively. It will be recognized that the particular counterion forming a part of any salt of this invention is not of a critical nature, so long as the salt as a whole is pharmaceutically-acceptable and as long as the counterion does not contribute undesired qualities to the salt as a whole. These salts may be prepared by methods known to the skilled artisan.
[0121] The term, “active ingredient” means the compounds generically described by Structural Formula I as well as the sterioisomers, salts, solvates, and hydrates,
[0122] The term “pharmaceutically acceptable” means that the carrier, diluent, excipients and salt are pharmaceutically compatible with the other ingredients of the composition. Pharmaceutical compositions of the present invention are prepared by procedures known in the art using well known and readily available ingredients.
[0123] “Preventing” refers to reducing the likelihood that the recipient will incur or develop any of the pathological conditions described herein. The term “preventing” is particularly applicable to a patient that is susceptible to the particular patholical condition.
[0124] “Treating” refers to mediating a disease or condition and preventing, or mitigating, its further progression or ameliorate the symptoms associated with the disease or condition.
[0125] “Pharmaceutically-effective amount” means that amount of active ingredientit, that will elicit the biological or medical response of a tissue, system, or mammal. Such an amount can be administered prophylactically to a patient thought to be susceptible to development of a disease or condition. Such amount when administered prophylactically to a patient can also be effective to prevent or lessen the severity of the mediated condition. Such an amount is intended to include an amount which is sufficient to modulate a selected PPAR receptor or to prevent or mediate a disease or condition. Generally, the effective amount of a Compound of Formula I will be between 0.02 through 5000 mg per day. Preferably the effective amount is between 1 through 1,500 mg per day. Preferably the dosage is from 1 through 1,000 mg per day. A most preferable the dose can be from 1 through 100 mg per day.
[0126] The desired dose may be presented in a single dose or as divisded doses administered at appropriate intervals.
[0127] A “mammal” is an individual animal that is a member of the taxonomic class Mammalia. The class Mammalia includes humans, monkeys, chimpanzees, gorillas, cattle, swine, horses, sheep, dogs, cats, mice, and rats.
[0128] Administration to a human is most preferred. The compounds and compositions of the present invention are useful for the treatment and/or prophylaxis of cardiovascular disease, for raising serum HDL cholesterol levels, for lowering serum triglyceride levels and for lower serum LDL cholesterol levels. Elevated triglyceride and LDL levels, and low HDL levels, are risk factors for the development of heart disease, stroke, and circulatory system disorders and diseases.
[0129] Further, the compound and compositions of the present invention may reduce the incidence of undesired cardiac events in patients. The physician of ordinary skill will know how to identify-humans who will benefit from administration of the compounds and compositions of the present invention.
[0130] The compounds and compositions of the present invention are also useful for treating and/or preventing obesity.
[0131] Further, these compounds and compositions are useful for the treatment and/or prophylaxis of non-insulin dependent diabetes mellitus (NIDDM) with reduced or no body weight gains by the patients. Furthermore, the compounds and compositions of the present invention are useful to treat or prevent acute or transient disorders in insulin sensitivity, such as sometimes occur following surgery, trauma, myocardial infarction, and the like. The physician of ordinary skill will know how to identify humans who will benefit from administration of the compounds and compositions of the present invention.
[0132] The present invention further provides a method for the treatment and/or prophylaxis of hyperglycemia in a human or non-human mammal which comprises administering an effective amount of active ingredient, as defined herein, to a hyperglycemic human or non-human mammal in need thereof.
[0133] The invention also relates to the use of a compound of Formula I as described above, for the manufacture of a medicament for treating a PPAR receptor mediated condition.
[0134] A therapeutically effective amount of a compound of Structural Formula I can be used for the preparation of a medicament useful for treating Metabolic Disorder, diabetes, treating obesity, lowering tryglyceride levels, lowering serum LDL levels, raising the plasma level of high density lipoprotein, and for treating, preventing or reducing the risk of developing atherosclerosis, and for preventing or reducing the risk of having a first or subsequent atherosclerotic disease event in mammals, particularly in humans. In general, a therapeutically effective amount of a compound of the present invention typically reduces serum triglyceride levels of a patient by about 20% or more, and increases serum HDL levels in a patient. Preferably, HDL levels will be increased by about 30% or more. In adition, a therapeutically effective amount of a compound, used to prevent or treat NIDDM, typically reduces serum glucose levels, or more specifically HbAlc, of a patient by about 0.7% or more.
[0135] When used herein Metabolic Syndrome includes pre-diabetic insulin resistance syndrome and the resulting complications thereof, insulin resistance, non-insulin dependent diabetes, dyslipidemia, hyperglycemia obesity, coagulopathy, hypertension and other complications associated with diabetes. The methods and treatments mentioned herein include the above and encompass the treatment and/or prophylaxis of any one of or any combination of the following: pre-diabetic insulin resistance syndrome, the resulting complications thereof, insulin resistance, Type II or non-insulin dependent diabetes, dyslipidemia, hyperglycemia, obesity and the complications associated with diabetes including cardiovascular disease, especially atherosclerosis. In addition, the methods and treatments mentioned herein include the above and encompass the treatment and/or prophylaxis of any one of or any combination of the following inflammatory and autoimmune diseases: adult respritory distress syndrome, rheumatoid arthritis, demyelinating disease, Chrohne's disease, asthma, systemic lupus erythematosus, psoriasis, and bursitis.
[0136] The compositions are formulated and administered in the same general manner as detailed herein. The compounds of the instant invention may be used effectively alone or in combination with one or more additional active agents depending on the desired target therapy. Combination therapy includes administration of a single pharmaceutical dosage composition which contains a compound of Structural Formula I, a stereoisomer, salt, solvate and/or hydrate thereof (“Active Igredient”) and one or more additional active agents, as well as administration of a compound of Active Ingredient and each active agent in its own separate pharmaceutical dosage formulation. For example, an Active Ingredient and an insulin secretogogue such as biguanides, thiazolidinediones, sulfonylureas, insulin, or α-glucosidose inhibitors can be administered to the patient together in a single oral dosage composition such as a tablet or capsule, or each agent administered in separate oral dosage formulations. Where separate dosage formulations are used, an Active Ingredient and one or more additional active agents can be administered at essentially the same time, i.e., concurrently, or at separately staggered times, i.e., sequentially; combination therapy is understood to include all these regimens.
[0137] An example of combination treatment or prevention of atherosclerosis may be wherein an Active Ingredient is administered in combination with one or more of the following active agents: antihyperlipidemic agents; plasma HDL-raising agents; antihypercholesterolemic agents, fibrates, vitamins, aspirin, and the like. As noted above, the Active Ingredient can be administered in combination with more than one additional active agent.
[0138] Another example of combination therapy can be seen in treating diabetes and related disorders wherein the Active Ingredient can be effectively used in combination with, for example, sulfonylureas, biguanides, thiazolidinediones, α-glucosidase inhibitors, other insulin secretogogues, insulin as well as the active agents discussed above for treating atherosclerosis.
[0139] The Active Ingredients of the present invention, have valuable pharmacological properties and can be used in pharmaceutical compositions containing a therapeutically effective amount of Active Ingredient of the present invention, in combination with one or more pharmaceutically acceptable excipients. Excipients are inert substances such as, without limitation carriers, diluents, fillers, flavoring agents, sweeteners, lubricants, solubilizers, suspending agents, wetting agents, binders, disintegrating agents, encapsulating material and other-conventional adjuvants. Proper formulation is dependent upon the route of administration chosen. Pharmaceutical compositions typically contain from about 1 to about 99 weight percent of the Active Ingredient of the present invention.
[0140] Preferably, the pharmaceutical formulation is in unit dosage form. A “unit dosage form” is a physically discrete unit containing a unit dose, suitable for administration in human subjects or other mammals. For example, a unit dosage form can be a capsule or tablet, or a number of capsules or tablets. A “unit dose” is a predetermined quantity of the Active Ingredient of the present invention, calculated to produce the desired therapeutic effect, in association with one or more pharmaceutically-acceptable excipients. The quantity of active ingredient in a unit dose may be varied or adjusted from about 0.1 to about 1500 milligrams or more according to the particular treatment involved. It may be preferred that the unit dosage is from about 1 mg to about 1000 mg.
[0141] The dosage regimen utilizing the compounds of the present invention is selected by one of ordinary skill in the medical or veterinary arts, in view of a variety of factors, including, without limitation, the species, age, weight, sex, and medical condition of the recipient, the severity of the condition to be treated, the route of administration, the level of metabolic and excretory function of the recipient, the dosage form employed, the particular compound and salt thereof employed, and the like.
[0142] Advantageously, compositions containing the compound of Structural Formula I or the salts thereof may be provided in dosage unit form, preferably each dosage unit containing from about 1 to about 500 mg be administered although it will, of course, readily be understood that the amount of the compound or compounds of Structural Formula I actually to be administered will be determined by a physician, in the light of all the relevant circumstances.
[0143] Preferably, the compounds of the present invention are administered in a single daily dose, or the total daily dose may be administered in divided doses, two, three, or more times per day. Where delivery is via transdermal forms, of course, administration is continuous.
[0144] Suitable routes of administration of pharmaceutical compositions of the present invention include, for example, oral, eyedrop, rectal, transmucosal, topical, or intestinal administration; parenteral delivery (bolus or infusion), including intramuscular, subcutaneous, intramedullary injections, as well as intrathecal, direct intraventricular, intravenous, intraperitoneal, intranasal, or intraocular injections. The compounds of the invention can also be administered in a targeted drug delivery system, such as, for example, in a liposome coated with endothelial cell-specific antibody.
[0145] Solid form formulations include powders, tablets and capsules.
[0146] Sterile liquid formulations include suspensions, emulsions, syrups, and elixirs.
[0147] Pharmaceutical compositions of the present invention can be manufactured in a manner that is itself known, e.g., by means of conventional mixing, dissolving, granulating, dragee-making, levigating, emulsifying, encapsulating, entrapping or lyophilizing processes.
[0148] The following pharmaceutical formulations 1 and 2 are illustrative only and are not intended to limit the scope of the invention in any way.
Formulation 1
[0149] Hard gelatin capsules are prepared using the following ingredients:
Quantity (mg/capsule) Active Ingredient 250 Starch, dried 200 Magnesium stearate 10 Total 460 mg
Formulation 2
[0150] A tablet is prepared using the ingredients below:
Quantity (mg/tablet) Active Ingredient 250 Cellulose, microcrystalline 400 Silicon dioxide, fumed 10 Stearic acid 5 Total 665 mg
[0151] The components are blended and compressed to form tablets each weighing 665 mg .
[0152] In yet another embodiment of the compounds of the present invention, the compound is radiolabelled, such as with carbon-14, or tritiated. Said radiolabelled or tritiated compounds are useful as reference standards for in vitro assays to identify new selective PPAR receptor agonists.
[0153] The compounds of the present invention can be useful for modulating insulin secretion and as research tools. Certain compounds and conditions within-the scope of this invention are preferred. The following conditions, invention embodiments, and compound characteristics listed in tabular form may be independently combined to produce a variety of preferred compounds and process conditions. The following list of embodiments of this invention is not intended to limit the scope of this invention in any way.
[0154] Some prefered characteristics of compounds of formula I are:
(a) R3 is methyl; (b) R4 is hydrogen; (c) R3 and R4 are each hydrogen; (d) R3 and R4 are each methyl; (e) A is carboxyl; (f) X is —O—; (g) X is —S—; (h) U is CH; (i) U is CH 2 CH; (j) R9 is methyl; (k) R9 is hydrogen; (l) R9 is C 1 -C 3 alkyl; (m) R8 is methyl; (n) R8 and R9 are each hydrogen; (o) R10 is CF 3 ; (p) R10 is haloalkyl; (q) R10 is haloalkyloxy; (r) R11 is hydrogen (s) R10 and R11 are each hydrogen; (t) R11 is haloalkyl; (u) Z3 is N; (v) Z2 and Z3 are each N; (w) Z1 and Z3 are each N; (x) Z3 is O; (y) R1 is optionally substituted C2-C3 arylalkyl; (z) R1 is substituted C2 arylalkyl; (aa) R2 is bonded to Z3; (bb) Z1 is N; (cc) Z3 is O; (dd) Z1, Z2, and Z3 are each N; (ee) Z1 and Z3 are each N and Z2 is C; (ff) R2 is bonded to Z2; (gg) Z1 is O, Z2 is N and Z3 is C; (hh) R2 is bonded to Z3; (ii) Z1 and Z3 are each N; (jj) — in the five membered ring each form a double bond at the designated position in Formula I; (kk) R1 is C 1 -C 4 alkyl; (ll) R32 is hydrogen; (mm) R2 is a bond; (nn) R2 is C 1 -C 2 alkyl; (oo) Y is O; (pp) Y is S; (qq) Y is C; (rr) Y is C, NH, or a bond; (ss) E is C(R3)(R4)A; (tt) R3 is hydrogen; (uu) R3 is C 1 -C 2 alkyl; (vv) R4 is C 1 -C 2 alkyl; (ww) R3 and R4 are each hydrogen; (xx) R3 and R4 are each methyl; (yy) A is COOH; (zz) Aliphatic linker is saturated; (aaa) Aliphatic linker is substituted with C 1 -C 3 alkyl; (bbb) Aliphatic linker is substituted with from one to three substituents each independently selected from R30; (ccc) Aliphatic linker is substituted with from one to two substituents each independently selected from R30; (ddd) Aliphatic linker is C 1 -C 3 alkyl; (eee) Aliphatic linker is C 1 -C 2 alkyl; (fff) Aliphatic linker is C 1 -C 3 alkyl and one carbon is replaced with an —O—; (ggg) A compound of Formula II:
(hhh) A compound of Formula III:
(iii) A compound of Formula IV:
(jjj) Aryl is a phenyl group; (kkk) Aryl is a naphthyl group; (lll) A compound of Formula I that is:
(mmm) A compound of Formula I that is
(nnn) A compound of Formula I that selectively modulates a delta receptor; (ooo) An Active Ingredient, as described herein, that is a PPAR coagaonist that modulates a gamma receptor and a delta receptor; (ppp) An Active Ingredient, as described herein, for use in the treatment of cardiovascular disease; (qqq) An Active Ingredient, as described herein, for use in the treatment of Metabolic Disorder; (rrr) An Active Ingredient for use in the control of obesity; (sss) An Active Ingredient for use in treating diabetes; (ttt) An Active Ingredient that is a PPAR receptor agonist; (uuu) A compound of Formula I selected from the group consisting of {2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenoxy}-acetic acid; 3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid; (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenoxy)-acetic acid; (R,S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenyl)-propionic acid; (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid; (R,S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid; (R,S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid; (R,S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid; (R,S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (R,S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid; (3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid; {3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-phenyl}-acetic acid; (3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-acetic acid; 2-(3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid; (3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenyl)-acetic acid; (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid; (R)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid; (S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid; (R)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid; (S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid; (R)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid; (S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid; (R)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid; (S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (R)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid; (R)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid; (S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; (R)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid; {4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; {4-[1-(3,5-Bis-trifluoromethyl-phenyl)-5-methyl-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; (4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid; 3-(4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid; 3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid; {4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; {4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; 3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid; {3-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid; 3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid; (S)-3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-2-methoxy-propionic acid; {3-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid; 3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid; 3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-2-methoxy-propionic acid; {2-Methyl-4-[2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethylsulfanyl]-phenoxy}-acetic acid; [2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid; [2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid; 3-[2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethoxy)-phenyl]-propionic acid; {2-Methyl-4-[1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-ylmethylsulfanyl]-phenoxy}-acetic acid; {2-Methyl-4-[5-methyl-1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-ylmethylsulfanyl]-phenoxy}-acetic acid; {4-[1-(3,5-Bis-trifluoromethyl-benzyl)-5-phenyl-1H-[1,2,3]triazol-4-ylmethanesulfonyl]-2-methyl-phenoxy}-acetic acid; 3-(2-Methyl-4-{1-[4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-ethoxy}-phenyl)-propionic acid; 3-{2-Methyl-4-[4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-ylmethoxy]-phenyl}-propionic acid; {4-[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; {4-[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid; {4-[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethoxy]-2-methyl-phenoxy}-acetic acid; and 3-{4-[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid;
(iii) A compound of Formula I selected from the group consisting of (R)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid, (S)-(2-Methyl-4-{1[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid, (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid, and (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid; and (jjj) A compound of Formula I that is (R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid.
Synthesis
[0288] Compounds of the present invention have been formed as specifically described in the examples. Further, many compounds are prepared as more generally using a) alkylation of phenol/thiophenol with a halide, b) a Mitsunobu protocol (O. Mitsunobu, 1981 Synthesis, p1); c) and other methods known to the skilled artisan. Alternative synthesis methods may also be effective and known to the skilled artisan.
[0289] For example, an intermediate like A is alkylated with an alkylating agent B in the presence of a base (e.g. K2CO3, Cs2CO3 etc.). Hydrolysis in the presence of aqueous NaOH or LiOH gave the acid product.
[0290] Alternatively, an intermediate like A is coupled with an alcohol C under Mitsunobu reaction condition (DEAD/PPh3, ADDP/Pbu3 etc.). Hydrolysis in the presence of aqueous NaOH or LiOH gave the acid product:
[0291] Thioether analogs could also be prepared by a ZnI2 mediated thioether formation reaction as shown below:
[0292] Intermediates B, C and D can be made in one of the following methods. Coupling reaction between pyrazole and aryl boronic acid or Aryl halide in the presence of copper gave the 1-arylpyrazole:
[0293] Formylation under Vilsmeier-Haack reaction condition of the 3-arylpyrazole gave the 3-formyl pyrazole, sodium borohydride reduction afforded the primary alcohol. The secondary alcohol intermediates can be obtained by alkylation with a Grignard reagent.
[0294] Alternatively, the pyrazole intermediates can be made by the following method starting from β-ketoesters:
[0295] A Wittig reaction is used to extend chain at 4-position as shown in scheme 4:
[0296] Imidazole intermediate can be made according to scheme 5:
[0297] Isoxazole intermediate is obtained by the following cycloaddition reaction:
[0298] Triazole intermediate can be made by the following method:
EXEMPLIFICATION
[0299] The Examples provided herein are illustrative of the invention claimed herein and are not intended to limit the scope of the claimed invention in any way.
[0000] Instrumental Analysis
[0300] Infrared spectra are recorded on a Perkin Elmer 781 spectrometer. 1 H NMR spectra are recorded on a Varian 400 MHz spectrometer at ambient temperature. Data are reported as follows: chemical shift in ppm from internal standard tetramethylsilane on the δ scale, multiplicity (b=broad, s=singlet, d=doublet, t=triplet, q=quartet, qn=quintet and m=multiplet), integration, coupling constant (Hz) and assignment. 13 C NMR are recorded on a Varian 400 MHz spectrometer at ambient temperature. Chemical shifts are reported in ppm from tetramethylsilane on the δ scale, with the solvent resonance employed as the internal standard (CDCl 3 at 77.0 ppm and DMSO-d 6 at 39.5 ppm). Combustion analyses are performed by Eli Lilly & Company Microanalytical Laboratory. High resolution mass spectra are obtained on VG ZAB 3F or VG 70 SE spectrometers. Analytical thin layer chromatography is performed on EM Reagent 0.25 mm silica gel 60-F plates. Visualization is accomplished with UV light.
[0000] Preparation 1
2-(4-Hydroxy-2-methyl-phenoxy)-2-methyl-propionic acid
[0301]
Step A
2-(4-Benzyloxy-2-formylphenoxy)-2-methyl propionic acid ethyl ester
[0302] 5-Benzyloxy-2-hydroxy-benzaldehyde (Kappe, T.; Witoszynskyj, T. Arch. Pharm., 1975, 308 (5), 339-346) (2.28 g, 10.0 mmol), ethyl bromoisobutyrate (2.2 mL, 15 mmol), and cesium carbonate (3.26 g, 10.0 mmol) in dry DMF (25 mL) are heated at 80° C. for 18 h. The reaction mixture is cooled and partitioned between water (30 mL) and ether (75 mL). The organic layer is washed with brine (15 mL). The aqueous layers are back-extracted with ethyl acetate (30 mL), and the organic layer is washed with brine (20 mL). The combined organic layers are dried (Na 2 SO 4 ) and concentrated to a brown oil. The crude product is purified by flash chromatography using hexanes:ethyl acetate (2.5:1) to give a pale yellow solid (3.04 g, 89%): mp 65° C.; 1 H NMR (400 MHz, CDCl 3 ) δ 1.24 (t, 3H, J=7.1 Hz), 1.62 (s, 6H), 4.23 (q, 2H, J=7.1 Hz), 6.81 (d, 1H, J=8.8 Hz), 7.10 (dd, 1H, J=4.6, 9.0 Hz), 7.30-7.43 (m, 6H); MS (ES) m/e 343.1 [M+1].
[0000] Step B
2-(4-Hydroxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester
[0303] 2-(4-Benzyloxy-2-formyl-phenoxy)-2-methyl-propionic acid ethyl ester (9.00 g, 26.3 mmol) in ethanol (250 mL) is treated with 5% Pd/C (1.25 g) and hydrogen (60 psi, rt, overnight). Additional 5% Pd/C (1.25 g) is added, and the reaction is continued for 6 h at 40° C. The mixture is filtered and concentrated to a tan oil (6.25 g). This oil contained 9 mol % of 2-(4-Hydroxy-2-hydroxymethyl-phenoxy)-2-methyl-propionic acid ethyl ester. 1 H NMR (400 MHz, CDCl 3 ) δ 1.26 (t, 3H, J=7.3 Hz), 1.51 (s, 6H), 2.14 (s, 3H), 4.24 (q, 2H, J=7.3 Hz), 5.68 (brs, 1H), 6.47 (dd, 1H, J=3.4, 8.8 Hz) , 6.59 (d, 1H, J=8.3 Hz), 6.60 (brs, 1H).
[0304] The following compound is prepared in a similar manner:
[0000] Preparation 2
2-(4-Hydroxy-2-methyl-phenoxy)-acetic acid
[0305]
[0306] 1 H NMR (400 MHz, CDCl3) δ 1.28 (t, 3H, J=7.1 Hz), 2.24 (s, 3H), 4.25 (q, 2H, J=7.1 Hz), 4.55 (s, 2H), 6.56 (dd, 1H, J=2.7, 8.5 Hz), 6.61 (d, 1H, J=8.3 Hz), 6.65 (d, 2H, J=2.9 Hz).
[0000] Preparation 3
(4-Hydroxy-2-propyl-phenoxy)-acetic acid ethyl ester
[0307]
Step A
4-Benzyloxy-2-propylphenol
[0308] 2-Allyl-4-benzyloxyphenol (WO 9728137 A1 19970807, Adams, A. D. et al.) (5.00 g, 20.8 mmol) in ethyl acetate (40 mL) is treated with 5% Pd/C (0.25 g) and hydrogen (1 atm) at ambient temperature for 18 h. The mixture is filtered and concentrated. The crude product is purified on a Biotage medium pressure chromatography system using a 40 L normal phase cartridge and eluted with 10% ethyl acetate in hexanes to give a tan solid (2.8 g, 56%). Rf=0.33 (25% EtOAc/Hexanes) ; 1 H NMR (400 MHz, CDCl 3 ) δ 7.44-7.31 (m, 5H) 6.78 (s, 1H), 6.69 (d, J=1.5 Hz, 2H), 5.00 (s, 2H), 4.31 (s, 1H), 2.55 (t, J=7.6 Hz, 2H), 1.64 (q, J=7.5 Hz, 2H), 0.97 (t, J=7.3 Hz, 3H).
[0000] Step B
(4-Benzyloxy-2-propylphenoxy)acetic acid ethyl ester
[0309] A solution of 4-benzyloxy-2-propylphenol (0.50 g, 1.94 mmol) in dry DMF (7 mL) is cooled in an ice bath and treated with NaH (0.15 g, 3.8 mmol, 60% oil dispersion). The ice bath is removed, ethyl bromoacetate (0.43 mL, 3.9 mmol) is added, and the mixture is placed in an oil bath (T=85° C.). After 18 h, the reaction mixture is cooled and concentrated in vacuo. The residue is diluted with EtOAc, washed with brine (2×), dried (Na 2 SO 4 ), and concentrated. The crude product is purified by radial chromatography using 10% ethyl acetate in hexanes to give a tan solid (0.62 g; 97%). 1 H NMR (400 MHz, CDCl 3 ) δ 7.44-7.31 (m, 5H), 6.82 (d, J=2.9 Hz, 1H), 6.72 (dd, J=8.8, 2.9 Hz, 1H), 6.66 (d, J=8.8 Hz, 1H), 5.00 (s, 2H), 4.57 (s, 2H), 4.25 (q, J=7.0 Hz, 2H), 2.63 (t, J=7.6 Hz, 2H), 1.64 (q, J=7.5 Hz, 2H), 1.29 (t, J=7.1 Hz, 3H), 0.95 (t, J=7.3 Hz, 3H); MS (FIA) m/e 329 (M+1).
[0000] Step C
(4-Hydroxy-2-propylphenoxy)acetic acid ethyl ester
[0310] A solution of (4-benzyloxy-2-propylphenoxy)acetic acid ethyl ester (0.60 g, 1.83 mmol) in THF (15 mL) is treated with 5% Pd/C (75 mg) and hydrogen (60 psi) at ambient temperature for 24 h. The mixture is filtered and concentrated. The crude product is purified by radial chromatography using 15% ethyl acetate in hexanes to give a tan solid (0.25 g, 57%). 1 H NMR (400 MHz, CDCl 3 ) δ 6.66 (d, J=2.9 Hz, 1H), 6.62 (d, J=8.8 Hz, 1H), 6.57 (dd, J=8.8, 2.9 Hz, 1H), 4.56 (s, 1H), 4.40 (s, 1H), 4.25 (q, J=7.2 Hz, 2H), 2.61 (t, J=7.6 Hz, 2H), 1.63 (q, J=7.5 Hz, 2H), 1.29 (t, J=7.1 Hz, 3H), 0.95 (t, J=7.3 Hz, 3H); MS (FIA) m/e 239 (M+1).
[0000] Preparation 4
(3-Bromo-4-hydroxy-phenoxy)-acetic acid ethyl ester
[0311]
[0312] To a solution of (4-hydroxy-phenoxy)-acetic acid ethyl ester (0.59 g, 3 mmol) in acetic acid (1.5 mL) is added bromine (0.48 g, 9 mmol) in acetic acid (0.5 mL) at room temperature. After 5 min, solvent is evaporated and purified by column chromatography on silica gel giving the title compound (0.6 g).
[0000] Preparation 5
(4-Mercapto-phenoxy)-acetic acid ethyl ester
[0313]
Step A
(4-Chlorosulfonyl-phenoxy)-acetic acid ethyl ester
[0314] Phenoxy-acetic acid ethyl ester (9.1 mL) is added to chlorosulfonic acid (15 mL) at 0° C. dropwise. The reaction is stirred at 0° C. for 30 min, it is allowed to warm to room temperature. After 2 hrs, the reaction mixture is poured into ice, solid product is collected by filtration and dried under vacuum.
[0000] Step B
(4-Mercapto-phenoxy)-acetic acid ethyl ester
[0315] To a mixture of (4-chlorosulfonyl-phenoxy)-acetic acid ethyl ester (0.98 g, 3.5 mmol) and tin powder (2.1 g) in ethanol (4.4 mL) is added HCl in dioxane (1.0 M, 4.4 mL) under nitrogen. The mixture is heated to reflux for 2 hrs, it is poured into ice and methylene chloride and filtered. The layers are separated and extracted with methylene chloride, dried and concentrated. The crude product is used for next step without purification.
[0316] The following compounds are made in a similar manner:
[0000] Preparation 6
(4-Mercapto-2-methyl-phenoxy)-acetic acid ethyl ester
[0317]
[0318] This compound can also be made by the following procedure: To a stirred suspension of Zn powder (10 μm, 78.16 g, 1.2 mol) and dichlorodimethyl silane (154.30 g, 145.02 mL, 1.2 mol) in 500 mL of dichloroethane is added a solution of (4-chlorosulfonyl-2-methyl-phenoxy)-acetic acid ethyl ester (100 g, 0.34 mol) and 1,3-dimethylimidazolidin-2-one (116.98 g, 112.05 mL, 1.02 mol) in 1 L of DCE. Addition is at a rate so as to maintain the internal temperature at ˜52° C., cooling with chilled water as necessary. After addition is complete, the mixture is heated at 75° C. for 1 hour. It is then cooled to room temperature, filtered and concentrated iv. Add MTBE, washed twice with saturated LiCl solution concentrate iv again. Take up the residue in CH 3 CN, wash with hexane (4×) and concentrate iv to yield a biphasic mixture. Let stand in a separatory funnel and separate layers, keeping the bottom layer for product. Filtration through a plug of silica gel (1 Kg, 25% EtOAc/hexane) and subsequent concentration yields 61 g (79%) of a clear, colorless oil.
[0319] NMR (DMSO-d 6 ) δ 7.1 (s, 1H), 7.05 (dd, 1H), 6.75 (d, 1H), 5.03 (s, 1H), 4.75 (s, 2H), 4.15 (q, 2H), 2.15 (s, 3H), 1.2 (t, 3H).
[0000] Preparation 7
(4-Mercapto-2-propyl-phenoxy)-acetic acid ethyl ester
[0320]
Preparation 8
3-(4-Hydroxy-2-methyl-phenyl)-propionic acid methyl ester
[0321]
Step A
4-Bromo-3-methyl-phenyl benzyl ester
[0322] To a solution of 4-Bromo-3-methyl-phenol (20.6 g, 0.0.11 mol) in DMF (100 mL) is added Cs2CO3 (54 g, 0.165 mol), followed by benzyl bromide (14.4 mL). After stirred at 60° C. for 40 h, the reaction mixture is diluted with ethyl acetate, filtered through celite. The filtrate is washed with water and brine, dried over sodium sulfate, concentration yields the title product (27 g).
[0000] Step B
3-(4-Benzyloxy-2-methyl-phenyl)-propionic acid methyl ester
[0323] To a solution of 4-bromo-3-methyl-phenyl benzyl ester (7.6 g, 27.4 mmol) in propronitrile (200 mL) is added methyl acrylate (10 mL) and diisopropylethyl amine (9.75 mL), the solution is degassed and filled with nitrogen for three times. To this mixture are added tri-o-tolyl-phosphane (3.36 g) and palladium acetate (1.25 g) under nitrogen, then heated at 110° C. overnight, cooled to room temperature, filtered through celite. The solvent is evaporated, the residue is taken into ethyl acetate and washed with water and brine, dried over sodium sulfate. Concentration and column chromatography on silica gel eluted with hexanes and ethyl acetate yields the title compound (6.33 g).
[0000] Step C
3-(4-Hydroxy-2-methyl-phenyl)-propionic acid methyl ester
[0324] A mixture of 3-(4-Benzyloxy-2-methyl-phenyl)-propionic acid methyl ester (13.7 g, 48.5 mmol) and Pd/C (5%, 13.7 g) in MeOH (423 mL) is stirred under 60 psi of hydrogen for 24 hrs. Catalyst is filtered off, filtrate is concentrated giving the title compound (8.8 g, 93.5%).
[0000] Preparation 9
3-(4-Mercapto-2-methyl-phenyl)-propionic acid methyl ester
[0325]
Step A
3-(4-Dimethylthiocarbamoyloxy-2-methyl-phenyl)-propionic acid methyl ester
[0326] 3-(4-Hydroxy-2-methyl-phenyl)-propionic acid methyl ester (5.0 g, 25.75 mmol) is dissolved into dry dioxane (100 mL) and combined with 4-dimethylamino pyridine (0.500 g, 2.6 mmol), triethylamine (7.0 mL, 51.5 mmol), and dimethylaminothiocarbomoyl chloride (4.5 g, 32.17 mmol). The reaction is heated to reflux under nitrogen. The reaction is monitored by TLC until all of the phenol is consumed, 20 h. After cooling to room temperature, the reaction is diluted with ethyl acetate (200 mL). Water (75 mL) is added and the two layers are separated. The organic layer is washed with brine (75 mL) then dried over anhydrous sodium sulfate. The solvent is removed and the residue is dried under vacuum.
[0000] Step B
3-(4-Dimethylcarbamoylsulfanyl-2-methyl-phenyl)-propionic acid methyl ester
[0327] 3-(4-Dimethylthiocarbamoyloxy-2-methyl-phenyl)-propionic acid methyl ester, taken crude from the previous step, is diluted with 75 mL of tetradecane and heated to reflux under nitrogen. The reaction is monitored by TLC until all the conversion is complete, 20h. The reaction is allowed to cool to room temperature, then the tetradecane is decanted away from the resulting oil. The residue is-rinsed several times with hexanes. This oil is then purified using flash column chromatography, yielding 5.01 g, or 69% (2 steps) of the product.
[0000] Step C
3-(4-Mercapto-2-methyl-phenyl)-propionic acid methyl ester
[0328] 3-(4-Dimethylcarbamoylsulfanyl-2-methyl-phenyl)-propionic acid methyl ester (5.01 g, 17.8 mmol)-is diluted with methanol (30 mL) and to this is added sodium methoxide (1.7 mL of 4M in methanol, 7.23 mmol). The reaction is heated to reflux under nitrogen and monitored by TLC. After complete conversion, 20 h., the reaction is allowed to cool to room temperature. The reaction is neutralized with 1N HCl (7.23 mL) and diluted with ethyl acetate (150 mL). The two phases are separated and the organic layer is washed with water (75 mL), then brine (75 mL). The organic layer is then dried over anhydrous sodium sulfate, then concentrated to yield 4.43 g crude product that is used without further purification.
[0000] Preparation 10
4-(2-Methoxycarbonyl-ethyl)-3-methyl-benzoic acid
[0329]
Step A
4-Bromo-3-methyl-benzoic acid benzyl ester
[0330] To a solution of 4-Bromo-3-methyl-benzoic acid benzyl (25.3 g, 0.118 mol) in DMF (200 mL) is added Cs2CO3 (76.6 g, 0.235 mol), followed by benzyl bromide (15.4 mL). After stirred at room temperature for 2 h, the reaction mixture is diluted with ethyl acetate, filtered through celite. The filtrate is washed with water and brine, dried over sodium sulfate, concentration yields the title product.
[0000] Step B
4-(2-Methoxycarbonyl-vinyl)-3-methyl-benzoic acid benzyl ester
[0331] To a solution of 4-bromo-3-methyl-benzoic acid benzyl ester (36 g, 118 mmol) in propronitrile (1000 mL) is added methyl acrylate (43.3 mL) and diisopropylethyl amine (42 mL), the solution is degassed and filled with nitrogen for three times. To this mixture are added tri-o-tolyl-phosphane (14.5 g) and palladium acetate (5.34 g) under nitrogen, then heated at 110° C. overnight, cooled to room temperature, filtered through celite. The solvent is evaporated, the residue is taken into ethyl acetate and washed with water and brine, dried over sodium sulfate. Concentration and column chromatography on silica gel-eluted with hexanes and ethyl acetate yields the title compound (31 g, 84.7%).
[0000] Step C
4-(2-Methoxycarbonyl-ethyl)-3-methyl-benzoic acid
[0332] A mixture of 4-(2-methoxycarbonyl-vinyl)-3-methyl-benzoic acid benzyl ester (11.6 g, 37.4 mmol) and Pd/C (5%, 1.5 g) in THF (300 mL) and methanol (100 mL) is stirred under 60 psi of hydrogen overnight. Catalyst is filtered off, filtrate is concentrated giving the title compound (8.3 g, 100%).
[0000] Preparation 11
(4-Hydroxy-2-methyl-phenyl)-acetic acid methyl ester
[0333]
Step A
[0334] 4-Methoxy-2-methylbenzoic acid (2.5 g, 15.04 mmol) is stirred in thionyl chloride (50 mL) at reflux 2 hr. The mixture is concentrated and diluted with toluene (10 mL) and concentrated. The resulting solid is dried under vacuum 18 hr. The resulting acid chloride is stirred in 20 mL ether at 0 deg C. A solution of diazomethane (39.6 mmol) in ether (150 mL) is added to the acid chloride solution and stirred 18 hr. The resulting diazoketone solution is concentrated. The residue is stirred in methanol (100 mL) and a solution of silver benzoate in triethylamine (1.0 g in 10 mL) is added and the reaction is heated to 60 deg C. and stirred 1 hr. The mixture is concentrated, diluted with 1.0 N aqueous hydrochloric acid (20 mL), extracted to three portions of ethyl acetate (50 mL each). The extracts are combined, washed with aqueous saturated sodium hydrogen carbonate, water, and brine (50 mL each), dried over anhydrous magnesium sulfate, filtered and concentrated. The residue is purified via silica gel chromatography eluting with 9:1 hexanes:ethyl acetate to afford 1.5 g (51%) of the homologated ester as a white solid.
[0000] Step B
[0335] (4-Methoxy-2-methyl-phenyl)-acetic acid methyl ester (1.5 g, 7.72 mmol) is stirred in dichloromethane (50 mL) at 0 deg. C. Aluminum chloride (4.13 g, 31 mmol) is added followed by ethane thiol (2.9 mL, 38.6 mmol) . The resulting mixture is stirred at room temperature for 2 hr. Water (50 mL) is added and the product is extracted into ethyl acetate (3×50 ml), the extracts are combined, dried over anhydrous magnesium sulfate, filtered, and concentrated to afford the title compound as a colorless oil, 1.4 g, 100%. MS M + +1 181. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 12
(3-Hydroxy-phenyl)-acetic acid methyl ester
[0336]
Step A
(3-Hydroxy-phenyl)-acetic acid methyl ester
[0337] (3-Hydroxy-phenyl)-acetic acid (5.0 g, 32.86 mmol) is stirred in methanol (100 mL) and concentrated (98%) sulfuric acid (3.0 mL,) is added. The mixture is heated to reflux 18 hr. The reaction is cooled and concentrated. The residue is diluted with water (100 mL) and extracted with ethyl acetate (3×50 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered, and concentrated to yield the title compound as an orange oil, 5.46 g, 100%. MS M + +1 167. The structure is confirmed by 1 H NMR spectroscopy.
[0338] The following compounds are made in a similar manner:
Preparation 13
(3-Hydroxy-4-methoxy-phenyl)-acetic acid methyl ester
[0339]
[0340] An orange oil. MS M + +1 197. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 14
3-(3-Hydroxy-phenyl)-propionic acid methyl ester
[0341]
Step A
3-(3-Hydroxy-phenyl)-propionic acid methyl ester
[0342] An orange oil. MS M + +1 181. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 15
(3-Mercapto-phenyl)-acetic acid methyl ester
[0343]
Step A
(3-Dimethylthiocarbamoyloxy-phenyl)-acetic acid methyl ester
[0344] A mixture of (3-Hydroxy-phenyl)-acetic acid methyl ester (5.5 g, 33.1 mmol) , N,N-dimethyl thiocarbamoyl chloride (5.11 g, 41.38 mmol), triethylamine (9.2 mL, 66.2 mmol), N,N-dimethylamino pyridine (0.4 g, 3.31 mmol) and dioxane (50 mL) is stirred at reflux 18 hr. The mixture is concentrated, partioned between 1M aqueous hydrochloric acid (200 mL) and ethyl acetate (3×75 mL). The combined organic extracts are dried over anhydrous magnesium sulfate, filtered, concentrated, and purified via silica chromatography eluting the product with dichloromethane to afford the title compound as a brown oil, 6.8 g, 81%. MS M + +1 254. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Step B
(3-Dimethylcarbamoylsulfanyl-phenyl)-acetic acid methyl ester
[0345] (3-Dimethylthiocarbamoyloxy-phenyl)-acetic acid methyl ester (6.8 g, 26.84 mmol) is stirred in tetradecane (30 mL) at 255 deg C. for 8 hr. The mixture is cooled, the residue is purified by silica chromatography eluting the product with hexanes to 1:1 hexanes:ethyl acetate to afford the title compound as an orange oil, 4.9 g, 58%. MS M + +1 254. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Step C
(3-Mercapto-phenyl)-acetic acid methyl ester
[0346] A mixture of (3-dimethylcarbamoylsulfanyl-phenyl)-acetic acid methyl ester (2.0 g, 7.9 mmol), potassium hydroxide (1.4 g, 24 mmol) methanol (50 mL), and water (5 mL) is stirred at reflux 3 hr. The mixture is concentrated, and product partitioned between 1M aqueous hydrochloric acid (50 mL) and ethyl acetate (3×75 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered and concentrated. The residue is taken up in methanol (50 mL), 2 mL concentrated sulfuric acid is added, and the mixture refluxed 3 hr. The mixture is concentrated, and the residue purified by silica chromatography eluting with 7:3 hexanes:ethyl acetate to afford the title compound as a pale yellow oil, 1.0 g, 69%. MS M + +1 183. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 16
3-(4-Iodomethyl-2-methyl-phenyl)-propionic acid methyl ester
[0347]
Step A
3-(4-Hydroxymethyl-2-methyl-phenyl)-acrylic acid methyl ester
[0348] A mixture of methyl-4-bromo-3-methylbenzoate (5.7 g, 24.88 mmol), lithium aluminum hydride (29 mL, 29 mmol, 1 M solution in tetrahydrofuran) and tetrahydrofuran (100 mL) is stirred in ice/water for 1 hr. The reaction is quenched with aqueous hydrochloric acid (50 mL, 1 M). The product is extracted into ethyl acetate (3×100 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered and concentrated. The crude product is taken up in propionitrile (100 mL). Methylacrylate (10 mL, 121.5 mmol), palladium acetate (1.12 g, 5 mmol), tri-o-tolylphosphine (3.0 g, 10 mmol), and N,N-diisopropyl ethylamine (8.7 mL, 50 mmol) are sequentially added and the resulting reaction mixture is heated to 110 deg C. 3 hr. The mixture is concentrated, and the residue diluted with aqueous hydrochloric acid (100 mL, 1M). The product is extracted with dichloromethane (2×100 mL) and ethyl acetate (100 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered, concentrated, and purified via silica chromatography eluting with 7:3 hexanes:ethyl acetate to 1:1 hexanes:ethyl acetate to afford the pure product as a yellow oil, 4.7 g, 91%. MS M + +1 207. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Step B
3-(4-Hydroxymethyl-2-methyl-phenyl)-propionic acid methyl ester
[0349] A mixture of 3-(4-Hydroxymethyl-2-methyl-phenyl)-acrylic acid methyl ester (4.7 g, 22.8 mmol), Raney nickel (0.668 g) and tetrahydrofuran (618 mL) is shaken under 60 psig. Hydrogen 24 hr. The catalyst is filtered off, and the mixture is concentrated to afford the product as a pale yellow oil, 4.3 g, 91%. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Step C
3-(4-Iodomethyl-2-methyl-phenyl)-propionic acid methyl ester
[0350] A mixture of 3-(4-Hydroxymethyl-2-methyl-phenyl)-propionic acid methyl ester (0.62 g, 2.98 mmol), triphenyl phosphine (0.86 g, 3.27 mmol) and dichloromethane (10 mL) is stirred at room temperature. A solution of iodine (0.83 g, 3.27 mmol) in benzene (5 mL) is added and the black mixture is stirred at room temperature 2 hr. The brown mixture is diluted with 10% aqueous sodium hydrogen sulfite (5 mL) and the resulting clear mixture is washed with ethyl acetate (3×50 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered and concentrated. The residue is purified via silica chromatography eluting with 9:1 hexanes:ethyl acetate to afford the title compound as a crystalline ivory solid, 0.68 g, 72%. MS M + +1 319. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 17
(4-Bromo-2-methyl-phenoxy)-acetic acid methyl ester
[0351]
Step A
(4-Bromo-2-methyl-phenoxy)-acetic acid methyl ester
[0352] A mixture of 4-bromo-2-methylphenol (1.0 g, 5.35 mmol), sodium hydride (0.26 g, 6.42 mmol, 60% mineral oil), N,N-dimethylformamide (10 mL), and methyl-2-bromoacetate (0.56 mL, 5.88 mmol) is stirred at room temperature 18 hr. The mixture is diluted with water (50 mL) and the product extracted to ethyl acetate (3×50 mL). The combined extracts are dried over anhydrous magnesium sulfate, filtered, concentrated and purified via silica chromatography eluting with 8:2 hexanes:ethyl acetate to afford title compound as a colorless oil, 1.03 g, 74%. MS M + 259. The structure is confirmed by 1 H NMR spectroscopy.
[0000] Preparation 18
3-(4-Amino-2-methyl-phenyl)-propionic acid methyl ester
[0353]
Step A
3-(2-Methyl-4-nitro-phenyl)-acrylic acid methyl ester
[0354] To a solution of 2-bromo-5-nitrotoluene (3.11 g, 14.39 mmol) in propionitrile (105 mL) is added DIPEA (5.1 mL, 29.28 mmol). The mixture is degassed three times. Methyl acrylate (5.2 mL, 57.74 mmol) is added and the mixture is degassed. Tri-o-tolylphosphine (1.77 g, 5.82 mmol) and Pd(OAc) 2 (0.64 g, 2.85 mmol) are added and the mixture is degassed a final two times followed by heating at 110° C. for 4 h. Upon cooling, the mixture is passed through Celite and the filtrate is concentrated. The residue is partitioned between Et 2 O and 1N HCl. The organics are washed with saturated NaHCO 3 and brine, and dried, with Na 2 SO 4 . The crude material is purified by flash chromatography to yield the title compound (2.90 g, 91%).
[0000] Step B
3-(4-Amino-2-methyl-phenyl)-propionic acid methyl ester
[0355] A mixture of 3-(2-Methyl-4-nitro-phenyl)-acrylic acid methyl ester (1.47 g, 6.64 mmol) and 5% Pd/C (0.29 g) in MeOH (100 mL) is exposed to a hydrogen atmosphere (60 psi) for 12 h. The mixture is filtered through Celite and purified by flash chromatography to yield the title compound (0.99 g, 77%).
[0000] Preparation 19
3-(2-Methyl-4-methylaminomethyl-phenyl)-propionic acid methyl ester TFA salt
[0356]
Step A
3-(4-Formyl-2-methyl-phenyl)-propionic acid methyl ester
[0357] A mixture of 3-(4-Hydroxymethyl-2-methyl-phenyl)-propionic acid methyl ester (0.49 g, 2.35 mmol) and MnO, (0.80 g, 9.20 mmol) in chloroform (5 mL) is stirred at RT for 4 days. The mixture is filtered through Celite; the Celite is washed with copious amounts of EtOAc. The filtrate is concentrated and purified by flash chromatography to yield the title compound (0.29 g, 60%).
[0000] Step B
3-(2-Methyl-4-methylaminomethyl-phenyl)-propionic acid methyl ester trifluoroacetic acid
[0358] To a mixture of 3-(4-Formyl-2-methyl-phenyl)-propionic acid methyl ester (0.27 gi 1.31 mmol) and methylamine (2M in THF, 0.60 mL, 1.20 mmol) in anhydrous CH 2 Cl 2 (10 mL) is added 4 Å molecular sieves followed by acetic acid (0.090 mL, 1.57 mmol). The mixture is stirred at RT for 1.5 h. Sodium triacetoxyborohydride (0.39 g, 1.85 mmol) is added, and the mixture is stirred overnight. The reaction is quenched with saturated NaHCO 3 . The organics are washed with saturated NaHCO 3 and brine, and dried with MgSO 4 . Upon concentration, the mixture is purified by reverse phase chromatography to yield the title compound (0.12 g, 455%).
[0000] Preparation 20
3-(4-Aminomethyl-2-methyl-phenyl)-propionic acid methyl ester
[0359]
Step A
3-(4-Chloromethyl-2-methyl-phenyl) -propionic acid methyl ester
[0360] To a 0° C. solution of 3-(4-Hydroxymethyl-2-methyl-phenyl)-propionic acid methyl ester (1.02 g, 4.90 mmol) in anhydrous CH 2 Cl 2 (15 mL) is added triethylamine (0.75 mL, 5.38 mmol) followed by thionyl chloride (0.40 mL, 5.48 mmol). The mixture is allowed to warm to RT overnight. Water is added, and the mixture is extracted with CH 2 Cl 2 . The organics are dried with MgSO 4 and concentrated. The crude material is purified by flash chromatography to yield the title compound (1.01 g, 91%).
[0000] Step B
3-(4-Azidomethyl-2-methyl-phenyl)-propionic acid methyl ester
[0361] To a solution of 3-(4-Chloromethyl-2-methyl-phenyl)-propionic acid methyl ester (0.52 g, 2.31 mmol) in DMF (7 mL) is added sodium azide (0.25.g, 3.84 mmol). The mixture is stirred overnight. Water is added, and the mixture is extracted with EtOAc. The organics are dried with Na 2 SO 4 and concentrated to yield the title compound (0.49 g, 91%). The material is used without further purification.
[0000] Step C
3-(4-Aminomethyl-2-methyl-phenyl)-propionic acid methyl ester
[0362] A mixture of 3-(4-Azidomethyl-2-methyl-phenyl)-propionic acid methyl ester (0.20 g, 0.86 mmol) and 5% Pd/C (32 mg) in EtOH (50 mL) is exposed to a hydrogen atmosphere (60 psi) at RT overnight. Upon filtering the mixture through Celite, the filtrate is concentrated-to yield the title compound (0.14 g, 78%). The material is used without further purification.
[0000] Preparation 21
(3-Chloro-4-mercapto-phenyl)-acetic acid methyl ester
[0363]
[0364] This compounds is made from the corresponding phenol analog based on the method outlined in preparation 9.
[0000] Preparation 22
2-(3-Hydroxy-phenyl)-2-methyl-propionic acid ethyl ester
[0365]
Step A
2-(3-Methoxy-phenyl)-propionic acid ethyl ester
[0366]
[0367] To a solution of LDA (2M, 16.5 mL) in THF (10 mL) at −70° C. is added a solution of (3-methoxy-phenyl)-acetic acid methyl ester (5.4 g, 30 mmol) in THF (10 mL). After 40 minutes at −70° C., iodomethane (2.5 mL, 40 mmol) is added. The mixture is stirred at room temperature overnight. It is diluted with EtOAc, washed with 1N HCl. The organic layer is dried over Na2SO4 and concentrated to give the titled compound as an oil: 5.9 g (quant.)
[0000] Step B
2-(3-Methoxy-phenyl)-2-methyl-propionic acid ethyl ester
[0368]
[0369] To a solution of LDA (2M, 11.4 mL) in THF (10 mL) at −70° C. is added a solution of 2-(3-methoxy-phenyl)-propionic acid ethyl ester (4g, 20.6 mmol) in THF (10 mL). After 1 hour at −70° C., iodomethane (1.7 mL, 26.8 mmol) is added and the mixture is stirred at room temperature overnight. It is diluted with EtOAc and washed with 1N HCl. The organic is concentrated to give the titled compound as an oil: 4 g (93%).
[0000] Step C
2-(3-Hydroxy-phenyl)-2-methyl-propionic acid ethyl ester
[0370]
[0371] To a solution of 2-(3-Methoxy-phenyl)-2-methyl-propionic acid ethyl ester (4 g, 19.2 mmol) in dichloromethane (20 mL) at 0 0C. is added BBr3 (1M in dichloromethane, 50 mL). After 2 hours at ambient temperature, it is quenched with MeOH. Solvent is evaporated and the residue is partitioned between EtOAc and 1N HCl. The organic is concentrated and purified by column chromatography (0 to 30% EtOAc in hexanes) to give the titled compound as a solid: 2.6 g (70%). ESMS—: 193 (M—1); 1H NMR is consistent with desired product.
[0000] Preparation 23
4-Chloromethyl-3-methyl-1-phenyl-1H-pyrazole
[0372]
Step A
3-Methyl-1-phenyl-1H-pyrazole-4-carbaldehyde
[0373]
[0374] Phosphoryl chloride (2.62 g, 17.1 mmol) is added dropwise to a solution of 3-methyl-1-phenyl-1H-pyrazole (2.7 g, 17.1 mmol) in DMF (1.25 g, 17.1 mmol) at 100° C. After heated 3hrs, the reaction mixture is cooled with ice bath and quenched by water. The resulting mixture is basified by 5N NaOH to pH=4, extracted with ethyl acetate, dried, concentrated. Column chromatography on silica gel yields the title compound.
[0000] Step B
(3-Methyl-1-phenyl-1H-pyrazol-4-yl)-methanol
[0375] To a solution of 3-Methyl-1-phenyl-1H-pyrazole-4-carbaldehyde (0.9 g, 4.84 mmol) in ethanol (20 mL) is added sodium borohydride (0.18 g, 4.84 mmol) at 0˜5° C., warmed to room temperature. After stirred for 2hrs, quenched by water, ethanol is evaporated. The resiude is diluted with water and extracted with ethyl acetate, dried over sodium sulfate. Concentration yields the title compound.
[0000] Step C
4-Chloromethyl-3-methyl-1-phenyl-1H-pyrazole
[0376] A solution of (3-methyl-1-phenyl-1H-pyrazol-4-yl)-methanol (0.7 g, 3.72 mmol) and triethyl amine (1.04 mL, 7.4 mmol) in methylene chloride (16 mL) is cooled to 0° C., then MeSO2Cl (0.46 mL, 5.95 mmol) is added dropwise. After 4 hrs, the reaction mixture is diluted with methylene chloride and washed with sodium bicarbonate, water and brine, dried over sodium sulfate. Concentration yields the crude title compound, which is used for the next step without further purification.
[0000] Preparation 24
4-Chloromethyl-3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-Pyrazole
[0377]
Step A
[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0378]
[0379] A THF (5 mL) solution of 3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carboxylic acid ethyl ester (1.0 g, 3.2 mmol) is cooled to 0° C. and a 1M LiAlH 4 (3.2 mL, 3.2 mmol) is added slowly. The reaction is warmed to room temperature slowly, after stirring at room temperature for 2 h, tlc (15% EtOAc/hexane) showed that all the starting ester had been consumed. The reaction is cooled and carefully quenched with water, 5N NaOH. The light tan solid is filter through celite and dried to give 0.86 g of the title compound.
[0000] Step B
4-Chloromethyl-3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0380] A solution of [3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol (0.86 g, 3.2 mmol) and triethyl amine 0.9 mL, 6.4 mmol) in methylene chloride (16 mL) is cooled to 0° C., then MeSO2Cl (0.4 mL) is added dropwise. After 2 hrs, TLC indicated that the reaction is not complete, 10 mol % more of triethyl amine and MeSO 2 Cl are added. After additional 2 hrs, the reaction mixture is diluted with methylene chloride and washed with sodium bicarbonate, water and brine, dried over sodium sulfate. Concentration yields the crude title compound, which is used for the next step without further purification.
[0381] The following compounds are made in a similar manner:
[0000] Preparation 25
1-(3,5-Bis-trifluoromethyl-phenyl)-4-chloromethyl-5-methyl-1H-pyrazole
[0382]
Preparation 26
[3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-methanol
[0383]
Step A
5-Methyl-2-(4-trifluoromethoxy-phenyl)-2,4-dihydro-pyrazol-3-one
[0384]
[0385] To a solution of the trifluoromethoxyphenyl hydrazine HCl salt (10.36 g, 45.3 mmol) and toluene (250.0 ml) at room temperature is added sodium hydroxide (1.04 g). After stirred overnight, the mixture is treated with ethyl acetoacetate (48.09 mL, 0.38 m). Reaction mixture is then stirred at room temperature for 66 hrs, diluted with ethyl acetate, washed with water, dried over sodium sulfate. Concentration and column chromatography on silica gel yields the title compound (9.3 g).
[0000] Step B
5-Chloro-3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde
[0386]
[0387] To DMF (5.03 mL) at 10° C. is added POCl 3 (6.1 mL) over a period of 30 minutes, to this solid is then added 5-Methyl-2-(4-trifluoromethoxy-phenyl)-2,4-dihydro-pyrazol-3-one (9.3 g, 32.4 mmol), followed by 5.03 mL of DMF. The reaction mixture is slowly heated to 100° C., an additional POCl 3 (6.1 mL) is added after 18 hrs. Heating is continued for another 6 hrs before the reaction mixture is very carefully reversed quenched into crushed ice, extracted with CH 2 Cl 2 , washed with 2N NaOH and brine, dried over sodium sulfate. Concentration and column chromatography on silica gel eluted with hexanes/ethyl acetate yields the title compound (9.6 g).
[0000] Step C
3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde
[0388]
[0389] To 5-chloro-3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde (5.7 g, 17 mmol) dissolved in EtOH (188 mL) is added Et 3 N (4.8 mL) and Lindlar catalyst (0.476 g). The mixture is then hydrogenated at room temperature (50 psi). After 2.5 hrs, reaction mixture is the filtered through celite, concentrated to a solid. Column chromatography n silica gel eluted with hexanes/ethyl acetate yields the title compound (3.4 g, 66.5% yiel, and [3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-methanol (0.85 g, 16.5% yield).
[0000] Step D
[3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-methanol
[0390]
[0391] To a solution of 3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde (0.76 g, 2.55 mmol) in ethanol (10 mL) is added NaBH4 (0.1 g, 2.64 mmol). After 2 hrs, the reaction is quenched by water, ethanol is evaporated and the residue is extracted with ethyl acetate, dried. Concentration yields the title compound (0.75 g).
[0000] Preparation 27
1-[3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethanol
[0392]
[0393] To a solution of 3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde (3.4 g, 11.4 mmol) tetrahydrofuran (80 mL) is added methyl magnesium bromide (4.6 mL, 13.7 mmol, 3 M in ether) dropwise at 0° C., the resulting mixture is allowed to stir at room temperature 30 min. The reaction mixture is quenched by aqueous ammonium chloride (30 mL), extracted with ethyl acetate, the combined extracts are dried over anhydrous magnesium sulfate, filtered and concentrated. Column chromatography on silica gel eluted with hexanes/ethyl acetate yields the title compound (3.3 g).
[0000] Preparation 28
[5-Chloro-3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-methanol
[0394]
[0395] To a solution of 5-chloro-3-methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazole-4-carbaldehyde (1.0 g, 3.0 mmol) in ethanol (10 mL) is added NaBH4 (0.113 g, 3 mmol). After 2 hrs, the reaction is quenched by water, ethanol is evaporated and the residue is extracted with ethyl acetate, dried. Concentration yields the title compound (0.95 g).
[0000] Preparation 29
[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0396]
Step A
[0397] The intermediate obtained from Step A is obtained from two separate methods.
[0000] Method 1
3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0398] To a solution of 4-(trifluoromethyl)phenylboronic acid (5.04 g, 26.5 mmol), 3-methylpyrazole (1.1 ml, 13.2 mmol), and pyridine (2.1 ml, 26.5 mmol) in dichloromethane (160 ml) is added copper (II) acetate (3.61 g, 19.9 mmol) and 4A molecular sieves (10.0 g). The suspension is stirred at ambient temperature in the open air for 48 hours, then filtered through Celite and concentrated in vacuo to a crude solid. Purification by silica flash chromatography (40:1 hexanes:ethyl acetate to 10:1 hexanes:ethyl acetate) yields the title compound as a white solid. MS: m/z (M+1) 227
[0000] Method 2
3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0399] A mixture of 4-iodobenzotrifluoride (246 g, 0.904 mol), 3-methylpyrazole (90 g, 1.09 mol) and potassium carbonate (254 g, 1.83 mol) in 1,4-dioxane (1L) under N 2 is treated with cupric iodide (1.75 g, 9.1 mmol) and trans-1,2-cyclohexanediamine (7.5 ml, 62.4 mmol) and heated at 110° C. for 30 hours. The mixture is cooled and diluted with water (1.5 L) and ethyl acetate (1.5 L). The organic layer is washed with water (1 L) and concentrated to an oil. Purification by silica flash chromatography (4:1 hexanes:ethyl acetate) yields the title compound as a white solid. MS: m/z (M+1) 227
[0000] Step B
3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde
[0400] This compound can be prepared by the following two different method:
[0000] Method I
[0401] To a solution of 3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (1.88 g, 8.31 mmol) in DMF (8.0 ml) heated at 90° C. is carefully added phosphorous oxychloride (1.0 ml, 10.8 mmol) and the resulting mixture heated at 90° C. for 7 hours. Additional phosphorous oxychloride (0.75 ml, 8.0 mmol) is added and the mixture heated for an additional 2 hours. The mixture is cooled at 0° C., then carefully treated with cold water (75 ml). After dilution with diethyl ether (40 ml) to dissolve solids, the mixture is adjusted to pH 3 with 5 N NaOH. The aqueous layer is extracted with diethyl ether (2×25 ml), the organic extracts then combined and washed with water, brine, dried (Na 2 SO 4 ) and concentrated to a crude solid. Purification by silica flash chromatography (20:1 hexanes:ethyl acetate to 5:1 hexanes:ethyl acetate) provided the title compound as a white solid. MS: m/z (M+1) 255.
[0000] Method II
[0402] Step A of method II
[0403] To a solution of the Trifluoromethylphenyl Hydrazine (60.4 g, 0.34 moles) and toluene (250.0 mL) at room temperature is added ethylacetoacetate (48.09 mL, 0.38 m). Reaction solution is then stirred overnight at r.t. for 12 hrs (N.B. reaction generally becomes hazy after an hour of stirring). Heated at reflux with continuous azeotropic removal of water and volatile organic solvents for another 12 hrs (note: the volume of toluene removed during azeotrope should be replaced during the course of the reaction). Reaction is monitored by TLC (1:1 EtoAc/Heptane). After the reaction is deemed to be complete, heptane (500.0 mL) is added to the hot solution. An off tan precipitate is observed upon equilibration to ambient temperature. The tan precipitate is filtered and the cake washed with heptane (75.0 mL), dried in an oven at 50° C. overnight (mass=75.39 g; 90% wt. Yield; 1 H (CDCl 3 +DMSO d 6 ) δ 1.82 (s, 3H), 3.16 (s, 2H), 7.22-7.25 (d, 2H, J=8.8 Hz), 7.57-7.59 (d, 1H, J=8.8 Hz), 7.66-7.68 (d, 1H, J=8.5 Hz).
Step B of method II
[0404] To DMF (44.56 mL, 0.57 m) at 10° C. is added POCl 3 (52.68 mL, 0.57 m) over a period of 30 minutes (caution solution solidifies after addition). To this solid is then added the pyrazolone (70.0 g, 0.28 m). Slowly heated mixture until dissolution is observed at 75-80° C. (To aid the dissolution, an extra 40 mL of DMF is added). The dark reaction solution is then heated at 90-100° C. for 18 hrs, after which an additional POCl 3 (52.6 mL) is added (reaction is monitored by TLC 1:1 EtoAc/Heptane). Heating is continued for another 6 hrs before the reaction mixture is very carefully reversed quenched into crushed ice over a period of 2 hrs. (Extreme caution: quenching is quite exothermic and should be done very carefully. Possible induction period can be observed during quenching of excess POCl 3 ). A dark brown precipitate is observed after quenching. On equilibration to r.t., the precipitate is extracted with CH 2 Cl 2 (500.0 mL), washed with 2N NaOH (2×500 ml), treated with Darco and anh. MgSO 4 . Subsequent filtration over hyflo and concentration at reduced pressure on the rotovap afforded a tan precipitate (mass=72.0 g). The purity of the precipitate can be upgraded by dissolving it in a hot EtoAc (200 ml), followed by a quick plug over silica gel. Concentration of the filtrate on the rotovap affords a tan solid (mass=68.4 g; 82% wt. Yield; 1 H (CDCl 3 ) δ 2.54 (s, 3H), 7.72-7.81 (m, 4H), 9.99 (s, 1H, C H O).
Step C of method II
[0405] To Chloro/formyl starting material (520 mg, 1.8 mm) dissolved in EtOH (20.0 mL) is added Et 3 N (0.5 mL) and Lindlar catalyst (0.05 g). The mixture is then hydrogenated at r.t (50 psi). After 2.5 hrs, 1 H nmr of an aliquot after a brief work up indicated product with no observable starting material. Reaction mixture is the filtered over hyflo, concentrated to a solid. To the solid is added CH 2 Cl 2 (40.0 mL) and 1NHCl (20.0 mL) with stirring. Subsequent separation of lower organic layer, drying and concentrating on the rotovap afforded a tan precipitate (mass=455 mg; 100% wt. yield; 1 H (CDCl 3 ) δ 2.57 (s, 3H), 7.71-7.74 (d, 2H, J=8.4 Hz), 7.82-7.85 (d, 2H, J=8.5 Hz), 8.43 (s, 1H), 10.00 (s, 1H, C H O).
[0000] Step C
[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0406] To a chilled (0° C.) suspension of 3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (350 mg, 1.37 mmol) in ethanol (6 ml) is added sodium borohydride (52 mg, 1.37 mmol) portionwise over two minutes. The reaction mixture is removed from the cold bath and stirred for one hour. After quenching with water (25 ml), the reaction mixture is extracted with diethyl ether (3×15 ml). The combined organic extracts are washed with water, brine, then dried (Na 2 SO 4 ) and concentrated to provide the title compound as a white solid. MS: m/z (M+1) 257.
[0000] Preparation 30
1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol
[0407]
[0408] To a cooled (0° C.) solution of 3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (500 mg, 1.96 mmol) in tetrahydrofuran (2.5 ml) is added a solution of methyl magnesium bromide (3M in diethyl ether)(0.98 ml, 2.94 mmol) over 4 minutes. The mixture is removed from the cold bath and stirred for two hours, then cooled again to 0° C. and treated with saturated aqueous ammonium chloride (30 ml) followed by water (20 ml). After extraction with ethyl acetate (3×20 ml), the combined organic extracts are washed with brine, then dried (Na 2 SO 4 ) and concentrated to a crude solid. Purification by silica flash chromatography (20:1 hexanes:ethyl acetate to 3:1 hexanes:ethyl acetate) provided the title compound as a racemic white solid.
[0409] MS: m/z (M+1) 271.
[0000] Preparation 31
1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0410]
[0411] To a cooled (0° C.) solution of 3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (300 mg, 1.18 mmol) in tetrahydrofuran (3.0 ml) is added a solution of ethyl magnesium bromide (3M in diethyl ether)(0.59 ml, 1.77 mmol) over 2 minutes. The mixture is removed from the cold bath and stirred for 3 hours, then cooled again to 0° C. and treated with saturated aqueous ammonium chloride and water. After extraction with ethyl acetate (3×15 ml), the combined organic extracts are washed with brine, then dried (Na 2 SO 4 ) and concentrated to a crude solid. Purification by silica flash chromatography (25:1 hexanes:ethyl acetate to 4:1 hexanes:ethyl acetate) provided the title compound as a racemic white solid. MS: m/z (M+1): 285.
[0000] Preparation 32
2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0412]
Step A
1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone
[0413] To a solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol (2.95 g, 10.9 mmol) in chloroform (80 ml) is added activated manganese (IV) dioxide (9.5 g, 109 mmol), and the resulting suspension heated at reflux for 36 hours. The mixture is cooled and filtered through Celite, washed with chloroform, and the filtrate concentrated to a crude solid. Purification by silica flash chromatography (20:1 hexanes:ethyl acetate to 2:1 hexanes:ethyl acetate) provided the title compound as a white solid. MS: m/z (M+1) 269.
[0000] Step B
4-(2-Methoxy-1-methyl-vinyl)-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0414] A solution of potassium tert-butoxide (3.74 g, 33.3 mmol) in tetrahydrofuran (25 ml) is added dropwise over 15 minutes to a cooled (0° C.) suspension of methoxymethyltriphenylphosphonium chloride (11.41 g, 33.3 mmol) in tetrahydrofuran (35 ml) . The mixture is stirred at 0° C. for 20 minutes and then treated dropwise over 5 minutes with a solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone (3.0 g, 11.1 mmol) in tetrahydrofuran (20 ml). After addition is complete, the mixture is removed from the cold bath and stirred for 2 hours, then diluted with brine (300 ml) and diethyl ether (150 ml). The organic layer is removed, and the remaining aqueous layer extracted with diethyl ether (2×25 ml). The organic extracts are combined, washed with brine, dried (Na 2 SO 4 ), and concentrated to an oil which is purified by silica flash chromatography (30:1 hexanes:ethyl acetate to 8:1 hexanes:ethyl acetate) to provide the title compound as an oil. MS: m/z (M+1) 297.
[0000] Step C
2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propionaldehyde
[0415] A cooled (0° C.) solution of 4-(2-Methoxy-1-methyl-vinyl)-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (2.7 g, 9.11 mmol) in tetrahydrofuran (25 ml) is treated dropwise over 5 minutes with concentrated hydrochloric acid (15 ml) and the mixture stirred at 0° C. for 3 hours. After dilution with diethyl ether (50 ml), the reaction mixture is adjusted to pH 7 with 1 N NaOH. The aqueous layer is extracted with diethyl ether (2×30 ml), the organic extracts then combined and washed with brine and dried (Na 2 SO 4 ). Concentration provided the title compound as an oil which slowly crystallized and is used without further purification. MS: m/z (M+1) 283.
[0000] Step D
2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0416] Sodium borohydride (132 mg, 3.5 mol) is added in one portion to a cooled (0° C.) solution of 2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propionaldehyde (2.0 g, 7.08 mmol) in ethanol (30 ml), and the mixture stirred at 0° C. for 1 hour. After quenching with water (55 ml), the reaction mixture is extracted with diethyl ether (3×25 ml). The combined organic extracts are washed with water, brine, then dried (Na 2 SO 4 ) and concentrated to a solid which is purified by silica flash chromatography (20:1 hexanes:ethyl acetate to 3:1 hexanes:ethyl acetate) to provide the title compound as a racemic solid. MS: m/z (M+1) 285.
[0000] Preparation 33
2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-2-ol
[0417]
[0418] To a cooled (0° C.) solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone (1.0 g, 3.72 mmol) in tetrahydrofuran (10 ml) is added methylmagnesium bromide (3M in diethyl ether) (1.9 ml, 5.6 mmol) dropwise over 3 minutes. After stirring at 0° C. for 90 minutes, the mixture is adjusted to pH 6 with 1 N HCl, and then diluted with diethyl ether (30 ml) and water (40 ml). The organic layer is removed and the remaining aqueous layer extracted with diethyl ether (2×25 ml). The combined organic extracts are combined and washed with water, brine, dried (Na 2 SO 4 ), and concentrated to an oil. Purification by silica chromatography (20:1 hexanes:ethyl acetate to 4:1 hexanes:ethyl acetate) provided the title compound as an oil. MS: m/z (M+1) 285.
[0000] Preparation 34
[3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0419]
Step A
3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazole
[0420] To a solution of 4-(trifluoromethyl)-phenylhydrazine (10 g, 56.77 mmol) in ethanol (150 mL), add 2,4-pentanedione (5.83 mL, 56.77 mmol) and a catalytic amount of p-toluenesulfonic acid. Heat the resulting mixture to reflux for 5 h. Then, allow the reaction mixture to cool to room temperature. Concentrate on rota-vapor. Partition the residue between EtOAc (150 mL) and H 2 O (100 mL). Wash the organic extract with brine (100 mL), dry over Na 2 SO 4 , filter and concentrate to afford title compound as an orange oil (quantitative yield) that is used directly for the next step. MPLC (M + +1=241.1).
[0000] Step B
3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde
[0421] To a solution of 3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (10.31 g, 42.92 mmol)) in DMF (42 mL) add POCl 3 (5.2 mL, 55.77 mmol). Stir the resulting mixture at 90° C. for 12 h, and then add POCl 3 (3.84 mL, 41.2 mmol) and stir again at 90° C. for additional 6 hours. Monitor the starting material consumption by TLC. When reaction is completed, then allow to cool to room temperature. Partition the residue between H 2 O (100 mL) and Et 2 O (3×100 mL), and extract again the aqueous layer with CH 2 Cl 2 (3×100 mL). Wash each organic extract separately with brine (2×100 mL), and dry over Na 2 SO 4 . Filter the solutions and concentrate together to afford the crude product. Purificate by silica gel column chromatography (0% to 25% EtOAc/hexanes) to obtain (7.04 g, 61%). 1 H NMR (CDCl 3 ): δ 10.05 (s, 1 H), 7.78 (d, J=8.4 Hz, 2 H), 7.59 (d, J=8.4 Hz, 2 H), 2.61 (s, 3 H), 2.53 (s, 3 H).
[0000] Step C
[3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0422] 3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (2.0 g, 7.46 mmol) is taken into EtOH (60 mL) at 0° C. (ice bath). Add sodium borohydride (0.141 g, 3.73 mmol), in one portion and let the mixture warm to room temperature while stirring for 12 h. Quench with H 2 O (80 mL), extract with EtOAc (3×50 mL). Wash the combined organic extracts with brine (3×30 mL), dry over NaSO 4 , filter and concentrate. Silica gel column chromatography yields the title compound as a white solid (1.97 g, 98%). MPLC (M + +1=271.1). 1 H NMR (CDCl 3 ): δ 7.73 (d, J=8.5 Hz, 2 H), 7.57 (d, J=8.5 Hz, 2 H), 4.58 (s, 2 H), 2.39 (s, 3 H), 2.36 (s, 3 H).
[0000] Preparation 35
1-[3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol
[0423]
[0424] Prepare a solution of 3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (7.04 g, 26.26 mmol) in THF (50 mL) and cool it to 0° C. using an ice bath. A solution of methyl magnesium bromide (1.0 M) (40 mL, 39.39 mmol) is added over 5 min. Once the addition is completed, remove the ice bath and stirred for additional 2 hours. Cool again to 0° C. and partition between saturated NH 4 Cl (80 mL) and EtOAc (150 mL). Wash the organic extract with H 2 O (2×50 mL), then with brine (3×50 mL), and dry over Na 2 SO 4 , filter and concentrate. Purify on silica gel column chromatography to afford the title compounds' as yellow solids (6.77 g, 91%). MPLC (M + +1=285.1).
[0425] The following compound is made in a similar way.
[0000] Preparation 36
1-[3,5-dimethyl-1-(4trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propanol
[0426] 1 H NMR (CDCl 3 : δ 7.71 (d, J=8.4 Hz, 2 H), 7.55 (d, J=8.4 Hz, 2 H), 4.66 (t, J=7.3 Hz, 1 H), 2.37 (s, 3 H), 2.35 (s, 3 H), 2.04-1.91 (m, 1 H), 1.85-1.78 (M, 1 H), 0.95 (t, J=7.3 Hz, 3 H).
[0000] Preparation 37
2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0427]
Step A
1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone
[0428] Dissolve 1-[3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-yl]-ethanol (5.09 g, 17.905 mmol) in CHCl 3 (80 mL) and to this solution, add activated manganese (IV) dioxide (15.57 g, 179.05 mmol). Heat to reflux the resulting suspension for 36 hours. After that time, allow to cool to room temperature, then filter through a short pad of Celite. Concentrate the filtrate to afford the title compound as an off-white solid, and use without further purification in next Reaction E. (4.87 g, 96%). MPLC (M + +1=283.1).
[0000] Step B
4-(2-methoxy-1-methyl-vinyl)-1H-pyrazol
[0429]
[0430] Suspend methoxymethyl triphenylphosphonium chloride (17.75 g, 51.79 mmol) in THF (40 mL) at room temperature and then cool to 0° C. (ice bath). Suspend potassium tert-butoxide (5.81 g, 51.79 mmol) in THF (30 mL). Add the potassium tert-butoxide suspension onto the methoxymethyl triphenylphosphonium chloride suspension in a dropwise fashion. Stir for 20 minutes. Then add dropwise a solution of 1-[3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-yl]-ethanone (4.87 g, 17.26 mmol) in THF (80 mL) along 5 minutes. After completion of the addition, remove the cooling bath. Stir for 2 additional hours. Partition the reaction mixture between EtOAc (250 mL) and H 2 O (100 mL). Wash the organic extract with brine (3×150 mL), dry over Na 2 SO 4 , filter and concentrate to afford the crude product. Purification using silica gel column chromatography (0% to 15% EtOAc/hexanes) gave the title compound as an off-white solid. (5.30 g, 99%). 1 H NMR (CDCl 3 ): δ 7.71 (d, J=8.7 Hz, 2 H), 7.60 (d, J=8.7 Hz, 2 H), 6.1 (s, 1 H), 3.62 (s, 3 H), 2.60 (s, 3 H), 1.83 (s, 3 H).
[0000] Step C
2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0431] Dissolve 4-(2-methoxy-1-methyl-vinyl)-1H-pyrazol (6.06 g, 19.52 mmol) in acetonitrile (200 mL) at room temperature. Add sodium iodide (2.93 g, 19.52 mmol) and stir the reaction mixture for 3 minutes. Cool while stirring to 0° C. (ice bath). Add trimethylsilylchloride (2.5 mL, 19.52 mmol) dropwise. Remove the ice bath and stir at room temperature for 2 hours. Monitor the consumption of the starting material by TLC. When the reaction is completed, add 5% sodium sulfate solution (100 mL) and EtOAc (250 mL). Extraction with EtOAc and wash the combined organic solutions with brine (100 mL×3). Dry over Na 2 SO 4 , and concentrate to obtain a yellow solid. This solid is taken up in 150 mL of EtOH and stirred at room temperature. Cool the mixture to 0° C. (ice bath) and add sodium borohydride (390 mg., 20.6 equivalents) in one portion. Remove the cooling bath after addition and stir the reaction mixture for 4 hours at room temperature. Monitor the reaction by TLC. Dilute with EtOAc, extract with 200 mL of EtOAc wash the combined organic phases with brine, (3×50 mL), dry over Na 2 SO 4 , and concentrate to obtain the title compound as a off-white solid. Purify by silica gel column chromatography with 30% EtOAc in Hexanes. (3.82 g, 62%). MPLC (M + +1=299.1).
[0000] Preparation 38
3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butan-1-ol
[0432]
Step A
1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone
[0433]
[0434] To an ambient temperature solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol (5.0 g, 18.50 mmol) in CH2Cl2 (100 ml) is added manganese (IV) dioxide (12.0 g, 138 mmol) and heated to reflux overnight. TLC (100% EtOAc) indicates complete consumption of starting material. The reaction mixture is filtered through a bed of silica gel resting on ceelite. The filtrate is concentrated and recrystallized from hot ethyl acetate/hexanes yields the title compound (4.93 g, 99%).
[0000] Step B
3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-but-2-enoic acid ethyl ester
[0435]
[0436] To a 0 C suspension of sodium hydride (7.2 g, 180 mmol, 60% oil dispersion) in THF (50 ml) prewashed with hexanes (100 ml) is added a solution of triethyl phosphonoacetate (32.5 ml, 163.7 mmol) in THF (50 ml). The reaction mixture is warmed to room temperature for 1 h and cooled back to 0 C. At which point a solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone (4.93 g, 16.37 mmol) in THF (100 ml) is added and the reaction mixture heated to reflux for 6 h. TLC (20% EtOAc/hexane) indicates complete consumption of starting material. Reaction is cooled to room temperature and quenched with saturated aqueous NH 4 Cl. The reaction mixture is concentrated and the aqueous layer extracted with EtOAC (3×200 ml). The combined organic layers are washed with brine (100 ml), dried (MgSO 4 ), filtered, concentrated and chromatographed (120 g SiO 2 , 10% EtOAc/Hexanes) to yield the title compound (5.41 g, 96%).
[0000] Step C
3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-but-2-en-1-ol
[0437]
[0438] To a 0 C solution of 3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-but-2-enoic acid ethyl ester (5.41 g, 15.99 mmol) in THF (200 ml) is added portion-wise lithium aluminum hydride (1.82 g, 47.97 mmol) and heated to reflux. After 1 h TLC (20% EtOAc/hexane) indicates complete consumption of starting material. The reaction is cooled to 0 C and quenched by the slow addition of water, 5N NaOH and water. The suspension, which is formed, is diluted with EtOAc (200 ml) and filtered. The filtrate is concentrated and chromatographed (120 g SiO 2 , 20% EtOAc/Hexanes) to yield (4.37 g, 86%) a 4:1 mixture of title compound and the saturated alkane.
[0000] Step D
3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butan-1-ol
[0439]
[0440] To an ambient temperature suspension of palladium on carbon (1.5 g, 10% wt) in a solution of 3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-but-2-en-1-ol (4.3 g, 14.51 mmol) in ethanol (30 ml) is added an atmosphere of hydrogen gas and continues to stir at room temperature. After 5 h LC/MS indiacated complete conversion of SM to desired product. Reaction mixture is filtered through ceelite and concentrated to yield the title compound (3.92 g, 91%).
[0000] Preparation 39
1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butan-1-ol
[0441]
Preparation 40
2-Methyl-1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0442]
Preparation 41
[3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0443]
Step A
5-tert-Butyl-2-(4-trifluoromethyl-phenyl)-2,4-dihydro-pyrazol-3-one
[0444]
[0445] To an ambient temperature solution of Trifluoromethylphenyl hydrazine (9.0 g, 51.1 mmol) is added 4,4-Dimethyl-3-oxo-pentanoic acid ethyl ester (9.13 ml, 57.1 mmol) and stirred overnight. The reaction mixture is then refluxed with continuous azeotropic removal of water and volatile organics for anther 6 hours. TLC (30% EtOAc/hexane) indicates complete consumption of starting material. Heptane is added to the hot solution. As the solution cools a tan solid precipitates and is filtered. The filter cake is washed with heptane and dried to yield the title compound (14.50 g, 99%).
[0000] Step B
3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde
[0446]
[0447] To a 10 C solution of phosphorous oxychloride (9.35 ml, 102.2 mmol) in DMF (30 ml) is added solid 5-tert-Butyl-2-(4-trifluoromethyl-phenyl)-2,4-dihydro-pyrazol-3-one (14.5 g, 51.1 mmol) and the reaction mixture is heated to 100 C overnight. TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction is quenched by pouring into ice (1 L). Once warmed to room temperature the mixture is extracted with CH 2 Cl 2 (3×300 ml). The combined organic layers are washed with 2N NaOH and water, dried (MgSO 4 ), filtered, concentrated and chromatographed (330 g SiO 2 , 10% EtOAc/Hexanes) to yield the title compound (14.7 g, 87%).
[0000] Step C
[3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0448]
[0449] To a 0 C solution of 3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (2.0 g, 6.05 mmol) in THF/MeOH (60/15 ml) is added portion-wise sodium borohydride (458 mg, 12.1 mmol) and warmed to room temperature. After 1 h TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction mixture is concentrated and the residue is partitioned between EtOAc (100 ml) and 0.2N HCl (50 ml). The aqueous layer is extracted with a second portion of EtOAc (50 ml). The combined organic layers are washed with brine, dried (MgSO 4 ), filtered and concentrated to yield the title compound (1.99 g, 99%).
[0000] Preparation 42
[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0450]
Step A
3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde
[0451] To an ambient temperature solution of 3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (9.0 g, 27.21 mmol) in EtOAC/Et 3 N (4/9 ml) is added 5% Pd/CaCO 3 (Pb) (908 mg). The reaction mixture is stirred under 60 psi of hydrogen overnight. Catalyst is filtered and the filtrate is concentrated giving the title compound (5.08 g, 63%).
[0000] Step B
[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0452]
[0453] To a 0 C solution of 3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (2.4 g, 8.1 mmol) in THF/MeOH (80/20 ml) is added portion-wise sodium borohydride (460 mg, 12.15 mmol) and warmed to room temperature. After 1 h TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction mixture is concentrated and the residue is partitioned between EtOAc (100 ml) and 0.2N HCl. (50 ml). The aqueous layer is extracted with a second portion of EtOAc (50 ml). The combined organic layers are washed with brine, dried (MgSO 4 ), filtered and concentrated to yield the title compound (2.28 g, 94%).
[0454] The following compounds were prepared in a similar manner using the appropriate β-keto esters.
[0000] Preparation 43
[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0455]
Preparation 44
[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol
[0456]
Preparation 45
1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol
[0457]
Preparation 46
1-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol
[0458]
Preparation 47
1-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol
[0459]
Preparation 48
2-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-2-ol
[0460]
Preparation 49
2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butan-1-ol
[0461]
Preparation 50
2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0462]
[0463] To a −78 C solution of 3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole-4-carbaldehyde (5.0 g, 16.87 mmol) in THF (170 ml) is added methylmagnesium bromide (24.1 ml, 33.75 mmol, 1.4 M in Et 2 O) dropwise and is allowed to warm to room temperature. After 1 h TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction is quenched with saturated aqueous NH 4 Cl. The reaction mixture is concentrated and the aqueous layer extracted with EtOAC (3×250 ml). The combined organic layers are washed with brine, dried (MgSO 4 ), filtered and concentrated to yield the title compound (5.27 g, 100%).
[0000] Step B
1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone
[0464] To an ambient temperature solution of 1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanol (5.27 g, 16.87 mmol) in CH 2 Cl 2 (100 ml) is added manganese (IV) dioxide (13.2 g, 152 mmol) and heated to reflux overnight. TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction mixture is filtered through a bed of silica gel resting on ceelite. The filtrate is concentrated and recrystallized from hot ethyl acetate/hexanes to yield the title compound (4.89 g, 93%).
[0000] Step C
3-tert-Butyl-4-(2-methoxy-1-methyl-vinyl)-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0465] To a an ambient temperature suspension of potassium tert-butoxide (4.01 g, 35.77 mmol) in THF (100 ml) is added (Methoxymethyl)triphenylphosphonium chloride (12.26 g, 35.57 mmol) and is stirred at room temperature for 30 min. 1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone (3.7 g, 11.92 mmol) is added and the reaction mixture continues to stir at room temperature. After 2 h TLC (30% EtOAc/hexane) indicates complete consumption of starting material. Reaction is quenched with saturated aqueous NH 4 Cl. The reaction mixture is concentrated and the aqueous layer extracted with EtOAc (3×200 ml). The combined organic layers are washed with brine, dried (MgSO 4 ), filtered, concentrated and chromatographed (120 g SiO 2 , 10% EtOAc/Hexanes) to yield the title compound (2.87 g, 71%).
[0000] Step D
2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propionaldehyde
[0466] To a 0 C solution of 3-tert-Butyl-4-(2-methoxy-1-methyl-vinyl)-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (2.66 g, 7.86 mmol) in THF (20 ml) is added dropwise concentrated hydrochloric acid (12.5 ml) and the reaction is warmed to room temperature. After 1 h TLC (30% EtOAc/hexane) indicates complete consumption of starting material. The reaction mixture is diluted with water and the pH is adjusted to 8 with solid NaHCO 3 . The reaction mixture is concentrated and the aqueous layer extracted with EtOAC (3×100 ml). The combined organic layers are washed with brine, dried (MgSO 4 ) , filtered, concentrated and chromatographed (120 g SiO 2 , 10% EtOAc/Hexanes) to yield the title compound (2.42 g, 95%).
[0000] Step E
2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0467] To a 0 C solution of 2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propionaldehyde (2.55 g, 7.86 mmol) in THF/MeOH (80/20 ml) is added portion-wise sodium borohydride (595 mg, 15.72 mmol) and warmed to room temperature. After 1 h TLC showed no SM. The reaction mixture is concentrated and the residue is partitioned between EtOAc (100 ml) and 0.2N HCl (50 ml). The aqueous layer is extracted with a second portion of EtOAc (50 ml). The combined organic layers are washed with brine, dried (MgSO 4 ), filtered and concentrated to yield the title compound (2.50 g, 98%).
[0000] Preparation 51
2-(3-Methyl-1-p-tolyl-1H-pyrazol-4-yl)-propan-1-ol
[0468]
Preparation 52
2-[3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-propan-1-ol
[0469]
Preparation 53
2-[1-(4-Chloro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propan-1-ol
[0470]
Preparation 54
2-[1-(4-Fluoro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propan-1-ol
[0471]
Preparation 55
[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-yl]-methanol
[0472]
Step A
4-Methyl-3-oxo-2-(triphenyl-15-phosphanylidene)-pentanoic acid methyl ester
[0473]
[0474] To a solution of isobutric acid (4.4 g, 50 mmol) and (triphenyl-15-phosphanylidene)-acetic acid methyl ester (16.7 g, 50 mmol)in methylene chloride (500 mL) is added DMAP (610 mg, 5 mmol) and EDCI (9.6 g, 50 mmol) at 0˜5° C., then warmed to room temperature. The reaction mixture is quenched by 1N NaOH, layers are separated, the organic layer is washed with water and brine, dried over sodium sulfate. Concentration yields the title compound.
[0000] Step B
4-Methyl-2,3-dioxo-pentanoic acid methyl ester
[0475]
[0476] To a solution of 4-Methyl-3-oxo-2-(triphenyl-15-phosphanylidene)-pentanoic acid methyl ester (2.0 g, 4.95 mmol) in methylene chloride is bubbled ozone for 30 min at −78° C., then the reaction mixture is loaded on silica gel column, eluted with hexanes and ethyl acetate giving 0.51 g of the title compound.
[0000] Step C
5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazole-4-carboxylic acid methyl ester
[0477]
[0478] To a slurry of NH40Ac (2.48 g) in acetic acid is added 4-Methyl-2,3-dioxo-pentanoic acid methyl ester (0.51 g, 3.22 mmol) and 4-Trifluoromethyl-benzaldehyde (1.11 g). The mixture is heated at 60° C. for 1 h, acetic acid is evaporated. The residue is dissolved in ethyl acetate, washed with NaHCO3, water and brine, dried over sodium sulfate. Concentration and column chromatography on silica gel yields the title compound (0.5 g).
[0000] Step D
[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-yl]-methanol
[0479]
[0480] A THF (5 mL) solution of 5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazole-4-carboxylic acid methyl ester (0.47 g, 1.51 mmol) is cooled to 0° C. and a 1M LiAlH 4 (1.51 mL, 1.51 mmol) is added slowly. The reaction is warmed to room temperature slowly, after stirring at room temperature for 2 h, tlc (15% EtOAc/hexane) showed that all the starting ester had been consumed. The reaction is cooled and carefully quenched with water, 5N NaOH. The light tan solid is filter through celite and dried to give 0.4 g of the title compound.
[0000] Preparation 56
[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-yl]-methanol
[0481]
Step A
5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazole-4-carboxylic acid methyl ester
[0482]
[0483] To a solution of 5-isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazole-4-carboxylic acid methyl ester (3.0 g, 9.6 mmol) in DMF (100 mL) is added sodium hydride (60%, 0.58 g) at 0˜5° C. The mixture is stirred at 0˜5° C. for 30 min methyl iodide (1.2 mL) is added. The reaction mixture is warmed to room temperature and stirred overnight, wuenched by water, extracted with ethyl acetate, dried over sodium sulfate. Concentration yields the title compound (2.5 g).
[0000] Step B
[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-yl]-methanol
[0484]
[0485] THF (10 mL) solution of 5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazole-4-carboxylic acid methyl ester(2.36 g, 7.23 mmol) is cooled to 0° C. and a 1M LiAlH 4 (7.5 mL, 7.5 mmol) is added slowly. The reaction is warmed to room temperature slowly, after stirring at room temperature for 2 h, tlc (15% EtOAc/hexane) showed that all the starting ester had been consumed. The reaction is cooled and carefully quenched with water, 5N NaOH. The light tan solid is filter through celite and dried to give 1.9 g of the title compound.
[0000] Preparation 57
1-[4-Methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-ethanol
[0486]
Step A
N-Hydroxyl-4-trifluoromethyl-benzimidoyl chloride
[0487]
[0488] 4-Trifluoromethyl-benzaldehyde (3.48 g, 20.0 mmol) in EtOH (50 mL) is added NH 2 OH—HCl (1.53 g, 22.0 mmol). The mixture is stirred and heated to reflux at 84° C. for 2 hours. It is then cooled down and concentrated and purified on silica gel chromatography column with 10-20% EtOAc/Hexanes to obtain the oxime intermediate.
[0489] The oxime intermediate (2.40 g, 12.7 mmol) is then dissolved in DMF (10 mL) and added the NCS (0.93 g, 6.95 mmol). Use heat gun to initiate the reaction and then add another portion of NCS (0.93 g, 6.95 mmol). The reaction mixture is stirred at room temperature for 2 hours and quenched with water (50 mL). The mixture is extracted with EtOAc (50 mL×2) and the combined organics are dried (Na 2 SO 4 ), concentrated,. and purified on silica gel chromatography column with 20-50% EtOAc/Hexanes to yield the title compound (2.60 g, 92%).
[0000] Step B
4-Methyl-3-(4-trifluoromethyl-phenyl)-isoxazole-5-carboxylic acid ethyl ester
[0490]
[0491] To a solution of N-Hydroxyl-4-trifluoromethyl-benzimidoyl chloride (0.65 g, 2.91 mmol) and but-2-ynoic acid ethyl ester (0.49 g, 4.36 mmol) in EtOAc (3.0 mL) is added Et 3 N dropwisely while stirred vigorously. The resulted suspension is heated to 80° C. for 12 hours. It is then filtered and the filtrate is purified on silica gel chromatography column with 10-15% EtOAc/Hexanes to obtain the product (410 mg, 47%).
[0000] Step C
[4-Methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-methanol
[0492]
[0493] A solution of 4-methyl-3-(4-trifluoromethyl-phenyl)isoxazole-5-carboxylic acid ethyl ester (810 mg, 2.71 mmol) in THF (30 mL) is treated with LiBH 4 (295 mg, 13.5 mmol). The suspension is stirred at room temperature for 48 hours and then quenched water (20 mL). The mixture is extracted with EtOAc (50 mL×2) and the combined organics are dried (Na 2 SO 4 ), concentrated, and purified on silica gel chromatography column with 50% EtOAc/Hexanes to yield the title compound (480 mg g, 69%).
[0000] Step D
1-[4-Methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-ethanol
[0494]
[0495] A solution of [4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-methanol (251 mg, 0.976 mmol) is treated with MnO 2 (168 mg, 1.95 mmol) and the suspension is stirred at 75° C. for 24 hours. The mixture is filtered and purified on silica gel chromatography column with 25% EtOAc/Hexanes to yield the aldehyde intermediate (165 mg).
[0496] A solution of that aldehyde intermediate (165 mg, 0.647 mmol) in THF (10 mL) at −78° C. is treated with MeMgBr (0.43 mL, 3.0 M). The mixture is stirred while warmed up to room temperature over 60 minutes. The reaction is then quenched with water (1.0 mL) and HCl (5 mL, 0.1 N). The mixture is extracted with EtOAc (50 mL×2) and the combined organics are dried (Na 2 SO 4 ), concentrated, and purified on silica gel chromatography column with 30% EtOAc/Hexanes to yield the title compound (160 mg, 91%).
[0000] Preparation 58
5-Chloromethyl-1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazole
[0497]
Step A
[0498] To a slurry of (4-Trifluoromethyl-phenyl)-hydrazine (1.8 g, 10.22 mmol) in water (50 mL) at 0° C. under nitrogen is slowly added concentrated hydrochloric acid (14 mL). In a separate round bottom flask, sodium nitrite (2.0 g, 34 mmol) is dissolved in water (10 mL) and transferred to the reaction slurry slowly by pipette. The mixture is allowed to stir at 0° C. open to air and monitored by TLC. Upon complete consumtion of starting material, the reaction is diluted with ethyl acetate and the two phases are seperated. The organic layer is washed, dried, filtered and concentrated. The crude 1-azido-4-trifluoromethyl-benzene is used immediately without further purification.
[0000] Step B
[0499] 1-azido-4-trifluoromethyl-benzene (10.22 mmol) is dissolved in anhydrous dimethyl formamide (4 mL) and methylpropriolate (3.6 mL, 40 mmol) is added with stirring under nitrogen at room temperature. The reaction is heated to 45° C. and monitored by TLC. After the starting material is completely consumed, the reaction is cooled to room temperature and concentrated. The reaction is diluted with chloroform and washed with water and brine, dried over sodium sulfate, then concentrated. The residue is further purified using flash column chromatography. The regioisomers 3-(4-Trifluoromethyl-phenyl)-3H-[1,2,3]triazole-4-carboxylic acid methyl ester (0.074 g, 0.2731 mmol), 4% yield, and 1-(4-Trifluoromethyl-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid methyl ester (0.510 g, 1.88 mmol), 18% yield, are formed in roughly a 1:4 ratio.
[0000] Step C
[0500] 1-(4-Trifluoromethyl-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid methyl ester (0.510 g, 1.88 mmol) is dissolved into anhydrous tetrahydrofuran (10 mL) and cooled to 0° C. under nitrogen. A solution of lithium aluminum hydride, 1.0 M in THF, (1.90 mL, 1.90 mmol) is slowly added and the reaction is monitored by TLC. Upon complete consumtion of starting material, the reaction is quenched with water, 20% sodium hydroxide, and water additions, diluted with diethyl ether, followed by filtration through a celite plug. The two phases are seperated. The organic layer is washed, dried, filtered and concentrated. The crude [1-(4-Trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-yl]-methanol (0.314 g, 1.29 mmol), 69% yield, is used without further purification.
[0000] Step D
[0501] [1-(4-Trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-yl]-methanol (0.314 g, 1.29 mmol), is dissolved into anhydrous dichloromethane (5 mL) and cooled to 0° C. under nitrogen. Triethyl amine (0.360 mL, 2.58 mmol) and methane sulfonyl chloride (0.150 mL, 1.94 mmol) are then slowly added and the reaction is monitored by TLC. Upon complete consumtion of starting material, the reaction is diluted with dichloromethane and extracted against saturated sodium bicarbonate solution. The organic layer is washed with water and brine, then dried over anhydrous sodium sulfate, and concentrated. The crude 4-Chloromethyl-1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazole (0.337 g, 1.29 mmol), 100% yield, is used without further purification.
Example 1
{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenoxy}-acetic acid
[0502]
Step A
4-Chloromethyl-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0503] To a cooled (0° C.) solution of [3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol (333 mg, 1.29 mmol) and triethylamine (0.36 ml, 2.58 mmol) in dichloromethane (5 ml) is added methanesulfonyl chloride (0.16 ml, 2.06 mmol) dropwise over 5 minutes. After stirring at 0° C. for 2 hours, the mixture is diluted with dichloromethane (15 ml) and washed with saturated aqueous sodium bicarbonate (2×15 ml). The organic layer is washed with water, brine, dried (Na 2 SO 4 ), and concentrated to the title compound as a solid and is used without further purification. MS: m/z (M+1) 275.
[0000] Step B
{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenoxy}-acetic acid methyl ester
[0504] To a solution of (4-Hydroxy-2-methyl-phenoxy)-acetic acid methyl ester (99.3 mg, 0.50 mmol) and 4-Chloromethyl-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (167 mg, 0.61 mmol) in acetonitrile (1.5 ml) is added cesium carbonate (260 mg, 0.80 mmol) and the resulting suspension stirred at ambient temperature for 18 hours. Filtration of the mixture and concentration of the filtrate yields a solid which is purified by silica chromatography (15:1 hexanes:ethyl acetate to 5:1 hexanes:ethyl acetate) to provide the title compound as a white solid. MS: m/z (M+1) 435
[0000] Step C
{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenoxy}-acetic acid
[0505] A solution of {2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenoxy}-acetic acid methyl ester (120 mg, 0.27 mmol) in methanol (10 ml) is treated with 5 N NaOH (0.54 ml, 2.7 mmol), and the solution is stirred at ambient temperature for 24 hours. The mixture is concentrated to dryness to give a solid which is dissolved in water (10 ml) and ethyl acetate (15 ml), and the solution is then adjusted to pH 3 with 6 N HCl. After extraction of the aqueous layer with ethyl acetate (2×15 ml), the organic extracts are combined and washed with water, brine, then dried (Na 2 SO 4 ) and concentrated to provide the title compound as a white solid. MS: m/z (M+1) 421. The structure is also confirmed by proton NMR.
[0506] The following compound is prepared substantially as described herein below:
Example 2
2-Methyl-2-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-propionic acid
[0507]
HRMS: Calcd. 447.1895, Found: 447.1901.
Example 3
3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid
[0508]
Step A
3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid methyl ester
[0509] To a cooled (0° C.) solution of [3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-methanol (135 mg, 0.52 mmol) and 3-(4-Hydroxy-2-methyl-phenyl)-propionic acid methyl ester (123 mg, 0.63 mmol) in tetrahydrofuran (5.0 ml) is added tri-n-butylphosphine (0.195 ml, 0.78 mmol) followed by addition of 1,1′-(azodicarbonyl)dipiperidine (197 mg, 0.78 mmol) portion-wise over 3 minutes. The mixture is stirred at 0° C. for 10 minutes, then removed from the cold bath and stirred for 18 hours. The mixture is diluted with hexanes (10 ml), filtered to remove insolubles, and the filtrate concentrated to an oil which is purified by silica flash chromatography (35:1 hexanes:ethyl acetate to 5:1 hexanes:ethyl acetate) to provide the title compound as a colorless oil. MS: m/z (M+1) 433.
[0000] Step B
3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid
[0510] A solution of 3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid methyl ester (98 mg, 0.22 mmol) in methanol (3 ml) is treated with 5N NaOH (0.11 ml, 0.56 mmol), and the solution is stirred at ambient temperature for 18 hours. The mixture is concentrated to dryness to give a solid, which is dissolved in water (10 ml) and ethyl acetate (15 ml), and the resulting solution is then adjusted to pH 3 with 6N HCl. After extraction of the aqueous layer with ethyl acetate (2×15 ml), the organic extracts are combined and washed with. water, brine, then dried (Na 2 SO 4 ) and concentrated to provide the title compound as a white solid. MS: m/z (M+1) 419. The structure is also confirmed by proton NMR.
[0511] The following compounds are prepared according to the procedure outlined above in Example 3:
Example 4
(R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenoxy)-acetic acid
[0512]
[0513] MS: m/z (M+1) 435. The structure is also confirmed by proton NMR.
Example 5
(R,S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenyl)-propionic acid
[0514]
[0515] MS: m/z (M+1) 433. The structure is also confirmed by proton NMR.
Example 6
(R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid
[0516]
[0517] MS: m/z (M+1) 451. The structure is also confirmed by proton NMR.
Example 7
(R,S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid
[0518]
[0519] MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 8
(R,S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid
[0520]
[0521] MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 9
(R,S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0522]
[0523] MS: m/z (M+1) 447. The structure is also confirmed by proton NMR.
Example 10
(R,S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0524]
[0525] MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 11
(R,S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid
[0526]
[0527] MS: m/z (M+1) 463. The structure is also confirmed by proton NMR.
Example 12
(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid
[0528]
[0529] MS (ES): 435 (M + +1). The structure is confirmed by 1 H NMR spectroscopy.
Example 13
{3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-phenyl}-acetic acid
[0530]
[0531] MS (ES) : 407 (M + +1) The structure is confirmed by 1 H NMR spectroscopy.
[0532] Example 14
(3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-acetic acid
[0533]
[0534] MS (ES): 421 (M + +1). The structure is confirmed by 1 H NMR spectroscopy.
Example 15
2-(3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid
[0535]
Step A
[0536] Lithium hexamethyldisilazane (0.51 mL, 0.51 mmol) is added dropwise to a solution of (3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-acetic acid methyl ester (0.20 g, 0.46 mmol) in 5 mL THF at −78 C. The resultant solution is stirred for 30 minutes and methyl iodide (0.034 mL, 0.55 mmol) is added dropwise. The solution is allowed to warm to room temperature over two hours and stirred overnight upon which it is poured into an aqueous solution of NH4Cl. The aqueous layer is extracted with ethyl acetate (3×25 mL) and washed with water (25 mL) and brine (25 mL). Chromatography (10% ethyl acetate/hexane) provided the ester.
[0000] Step B
[0537] The ester is hydrolyzed in a similar fashion providing the titled compound. MS (ES) 435 (M + +1). The structure is confirmed by 1 H NMR spectroscopy.
Example 16
(3-{1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenyl)-acetic acid
[0538]
[0539] MS (ES): 405 (M + +1). The structure is confirmed by 1H NMR spectroscopy.
Example 17
(R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0540]
Step A
(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid ethyl ester
[0541] Zinc iodide (105 mg, 0.33 mmol) is added to a solution of 1-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol (185 mg, 0.65 mmol) and (4-Mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (176 mg, 0.78 mmol) in 1,2-dichloroethane (1 ml) and the solution stirred at ambient temperature for 1 hour. The mixture is diluted with water (20 ml) and dichloromethane (10 ml), the organic layer is removed, and the remaining aqueous layer extracted with dichloromethane (2×10 ml). The combined organic extracts are combined and washed with brine, then dried (Na 2 SO 4 ) and concentrated to an oil which is purified by silica chromatography (15:1 hexanes:ethyl acetate to 10:1 hexanes:ethyl acetate) to give the title compound as a colorless oil. MS: m/z (M+1) 493.
[0000] Step B
(R,S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0542] A solution of (2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid ethyl ester (239 mg, 0.48 mmol) in methanol (4 ml) is treated with 2N NaOH (0.72 ml, 1.44 mmol), and the solution is stirred at ambient temperature for 16 hours. The mixture is concentrated to dryness to give a solid, which is dissolved in water (15 ml) and ethyl acetate (15 ml), and the resulting solution is then adjusted to pH 3 with 6N HCl. After extraction of the aqueous layer with ethyl acetate (2×20 ml), the organic extracts are combined and washed with water, brine, then dried (Na 2 SO 4 ) and concentrated to provide the title compound as a white solid. MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 18
(S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid
[0543]
[0544] The title compound is obtained via chiral chromatography of the racemate on a Chiralcel OD (4.6×250 mm) column with an eluent consisting of 10% n-propanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 451. The structure is also confirmed by proton NMR.
Example 19
(R)-(2-Methyl-4-{1[-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-acetic acid
[0545]
[0546] The title compound is obtained via chiral chromatography of the racemate on a Chiralcel OD (4.6×250 mm) column with an eluent consisting of 10% n-propanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 451. The structure is also confirmed by proton NMR.
Example 20
(S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0547]
[0548] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 447. The structure is also confirmed by proton NMR.
Example 21
(R)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0549]
[0550] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 447. The structure is also confirmed by proton NMR.
Example 22
(S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid
[0551]
[0552] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 23
(R)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-acetic acid
[0553]
[0554] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 24
(S)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid
[0555]
[0556] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 25
(R)-3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid
[0557]
[0558] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 20% isopropanol in heptane containing 0.2% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 449. The structure is also confirmed by proton NMR.
Example 26
(S)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0559]
[0560] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 10% ethanol in heptane containing 0.1% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 27
(R)-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0561]
[0562] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 10% ethanol in heptane containing 0.1% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 28
(S)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid
[0563]
[0564] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 15% ethanol in heptane containing 0.1% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 463. The structure is also confirmed by proton NMR.
Example 29
(R)-3-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid
[0565]
[0566] The title compound is obtained via chiral chromatography of the racemate on a Chiralpak AD (4.6×250 mm) column with an eluent consisting of 15% ethanol in heptane containing 0.1% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 463. The structure is also confirmed by proton NMR.
Example 30
(S)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0567]
[0568] The title compound is obtained via chiral chromatography of the racemate on a Chiralcel OJ (4.6×250 mm) column with an eluent consisting of 100% ethanol containing 0.2% trifluoroacetic acid as buffer, and eluted as the first enantiomer. MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 31
(R)-(2-Methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0569]
[0570] The title compound is obtained via chiral chromatography of the racemate on a Chiralcel OJ (4.6×250 mm) column with an eluent consisting of 100% ethanol containing 0.2% trifluoroacetic acid as buffer, and eluted as the second enantiomer. MS: m/z (M+1) 465. The structure is also confirmed by proton NMR.
Example 32
{4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0571]
Step A
{4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid ethyl ester
[0572] To a solution of 4-Chloromethyl-3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (172 mg, 0.6 mmol) and (4-Mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (152 mg, 0.67 mmol) in acetonitrile (2.5 mL) is added Ca 2 CO 3 (325 mg, 1 mmol). The mixture is stirred at room temperature over night, quenched by water, extracted with ethyl acetate, dried over sodium sulfate. Concentration yields the crude product.
[0000] Step B
{4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0573] To a solution of {4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid ethyl ester from step A in THF (1 mL is added LiOH (1.0 M, 1 mL). It is stirred at room temperature for 2 hrs, is acidified with 5 N HCl, extracted with ether, dried over sodium sulfate. Concentration and reversed phase HPLC purification (acetone/water/TFA as eluent) yields the title compound (62 mg) . MS (ES): 453 (M + +1); the structure is also confirmed by 1 H NMR.
Example 33
{4-[1-(3,5-Bis-trifluoromethyl-phenyl)-5-methyl-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0574]
[0575] MS (ES): 505.1 (M + +1); the structure is also confirmed by 1 H NMR.
Example 34
(4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0576]
Step A
(4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid ethyl ester
[0577] To a solution of 1-[3-Methyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethanol (314 mg, 1 mmol) in 1,2-dichloroethane (4 mL) is added ZnI 2 (160 mg, 0.5 mmol), followed by addition of (4-mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (270 mg, 0.1.2 mmol). After 2 hrs, the reaction mixture is loaded on silica gel column directly and eluted with hexanes/ethyl acetate giving the title compound (498 mg).
[0000] Step B
(4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0578] To a solution of (4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid ethyl ester (110 mg) from step A in ethanol (1 mL is added NaOH (5.0 M, 1 mL). After stirring at 50° C. for 2 hrs, it is acidified with 5 N HCl, extracted with ether, dried over sodium sulfate. Concentration and reversed phase HPLC purification (acetone/water/TFA as eluent) yields the title compound (86 mg). MS (ES): 493.3 (M + −1).
[0579] The following compounds are made in a similar manner:
Example 35
3-(4-{1-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0580]
[0581] MS (ES): 491.3 (M + −1).
Example 36
3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid
[0582]
[0583] MS (ES): 479.1 (M + +1).
Example 37
[0584]
{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0585] MS (ES): 481.1 (M + +1).
Example 38
{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0586]
[0587] MS (ES): 513.1 (M + +1, 37 Cl)
Example 39
3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid
[0588]
[0589] MS (ES): 515.1 (M + +1, 37 Cl).
Example 40
{3-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid
[0590]
Step A
{3-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid ethyl ester
[0591] A solution of [5-chloro-1-(4-difluoromethoxy-phenyl)-3-isopropyl-1H-pyrazol-4-yl]-methanol (100 mg, 0.3 mmol) in toluene (3.0 mL) is degassed and filled with nitrogen for 3 times. 1,1′-(Azodicarbonyl)-dipiperidine (120 mg, 0.5 mmol) is added to the reaction mixture under nitrogen at 0° C., followed by the addition of tributylphosphine (0.124 mL, 0.5 mmol) and (3-hydroxy-phenyl)-acetic acid (83 mg, 0.5 mmol). The reaction mixture is allowed to warm to room temperature and stirred overnight, the mixture is loaded on silica gel column. Chromatography yields the title compound (120 mg).
[0000] Step B
{3-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid
[0592] {3-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid ethyl ester (120 m) from step A is taken into ethanol (1 mL) and treated with NaOH (5.0 N, 1 mL) at 50° C. for 2 hrs. The reaction mixture is acidified with 5 N HCl, extracted with ethyl ether, dried over sodium sulfate. Concentration yields the title compound (120 mg). MS (ES): 469.1 (M + −1), the structure is also confirmed by proton NMR.
[0593] The following compounds are made in a similar manner:
Example 41
3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0594]
[0595] MS (ES): 497.1 (M + +1), the structure is also confirmed by proton NMR.
Example 42
(S)-3-{4-[5-Chloro-3-isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-2-methoxy-propionic acid
[0596]
[0597] MS (ES): 513.1 (M + +1), the structure is also confirmed by proton NMR.
Example 43
{3-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid
[0598]
[0599] MS (ES): 435.5 (M + +1), the structure is also confirmed by proton NMR.
Example 44
3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0600]
[0601] MS (ES): 463.4 (M + +1), the structure is also confirmed by proton NMR.
Example 45
3-{4-[3-Isopropyl-1-(4-trifluoromethoxy-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-2-methoxy-propionic acid
[0602]
[0603] MS (ES): 479.5 (M + +1), the structure is also confirmed by proton NMR.
Example 46
{2-Methyl-4-[2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethylsulfanyl]-phenoxy}-acetic acid
[0604]
Step 1
[0605] (4-Mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (113 mg, 0.500 mmol) is dissolved into anhydrous acetonitrile(ACN) (2 mL). Toluene-4-sulfonic acid 2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethyl ester (176 mg, 0.495 mmol) is added to the reaction, followed by the addition of cesium carbonate (326 mg, 1.00 mmol). The reaction is allowed to stir under nitrogen at room temperature and monitored by TLC and HPLC. Upon complete consumption of the tosylate, the reaction is diluted with diethyl ether and quenched with 0.1N NaOH. The two phases are separated, then the organic layer washed with water and brine. The organic phase is dried over anhydrous sodium sulfate and concentrated under vacuum. The residue is further purified using either EtOAc/Hexanes (1:9) or Acetone/Hexanes (1:9) gradients on silica gel chromatography to yield {2-Methyl-4-[2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethylsulfanyl]-phenoxy}-acetic acid ethyl ester (133 mg, 0.346 mmol) or 70%.
[0000] Step 2
[0606] {2-Methyl-4-[2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethylsulfanyl]-phenoxy}-acetic acid ethyl ester (133 mg, 0.346 mmol) is dissolved in tetrahydrofuran (1 mL) and 1N LiOH (1 mL) is added. The mixture is heated to reflux until the conversion is complete. Upon complete conversion, the reaction is cooled to room temperature and 1N HCl (1 mL) is added. The mixture is diluted with diethyl ether and extracted with 1N HCl. The organic layer is washed with water and brine, then dried over anhydrous sodium sulfate.
[0607] Concentration of the solvent reveals the pure {2-Methyl-4-[2-(5-methyl-3-phenyl-pyrazol-1-yl)-ethylsulfanyl]-phenoxy}-acetic acid in near quantitative yield (130 mg, 0.340 mmol).
Example 47
[2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid
[0608]
Step 1
[0609] (4-Mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (113 mg, 0.500 mmol) is dissolved into anhydrous acetonitrile(ACN) (2 mL). Cesium carbonate (326 mg, 1.00 mmol) is added to the reaction, followed by the addition of 4-Chloromethyl-5-methyl-1-phenyl-1H-pyrazole (102 mg, 0.495 mmol). The reaction is allowed to stir under nitrogen at room temperature and monitored by TLC and HPLC. Upon complete consumption of the chloride, the reaction is diluted with diethyl ether and quenched with 0.1N NaOH. The two phases are separated, then the organic layer washed with water and brine. The organic phase is dried over anhydrous sodium sulfate and concentrated under vacuum. The residue is further purified using either EtOAc/Hexanes (1:9) or Acetone/Hexanes (1:9) gradients on silica gel chromatography to yield [2-Methyl-4-(5-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid ethyl ester (157 mg, 0.396 mmol) or 80%.
[0000] Step 2
[0610] [2-Methyl-4-(5-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid ethyl ester (157 mg, 0.396 mmol) is dissolved in tetrahydrofuran (1 mL) and 1N LiOH (1 mL) is added. The mixture is heated to reflux until the conversion is complete. Upon complete conversion, the reaction is cooled to room temperature and 1N HCl (1 mL) is added. The mixture is diluted with diethyl ether and extracted with 1N HCl. The organic layer is washed with water and brine, then dried over anhydrous sodium sulfate. Concentration of the solvent reveals the pure [2-Methyl-4-(5-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid in near quantitative yield (138 mg, 0.375 mmol).
[0611] The following compounds are made in a substantially similar manner:
Example 48
[2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethylsulfanyl)-phenoxy]-acetic acid
[0612]
[0613] MS (ES): 351.13 (M + +H)
Example 49
3-[2-Methyl-4-(3-methyl-1-phenyl-1H-pyrazol-4-ylmethoxy)-phenyl]-propionic acid
[0614]
[0615] MS (ES): 369.04 (M + +H)
Example 50
{2-Methyl-4-[1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-ylmethylsulfanyl]-phenoxy}-acetic acid
[0616]
[0617] MS (ES) : 424.4 (M + +H).
Example 51
{2-Methyl-4-[5-methyl-1-(4-trifluoromethyl-phenyl)-1H-[1,2,3]triazol-4-ylmethylsulfanyl]-phenoxy}-acetic acid
[0618]
[0619] MS (ES): 438.4 (M + +H).
Example 52
{4-[1-(3,5-Bis-trifluoromethyl-benzyl)-5-phenyl-1H-[1,2,3]triazol-4-ylmethanesulfonyl]-2-methyl-phenoxy}-acetic acid
[0620]
[0621] MS (ES): 614.5 (M + +H).
Example 53
[0622]
3-(2-Methyl-4-{1-[4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-ethoxy}-phenyl)-propionic acid
[0623] A solution of 3-(4-hydroxy-2-methyl-phenyl)-propionic acid methyl ester (88 mg, 0.45 mmol) and 1-[4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-yl]-ethanol (81 mg, 0.30 mmol) in toluene (10 mL) is degassed and filled with nitrogen for 3 times. Tributylphosphine (91 mg, 0.45 mmol) is added to the reaction mixture under nitrogen at 0° C., followed by addition of of 1,1′-(azodicarbonyl)-dipiperidine (88 mg, 0.45 mmol). The reaction mixture is allowed to warm to room temperature and stirred for 48 hours. The mixture is loaded directly on silica gel chromatography with 25% EtOAc/Hexanes to obtain the intermediate ester. This intermediate is taken into THF (0.5 mL) and MeOH 1.0 mL), and is treated with NaOH (2.0 N, 1.5 mL) for 2 hours. The reaction mixture is acidified with 5 N HCl, extracted with ethyl ether, dried over sodium sulfate. Concentration yields the title compound (21 mg, 16%). MS (ES): 434.3; the structure is also confirmed by proton NMR.
Example 54
3-{2-Methyl-4-[4-methyl-3-(4-trifluoromethyl-phenyl)-isoxazol-5-ylmethoxy]-phenyl}-propionic acid
[0624]
[0625] MS (ES): 420.2; the structure is also confirmed by proton NMR.
Example 55
{4-[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0626]
Step A
{4-[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid ethyl ester
[0627] A solution of (4-mercapto-2-methyl-phenoxy)-acetic acid ethyl ester (120 mg, 0.53 mmol) and [5-isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-yl]-methanol (100 mg, 0.35 mmol) in toluene (3.0 mL) is degassed and filled with nitrogen for 3 times. Tributylphosphine (0.13 mL) is added to the reaction mixture under nitrogen at 0° C., followed by addition of of 1,1′-(azodicarbonyl)-dipiperidine (134 mg). The reaction mixture is allowed to warm to room temperature and stirred overnight, the mixture is loaded on silica gel column. Chromatography yields the title compound (120 mg).
[0000] Step B
{4-[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0628] ({4-[5-Isopropyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid ethyl ester (120 mg) is taken into THF (2 mL) and treated with LiOH (1.0 N, 2 mL) for 2 hrs. The reaction mixture is acidified with 5 N HCl, extracted with ethyl ether, dried over sodium sulfate. Concentration yields the title compound. MS (ES): 465.2 (M + +1), the structure is also confirmed by proton NMR.
[0629] The following compounds are made in a similar manner:
Example 56
{4-[5-Isopropyl-3-methyl-2-4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0630]
[0631] MS (ES): 477.2 (M + −1), the structure is also confirmed by proton NMR.
Example 57
{4-[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethoxy]-2-methyl-phenoxy}-acetic acid
[0632]
[0633] MS (ES): 463.2 (M + +1), the structure is also confirmed by proton NMR.
Example 58
3-{4-[5-Isopropyl-3-methyl-2-(4-trifluoromethyl-phenyl)-3H-imidazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0634]
[0635] MS (ES): 461.2 (M + +1), the structure is also confirmed by proton NMR.
Example 59
(3-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid
[0636]
Step A
[0637] (3-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid methyl ester Dissolve 2-[3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-1-ol (219 mg. 0.74 mmol) in toluene (20 mL). Add (3-mercapto-phenyl)-acetic acid methyl ester (175 mg., 0.96 mmol) while stirring. This mixture is degassed passing Argon for 10 minutes. Then, add n-tributyl phosphine (0.3 mL, 1.18 mmol) dropwise. Cool the reaction mixture to 0° C. (ice bath). Add Azo-dicarbonyldipiperidine (ADDP) (261 mg., 1.04 mmol) portionwise. Allow the reaction mixture to warm slowly to room temperature overnight. The next day, remove the solvent on rotavapor. Take up the resulting solid in ethyl ether (70 mL), filter off the solids and wash the filtrate with saturated sodium bicarbonate solution (3×30 mL), brine (3×30 mL), dry over Na 2 SO 4 , and concentrate to afford the crude compound. Purify by silica gel column chromatography (40% EtOAc in Hexanes) to yield 330 mg. of pure title compound (97%). MPLC (M + +1=463.3).
[0000] Step B
(3-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid
[0638] Dissolve (3-{2-[3,5-dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl) acetic acid methyl ester (114 mg., 0.25 mmol) in THF (5 ml) and MeOH (10 mL) at room temperature. Cool to 0° C. (ice bath) and add 2.5 mL of a 2N aqueous solution of KOH. Stir the reaction at room temperature overnight. The following day, add 2N HCl until the solution reach pH=3-4. Extract with EtOAc (70 mL), wash the organic phase with brine (3×30 mL), and dry over Na 2 SO 4 .to afford 110 mg. of title compound (99%). MPLC (M + +1=449.3).
[0639] The following compounds were made in a similar manner:
Example 60
(4-{1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-2-methyl-phenoxy)-acetic acid
[0640]
[0641] MS (M + +1=449.1).
Example 61
(4-{1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0642]
[0643] MS (M + +1=465.1).
Example 62
(4-{1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenoxy)-acetic acid
[0644]
[0645] MS (M + +1=463.1).
Example 63
(4-{1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0646]
[0647] MS (M + +1=478.1).
Example 64
3-(4-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenyl)-propionic acid
[0648]
[0649] MS (M + +1=461.1.1).
Example 65
3-(4-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-2-methyl-phenyl)-propionic acid
[0650]
[0651] MS (M + +1477.1).
Example 66
3-(4-{1-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-2-methyl-phenyl)-propionic acid
[0652]
[0653] MS (M + +1=447.1).
Example 67
3-{4-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0654]
[0655] MS (M + +1=433.1).
Example 68
(3-{2-[3,5-Dimethyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-acetic acid
[0656]
[0657] MS (M + +1=433.1).
Example 69
3-{2-Methyl-4-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-phenyl}-propionic acid
[0658]
[0659] HRMS: Calcd. 435.1354, Found: 435.1351.
Example 70
3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid
[0660]
[0661] HRMS: Calcd. 463.1667, Found: 463.1651.
Example 71
3-(2-Methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-propionic acid
[0662]
[0663] HRMS: Calcd. 477.1823, Found: 477.1825.
Example 72
3-(2-Methyl-4-{2-methyl-1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-propionic acid
[0664]
[0665] HRMS: Calcd. 477.1823, Found: 477.1817
Example 73
3-(2-Methyl-4-{1-methyl-1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenyl)-propionic acid
[0666]
[0667] HRMS: Calcd. 463.1667, Found: 463.1654.
Example 74
(2-Methyl-4-{1-methyl-1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl-]-ethylsulfanyl}-phenoxy)-acetic acid
[0668]
[0669] HRMS: Calcd. 465.1460, Found: 465.1444
Example 75
3-{4-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid
[0670]
[0671] HRMS: Calcd. 463.1667, Found: 463.1669.
Example 76
3-{4-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0672]
[0673] HRMS: Calcd. 447.1895, Found: 447.1893.
Example 77
{4-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0674]
[0675] HRMS: Calcd. 465.1460, Found: 465.1439.
Example 78
{4-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenylsulfanyl}-acetic acid
[0676]
[0677] HRMS: Calcd. 465.1460, Found: 465.1451
Example 79
3-{3-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-propionic acid
[0678]
[0679] HRMS: Calcd. 433.1739, Found: 433.1736.
Example 80
3-(4-{1-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0680]
[0681] HRMS: Calcd. 477.1823, Found: 477.1820.
Example 81
3-(4-{1-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-1-methyl-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0682]
[0683] HRMS: Calcd. 491.1980, Found: 491.1977.
Example 82
(4-{1-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-1-methyl-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0684]
[0685] HRMS: Calcd. 493.1773, Found: 493.1762.
Example 83
3-{4-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid
[0686]
[0687] HRMS: Calcd. 477.1823, Found: 477.1810.
Example 84
3-(4-{1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0688]
[0689] HRMS: Calcd. 491.1980, Found: 491.1970.
Example 85
3-(4-{1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-ethyl-phenyl)-propionic acid
[0690]
[0691] HRMS: Calcd. 505.2137, Found: 505.2125.
Example 86
(4-{1-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0692]
[0693] HRMS: Calcd. 493.1773, Found: 493.1779.
Example 87
(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenyl)-acetic acid
[0694]
[0695] HRMS: Calcd. 433.1739, Found: 433.1745.
Example 88
(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-acetic acid
[0696]
[0697] HRMS: Calcd. 449.1511, Found: 449.1502.
Example 89
(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-acetic acid
[0698]
[0699] Isomer-1, HRMS: Calcd. 449.1511, Found: 449.1517;
[0700] Isomer-2, HRMS: Calcd. 449.1511, Found: 449.1514.
Example 90
2-Methyl-2-(2-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenoxy)-propionic acid
[0701]
[0702] HRMS: Calcd. 491.2158, Found: 491.2137.
Example 91
2-Methyl-2-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenoxy)-propionic acid
[0703]
[0704] HRMS: Calcd. 477.2001, Found: 477.1977.
Example 92
2-Methyl-2-(3-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0705]
[0706] HRMS: Calcd. 447.1895, Found: 447.1882.
Example 93
2-Methyl-2-(3-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-propionic acid
[0707]
[0708] HRMS: Calcd. 463.1844, Found: 463.1824.
Example 94
2-Methyl-2-(2-methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethoxy}-phenoxy)-propionic acid
[0709]
[0710] ESMS+: 463 (M+H).
Example 95
2-Methyl-2-(2-methyl-4-{1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-phenoxy)-propionic acid
[0711]
[0712] HRMS: Calcd. 479.1616, Found, 479.1618.
Example 96
2-Methyl-2-(3-methyl-4-{2- [3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-propionic acid
[0713]
[0714] High Res. EI-MS: 463.1827; calc. 463.1844.
Example 97
2-Methyl-2-(3-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenylsulfanyl)-propionic acid
[0715]
[0716] High Res. EI-MS: 493.1757; calc. 493.1773.
Example 98
3-(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0717]
[0718] High Res. EI-MS: 433.1724; calc. 493.1739.
Example 99
2-Methyl-2-(3-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-propionic acid
[0719]
[0720] High Res. EI-MS: 477.1998; calc. 477.2001.
Example 100
2-Methoxy-3-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0721]
[0722] High Res. EI-MS: 463.1837; calc. 463.1844.
Example 101
2,2-Dimethyl-3-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0723]
[0724] High Res. EI-MS: 475.2201; calc. 475.2208.
Example 102
3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-benzoic acid
[0725]
[0726] High Res. EI-MS: 405.1428; calc. 405.1426.
Example 103
3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-benzoic acid
[0727]
[0728] High Res. EI-MS: 421.1209; calc. 421.1198.
Example 104
(3-{3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenyl)-acetic acid
[0729]
[0730] High Res. EI-MS: 433.1729; calc. 433.1739.
Example 105
2-Methyl-2-(4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenoxy)-propionic acid
[0731]
[0732] High Res. EI-MS: 477.1998; calc. 477.2001.
Example 106
2-Methyl-2-(2-methyl-4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenoxy)-propionic acid
[0733]
[0734] High Res. EI-MS: 491.2146; calc. 491.2158.
Example 107
(2-Methyl-4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-acetic acid
[0735]
[0736] High Res. EI-MS: 479.1605; calc. 479.1616.
Example 108
3-{3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-benzoic acid
[0737]
[0738] High Res. EI-MS: 435.1348; calc. 435.1354.
Example 109
2,2-Dimethyl-3-(2-methyl-4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenyl)-propionic acid
[0739]
[0740] High Res. EI-MS: 489.2325; calc. 489.2365.
Example 110
(3-{3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-acetic acid
[0741]
[0742] High Res. EI-MS: 449.1524; calc. 449.1511.
Example 111
3-{4-[3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0743]
[0744] High Res. EI-MS: 495.1656; calc. 495.1662.
Example 112
{4-[3-tert-Butyl-5-chloro-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0745]
[0746] High Res. EI-MS: 513.1224; calc. 513.1226.
Example 113
3-{4-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0747]
[0748] MS (ES): 461.2 (M+1)
Example 114
{4-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0749]
[0750] MS (ES): 479.2 (M+1)
Example 115
(4-{1-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0751]
[0752] High Res. EI-MS: 559.1672; calc. 559.1678.
Example 116
3-(4-{1-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0753]
[0754] High Res. EI-MS: 557.1864; calc. 557.1866.
Example 117
{4-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenoxy}-acetic acid
[0755]
[0756] High Res. EI-MS: 545.1512; calc. 545.1522.
Example 118
3-{4-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethylsulfanyl]-2-methyl-phenyl}-propionic acid
[0757]
[0758] High Res. EI-MS: 543.1706; calc. 543.1729.
Example 119
{3-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-phenyl}-acetic acid
[0759]
[0760] High Res. EI-MS: 499.1647; calc. 499.1645.
Example 120
3-{4-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-ylmethoxy]-2-methyl-phenyl}-propionic acid
[0761]
[0762] High Res. EI-MS: 527.1953; calc. 527.1957.
Example 121
(4-{2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0763]
[0764] High Res. EI-MS: 507.1917; calc. 507.1929.
Example 122
(3-{2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propylsulfanyl}-phenyl)-acetic acid
[0765]
[0766] High Res. EI-MS: 461.2061; calc. 461.2025.
Example 123
(3-{2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-acetic acid
[0767]
[0768] High Res. EI-MS: 447.1830; calc. 447.1823.
Example 124
3-(4-{2-[3-tert-Butyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenyl)-propionic acid
[0769]
[0770] High Res. EI-MS: 489.2371; calc. 489.2365.
Example 125
2-(4-{2-[1-(4-Fluoro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenoxy)-2-methyl-propionic acid
[0771]
Example 126
2-(4-{2-[3-(4-Chloro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenoxy)-2-methyl-propionic acid
[0772]
Example 127
2-Methyl-2-{2-methyl-4-[2-(3-methyl-1-p-tolyl-1H-pyrazol-4-yl)-propoxy]-phenoxy}-propionic acid
[0773]
Example 128
(3-{2-[1-(4-Fluoro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-phenyl)-acetic acid
[0774]
Example 129
{3-[2-(3-Methyl-1-p-tolyl-1H-pyrazol-4-yl)-propoxy]-phenyl}-acetic acid
[0775]
[0776] The following single enantiomers were obtained by chiral separation using chiral HPLC column:
Example 130
3-(4-{1-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl) -propionic acid
[0777]
[0778] Isomer 1, High Res. El-MS: 557.1886; calc. 557.1866.
[0779] Isomer 2, High Res. El-MS: 557.1922; calc. 557.1866.
Example 131
(4-{1-[3-[2-(2-Fluoro-phenyl)-ethyl]-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenoxy)-acetic acid
[0780]
[0781] Isomer 1, High Res. El-MS: 559.1665; calc. 559.1678.
[0782] Isomer 2, High Res. EI-MS: 559.1666; calc. 559.1678.
Example 132
(3-{3-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenyl)-acetic acid
[0783]
[0784] Isomer 1, High Res. EI-MS: 433.1728; calc. 433.1739.
[0785] Isomer 2, High Res. EI-MS: 433.1732; calc. 433.1739.
Example 133
2-Methyl-2-(4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenoxy)-propionic acid
[0786]
[0787] Isomer 1, High Res. EI-MS: 477.1986; calc. 477.2001.
[0788] Isomer 2, High Res. EI-MS: 477.1985; calc. 477.2001.
Example 134
(2-Methyl-4-{3-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butylsulfanyl}-phenyl)-acetic acid
[0789]
[0790] Isomer 1, High Res. EI-MS: 479.1611; calc. 479.1616.
[0791] Isomer 2, High Res. EI-MS: 479.1610; calc. 479.1616.
Example 135
3-(4-{1-[3-Isopropyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethylsulfanyl}-2-methyl-phenyl)-propionic acid
[0792]
[0793] Isomer-1: HRMS: Calcd. 477.1823, Found: 477.1810;
[0794] Isomer-2: HRMS: Calcd. 477.1823, Found: 477.1812.
Example 136
(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-butoxy}-phenyl)-acetic acid
[0795]
[0796] Isomer-2, ESMS+: 433 (M+H);
[0797] Isomer-2, ESMS+: 433 (M+H). Example 137
2-Methyl-2-(3-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-propionic acid
[0798]
[0799] Isomer 1; High Res. EI-MS: 463.1886; calc. 463.1844.
[0800] Isomer 2, High Res. EI-M$: 463.1839; calc. 463.1844.
Example 138
2-Methyl-2-(3-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenylsulfanyl)-propionic acid
[0801]
[0802] Isomer 1, High Res. EI-MS: 493.1785; calc. 493.1773.
[0803] Isomer 2, High Res. EI-MS: 493.1757; calc. 493.1773.
Example 139
3-(3-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0804]
[0805] Isomer 1, High Res. EI-MS: 433.1745; calc. 493.1739.
[0806] Isomer 2, High Res. EI-MS: 433.1719; calc. 493.1739.
Example 140
2-Methyl-2-(3-methyl-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenoxy)-propionic acid
[0807]
[0808] Isomer 1, High Res. EI-MS: 477.1989; calc. 477.2001.
[0809] Isomer 2, High Res. EI-MS: 477.1989; calc. 477.2001.
Example 141
2-Methoxy-3-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propoxy}-phenyl)-propionic acid
[0810]
[0811] Isomer 1, High Res. EI-MS: 463.1838; calc. 463.1844.
[0812] Isomer 2, High Res. EI-MS: 463.1854; calc. 463.1844.
Example 142
2-(4′-{2-[1-(4-Chloro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenoxy)-2-methyl-propionic acid
[0813]
[0814] Isomer-1 and Isomer-2.
Example 143
2-Methyl-2-{2-methyl-4-[2-(3-methyl-1-p-tolyl-1H-pyrazol-4-yl)-propoxy]-phenoxy}-propionic acid
[0815]
[0816] Isomer-1: and Isomer-2.
Example 144
2-(4-{2-[1-(4-Fluoro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-2-methyl-phenoxy)-2-methyl-propionic acid
[0817]
[0818] Isomer-1 and Isomer-2.
Example 145
(3-{2-[1-(4-Fluoro-phenyl)-3-methyl-1H-pyrazol-4-yl]-propoxy}-phenyl)-acetic acid
[0819]
[0820] Isomer-1 and Isomer-2.
Example 146
{3-[2-(3-Methyl-1-p-tolyl-1H-pyrazol-4-yl)-propoxy]-phenyl}-acetic acid
[0821]
[0822] Isomer-1 and Isomer-2.
[0823] The following compounds were also made:
Example 147
(4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethyl)}-phenoxy)-acetic acid
[0824]
[0825] HRMS: Calcd. 405.1426, Found: 405.1412.
Example 148
2-Methyl-2-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethyl}-phenoxy)-propionic acid
[0826]
[0827] HRMS: Calcd. 433.1739, Found: 433.1731.
Example 149
(4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-acetic acid
[0828]
[0829] HRMS: Calcd. 419.1582, Found: 419.1594.
Example 150
2-Methyl-2-(4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-propionic acid
[0830]
Step A
(R,S)-1-(4-Methoxy-phenyl)-2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-2-ol
[0831]
[0832] To a solution of 1-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-ethanone (804 mg, 3 mmol) in THF (20 mL) at −80 0C. is added 4-methoxylbenzyl magnesium chloride (0.25 M in THF, 24 mL) and the mixture is stirred at ambient temperature overnight. It is quenched with 0.2 N HCl, extracted with EtOAc. The organic layer is concentrated to give the titled compound as an oil. This is used for the next reaction without further purification.
[0833] ESMS+: 391 (M+H)
Step B
(R,S)-4-[2-(4-Methoxy-phenyl)-1-methyl-ethyl]-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole
[0834]
[0835] To a solution of (R, S)-1-(4-methoxy-phenyl)-2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propan-2-ol (3 mmol) in dichloromethane (20 mL) at room temperature is added TFA (1.2 mL, 15 mmol) followed by Et3SiH (2.4 mL, 15 mmol). After 3 hours, it is quenched with saturated NaHCO3, extracted with dichloromethane. The organic layer is concentrated and purified by column chromatography (0-5% EtOAc in hexanes) to give a white solid. This is subjected to hydrogenation (5% Pd/C, 60 psi) in EtOH overnight. It is filtered and washed with EtOH. Combined filtrate is concentrated to give an oil: 760 mg (84%). This is used for the next reaction without further purification.
Step C
(R,S)-4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenol
[0836]
[0837] (R,S)-4-[2-(4-Methoxy-phenyl)-1-methyl-ethyl]-3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazole (760 mg, 2 mmol) is treated with BBr3/CH2Cl2 (1M, 6 mL) from 0 0C to room temperature for 3 hours. It is quenched with MeOH and evaporated to dryness. The residue is purified by column chromatography (0-20% EtOAc in hexanes) to give the titled compound as a solid: 320 mg (44%)
[0838] ESMS−: 359 (M−1).
Step D
(R,S)-(4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-acetic acid methyl ester
[0839]
[0840] A mixture of (R,S)-4-{2-[3-methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenol (150 mg, 0.42 mmol), methyl bromoacetate (0.096 mL, 1 mmol) and potassium carbonate (172 mg, 1.26 mmol) in acetonitrile (7 mL) is stirred at reflux overnight. It is filtered and washed with EtOAc. The combined filtrate is concentrated and purified by column chromatography (0-20% EtOAc in hexanes) to give the titled compound: 135 mg (75%).
[0841] ESMS+: 433 (M+H).
Step E
(R,S)-(4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-acetic acid
[0842]
[0843] (R,S)-(4-{2-[3-Methyl-1-(4-trifluoromethyl-phenyl)-1H-pyrazol-4-yl]-propyl}-phenoxy)-acetic acid methyl ester (135 mg, 0.3 mmol) is treated in a mixture of 2N LiOH/H2O and dioxane at 80 0C. for 3 hours. Solvent is evaporated and the residue partitioned between EtOAc and 1N HCl. The organic layer is concentrated to give the titled compound as a solid: 126 mg (96%).
[0844] HRMS: Calcd. 419.1582, Found: 419.1594.
Example 151
{3-[2-Methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenyl}-acetic acid
[0845]
[0846] HRMS: Calcd. 391.1270, found, 391.1253.
Example 152
{2-Methyl-4-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethylsulfanyl]-phenoxy}-acetic acid
[0847]
[0848] HRMS: Calcd. 437.1147, found, 437.1144.
Example 153
2-Methyl-2-{4-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenoxy}-propionic acid
[0849]
[0850] HRMS: Calcd. 435.1532, found, 435.1527.
Example 154
2-Methyl-2-{2-methyl-4-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenoxy}-propionic acid
[0851]
[0852] HRMS: Calcd. 449.1688, found, 449.1690.
Example 155
(S)-2-Methoxy-3-{4-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenyl}-propionic acid
[0853]
[0854] HRMS: Calcd. 435.1532, found, 435.1544.
Example 156
2,2-Dimethyl-3-{4-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenyl}-propionic acid
[0855]
[0856] HRMS: Calcd. 447.1895, found, 447.1890.
Example 157
3-{3-[2-Methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethoxy]-phenyl}-propionic acid
[0857]
[0858] HRMS: Calcd. 405.1426, found, 405.1413.
Example 158
3-[2-Methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-ylmethylsulfanyl]-benzoic acid
[0859]
[0860] HRMS: Calcd. 393.0884, found, 393.0875.
Example 159
(R,S)-(3-{2-[2-Methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-yl]-propoxy}-phenyl)-acetic acid
[0861]
[0862] HRMS: Calcd. 419.1582, found, 419.1583.
Example 160
(R,S)-(3-{2-[2-Methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-yl]-propylsulfanyl}-phenyl)-acetic acid
[0863]
[0864] HRMS: Calcd. 435.1354, found, 435.1351.
Example 161
(R,S)-(2-Methyl-4-{2-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-yl]-propylsulfanyl}-phenoxy)-acetic acid
[0865]
[0866] HRMS: Calcd. 465.1460, found, 465.1451.
Example 162
(R,S)-3-(2-Methyl-4-{2-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-yl]-propoxy}-phenyl)-propionic acid
[0867]
[0868] HRMS: Calcd. 447.1895, found, 447.1873.
Example 163
(R,S)-2-Methyl-2-(2-methyl-4-{2-[2-methyl-5-(4-trifluoromethyl-phenyl)-2H-pyrazol-3-yl]-propoxy}-phenoxy)-propionic acid
[0869]
[0870] HRMS: Calcd. 477.2001, found, 477.1989.
Biological Assays
Binding and Cotransfection Studies
[0871] The in vitro potency of compounds in modulating PPARα receptors are determined by the procedures detailed below. DNA-dependent binding (ABCD binding) is carried out using SPA technology with PPAR receptors. Tritium-labeled PPARα agonists are used as radioligands for generating displacement curves and IC 50 values with compounds of the invention. Cotransfection assays are carried out in CV-1 cells. The reporter plasmid contained an acylCoA oxidase (AOX) PPRE and TK promoter upstream of the luciferase reporter cDNA. Appropriate PPARs are constitutively expressed using plasmids containing the CMV promoter. For PPARα, interference by endogenous PPARγ in CV-1 cells is an issue. In order to eliminate such interference, a GAL4 chimeric system is used in which the DNA binding domain of the transfected PPAR is replaced by that of GAL4, and the GAL4 response element is utilized in place of the AOX PPRE. Cotransfection efficacy is determined relative to PPARα agonist reference molecules. Efficacies are determined by computer fit to a concentration-response curve, or in some cases at a single high concentration of agonist (10 μM).
[0872] These studies are carried out to evaluate the ability of compounds of the invention to bind to and/or activate various nuclear transcription factors, particularly huPPARα (“hu” indicates “human”). These studies provide in vitro data concerning efficacy and selectivity of compounds of the invention. Furthermore, binding and cotransfection data for compounds of the invention are compared with corresponding data for marketed compounds that act on huPPARα.
[0873] The binding and cotransfection efficacy values for compounds of the invention which are especially useful for modulating a PPAR receptor, are ≦100 nM and ≧50%, respectively.
Evaluation of Triglyceride Reduction and HDL Cholesterol Elevation in HuapoAI Transgenic Mice
[0874] Compounds of the present invention are studied for effects upon HDL and triglyceride levels in human apoAI mice. For each compound tested, seven to eight week old male mice, transgenic for human apoAI (C57BL/6-tgn(apoa1)1rub, Jackson Laboratory, Bar Harbor, Me.) are acclimated in individual cages for two weeks with standard chow diet (Purina 5001) and water provided ad libitum. After the acclimation, mice and chow are weighed and assigned to test groups (n=5) with randomization by body weight. Mice are dosed daily by oral gavage for 8 days using a 29 gauge, 1½ inch curved feeding needle (Popper & Sons). The vehicle for the controls, test compounds and the positive control (fenofibrate 100 mg/kg) is 1% carboxymethylcellulose (w/v) with 0.25% tween 80 (w/v). All mice are dosed daily between 6 and 8 a.m. with a dosing volume of 0.2 ml. Prior to termination, animals and diets are weighed and body weight change and food consumption are calculated. Three hours after last dose, mice are euthanized with CO2 and blood is removed (0.5-1.0 ml) by cardiac puncture. After sacrifice, the liver, heart, and epididymal fat pad are excised and weighed. Blood is permitted to clot and serum is separated from the blood by centrifugation.
[0875] Cholesterol and triglycerides are measured colorimetrically using commercially prepared reagents (for example, as available from Sigma #339-1000 and Roche #450061 for triglycerides and cholesterol, respectively). The procedures are modified from published work (McGowan M. W. et al., Clin Chem 29:538-542, 1983; Allain C. C. et al., Clin Chem 20:470-475, 1974. Commercially available standards for triglycerides and total cholesterol, respectively, commercial quality control plasma, and samples are measured in duplicate using 200 μl of reagent. An additional aliquot of sample, added to a well containing 200 μl water, provided a blank for each specimen. Plates are incubated at room temperature on a plate shaker and absorbance is read at 500 nm and 540 nm for total cholesterol and triglycerides, respectively. Values for the positive control are always within the expected range and the coefficient of variation for samples is below 10%. All samples from an experiment are assayed at the same time to minimize inter-assay variability.
[0876] Serum lipoproteins are separated and cholesterol quantitated by fast protein liquid chromatography (FPLC) coupled to an in line detection system. Samples are applied to a Superose 6 HR size exclusion column (Amersham Pharmacia Biotech) and eluted with phosphate buffered saline-EDTA at 0.5 ml/min. Cholesterol reagent (Roche Diagnostics Chol/HP 704036) at 0.16 ml/min mixed with the column effluent through a T-connection and the mixture passed through a 15 m×0.5 mm id knitted tubing reactor immersed in a 37 C water bath. The colored product produced in the presence of cholesterol is monitored in the flow strem at 505 nm and the analog voltage from the monitor is converted to a digital signal for collection and analysis. The change in voltage corresponding to change in cholesterol concentration is plotted vs time and the area under the curve corresponding to the elution of very low density lipoprotein (VLDL), low density lipoprotein (LDL) and high density lipoprotein (HDL) is calculated using Perkin Elmer Turbochrome software.
[0877] Triglyceride Serum Levels in Mice Dosed with a Compound of the Invention is Compared to Mice Receiving the Vehicle to identify compounds which could be particularly useful for lowering triglycerides. Generally, triglyceride decreases of greater than or equal to 30% (thirty percent) compared to control following a 30 mg/kg dose suggests a compound that can be especially useful for lowering triglyceride levels.
[0878] The percent increase of HDLc serum levels in mice receiving a compound of the invention is compared to mice receiving vehicle to identify compounds of the invention that could be particularly useful for elevating HDL levels. Generally, and increase of greater than or equal to 25% (twenty five percent) increase in HDLc level following a 30 mg/kg dose suggests a compound that can be especially useful for elevating HDLc levels.
[0879] It may be particularly desirable to select compounds of this invention that both lower triglyceride levels and increase HDLc levels. However, compounds that either lower triglyceride levels or increase HDLc levels may be desirable as well.
Evaluation of Glucose Levels in db/db Mice
[0880] The effects upon plasma glucose associated with administering various dose levels of different compounds of the present invention and the PPAR gamma agonist rosiglitazone (BRL49653) or the PPAR alpha agonist fenofibrate, and the control, to male db/db mice, are studied.
[0881] Five week old male diabetic (db/db) mice [for example, C57BlKs/j-m+/+Lepr(db), Jackson Laboratory, Bar Harbor, Me.] or lean littermates are housed 6 per cage with food and water available at all times. After an acclimation period of 2 weeks, animals are individually identified by ear notches, weighed, and bled via the tail vein for determination of initial glucose levels. Blood is collected (100 μl) from unfasted animals by wrapping each mouse in a towel, cutting the tip of the tail with a scalpel, and milking blood from the tail into a heparinized capillary tube. Sample is discharged into a heparinized microtainer with gel separator and retained on ice. Plasma is obtained after centrifugation at 4° C. and glucose measured immediately. Remaining plasma is frozen until the completion of the experiment, when glucose and triglycerides are assayed in all samples. Animals are grouped based on initial glucose levels and body weights. Beginning the following morning, mice are dosed daily by oral gavage for 7 days. Treatments are test compounds (30 mg/kg), a positive control agent (30 mg/kg) or vehicle [1% carboxymethylcellulose (w/v)/0.25% Tween80 (w/v); 0.3 ml/mouse]. On day 7, mice are weighed and bled (tail vein) 3 hours after dosing. Twenty-four hours after the 7 th dose (i.e., day 8), animals are bled again (tail vein). Samples obtained from conscious animals on days 0, 7 and 8 are assayed for glucose. After the 24-hour bleed, animals are weighed and dosed for the final time. Three hours after dosing on day 8, animals are anesthetized by inhalation of isoflurane and blood obtained via cardiac puncture (0.5-0.7 ml). Whole blood is transferred to serum separator tubes, chilled on ice and permitted to clot. Serum is obtained after centrifugation at 4° C. and frozen until analysis for compound levels. After sacrifice by cervical dislocation, the liver, heart and epididymal fat pads are excised and weighed.
[0882] Glucose is measured calorimetrically using commercially purchased reagents. According to the manufacturers, the procedures are modified from published work (McGowan, M. W., Artiss, J. D., Strandbergh, D. R. & Zak, B. Clin Chem, 20:470-5 (1974) and Keston, A. Specific colorimetric enzymatic analytical reagents for glucose. Abstract of papers 129th Meeting ACS, 31C (1956).); and depend on the release of a mole of hydrogen peroxide for each mole of analyte, coupled with a color reaction first described by Trinder (Trinder, P. Determination of glucose in blood using glucose oxidase with an alternative oxygen acceptor. Ann Clin Biochem, 6:24 (1969)). The absorbance of the dye produced is linearly related to the analyte in the sample. The assays are further modified in our laboratory for use in a 96 well format. The commercially available standard for glucose, commercially available quality control plasma, and samples (2 or 5 μl/well) are measured in duplicate using 200 μl of reagent. An additional aliquot of sample, pipetted to a third well and diluted in 200 μl water, provided a blank for each specimen. Plates are incubated at room temperature for 18 minutes for glucose on a plate shaker (DPC Micormix 5) and absorbance read at 500 nm on a plate reader. Sample absorbances are compared to a standard curve (100-800 for glucose). Values for the quality control sample are always within the expected range and the coefficient of variation for samples is below 10%. All samples from an experiment are assayed at the same time to minimize inter-assay variability.
Evaluation of the Effects of Compounds of the Present Invention upon A y Mice Body Weight, Fat Mass, Glucose and Insulin Levels
[0000] Female A y Mice
[0883] Female A y mice are singly housed, maintained under standardized conditions (22° C., 12 h light:dark cycle), and provided free access to food and water throughout the duration of the study. At twenty weeks of age the mice are randomly assigned to vehicle control and treated groups based on body weight and body fat content as assessed by DEXA scanning (N=6). Mice are then dosed via oral gavage with either vehicle or a Compound of this invention (50 mg/kg) one hour after the initiation-of the light cycle (for example, about 7 A.M.) for 18 days. Body weights are measured daily throughout the study. On day 14 mice are maintained in individual metabolic chambers for indirect calorimetry assessment of energy expenditure and fuel utilization. On day 18 mice are again subjected to DEXA scanning for post treatment measurement of body composition.
[0884] The results of p.o. dosing of compound for 18 days on body weight, fat mass, and lean mass are evaluated and suggest which compounds of this invention can be especially useful for maintaining desirable weight and/or promoting desired lean to fat mass.
[0885] Indirect calorimetry measurements revealing a significant reduction in respiratory quotient (RQ) in treated animals during the dark cycle [0.864±0.013 (Control) vs. 0.803±0.007 (Treated); p<0.001] is indicative of an increased utilization of fat during the animals' active (dark) cycle and can be used to selected especially desired compounds of this invention. Additionally, treated animals displaying significantly higher rates of energy expenditure than control animals suggest such compounds of this invention can be especially desired.
[0000] Male KK/A y Mice
[0886] Male KK/A y mice are singly housed, maintained under standardized conditions (22° C., 12 h light:dark cycle), and provided free access to food and water throughout the duration of the study. At twenty-two weeks of age the mice are randomly assigned to vehicle control and treated groups based on plasma glucose levels. Mice are then dosed via oral gavage with either vehicle or a Compound of this invention (30 mg/kg) one hour after the initiation of the light cycle (7 A.M.) for 14 days. Plasma glucose, triglyceride, and insulin levels are assessed on day 14.
[0887] The results of p.o. dosing of compound for 14 days on plasma glucose, triglycerides, and insulin are evaluated to identify compounds of this invention which may be especially desired.
[0000] Method to Elucidate the LDL-cholesterol Total-cholesterol and Triglyceride Lowering Effect
[0888] Male Syrian hamsters (Harlan Sprague Dawley) weighing 80-120 g are placed on a high-fat cholesterol-rich diet for two to three weeks prior to use. Feed and water are provided ad libitum throughout the course of the experiment. Under these conditions, hamsters become hypercholesterolemic showing plasma cholesterol levels between 180-280 mg/dl. (Hamsters fed with normal chow have a total plasma cholesterol level between 100-150 mg/dl.) Hamsters with high plasma cholesterol (180 mg/dl and above) are randomized into treatment groups based on their total cholesterol level using the GroupOptimizeV211.xls program.
[0889] A Compound of this invention is dissolved in an aqueous vehicle (containing CMC with Tween 80) such that each hamster received once a day approx. 1 ml of the solution by garvage at doses 3 and 30 mg/kg body weight. Fenofibrate (Sigma Chemical, prepared as a suspension in the same vehicle) is given as a known alpha-agonist control at a dose of 200 mg/kg, and the blank control is vehicle alone. Dosing is performed daily in the early morning for 14 days.
[0890] Quantification of Plasma Lipids:
[0891] On the last day of the test, hamsters are bled (400 ul) from the suborbital sinus while under isoflurane anesthesia 2 h after dosing. Blood samples are collected into heparinized microfuge tubes chilled in ice bath. Plasma samples are separated from the blood cells by brief centrifugation. Total cholesterol and triglycerides are determined by means of enzymatic assays carried out automatically in the Monarch equipment (Instrumentation Laboratory) following the manufacturer's precedure. Plasma lipoproteins (VLDL, LDL and HDL) are resolved by injecting 25 ul of the pooled plasma samples into an FPLC system eluted with phosphate buffered saline at 0.5 ml/min through a Superose 6 HR 10/30 column (Pharmacia) maintained room temp. Detection and characterization of the isolated plasma lipids are accomplished by postcolumn incubation of the effluent with a Cholesterol/HP reagent (for example, Roche Lab System; infused at 0.12 ml/min) in a knitted reaction coil maintained at 37° C. The intensity of the color formed is proportional to the cholesterol concentration and is measured photometrically at 505 nm.
[0892] The effect of administration of a Compound of this invention for 14 days is studied for the percent reduction in LDL level with reference to the vehicle group. Especially desired compounds are markedly more potent than fenofibrate in LDL-lowering efficacy. Compounds of this invention that decrease LDL greater than or equal to 30% (thirty percent) compared to vehicle can be especially desired.
[0893] The total-cholesterol and triglyceride lowering effects of a Compound of this invention is also studied. The data for reduction in total cholesterol and triglyceride levels after treatment with a compound of this invention for 14 days is compared to the vehicle to suggest compounds that can be particularly desired. The known control fenofibrate did not show significant efficacy under the same experimental conditions.
[0000] Method to Elucidate the Fibrinogen-Lowering Effect of PPAR Modulators
[0000] Zucker Fatty Rat Model:
[0894] The life phase of the study on fibrinogen-lowering effect of compounds of this invention is part of the life phase procedures for the antidiabetic studies of the same compounds. On the last (14 th ) day of the treatment period, with the animals placed under surgical anesthesia, ˜3 ml of blood is collected, by cardiac puncture, into a syringe containing citrate buffer. The blood sample is chilled and centrifuged at 4° C. to isolate the plasma that is stored at −70° C. prior to fibrinogen assay.
[0000] Quantification of Rat Plasma Fibrinogen:
[0895] Rat plasma fibrinogen levels are quantified by using a commercial assay system consists of a coagulation instrument following the manufacturer's protocol. In essence, 100 ul of plasma is sampled from each specimen and a 1/20 dilution is prepared with buffer. The diluted plasma is incubated at 37° C. for 240 seconds. Fifty microliters of clotting reagent thrombin solution (provided by the instrument's manufacturer in a standard concentration) is then added. The instrument monitors the clotting time, a function of fibrinogen concentration quantified with reference to standard samples. Compounds that lower fibrinogen level greater than vehicle can be especially desired.
[0896] Cholesterol and triglyceride lowering effects of compounds of this invention are also studied in Zucker rats.
[0000] Method to Elucidate the Anti-Body Weight Gain and Anti-Appetite Effects of Compounds of this Invention
[0000] Fourteen-Day Study in Zucker Fatty Rat 1 or ZDF Rat 2 Models:
[0897] Male Zucker Fatty rats, non-diabetic (Charles River Laboratories, Wilmington, Mass.) or male ZDF rats (Genetic Models, Inc, Indianapolis, Ind.) of comparable age and weight are acclimated for 1 week prior to treatment. Rats are on normal chow and water is provided ad libitum throughout the course of the experiment.
[0898] Compounds of this invention are dissolved in an aqueous vehicle such that each rat received once a day approximately 1 ml of the solution by garvage at doses 0.1, 0.3, 1 and 3 mg/kg body weight. Fenofibrate (Sigma Chemical, prepared as a suspension in the same vehicle) a known alpha-agonist given at doses of 300 mg/kg, as well as the vehicle are controls. Dosing is performed daily in the early morning for 14 days. Over the course of the experiment, body weight and food consumption are monitored.
[0899] Using this assay, compounds of this invention are identified to determine which can be associated with a significant weight reduction.
[0000] Method to Elucidate the Activation of the PPAR Delta Receptor in Vivo
[0900] This method is particularly useful for measuring the in vivo PPARdelta receptor activation of compounds of this invention that are determined to possess significant in vitro activity for that receptor isoform over the PPAR gamma isoform.
[0901] Male PPARa null mice (129s4 SvJae-PPARa<tm1Gonz>mice; Jackson Laboratories) of 8-9 weeks of age are maintained on Purina 5001 chow with water ad libitum for at least one week prior to use. Feed and water are provided ad libitum throughout the course of the experiment. Using the GroupOptimizeV211.xls program, mice are randomized into treatment groups of five animals each based on their body weight.
[0902] Compounds of this invention are suspended in an aqueous vehicle of 1% (w/v) carboxymethylcellulose and 0.25% Tween 80 such that each mouse receives once a day approx. 0.2 ml of the solution by gavage at doses ranging from 0.2 to 20 mg/kg body weight. A control group of mice is included in each experiment whereby they are dosed in parallel with vehicle alone. Dosing is performed daily in the early morning for 7 days.
[0903] On the last day of dosing, mice are euthanized by CO2 asphyxiation 3 hours after the final dose. Blood samples are collected by heart draw into EDTA-containing microfuge tubes and chilled on ice. Liver samples are collected by necropsy and are flash-frozen in liquid nitrogen and stored at ˜80 degrees Celsius. For RNA isolation from liver, five to ten mg of frozen liver is placed in 700 μl of 1× Nucleic Acid Lysis Solution (Applied Biosystems Inc., Foster City, Calif.) and homogenized using a hand-held tissue macerator (Biospec Products Inc., Bartlesville, Okla.). The homogenate is filtered through an ABI Tissue pre-filter (Applied Biosystems Inc., Foster City, Calif.) and collected in a deep well plate on an ABI 6100 Nucleic Acid prep station (Applied Biosystems Inc., Foster City, Calif.). The filtered homogenate is then loaded onto an RNA isolation plate and the RNA Tissue-Filter-DNA method is run on the ABI 6100. The isolated RNA is eluted in 150 μl of RNase free water. For quality assessment, 9 μl of the isolated RNA solution is loaded onto a 1% TBE agarose gel, and the RNA is visualized by ethidium-bromide fluorescence.
[0904] Complementary DNA (cDNA) is synthesized using the ABI High Capacity Archive Kit (Applied Biosystems Inc., Foster City, Calif.). Briefly, a 2× reverse transcriptase Master Mix is prepared according to the manufacturer's protocol for the appropriate number of samples (RT Buffer, dNTP, Random Primers, MultiScribe RT (50U/μl), RNase free water). For each reaction, 50 μl of 2× RT Master Mix is added to 50 μl of isolated RNA in a PCR tube that is incubated in a thermocycler (25° C. for 10 minutes followed by 37° C. for 2 hours). The resultant cDNA preparation is diluted 1:100 in dH2O for analysis by real-time PCR. Also, a standard curve of cDNA is diluted 1:20, 1:100, 1:400, 1:2000, 1:10,000 for use in final quantitation.
[0905] A real-time PCR Master Mix for mouse Cyp4A1 gene expression is mixed to contain:
1× Taqman Universal PCR Master Mix (Applied Biosystems Inc., Foster City, Calif.) 6 micromolar final concentration Forward primer;. Qiagen/Operon Technologies, Alameda, Calif.) 6 micromolar final concentration Reverse primer (Qiagen/Operon Technologies, Alameda, Calif.) 0.15 micromolar final concentration Probe (5′ 6-FAM and 3′ Tamra-Q; Qiagen/Operon Technologies, Alameda, Calif.) RNase free water to 10 microliters
A real-time PCR Master Mix for the 18S ribosomal RNA control gene expression is mixed to contain
1× Taqman Universal PCR Master Mix (Applied Biosystems Inc., Foster City, Calif.) 0.34 micromolar Probe/Primer TaqMan® Ribosomal RNA Control Reagents #4308329 Applied Biosystems Inc., Foster City, Calif.) RNase free water to 10 microliters
[0914] For the real-time PCR analysis, 6 ul of the respective Master Mix solution (either Cyp4A1 or 18S) and 4 ul either of diluted cDNA or of Standard Curve samples is added to individual wells of a 384-well plate (n=2 for Standards; n=4 for unknowns). Reactions are performed using the ABI 7900 HT standard universal RT-PCR cycling protocol. Data are analyzed using SDS 2.1 (Applied Biosystems Inc., Foster City, Calif.). Average quantity and standard deviation are calculated automatically for each individual sample, according to the standard curve values. Using Microsoft Excel 2000, mean values for each group of five individual mice is calculated. The mean value of each compound-treated group is divided by the mean value of the vehicle-treated group. The fold induction over the vehicle group is determined by assigning the vehicle group to the value of 1.0, and the fold change of the mean value for each group is expressed as fold-induction versus vehicle (1.0). Data are plotted using Jandel SigmaPlot 8.0.
Monkey Studies
Efficacy Studies
[0915] Compounds of the invention may be examined in a dyslipidemic rhesus monkey model. After an oral dose-escalation study for 28 days in obese, non-diabetic rhesus monkeys a determination of HDL-c elevation is made with each dose and compared with pretreatment levels. LDL cholesterol is also determined with each dose. C-reactive protein levels are measured and compared to pretreatment levels.
[0916] Compound of Formula I may be shown to elevate plasma HDL-cholesterol levels in an African Green Monkey model in a manner similar to that described above in rhesus monkeys.
[0917] Two groups of monkeys are placed in a dose-escalating study that consists of one week of baseline measurements, 9 weeks of treatments (vehicle, Compound of Formula I), and four weeks of washout. During baseline, monkeys in all three groups are administered vehicle once daily for seven days. Test compound of Formula I, is administered in vehicle once daily for three weeks, then at a greater concentration (double the dose may be desired) once daily for three weeks, and then a still greater concentration (double the most recent dose may be desired) once daily for three weeks. At the completion of treatment, monkeys in both groups are administered vehicle once daily and monitored for an additional six weeks.
[0918] Animals are fasted overnight and then sedated for body weight measurements and blood collection at weeks 1 (vehicle), 2, 3, 4, 6, 7, 9, 10, 12, and 14 of the study.
[0000] Parameters to Measured, for Example:
[0000]
Body weight
Total plasma cholesterol
HDL
LDL
Triglycerides
Insulin
Glucose
PK parameters at week 4, 7, and 10 (plasma drug concentration at last week of each dose)
ApoAI
ApoAII
ApoB
ApoCIII
Liver enzymes (SGPT, SGOT, □GT)
Complete blood count
[0933] Additionally, other measures may be made, as appropriate, and consistent with the stated study design.
[0000] Equivalents:
[0934] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
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The present invention is directed to compounds represented by the following structural formula, Formula I: wherein: (a) X is selected from the group consisting of a single bond, O, S, S(O)2 and N; (b) U is an aliphatic linker; (c) Y is selected from the group consisting of O, C, S, NH and a single bond; (d) E is C(R3)(R4)A or A and wherein (i) A is selected from the group consisting of carboxyl, tetrazole, C1-C6 alkylnitrile, carboxamide, sulfonamide and acylsulfonamide; (e) Z1 and Z2 are each independently selected from the group consisting of N, O, and C with the proviso that at least one of Z1 and Z2 is N; (f) Z3 is selected from the group consisting of N, O, and C. (g) R8 is selected from the group consisting of hydrogen, C1-C6 alkyl, C1-C4 alkylenyl and halo; (h) R9 is selected from the group consisting of hydrogen, C1-C4 alkyl, C1-C4 alkylenyl, halo, aryl-C0-C4 alkyl, heteroaryl, C1-C6 allyl, and OR29.
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TECHNICAL FIELD OF THE INVENTION
[0001] The invention relates to a game, and more particularly to a game using a firearm with specialized ammunition.
SUMMARY OF THE INVENTION
[0002] A gaming apparatus and method is provided that includes the use and application of a combination of a firearm with specialized ammunition, gates, targets, a motorized vehicle and a game track or course. In practice of the game, a rider maneuvers through the course discharging the firearm at targets. Ammunition is provided that is capable of short range use to damage or to destroy the reactive targets while offering reasonable safety to the rider and spectators. The reactive targets may include electronics that act as gating and storing indicators. The reactive targets and the gates can also act as communication points for relay of gating and scoring information to a wireless network device.
BRIEF DESCRIPTION OF THE DRAWINGS
[0003] For a more complete understanding of the features and advantages of the present invention, reference is now made to the detailed description of the invention along with the accompanying figures in which corresponding numerals in the different figures refer to corresponding parts and in which:
[0004] FIG. 1 is a schematic plan view of a game track and targets;
[0005] FIG. 2 is an enlarged view of a player, motorized vehicle and target;
[0006] FIG. 3 is a cut away view of a preferred embodiment of the ammunition used to conduct the game;
[0007] FIG. 4 is a schematic representation of an embodiment of the communication between network components of the invention; and
[0008] FIG. 5 is flow diagram of steps executed by a network controller.
DETAILED DESCRIPTION OF THE INVENTION
[0009] FIGS. 1 and 2 show in detail one embodiment of the game in accordance with the present invention. The game comprises course 17 , gates 13 , targets 14 , barrels 12 , vehicle 15 and firearm 21 . The firearm includes a novel type of blank ammunition. In an additional embodiment, the game comprises course 17 , gates 13 , targets 14 , vehicle 15 and firearm 21 . In an additional embodiment, the game comprises course 17 , barrel 12 , targets 13 , vehicle 15 and firearm 21 .
[0010] In the preferred embodiment, course 17 includes a start/finish gate 11 , path 16 , multiple gates 13 , multiple targets 14 and multiple barrels 12 . However in other embodiments, the course can include either a start/finish gate, gates and targets or the course can include either a start/finish gate, gates and barrels. In the preferred embodiment course 17 is generally planar. The dimensions of course 17 should be approximately 280 feet by approximately 100 feet. The area of the course can be larger or smaller and the topography of the course may vary.
[0011] The arrangement of gates 13 , targets 14 and barrels 12 determine path 16 of course 17 . The rider travels along path 16 in the direction of arrows 10 through all of gates 13 and around all of barrels 12 . The course shown in FIG. 1 is just one arrangement of the gates, targets and barrels. In FIG. 1 , all of gates 13 are shown as a triangle, all of targets 14 are shown as a circle and all of barrels 12 are shown as squares. Gates 13 , targets 14 and barrels 12 can be arranged in a multitude of different patterns in order to provide different challenges to the riders including testing their maneuvering and shooting abilities. For example, group 40 of gates 13 requires the rider to perform a 360 degree turn around gates 13 . While arrangement 41 of gates 13 , requires the rider to perform an “s-like” pattern. The distance between gates 13 and targets 14 varies throughout the entire course.
[0012] In the preferred embodiment, gates 13 are standard rubber construction cones that are approximately 18 inches to 24 inches high. A standard construction cone is a hollow cylindrical stanchion having a flat base and is adapted to stand upright on flat and inclined surfaces. In the preferred embodiment, the gates are fluorescent or “day glow” in color. Gates 13 can be composed of a variety of materials including wood, steel, aluminum, plastic, rubber. In an alternate embodiment, the cones are to be lighted from the inside to aid in visibility.
[0013] In the preferred embodiment, targets 14 comprise reactive target 22 , stanchion 23 and target stand 24 . In this embodiment, reactive target 22 and target stand 24 are fluorescent or “day glow”. Reactive target 22 and target stand 24 can be the same color but do not have to be. In the preferred embodiment, reactive target 22 is a helium balloon that has a diameter between approximately 9 inches to approximately 12 inches when inflated. In an additional embodiment, clay targets can also be employed suspended by appropriate stanchions. However, objects with a diameter of at least 5 inches that can be punctured, broken or moved by ammunition 26 also serve as useful targets. However, in other embodiments, when reactive target 22 is a helium balloon, reactive target further comprises a standard automobile tire valve. In this embodiment, the reactive target is inflated through the tire valve and removably attached to the reactive target with a standard O-ring. In the preferred embodiment, stanchion 23 is an indentation on target stand 24 that allows reactive target 22 to be removably affixed to target stand 24 . In the preferred embodiment, target stand 24 is a standard rubber construction cone that is approximately 3 feet high. Target stand 24 can be composed of a variety of materials however, plastic or rubber is preferred for safety considerations.
[0014] In the preferred embodiment, targets 14 are identical. However, in alternate embodiments, targets 14 may vary within course 17 . Such as the targets may be different colors, may be different heights or may contained different reactive targets scored differently.
[0015] FIG. 4 shows a schematic representation of network components and a controller that are present in any embodiment of the novel game that includes an automated scoring system. In this embodiment, electrical motion sensing devices 403 are incorporated in first stanchion 401 , second stanchion 402 and first target stand 409 for registering movement of target 408 or displacement of first stanchion 401 , second stanchion 402 or first target 409 . In this embodiment, first stanchion 401 contains optical receiver 404 and second stanchion 402 contains optical transmitter 406 . The optical transmitter and receiver are diametrically opposed on the course so that in use when a beam of light from the transmitter to the receiver is broken, passage of the gate is registered in the memory of the controller. Optical receivers and optical transmitters known in the art are used to register the passage of the player through the stanchions while playing the game. In yet another embodiment, the stanchion is a rectangular or square box that is approximately 1 inch tall and contains a motion sensing device. In this embodiment, the rider must travel directly over the gate. First stanchion 401 and first target 409 further contains processor 405 . Processor 405 contains a programmer, memory and transceiver as known in the art to store information gathered by first stanchion 401 , second stanchion 402 or first target 409 for transmission of data to controller 410 . In one preferred embodiment, this information can be transmitted to a central controller by a wireless data transmission device, as known in the art. In the preferred embodiment, control 410 is a personal computer is used for communication of the electrical data from the wireless data transmission device.
[0016] The electrical data transmitted is used to calculate the time required to complete the course, score and any necessary penalties. Standard wireless equipment and associated hardware and software known by those of ordinary skill in the art is used.
[0017] FIG. 5 is a flow diagram of processes 500 , which is performed on the electrical data transmitted to controller 410 in the preferred embodiment. The process begins with step 501 when electrical data transmitted to controller 410 signals that the rider has entered the course. Once the program starts, it performs step 502 by logging the time when the rider started the course, then step 503 by registering each gate that the rider passes through. Step 504 processes any movement by the gates/stanchions or targets. Then, step 505 adds additional time to the elapsed time as a result of events such as displacement of the gates. Next, step 506 registers the number of targets that the rider hit with the ammunition. Step 507 logs the time that the rider completed the course. Then process completes step 508 by analyzing the length of time it took the rider to complete the course. Next step 509 analyzes the point total of the rider receives based on his placement in the game. Finally step 510 logs the results and calculates the riders elapsed time, penalty points, and placement in the game.
[0018] In the preferred embodiment, holster 17 is on rider 20 . Holster 17 holds firearm 21 in a safe manner when it is not in use. Holster 17 can be composed of a variety of materials including leather, plastic or nylon. In another embodiment, holster 17 is on vehicle 15 . In alternate embodiments more than one holster is on rider 20 or vehicle 15 .
[0019] Vehicle 15 can be any motorized vehicle. In the preferred embodiment vehicle 15 is an all terrain vehicle (ATV). However, vehicle 15 can also be a motorcycle, golf cart or snow mobile without departing from the spirit of the invention. In an alternate embodiment, the vehicle accommodates more than one person. In this alternate embodiment, one person is designated “driver” while the other(s) are designated “shooters”.
[0020] Firearm 21 is an object that is capable of firing ammunition 26 . In the preferred embodiment, firearm 21 is a revolver pistol such as a 44 Magnum or 45 Long Colt Revolver. In yet additional embodiments, firearm 21 may be replaced by other devices capable of firing a projectile such as a sling shot, spear gun, air gun or cross bow. In alternate embodiments, more than one firearm is utilized.
[0021] FIG. 3 is a cut away view of ammunition 26 . Ammunition 26 is blank ammunition. In the preferred embodiment, ammunition 26 has a limited range. For example, ammunition 26 must break reactive target 22 at approximately 10 feet but not be capable of breaking reactive target 22 past approximately 18 feet. Ammunition 26 comprises cartridge 31 , fibers filler 32 , propellant 33 and primer 34 . In the preferred embodiment cartridge 31 is composed of plastic. In another embodiment, the cartridge is composed of brass, steel or aluminum. In the preferred embodiment, fibers filler 32 is crushed walnut hull. However fibers filler 32 can be other media such as grits, crushed corn or wood fibers. In the preferred embodiment, propellant 33 is smokeless gun powder. In another embodiment, the propellant can be black powder. In the preferred embodiment, primer 34 is a chemical primer, but other primers can be used without departing from the spirit of the invention. In the preferred embodiment, fibers filler 32 , propellant 33 and primer 34 are maintained in cartridge 31 by star. crimping end 35 of cartridge 31 . In other embodiment, other crimping or sealing means can be used to keep fibers filler 32 , propellant 33 and primer 34 within cartridge 31 . Propellant 33 and primer 34 are introduced in the cartridge to project the fibers filler only about 10 feet. In another embodiment the fibers filler and propellant are replaced by a concussion load capable of breaking the target by a shock wave or sound wave.
[0022] Engaged in the novel game, rider 20 enters course 17 on vehicle 15 through start/finish gate 11 . As soon as rider 20 travels through the start/finish gate, a timing device will be activated by a motion sensor or optical signal. Rider 20 continues around course 17 by traveling through gates 13 and/or around barrels 12 in order to shoot at each target 14 with firearm 21 by employing ammunition 26 . In embodiments where no motion sensor or optical signal is present, a manual timer is used and activated by a game observer.
[0023] Rider 20 travels through each gate 13 . In the preferred embodiment, rider 20 only has to travel through gates 13 . However, in other embodiments, rider 20 might have to perform different tasks such as driving vehicle 15 a full 360 degrees around a gate.
[0024] When rider 20 approaches target 14 , rider 20 aims firearm 21 towards reactive target 22 on target 14 . In the preferred embodiment, target 14 should be approximately 18 feet from each gate 13 . However, distances between approximately 5 feet and approximately 20 feet will work with equal success.
[0025] After rider 21 has driven through all gates 13 , shot or attempted to shoot at targets 14 and travels back through start/finish gate 11 . Sensors in the start/finish gates mark the time required to complete the course. In embodiments without electronic sensors, a manual observer logs the completion time.
[0026] In a preferred embodiment, a scoring method is provided to rank players. In this embodiment, numerous riders compete in a series by playing one or more games on a course. Each game can be won or lost. The series can be won or lost as well. The winner of the series is the rider that gains the most points. A rider's placement is determined by adding the time to complete the course with any applicable penalties, the shortest time wins. In the preferred embodiment, the applicable penalties are as follows:
a. Missed target=add 5 seconds; b. Knocked over gate=add 5 seconds; c. Failure to follow the course=add 10 seconds; d. Dropped firearm=add 5 seconds; e. Failure to holster first firearm=add 20 seconds; f. No show at course=add 99.9 seconds; g. Dismounting during course=add 99.9 seconds; and h. Safety infraction results in a disqualification from the series.
[0035] A safety infraction includes discharging the firearm at a spectator. First place is awarded to the rider with the shortest overall time. While, second place is awarded to the rider with the second shortest time, etc.
[0036] A series of games is provided in which scores from different games for each individual rider are combined to arrive at a winner for each series. A rider will receive one point for each individual game that the rider completes. If more than 5 riders enter into a specific game, the points will be awarded as follows:
i. 1 st place=5 points; ii. 2 nd place=4 points; iii. 3 rd place=3 points; iv. 4 th place=2 points; and v. 5 th place=1 point.
[0042] If 4 riders enter into a specific game, the points will be awarded as follows:
vi. 1 st place=3 points; vii. 2 nd place=2 points; and viii. 3 rd place=1 points.
[0046] If less than four riders enter the game, no additional points will be awarded.
[0047] The novel game provides a method for ranking contestants. Riders are classified into various contestant levels. The contestant levels allow riders of similar riding and shooting ability to compete against each other. All entry level riders are considered at Level 1. A rider moves up to Level 2 after he earns two first place wins at that level. A rider reaches Level 3 status when he earns three first place wins at that level. Level 4 status is achieved when the rider earns four first place wins at that level. A rider attains Level 5 status when he has five first place wins at that level. Finally, a rider achieves Level 6 status when he has at least six first place wins at that level. Of course other levels are possible.
[0048] While this invention has been described in reference to illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications and combinations of the illustrative embodiments, as well as other embodiments of the invention, will be apparent to persons skilled in the art upon reference to the description. It is therefore intended that the appended claims encompass any such modifications or embodiments.
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The current invention is a gaming apparatus and method wherein players ride on a motorized vehicle around a course through a variety of gates and a variety of barrels while shooting at targets with a firearm loaded with specialized blank ammunition. The blank ammunition is capable of short range use to damage or destroy the targets.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The present application claims priority to Korean Patent Application No. 10-2011-0015253 filed in the Republic of Korea on Feb. 21, 2011, and PCT Application No. PCT/KR2012/001256 filed on Feb. 20, 2012, the disclosures of which are incorporated herein by reference.
TECHNICAL FIELD
The present invention relates to a method for using an enzyme under a high pressure condition, a method for promoting the activity of the enzyme; and a method for measuring the activity of the enzyme.
BACKGROUND
Enzymes do not have any kind of side reaction during physicochemical hydrolysis, have low energy consumption due to their high catalytic activity, and does not have to be removed after processing. Accordingly, they widely are used in various industries.
Enzymes in the past have been mainly used for food production using glycolysis saccharifying starch, but recently, their range of use has expanded to being used for producing medicine, fine chemical products, and food, drugs and chemicals for special use. Specifically, food enzymes are being used in a variety of fields such as syrup production, alcohol fermentation such as beer, dairy, bread, fruit and vegetable juice production, crop-processing, food preservation, egg-processing, food lipid-processing, fish-processing, flavor production, animal feed production. Further, they are also being used as a detergent, with the trend increasing towards the use of enzyme as a dishwashing detergent, which has largely contributed to the growing market for using enzymes as a detergent. Recently, the use of the enzymes in the textile industry has also gradually increased. Accordingly, in the case of wool, a biocarbonsation process, which removes impurities existing in the fibers by using enzymes, is being developed, and the enzymes are also used in a polishing process, which removes naps on the textile, for improving clearness of dyeing, visibility of colors, feel of the surface, wrinkle resistance and softness. In the case of pulp, the enzymes are also used for removing impurities, and the enzymes also may be used in a deinking process, which removes ink when recycling printed papers. In the case of the leather industry, which is a representative industry for causing environmental pollution, a process for using the enzymes instead of strong acid during soaking, unhairing or defatting process, are being developed in order to solve the said problem. In addition, the enzymes are also used in various chemical industries such as amino acid industry, steroid conversion, antibiotic material production, peptide synthesis, ester conversion and synthesis, and organic chemistry. Furthermore, as therapeutic enzymes, digestive enzymes, anti-inflammatory enzymes, thrombolytic enzymes, anti-tumor enzymes, enzymes for the circulating system and the like are being developed, and clinical diagnosis field using enzymes are also being developed step by step. Particularly, in Korea, enzymes are often used because an enzyme hydrolysis method, which produces animal and vegetable protein hydrolysates through protein hydrolysis by directly adding enzymes to raw materials is used in order to prepare traditional natural flavoring substances.
On the other hand, under high pressure, a chemical reaction is stimulated toward the direction where volume is decreased, according to the LE Chartelier's principle. Thus, the reaction may be accelerated when the volume is decreased according to the increased pressure. Accordingly, for the purpose of accelerating the reaction using various enzymes described above, a high pressure process is used. Particularly, when conducting reactions for producing foods under the high pressure condition, it may affect the hydrogen bonds, thereby changing three dimensional structures of macro molecules, which will maintain the natural flavor, taste, color and nutritional ingredients, increase solubility and extraction rate, and also improve preservation. In addition, when using the high pressure process, high-quality foods may be produced so that functional characteristics are excellent and nutritional ingredients are preserved. Such a high pressure process is an eco-friendly economic process with low energy consumption. When using the high pressure process, there are advantages in that growth of microorganisms may be inhibited, the enzyme function is stimulated, the treatment process is simple, and addition of additive salt and alcohol may be excluded. For example, when producing extracts such as red ginseng extract, green tea extract, bamboo extract and adlay extract, if the high pressure enzyme reaction is used, the effect and physical properties of the extract may be changed.
However, generally under the high pressure condition, water penetrated into the tertiary structure of the enzyme may destruct the bonding force of the tertiary structure (e.g., hydrophobic bond), which will make it lose its enzyme activity making it difficult to use the enzymes under high pressure condition.
SUMMARY
The present invention is designed to solve the problems of the prior art, and therefore it is an object of at least at least one embodiment of the present invention to provide a method for using a high pressure-resistant enzyme in a high pressure condition; a method for promoting the activity of the high pressure-resistant enzyme by improving the thermal stability of the enzyme by means of a high pressure treatment; a composition, which contains the high pressure-resistant enzyme, for decomposing proteins under a high pressure condition; a composition, which contains the composition for decomposing proteins, for preparing natural flavoring substances; a container for high pressure treatment, which contains the composition for decomposing proteins; and a method for measuring the activity of the high pressure-resistant enzyme, which comprises a step of decomposing an azocasein solution serving as a substrate by using the high pressure-resistant enzyme treated under a high pressure condition.
In order to solve the above problems, as one embodiment, the present invention relates to a method for using an enzyme under a high pressure condition, wherein the enzyme is at least one selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E (preferably, Marugoto E™) and alcalase.
More preferably, the high pressure condition may be 100 to 400 MPa.
The present inventors confirmed that α-chymotrypsin, pepsin, trypsin and trypsin acetylated are excellent in pressure resistance, with the trypsin being the most excellent in that when treated at high pressure of 300 MPa for 300 min, the enzyme activity increased 40% compared with the trypsin treated at ambient pressure, as well as enzyme activity increasing at 300 MPa as time passed. Further, the α-chymotrypsin showed a tendency to increase the enzyme activity at 300 MPa as time passed, and when it was treated at high pressure for 300 min, its relative activity was over 100%. Further, the trypsin acetylated also showed a tendency to increase the enzyme activity at 300 MPa as time passed, and when treated at high pressure for 300 min, its relative activity was also 100%, which was almost similar to the case in which it was treated at ambient pressure for 300 min. Further, the pepsin treated at high pressure also showed the same enzyme activity with the case when treated at ambient pressure.
In addition, it was confirmed that flavourzyme, protease E and alcalase were also excellent in pressure resistant characteristic. When the flavourzyme and the protease E were treated at high pressure for 300 min, its enzyme activity was almost similar with when treated at ambient pressure, and its relative activity was about 100%. Further, the alcalase was also excellent in pressure resistance. Accordingly, when it was treated at high pressure of 300 MPa for 300 min, it showed almost similar enzyme activity with the alcalase treated at ambient pressure for the same duration, and also showed a tendency to increase the relative activity at 300 MPa as time passed.
Therefore, the present invention was completed by finding that the α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase have high pressure resistance (see FIGS. 7 to 10 ).
According to at least at least one embodiment of the present invention, by means of using the high pressure-resistant enzymes, a method for using the enzymes under a high pressure condition while keeping the enzyme activities, preferably reactions, such as protein decomposition, carbohydrate decomposition, lipid decomposition, bioactive compound extractions, protein enzyme modification, enzyme synthesis for functional ingredients and the like, under a high pressure condition may be conducted. More preferably, the bioactive compound extraction may be extracting the bioactive compounds from plants having thick cell walls, the protein enzyme modification may be objected to improve digestibility and the like, and in the enzyme synthesis for functional ingredients, the functional ingredients may include sweeteners, peptides, enantio selective esters and the like.
In addition, the method for using the enzymes may be more favorable for accomplishing the object of using the enzymes when the activities of the enzymes are promoted. Accordingly, the method for using enzymes, preferably reactions, such as protein decomposition, carbohydrate decomposition, lipid decomposition, bioactive compound extractions, protein enzyme modification, enzyme synthesis for functional ingredients and the like, under a high pressure condition may be applied to a method for promoting the activities of the enzymes.
Therefore, as another embodiment, the present invention provides a composition for decomposing proteins, a composition for decomposing carbohydrates, a composition for decomposing lipids, a composition for extracting bioactive compounds, a composition for modifying protein enzymes or a composition for synthesizing functional ingredients with enzymes, which contains at least one enzyme selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase, under a high pressure condition. Preferably, the high pressure condition may be 100 to 400 MPa.
The term “protein decomposition”, used herein refers to a chemical reaction making amino acids or peptide mixtures by hydrolyzing peptide bonds of proteins and peptides.
The term “high pressure resistance”, used herein refers to a characteristic in which the activity is maintained or increased under a high pressure condition, and the high pressure may be 100 MPa or more, preferably 100 to 400 MPa, more preferably 100 to 300 MPa.
The α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase are known as an enzyme, and can be easily obtained in the art through commercial routes. The α-chymotrypsin may be one derived from bovine pancreas, the pepsin may be one derived from pig gastric mucous membrane, the trypsin may be one derived from bovine pancreas, the trypsin acetylated may be one derived from bovine pancreas, the flavourzyme may be one derived from Aspergillusoryzae, the protease E may be one derived from microorganisms, or the alcalase may be one derived from Bacillus licheniformis , preferably, but is not limited thereto. Preferably, the protease E may be Marugoto E™, but is not limited thereto.
It was estimated that among the said enzymes, serine-based enzymes, alcalase, α-chymotrypsin, trypsin and trypsin acetylated, have a common acyl-enzyme intermediate as a covalent intermediate, and since covalent bondings at their active site are not destructed even when treated at high pressure, the bondings are estimated to contribute to maintaining the enzyme activity (see FIG. 11 ). On the contrary, in the case of thermolysin, which is a metalloprotease, a zinc ion is essential for expressing the activity of the enzyme. It is estimated that the zinc ion is coordinately bonded to amino acids on an active site, and the coordinate bondings are destructed when treated at high pressure, which will make it lose its enzyme activity (see FIG. 12 ). But, for this reason, it is not limited to only covalent bonds existing at the active site of all of the α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and the alcalase, and the present invention is not construed to be limited by these assumptions or guesses.
Proper enzyme may be selected depending on the type of the substrate, and at least one selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase may be used alone or in a mixture thereof. If used in a mixture, the enzymes may be used simultaneously or sequentially. The present inventors confirmed that when the mixture of the high pressure-resistant enzymes was used, the enzyme hydrolysis improved, and particularly, the enzyme hydrolysis improved in proportion to the number of the enzyme to be mixed (see Tables 8 to 10). Accordingly, preferably, a mixture of two or more selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase may be used. More preferably, a mixture of three or more, four or more, five or more, or six or more, and most preferably, a mixture of seven or more may be used.
Further, if the activity of the enzyme used in the present invention is maintained, it may also include being chemically or physically treated before use, as well as being treated at high pressure treatment before use.
In at least at least one embodiment of the present invention, the pressurizing time (PT, time to maintain a certain pressure after reaching the pressure) of the high pressure condition may be properly selected by a person skilled in the art depending on the type of the substrate to be hydrolyzed, a method for using the enzyme, the type of the enzyme, the type of the solvent and the like, and the enzyme may maintain its high pressure resistance for 60 min or more at 100 to 400 MPa, preferably 60 to 300 min, and therefore, the PT may be 60 min or more, for example, 60 to 300 min.
In at least at least one embodiment of the present invention, although the high pressure may be formed by various methods known in the art such as gas, heat and liquid, it may more preferably be hydraulic pressure formed by water.
The present invention may be conducted in both an open-type reaction system and a closed-type reaction system, but more preferably the closed-type reaction system may be used to prepare natural flavoring substances in order to improve flavor. For example, the reaction may be conducted in the high pressure enzyme hydrolysis system illustrated in FIG. 1 , but is not limited thereto.
Further, in at least at least one embodiment of the present invention, the reaction temperature may be properly selected by a person skilled in the art depending on the type of the substrate to be hydrolyzed, a method for using the enzyme, the type of the enzyme, the type of the solvent and the like, but the reaction rate and/or the reaction yield may be increased by heating in the temperature range where the enzyme and the substrate are not denatured.
Particularly, the present inventors confirmed that the thermal stability of the enzyme largely increased after the high pressure treatment, and therefore, the enzyme activity improved when heated under high pressure condition, compared with the ambient pressure condition (Tables 3 to 6, FIGS. 13 to 16 ). Accordingly, when using the high pressure-resistant enzyme, the yield of the heat-treated reaction under the high pressure condition, for example, the yield of protein hydrolysate may be improved.
The heat treatment may include heating at 40° C. or higher for 2 min or longer, preferably at 40 to 85° C. or higher for 2 min or longer, more preferably at 40 to 85° C. or higher for 2 to 120 min.
Therefore, as another embodiment, the present invention provides a method for improving the activity of at least one enzyme selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase, wherein the enzyme is treated at high pressure when heating. Preferably, the high pressure condition may be 100 to 400 MPa, and more preferably 100 to 300 MPa.
The high pressure treatment and the heat treatment may be conducted simultaneously or independently. When conducted independently, they may be conducted sequentially, and the high pressure treatment may precede the heat treatment. But it is preferred that they be conducted simultaneously.
Natural flavoring substances may be prepared by using the method and the composition according to the present invention. Accordingly, as another embodiment, the present invention relates to a method for preparing natural flavoring substances, which comprises a step of hydrolyzing proteins under the high pressure condition by using the high pressure-resistant protein hydrolysis enzyme, and a composition for preparing natural flavoring substances, which comprises the composition for hydrolyzing proteins under the high pressure condition. Namely, at least at least one embodiment of the present invention provides the method for preparing natural flavoring substances, which comprises a step of reacting at high pressure by using at least one enzyme selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase, and the natural flavoring substances prepared by the said method. Preferably, in this method, the said heat treatment (for example, heating at 40° C. or higher for 2 min or longer) may be conducted at the same time. Preferably, the high pressure condition may be 100 to 400 MPa.
During the preparing process, any natural flavoring substance, which may include a step of hydrolyzing proteins by a protein hydrolysis enzyme, may be included in the said natural flavoring substances.
Other processes other than the step of hydrolyzing proteins may be properly selected by a person skilled in the art depending on the type of the natural flavoring substances to be prepared.
The method for preparing natural flavoring substances and the composition for preparing natural flavoring substances are exemplified as the method for hydrolyzing proteins and the composition for hydrolyzing proteins according to the present invention. It should be appreciated by those skilled in the art that the present invention is not limited to the exemplary uses and may be applied to other various uses and such equivalent uses do not depart from the spirit and scope of the invention.
As further another embodiment, the present invention relates to a container for high pressure treatment, which comprises the composition according to the present invention. Preferably, the high pressure condition may be 100 to 400 MPa.
The container may be any container, if it is durable to the high pressure treatment, and high pressure can be transferred into the container, regardless of shapes, structures and materials.
The container for high pressure treatment containing the high pressure-resistant enzymes may be applied to various uses because it can conduct treatments using the high pressure-resistant enzymes even under the high pressure treatment condition.
As further another embodiment of the present invention, the present invention related to a method for measuring the activity of the enzyme, which comprises a step of hydrolyzing an azocasein solution serving as a substrate by using the enzyme, which is at least one selected from the group consisting of α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase, and treated under a high pressure condition. Preferably, the high pressure condition may be 100 to 400 MPa.
The present inventors confirmed that the activities of the enzymes treated at high pressure may be easily and accurately measured by using the azocasein solution as a substrate ( FIG. 4 ). The said enzymes have the substrate specificity to various substrates including azocasein.
The concentration of the azocasein may be 2 to 5%, preferably 3%.
As seen from the above, according to at least at least one embodiment of the present invention, the reaction rate and/or reaction yield of a method for using an enzyme may be improved. Therefore, the present invention is expected to be used in various industry fields, and particularly, if it is used for producing food favoring substances, it is expected to bring significant changes in the entire food material industries using enzymes.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and aspects of the present invention will become apparent from the following descriptions of the embodiments with reference to the accompanying drawings in which:
FIG. 1 shows a high pressure enzyme hydrolysis system (high pressure bio-hydrolysis enzyme reactor);
FIG. 2 shows a method for evaluating the enzyme activity. The sample is the case of activating an enzyme, and the blank is the case of inactivating an enzyme.
FIG. 3 shows a method for measuring the enzyme activity by using azocasein as a substrate;
FIG. 4 shows the optimized substrate concentration for enzyme analysis (Trypsin concentrations (mg/mL): A, 0.5; B, 5; C, 0.5; D, 5);
FIG. 5 shows the effects of the concentrations of catalog hydrolysis enzymes on the activity, measured by the azocasein analysis;
FIG. 6 shows the effects of the concentrations of industrial enzymes on the activity, measured by the azocasein analysis;
FIG. 7 shows the activities of the enzymes according to the time treated at 100 MPa;
FIG. 8 shows the activities of the enzymes according to the time treated at 300 MPa;
FIG. 9 shows the change on the activity of each catalog hydrolysis enzyme during high pressure treatment;
FIG. 10 shows the change on the activity of each industrial hydrolysis enzyme during high pressure treatment;
FIG. 11 are pictures comparing active sites of trypsin and thermolysin;
FIG. 12 shows a catalytic mechanism in which the coordinate bondings formed by zinc are destructed depending on the high pressure treatment;
FIG. 13A-B show thermal inactivation profiles of trypsin (◯, 40° C.; ●, 45° C.; □, 50° C.; ▪, 55° C.; Δ, 60° C.);
FIG. 14A-B show the result of dynamics analysis of the thermal inactivation profiles of trypsin (◯, 40° C.; ●, 45° C.; □, 50° C.; ▪, 55° C.; Δ, 60° C.);
FIG. 15A-B show thermal inactivation profiles of protease E (◯, 40° C.; ●, 45° C.; □, 50° C.; ▪, 55° C.; Δ, 60° C.);
FIG. 16A-B show the result of dynamics analysis of the thermal inactivation profiles of protease E (◯, 40° C.; ●, 45° C.; □, 50° C.; ▪, 55° C.; Δ, 60° C.);
FIG. 17 is a graph comparing a non-enzyme reaction and enzyme reactions under the ambient pressure and at the high pressure;
FIG. 18 shows electrophoresis patterns of enzyme hydrolysates according to treatment with one enzyme (1, markers; 2, non-enzyme treated 12% protein (AP); 3, F (AP); 4, F (HP); 5, A (AP); 6, A (HP); 7, P (AP); 8, P (HP); 9, M (AP); 10, M (HP); AP, ambient pressure; HP, 300 MPa. F, flavourzyme; A, alcalase; P, Protamex; M, MarugotoE);
FIG. 19 shows electrophoresis patterns of enzyme hydrolysates according to treatment with two enzymes (1,10, markers; 2, non-enzyme treated 12% protein (AP); 3, FA (AP); 4, FA (HP); 5, FP (AP); 6, FP (HP); 7, FM (AP); 8, FM (HP); 9, 12% non-enzyme treated 12% protein; AP, ambient pressure; HP, 300 MPa; F, flavourzyme; A, alcalase; P, Protamex; M, Marugoto E);
FIG. 20 shows electrophoresis patterns of enzyme hydrolysates according to treatment with three enzymes (1,10, markers; 2, non-enzyme treated 12% protein (AP); 3, FAP (AP); 4, FAP (HP); 5, FAM (AP); 6, FAM (HP); 7, FPM (AP); 8, FPM (HP); 9, non-enzyme treated 12% protein (HP); AP, ambient pressure; HP, 300 MPa; F, flavourzyme; A, alcalase; P, Protamex; M, Marugoto E);
FIG. 21 shows an electrophoresis pattern of enzyme hydrolysates according to treatment with four enzymes (1,10, markers; 2, non-enzyme treated 12% wheat gluten (AP); 3, non-enzyme treated 12% wheat gluten (HP); 4, WG (AP); 5, WG (HP); 6, AFP (AP); 7, AFP (HP); 8, non-enzyme treated 12% anchovy fine powder (AP); 9, non-enzyme treated 12% anchovy fine powder (HP); AP, ambient pressure; HP, 300 MPa; F, flavourzyme; A, alcalase; P, Protamex; M, Marugoto E);
FIG. 22 shows an electrophoresis pattern in the case of not treating any enzyme (1,8, marker; 2, 12% WG; 3, 12% WG (AP); 4, 12% WG (HP); 5, 12% AFP; 6, 12% AFP (AP); 7, 12% AFP (HP); AP, ambient pressure; HP, 300 MPa; F, flavourzyme; A, alcalase; P, Protamex; M, Marugoto E);
FIG. 23 shows electrophoregrams of the enzyme hydrolysates of the wheat gluten (AP, ambient pressure; HP, 300 MPa);
FIG. 24 shows electrophoregrams of the enzyme hydrolysates of the anchovy fine powder (AP, ambient pressure; HP, 300 MPa);
FIG. 25 shows the results of measuring the soluble solids of the enzyme hydrolysates according to the treatment with one enzyme;
FIG. 26 shows the results of measuring the soluble solids of the enzyme hydrolysates according to the treatment with two enzymes;
FIG. 27 shows the results of measuring the soluble solids of the enzyme hydrolysates according to the treatment with three enzymes;
FIG. 28 shows the results of measuring the soluble solids of the enzyme hydrolysates according to the treatment with four enzymes;
FIG. 29 are results of measuring soluble nitrogen contents of the enzyme hydrolytes of the wheat gluten and the anchovy fine powder (o, Total soluble N (AP); ●, TCA soluble N (AP); □, Total soluble N (HP); ▪, TCA soluble N (HP); AP, ambient pressure; HP, 300 MPa);
FIG. 30 shows DHN of the enzyme hydrolysates of the wheat gluten and the anchovy fine powder (◯, wheat gluten (AP); ●, wheat gluten (HP); □, anchovy fine powder (AP); ▪, anchovy fine powder (HP); AP, ambient pressure; HP, 300 MPa); and
FIG. 31 shows the solubility of the enzyme hydrolysates of the wheat gluten and the anchovy fine powder (◯, wheat gluten (AP); ●, wheat gluten (HP); □, anchovy fine powder (AP); ▪, anchovy fine powder (HP); AP, ambient pressure; HP, 300 MPa.
DETAILED DESCRIPTION
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. Prior to the description, it should be understood that the terms used in the specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present disclosure on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Therefore, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
Example 1
Constructing and Using High Pressure Enzymatic Hydrolysis System
(High Pressure Bio-Hydrolysis Enzyme Reactor)
A high pressure enzymatic hydrolysis system was constructed in order to conduct a high pressure bio-hydrolysis reaction by an enzyme by means of hydraulic pressure, which was generated from water used as a pressure medium (see FIG. 1 ). This system, whose workable maximum reaction temperature and pressure were 70° C. and 4000 bar (400 MPa), respectively, was able to conduct various high pressure hydrolysis reaction by food enzymes, objected by the present study, and was able to increase in enzymatic hydrolysis and in production yield of the hydrolyzed products in a short time, by promoting enzyme activities and changing structures of hydrolysis substrates under a high pressure condition. By using a closed-type reaction system, flavors of reaction products such as salt-free natural flavoring substances were able to be enhanced.
Example 2
Securing Various Enzyme Groups
Enzymes, which will be used for producing natural flavoring substances by using the high pressure bio-hydrolysis technology were secured as follows, based on industrial enzymes and catalog enzymes.
A. Catalog Enzymes
Pepsin (from porcine gastric mucosa), trypsin (from bovine pancreas), α-chymotrypsin (from bovine pancreas), thermolysin (from Bacillus thermoproteolyticus rokko), papain (from papaya latex), papain (from Carica papaya ), bromelain (from pineapple), trypsin (acetylated), ficin (from fig tree).
B. Industrial Enzymes
Alcalase 2.4 L (subtilisin, from Bacillus licheniformis , Novozyme), flavourzyme (aminopeptidase, from Aspergillusoryzae, Novozyme), Protamex (from Bacillus licheniformis and B. amyloliquefaciens , Novozyme), protease E (from microorganisms, Supercritical technology research corporation, Toyo Koatsu Co. Ltd.)
Example 3
Constructing Enzyme Activity Evaluation System
Enzyme activities were searched over azoalbumin and azocasein combined with an azo dye as a chromogen. An advantage of this method is that the enzyme activity evaluation can be easily and accurately conducted. At this time, blank was an enzyme solution inactivated with 30% TCA solution in advance, and then treated in the same manner as the samples (see FIG. 2 ). Entire experiment processes were illustrated as shown in FIG. 3 .
Example 4
Measuring Enzyme Activity Change Depending on Reaction Variables and High Pressure Condition
A. Optimizing Substrate Concentration for Enzyme Reaction
The substrate concentration for measuring the enzyme activity was optimized in order to test the change on the enzyme activity depending on the high pressure condition against the hydrolysis enzyme group secured above. Trypsin was dissolved in 0.1 M phosphate buffer solution (pH 7.5) at concentrations of 0.5 and 5 mg/mL, and then the enzyme activity was measured via the process illustrated in FIG. 3 while changing the substrate concentration from 0.2 to 9.5% (w/v).
While changing the substrate concentration, the enzyme activity was measured, and the result obtained there from showed a typical saturation curve ( FIG. 4 ). The lowest concentration in the substrate concentration region where the saturation curve began to appear was selected as the optimum substrate concentration to avoid the K M region which has a big activity dynamic range according to the increase of the substrate concentration. The enzyme activity of trypsin was saturated at the azoalbumin concentration of 3% when trypsin concentration was 5 mg/mL, but in the case of azocasein, the enzyme activity of trypsin was saturated at the trypsin concentration of 0.5 mg/mL. Thus, it was observed that the reactivity of azocasein was better than that of azoalbumin. Accordingly, the 3% azocasein solution was used as a substrate solution in the later experiments.
B. Optimizing Enzyme Concentration for High Pressure Reaction
Then, in order to determine the enzyme concentration for high pressure treatment, the enzyme activity according to the concentration change was measured with the 3% azocasein as a substrate solution under the conditions of Table 1.
TABLE 1
Design for Test for Selecting Enzyme Concentration of
High Pressure Treatment
Enzyme
Temperature
concentration
Enzyme
(° C.)
pH
(mg/mL)
Pepsin a
37
0.01N HCl
0.05, 0.1, 0.5, 1, 5
α-Chymotrypsin a
37
7.5
0.05, 0.1, 0.5, 1, 5
Papain
37
6.5
0.05, 0.1, 0.5, 1, 5
(from papaya latex) a
Papain
37
6.5
0.05, 0.1, 0.5, 1, 5
(from Carica papaya ) b
Bromelain a
37
5
0.05, 0.1, 0.5, 1, 5
Trypsin acetylated c
37
7.5
0.05, 0.1, 0.5, 1, 5
Thermolysin a
37
7.5
0.05, 0.1, 0.5, 1, 5
Trypsin a
37
7.5
0.5
Ficin a
37
6.5
0.05, 0.1, 0.5, 1, 5
Flavourzyme 500 MG d
37
6.5
0.25, 0.5, 2.5, 5, 25
Protamex d
37
7
0.25, 0.5, 2.5, 5, 25
Alcalase 2.4L e
37
7.5
0.25, 0.5, 25, 5, 25
Protease E d
37
7
0.25, 0.5, 2.5, 5, 25
a Lyophilized powder,
b powder,
c synthetic,
d crude powder,
e liquid
The results were illustrated in FIG. 5 and FIG. 6 . As a result of measuring the activity change according to the concentration of the enzyme, divided into the catalog enzyme and the industrial enzyme, a pattern in which the enzyme activity was saturated according to the increase of the enzyme concentration, similar with when the substrate was increased was observed. In this case, the important thing to consider when selecting the enzyme concentration is to select the enzyme concentration at the section where the enzyme activity increased, and it was judged that the effect of the high pressure treatment may be properly reflected in the enzyme activity at this enzyme concentration. The enzyme concentrations of the pepsin, α-chymotrypsin, papain (from papaya latex), papain (from Carica papaya ), bromelain, trypsin acetylated, thermolysin, trypsin, ficin, flavourzyme, Protamex, alcalase and protease E, selected through the said process, were 5, 5, 5, 5, 5, 0.5, 0.1, 0.5, 1, 5, 2.5, 0.5 and 2.5 mg/mL, respectively.
C. Changing on Enzyme Activity Depending on High Pressure Treatment Condition
The enzyme activity depending on the high pressure treatment condition was compared with the enzyme activity under the ambient pressure (0.1 MPa) at the enzyme concentration selected in the above experiment. The specific experiment conditions were as listed in Table 2, and the changes on the enzyme activity when treated at 100 and 300 MPa for 60, 120 and 300 min were illustrated in FIG. 7 and FIG. 8 , respectively.
The patterns of the enzyme activity were mostly similar at 100 and 300 MPa. However, some of the enzymes showed high pressure-resistance, but other enzymes did not show high pressure-resistance. Representatively, the activity of the trypsin increased even more depending on the time treated at high pressure at 300 MPa while the activity of the thermolysin almost completely disappeared at 300 MPa, thereby showing very weak characteristic on high pressure.
TABLE 2
Design for Test for Treating Various Protein Hydrolysis
Enzymes under High Pressure Condition
Vessel
Enzyme
temperature
Vessel
Reaction
concentration
Enzyme
(° C.)
pressure (MPa)
time (min)
(mg/mL)
Pepsin
37
100, 300
60, 120, 300
5
α-Chymotrypsin
37
100, 300
60, 120, 300
5
Papain (from papaya latex)
37
100, 300
60, 120, 300
5
Papain (from Carica
37
100, 300
60, 120, 300
5
papaya )
Bromelain
37
100, 300
60, 120, 300
5
Trypsin acetylated
37
100, 300
60, 120, 300
0.5
Thermolysin
37
100, 300
60, 120, 300
0.1
Trypsin
31
100, 300
60, 120, 300
0.5
Ficin
37
100, 300
60, 120, 300
1
Flavourzyme 500 MG
37
100, 300
60, 120, 300
5
Protamex
37
100, 300
60, 120, 300
2.5
Alcalase 2.4L
37
100, 300
60, 120, 300
0.5
Protease E
37
100, 300
60, 120, 300
2.5
In order to more clearly investigate the pressure-resistance characteristic of some enzymes, the activities of each enzyme according to the time treated at high pressure at 100 and 300 MPa were expressed as relative activity (%) when regarding the enzyme activity at the ambient pressure as 100, respectively (see FIGS. 9 and 10 ). Among the catalog enzymes, α-chymotrypsin, pepsin, trypsin and trypsin acetylated were excellent in the pressure-resistance, and trypsin was the most excellent in pressure-resistance as its enzyme activity when treated at 300 MPa for 300 min was 40% higher than when treated at ambient pressure. However, the residual activity of the thermolysin when treated at 300 MPa for 300 min was only 5% or less. Among the industrial enzymes, Protamex was relatively weak on the high pressure treatment, but flavourzyme, protease E and alcalase were excellent in pressure-resistance. Accordingly, the present inventors could find that α-chymotrypsin, pepsin, trypsin, trypsin acetylated, flavourzyme, protease E and alcalase had high pressure-resistance.
Here, it was determined that the extreme difference between the trypsin and the thermolysin on the pressure-resistance was closely related to mechanisms of the two enzymes (see FIG. 11 ). When comparing active site structures of these enzymes, it was judged that the active site of the trypsin, one of the serine-based enzymes, was not destructed by the high pressure treatment because there was only covalent bondings. On the contrary, since in the case of the thermolysin, one of the metallic enzymes, wherein a zinc (Zn) ion is bonded to histidine and glutamic acid, amino acids on the active site, by coordinate bondings, also plays an important role in catalytic function of the enzyme (see FIG. 12 ), it was assumed that the high pressure treatment destructed the coordinate bondings by the zinc, thereby losing the enzyme activity of the thermolysin.
D. Thermal Inactivation Under High Pressure and Ambient Pressure by Using High Pressure-Resistant Enzyme
Among the high pressure-resistant enzymes selected in the above experiment, the trypsin as the catalog enzyme and the protease E as the industrial enzyme were subjected to a time-dependent thermal inactivation test under the ambient pressure and the high pressure, and the heat was treated for 2, 5, 10, 15, 20, 30, 45 and 60 min at each temperature, respectively.
Tables 3 and 4 showed the result of the thermal inactivation test against the trypsin under the high pressure and the ambient pressure. As shown in the following table, it was found that the high pressure treatment largely increased the thermal stability of the enzyme at all temperature conditions.
TABLE 3
Time-Dependent Thermal Inactivation of Trypsin at 300 MPa
Pressurizing
Heat treatment (° C.)
time (min)
40
45
50
55
60
2
1.178 ± 0.054 a
1.186 ± 0.015
1.150 ± 0.015
1.082 ± 0.045
0.928 ± 0.008
5
1.238 ± 0.005
1.201 ± 0.013
1.140 ± 0.023
1.090 ± 0.009
0.845 ± 0.021
10
1.238 ± 0.004
1.200 ± 0.004
1.130 ± 0.001
1.058 ± 0.016
0.749 ± 0.021
15
1.231 ± 0.010
1.169 ± 0.015
1.137 ± 0.010
1.011 ± 0.009
0.459 ± 0.022
20
1.204 ± 0.001
1.185 ± 0.006
1.079 ± 0.032
0.944 ± 0.012
0.511 ± 0.010
30
1.180 ± 0.011
1.148 ± 0.003
1.075 ± 0.011
0.864 ± 0.011
0.366 ± 0.007
45
1.172 ± 0.014
1.137 ± 0.005
0.974 ± 0.010
0.735 ± 0.005
0.223 ± 0.011
60
1.162 ± 0.008
1.077 ± 0.005
0.949 ± 0.012
0.699 ± 0.011
0.162 ± 0.003
a Mean ± SD (n = 3).
TABLE 4
Time-Dependent Thermal Inactivation of Trypsin at Ambient Pressure
Heat treatment (° C.)
Time (min)
40
45
50
55
60
2
1.201 ± 0.067 a
1.085 ± 0.025
0.683 ± 0.014
0.236 ± 0.008
0.246 ± 0.008
5
1.237 ± 0.007
1.029 ± 0.006
0.372 ± 0.010
0.420 ± 0.002
0.258 ± 0.013
10
1.192 ± 0.026
0.907 ± 0.014
0.285 ± 0.013
0.128 ± 0.010
0.106 ± 0.003
15
1.149 ± 0.003
0.813 ± 0.003
0.446 ± 0.007
0.147 ± 0.017
0.087 ± 0.000
20
1.129 ± 0.006
0.795 ± 0.016
0.240 ± 0.015
0.125 ± 0.002
0.085 ± 0.001
30
1.068 ± 0.002
0.778 ± 0.023
0.334 ± 0.004
0.095 ± 0.009
0.076 ± 0.013
45
1.023 ± 0.011
0.647 ± 0.005
0.113 ± 0.013
0.225 ± 0.008
0.073 ± 0.005
60
0.949 ± 0.009
0.477 ± 0.009
0.228 ± 0.009
0.067 ± 0.008
0.069 ± 0.005
a Mean ± SD (n = 3).
When regarding the enzyme activity of the control group measured right after preparing the enzyme solution as 100, the residual activity (%) according to the heat treatment was measured and illustrated in FIG. 13 . This result was plotted on as emi-logarithmic scale, and then the rate constant of the first order reaction by the thermal inactivation depending on temperature was calculated ( FIG. 14 ).
The results of the thermal inactivation tests against the protease E under the high pressure and the ambient pressure were expressed in Tables 5 and 6. Like in the case of trypsin, the thermal stability of the enzyme after the high pressure treatment largely increased at all temperature conditions, and the degree of the increase was larger than the case of trypsin.
When regarding the activity of the control group as 100, the residual activity according to the heat treatment was measured and illustrated in FIG. 15 . This result was plotted on as emi-logarithmic scale, and then the rate constant of first order reaction by the thermal inactivation depending on temperature was calculated ( FIG. 16 ).
TABLE 5
Time-Dependent Thermal Inactivation of Protease E at 300 MPa
Pressurizing
Heat treatment (° C.)
time (min)
40
45
50
55
60
2
1.252 ± 0.006 a
1.263 ± 0.029
1.280 ± 0.007
1.286 ± 0.020
1.141 ± 0.0021
5
1.252 ± 0.016
1.259 ± 0.005
1.282 ± 0.024
1.219 ± 0.026
0.865 ± 0.0448
10
1.222 ± 0.015
1.223 ± 0.070
1.282 ± 0.008
1.196 ± 0.028
0.800 ± 0.0176
15
1.235 ± 0.011
1.254 ± 0.032
1.265 ± 0.029
1.196 ± 0.002
0.726 ± 0.0141
20
1.279 ± 0.019
1.242 ± 0.019
1.220 ± 0.009
1.144 ± 0.024
0.627 ± 0.0010
30
1.262 ± 0.020
1.183 ± 0.017
1.230 ± 0.013
1.089 ± 0.032
0.437 ± 0.0080
45
1.235 ± 0.004
1.232 ± 0.002
1.178 ± 0.013
1.014 ± 0.004
0.328 ± 0.0247
60
1.240 ± 0.008
1.186 ± 0.005
1.181 ± 0.003
0.942 ± 0.022
0.271 ± 0.0106
a Mean ± SD (n = 3).
TABLE 6
Time-Dependent Thermal Inactivation of Protease E at Ambient Pressure
Heat treatment (° C.)
Time (min)
40
45
50
55
60
2
1.275 ± 0.015 a
1.197 ± 0.007
1.152 ± 0.034
0.207 ± 0.008
0.157 ± 0.0053
5
1.256 ± 0.020
1.119 ± 0.008
0.965 ± 0.044
0.176 ± 0.011
0.174 ± 0.0028
10
1.164 ± 0.029
1.108 ± 0.016
0.913 ± 0.017
0.173 ± 0.007
0.111 ± 0.0017
15
1.196 ± 0.047
1.100 ± 0.082
0.737 ± 0.007
0.174 ± 0.009
0.098 ± 0.0040
20
1.237 ± 0.024
0.939 ± 0.023
0.696 ± 0.008
0.154 ± 0.012
0.076 ± 0.0068
30
1.235 ± 0.011
0.805 ± 0.046
0.605 ± 0.031
0.123 ± 0.016
0.070 ± 0.0047
45
1.229 ± 0.029
0.594 ± 0.016
0.383 ± 0.019
0.135 ± 0.007
0.059 ± 0.0018
60
1.182 ± 0.007
0.525 ± 0.020
0.311 ± 0.014
0.137 ± 0.005
0.103 ± 0.0028
a Mean ± SD (n = 3).
The result of calculating the activation energy (Ea) from the rate constant of the first order reaction of FIG. 14 and FIG. 16 by Arrhenius plot was shown in Table 7. Activation energies of the trypsin and the protease E at high pressure reaction were 38.9 and 51.5 kcal/mol, and were lower than those of the ambient pressure reaction of 60.2 and 76.5 kcal/mol. Consequently, the high pressure condition increased the reaction rate of the enzyme by lowering the activation energy of the enzyme reaction (see FIG. 17 ), and it was estimated that this may be expressed as the yield increase of the reaction product.
TABLE 7
First Order Rate Constant of Trypsin and Protease E at 300 MPa and Ambient Pressure
k × 10 −2 (min −1 )
E a
enzyme
40° C.
45° C.
50° C.
55° C.
60° C.
(cal mol −1 K −1 )
Trypsin
A
0.0496 × 10 −2
0.0880 × 10 −2
0.1772 × 10 −2
0.4014 × 10 −2
6.9233 × 10 −2
38993
B
0.1996 × 10 −2
0.5949 × 10 −2
13.582 × 10 −2
36.641 × 10 −2
35.722 × 10 −2
60289
Protease
A
0.0113 × 10 −2
0.0464 × 10 −2
0.0709 × 10 −2
0.2229 × 10 −2
2.6283 × 10 −2
51509
E
B
0.0347 × 10 −2
0.6635 × 10 −2
0.9998 × 10 −2
39.659 × 10 −2
45.682 × 10 −2
76505
A, High pressure treatment; B. ambient pressure treatment.
Example 5
Preparation of Enzyme Hydrolysate Under High Pressure Hydrolysis Condition from Agricultural and Fishery Protein
Hydrolysis test for each type of enzymes was conducted as follows by using wheat gluten and anchovy fine powder as a reaction substrate and water as a reaction solvent. The wheat gluten and the anchovy fine powder were dissolved in distilled water to make a 12% solution. The hydrolysis enzyme used herein were alcalase, Protamex, Marugoto E (protease E) and flavourzyme, and of them, one, two, three and four enzymes were combined before treating. As a method for treating the enzyme, in the case of the ambient pressure treatment, the substrate was hydrolyzed with the enzyme in a beaker in a 50° C. water bath for 1 hour, and in the case of the high pressure treatment, the substrate was hydrolyzed with the enzyme in a vinyl pouch at 50° C. and 300 MPa for 1 hour. The thermal inactivation was conducted by heating in a 90° C. water bath for 10 min Centrifugation after the enzyme hydrolysis was conducted at 10000 g and 10° C. for 30 min. The enzyme hydrolysate was electrophoresed, and then suspended solid (SS) was measured by water determination method using sea sand in a 105° C. dry oven. Further, degree of hydrolysis nitrogen (DHN) was measured by measuring nitrogen content against a TCA-soluble fraction and a total soluble fraction of hydrolysates, and a 12% sample suspension not treated with any enzyme by Kjeldahlanalysis.
A. Result of Electrophoresis Pattern of Enzyme Hydrolysate
Electrophoresis pattern of the enzyme hydrolysate obtained from the hydrolysis test conducted by the above process was examined. As the result, when comparing bands of the case treated with one enzyme ( FIG. 18 ), the case treated with two enzymes ( FIG. 19 ), the case treated with three enzymes ( FIG. 20 ) and the case treated with four enzymes ( FIG. 21 ), and the case not treated with any enzyme ( FIG. 22 ), it was confirmed that the hydrolysates treated with the enzymes showed more band patterns of molecular weight of thousands or less than the case not treated with any enzyme.
An electrophoregram was drawn from the electrophoresis patterns of the enzyme hydrolysates obtained from the cases treating one enzyme and three enzymes to the wheat gluten ( FIG. 23 ). It was confirmed that there was little difference according to enzyme treating groups, but when compared with the group not treated with any enzyme, the effect of the changes on the electrophoregrams by hydrolysis was obvious.
The electrophoregram of the anchovy fine powder showed a similar pattern with the result of the wheat gluten ( FIG. 24 ).
B. Result of Measuring Soluble Solid (SS) of Enzyme Hydrolysate
Results of measuring the soluble solid (SS) of the enzyme hydrolysates treated with one enzyme, two enzymes, three enzymes and four enzymes by the 105° C. drying method using sea sand were shown in Table 8. The SS was higher in the case of four enzymes than the case of one enzyme, and at the high pressure than at the ambient pressure, and there from, it was concluded that the enzyme was hydrolyzed better as the number of the enzyme used for the enzyme hydrolysis increased, and at high pressure condition.
TABLE 8
Wheat gluten
Anchovy fine powder
Enzyme
AP (%) a
HP (%) b
AP (%)
HP (%)
F
42.00 ± 0.18
67.23 ± 0.24
39.66 ± 0.05
43.70 ± 0.31
P
50.85 ± 0.36
49.43 ± 0.33
40.75 ± 0.23
47.12 ± 0.56
A
25.58 ± 0.21
43.61 ± 0.50
36.44 ± 0.33
45.33 ± 0.36
M
49.48 ± 0.38
74.08 ± 0.84
37.62 ± 0.06
48.89 ± 0.13
FA
75.78 ± 3.15
80.84 ± 1.15
46.27 ± 0.35
59.63 ± 0.69
FP
76.06 ± 0.36
81.06 ± 0.27
46.17 ± 0.22
57.54 ± 0.58
FM
69.10 ± 0.88
78.05 ± 1.15
44.57 ± 0.26
54.80 ± 4.97
FAP
77.10 ± 0.68
83.04 ± 0.63
48.26 ± 0.31
64.51 ± 0.84
FAM
76.84 ± 0.65
84.32 ± 0.45
47.74 ± 0.29
63.01 ± 0.22
FPM
78.29 ± 0.79
84.19 ± 0.26
49.06 ± 0.38
62.40 ± 0.60
FAPM
79.37 ± 0.90
87.23 ± 1.97
53.74 ± 0.31
69.23 ± 0.28
a Treatment at ambient pressure.
b Treatment at 300 MPa.
F. Flavourzyme;
P. Protamex;
A. Alcalase;
M. Marugoto E.
The relationship in Table 8 was expressed in graphs of FIGS. 25 to 28 , and they visually show the relationship between the SS content and the enzyme hydrolysis under the high pressure and the ambient pressure conditions.
C. Result of Measuring Degree of Hydrolysis Nitrogen (DHN) of Enzyme Hydrolysate
Results of measuring the degree of hydrolysis nitrogen (DHN) of the hydrolysate hydrolyzed by the protease were shown in Table 9 and Table 10. The DHN is used as one of the standards for the ratio of the number of hydrolyzed peptide bonds to the total number of the peptide bonds, and as the result of measuring the SS, the DHN and the solubility were higher as the number of the treated enzyme was increased and the enzyme hydrolysis was conducted under the high pressure condition than at the ambient pressure because the number of the hydrolyzed peptide was more. When compared with the value of the Blank, it could be found that the effect of the hydrolysis was higher as the number of the treated enzyme increased. The result of treating under the ambient pressure was shown in Table 9, and the result of treating under the high pressure (300 MPa) was shown in Table 10.
TABLE 9
Wheat gluten
Anchovy fine powder
Total
Total
soluble-N
TCA-soluble-N
Solubility
DHN
soluble-N
TCA-soluble-N
Solubility
DHN
Enzyme
(%)
(%)
(%)
(%)
(%)
(%)
(%)
(%)
Blank a
0.27 ± 0.04
0.19 ± 0.01
2.52
1.77
0.91 ± 0.02
0.71 ± 0.02
12.08
9.43
F
3.77 ± 0.08
2.54 ± 0.01
35.14
23.67
2.46 ± 0.04
2.43 ± 0.01
32.67
32.27
FA
6.18 ± 0.38
3.02 ± 0.04
57.60
28.15
3.25 ± 0.05
3.17 ± 0.07
43.16
42.10
FAM
7.14 ± 0.21
6.82 ± 0.07
66.54
63.56
3.24 ± 0.13
2.77 ± 0.01
43.03
36.79
FAMP
7.14 ± 0.23
6.87 ± 0.08
66.54
64.03
3.65 ± 0.13
3.58 ± 0.11
48.47
47.54
a Without enzyme treatment.
Tatal-N = Wheat gluten. 10.73 ± 0.07%: Anchovy fine powder, 7.53 ± 0.02%.
DHN (%) = TCA-soluble-N/Tatal-N * 100
TABLE 10
Wheat gluten
Anchovy fine powder
Total
Total
soluble-N
TCA-soluble-N
Solubility
DHN
soluble-N
TCA-soluble-N
Solubility
DHN
Enzyme
(%)
(%)
(%)
(%)
(%)
(%)
(%)
(%)
Blank a
0.35 ± 0.02
0.32 ± 0.02
3.26
2.98
0.98 ± 0.03
0.78 ± 0.02
13.01
10.36
F
6.25 ± 0.28
5.77 ± 0.07
58.25
53.77
3.56 ± 0.07
3.51 ± 0.04
47.28
46.61
FA
6.79 ± 0.18
6.4 ± 0.1
63.28
59.65
4.15 ± 0.1
4.14 ± 0.02
55.11
54.98
FAM
7.69 ± 0.14
7.53 ± 0.79
71.67
70.18
4.43 ± 0.15
4.3 ± 0.02
58.83
57.10
FAMP
8.09 ± 0.12
7.73 ± 0.1
75.40
72.04
4.87 ± 0.09
4.7 ± 0.06
64.67
62.42
a Without enzyme treatment.
Tatal-N = Wheat gluten, 10.73 ± 0.07%; Anchovy fine powder, 7.53 ± 0.02%.
DHN (%) = TCA-soluble-N/Tatal-N * 100
The relationship in Table 9 and Table 10 were expressed in graphs of FIGS. 29 to 31 , and they visually show the relationship between the enzyme hydrolysis, and the DHN and the solubility under the high pressure and the ambient pressure conditions well.
The present invention has been described in detail. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
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At least at least one embodiment of the present invention relates to a method for using a high pressure-resistant enzyme in a high pressure condition; a method for promoting the activity of the high pressure-resistant enzyme by means of a high pressure treatment; a composition, which contains the high pressure-resistant enzyme, for decomposing proteins under a high pressure condition; a composition, which contains the composition for decomposing proteins, for preparing natural flavoring substances; a container for high pressure treatment, which contains the composition for decomposing proteins; and a method for measuring the activity of the high pressure-resistant enzyme, which comprises a step of decomposing an azocasein solution serving as a substrate by using the high pressure-resistant enzyme treated under a high pressure condition.
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PRIORITY
This application claims priority to a provisional application entitled “Optical Tomography Using Independent Component Analysis For Detection And Localization Of Targets In Turbid Media,” which was filed in the U.S. Patent and Trademark Office on Dec. 7, 2004, and assigned Ser. No. 60/633,412, the contents of which are incorporated herein by reference.
GOVERNMENTAL INFORMATION
This invention is supported in part by the U.S. Army Medical Research and Material Command, National Aeronautics and Space Administration, Office of Naval Research.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a system and method for detecting, imaging, and determining the location of objects in a turbid medium using light as a probe, and more particularly relates to a system and method for finding and locating objects including, tumors in living tissue, an individual, a building, or a vehicle such as an aircraft, a missile, etc. located in smoke, fog, and vehicles and objects such as submarines and mines located in shallow and/or murky water using independent component analysis (ICA).
2. Description of the Related Art
With the pervasiveness of cancer and terrorism in modern times, it has become common to screen for undesired objects. For example, it is common to screen the human body for tumors which can include cancerous as well as benign tumors. Moreover, with the pervasiveness of terrorism, it is common to patrol and screen secure areas for objects and individuals that should not be in the secure areas. For example, border crossings, military bases, airports, governmental buildings, high-occupancy buildings and other selected locations are typically under constant surveillance to assure the security of these areas. Finding objects in a turbid medium has been researched in the past. Basic principles and simulation as well as experimental results of finding objects in a turbid medium are known. For example, see M. Xu et al. “Simulated And Experimental Separation And Characterization Of Absorptive Inhomogeneities Embedded In Turbid Media,” OSA Biomedical Topical Meeting, April, 2004; M. Alrubaiee et al. “Time-Resolved And Quasi-Continuous Wave Three-Dimensional Tomographic Imaging,” Femtosecond Laser Applications in Biology, Proceedings of SPIE, vol. 5463, April, 2004; M. Xu et al. “Information Theory Approach To Detect Small Inhomogeneities Within Tissue-Like Turbid Media,” the 4 th Inter-institute Workshop on Optical Diagnostic Imaging from Bench to Bedside, National Institutes of Health, Natcher Conference Center, Sep. 20-22, 2004; M. Alrubaiee et al. “Three-Dimensional Localization And Reconstruction Of Objects In A Turbid Medium Using Independent Component Analysis Of Optical Transmission And Fluorescence Measurements,” the 4 th Inter-institute Workshop on Optical Diagnostic Imaging from Bench to Bedside, National Institutes of Health, Sep. 20-22, 2004, the contents of all of which are incorporated herein by reference.
Additionally, on the medical side, noninvasive optical probing of tumors and functional monitoring of physiological activities in a human body using near infrared (NIR) light has been investigated by many investigators as compiled in G. Muller, R. R. Alfano, et al. Medical Optical Tomography: Functional Imaging and Monitoring, Vol. IS11 of SPIE Institute Series, 1993; S. K. Gayen and R. R. Alfano, “Emerging Optical Biomedical Imaging Techniques,” Opt. Photon. News 7, 17-22 1996; J. C. Hebden, et al. “Optical Imaging In Medicine: I. Experimental Techniques,” Phys. Med. Biol. 42, 825-840, 1997; S. R. Arridge et al., “Optical Imaging In Medicine: II. Modeling And Reconstruction,” Phys Med Biol. 42, 841-853, 1997, the contents of all of which are incorporated herein by reference. While some optical imaging techniques use a difference in light scattering and absorption characteristics between normal and cancerous tissues, other optical image techniques detect fluorescence of externally administered contrast agents that attach selectively to the tumors, or native tissue fluorescence. For example, see Ntziachristos et al., “Experimental Three-Dimensional Fluorescence Reconstruction Of Diffuse Media By Use Of A Normalized Born Approximation,” Opt. Lett. 26, 893-895, (2001); A. B. Milstein, et al., “Fluorescence Optical Diffusion Tomography,” Appl. Opt. 42, 3081-3094 (2003), the contents of all which are incorporated herein by reference.
Although both direct imaging, for example as disclosed in L. Wang, R. R. Alfano et al., “Ballistic 2-D Imaging Through Scattering Walls Using An Ultrafast Optical Kerr Gate,” Science 253, 769-771, 1991, and inverse reconstruction, for example as disclosed in R. Arridge, “Optical Tomography In Medical Imaging,” Inverse Problems 15, R41-R93, 1999, approaches have been used to obtain images of a target embedded in various types of turbid media, these methods still leave much to be desired. For example, the direct imaging approach uses different techniques to sort out image bearing ballistic and snake light, and to reject image blurring multiple scattered light in order to obtain a desired image, for example see U.S. Pat. No. 5,140,463, entitled “Method And Apparatus For Improving The Signal To Noise Ratio Of An Image Formed Of An Object Hidden In Or Behind A Semi-Opaque Random Media,” to Yoo et. al.; U.S. Pat. No. 5,142,372, to R. R. Alfano et. al., entitled U.S. Pat. No. 5,227,912, entitled “Multiple-Stage Optical Kerr Gate System,” to Ho et. al., U.S. Pat. No. 5,371,368, entitled “Ultrafast Optical Imaging Of Objects In A Scattering Medium,” to R. R. Alfano et. al.; Gayen and R. R. Alfano, “Sensing Lesions In Tissues With Light,” Optics Express Vol. 4, pp. 475-480 (1999); Gayen et. al., “Two-Dimensional Near-Infrared Transillumination Imaging Of Biomedical Media With A Chromium-Doped Forsterite Laser,” Appl. Opt. Vol. 37, pp. 5327-5336 (1998); Gayen, et. al. “Near-Infrared Laser Spectroscopic Imaging: A Step Towards Diagnostic Optical Imaging Of Human Tissues,” Lasers in the Life Sciences Vol. 37, pp. 187-198, (1999); Gayen, et. al., “Time-Sliced Transillumination Imaging Of Normal And Cancerous Breast Tissues,” in OSA Trends in Optics and Photonics Series Vol. 21 on Advances in Optical Imaging and Photon Migration, pp. 63-66, (1998); Dolne et. al, “IR Fourier Space Gate And Absorption Imaging Through Random Media,” Lasers in the Life Sciences Vol. 6, pp. 131-141, (1994); Das et. al. “Ultrafast Time-Gated Imaging In Thick Tissues: A Step Toward Optical Mammography,” Opt. Lett. Vol. 18, pp. 1002-1004, (1993); Hebden et. al., “Time Resolved Imaging Through A Highly Scattering Medium,” Appl. Opt. Vol. 30, pp. 788-794, (1991); and Demos et. al., “Time-Resolved Degree Of Polarization For Human Breast Tissue,” Opt. Commun. Vol. 124, pp. 439-442, (1996); the contents of all of which is incorporated herein by reference.
Although the above disclosed methods are typically suitable for turbid mediums whose thickness is less than 10 times the transport-mean-free-path, it is now accepted that for the turbid medium thickness which is greater than 10 times the transport-mean-free-path, direct shadowgram imaging is not feasible, and one has to resort to inverse reconstruction technique.
The conventional inverse reconstruction approach to locate and characterize the targets, matches the detected light intensities on the boundaries to that computed by a forward model of light propagation in the medium. The absorption and scattering coefficient distribution of the full medium is updated iteratively until the emerging light intensities on the boundaries predicted by the forward model are close to the observed values. Various approaches using time-resolved, frequency-domain, or steady-state lasers have been explored for inverse image reconstruction. Examples of inverse reconstruction methods include U.S. Pat. No. 5,813,988, entitled “Time-Resolved Diffusion Tomographic Imaging In Highly Scattering Turbid Media,” to R. R. Alfano et. al.; U.S. Pat. No. 5,931,789, entitled “Time-Resolved Diffusion Tomographic 2d And 3d Imaging In Highly Scattering Turbid Media,” to R. R. Alfano et. al.; Cai et. al., “Optical Tomographic Image Reconstruction From Ultrafast Time-Sliced Transmission Measurements,” Appl. Opt. Vol. 38, pp. 4237-4246 (1999); Cai et. al., “Time-Resolved Optical Diffusion Tomographic Image Reconstruction In Highly Scattering Turbid Media,” Proc. Natl. Acad. Sci. USA, Vol. 93, pp. 13561-13564, (1996); U.S. Pat. No. 6,665,557 B1, entitled “Sprectroscopic And Time-Resolved Optical Methods And Apparatus For Imaging Objects In Turbed Media,” to R. R. Alfano et. al.; S. R. Arridge, “The Forward And Inverse Problems In Time-Resolved Infrared Imaging,” published in the Medical Optical Tomography: Functional Imaging and Monitoring, SPIE, vol. IS11, C. Muller ed., PP. 31-64, (1993); and Singer et. al., “Image Reconstruction Of Interior Bodies That Diffuse Radiation,” Science, Vol. 248, pp 990-993, (1993); the contents of each of which are incorporated herein by reference.
SUMMARY OF THE INVENTION
Typical three-dimensional inverse reconstruction approaches suffer from the following limitations. Firstly, the iterative inverse reconstruction approach is time-consuming and not applicable to real-time imaging; and secondly, the spatial resolution in tissues is moderate and there is an inability to discern small targets with a size of less than 5 mm, such as, tumors at an earlier stage deep within the tissue. This limitation can be attributed to the following reasons: (1) light is highly scattered in tissue; and (2) the perturbation of the emerging light intensities due to the presence of targets is weak. Thus, the inverse reconstruction is highly ill-posed and requires regularization to stabilize the inversion at the cost of losing resolution. Moreover, a weak signal from a target is hard to differentiate using conventional methods.
Accordingly, there is a need for a system and a method for detecting and locating a target in a turbid medium, which can overcome the limitation of current inverse reconstruction methods.
Accordingly, it is an object of the present invention to provide a system and a method for detecting and locating a target in a turbid medium, which can overcome the limitations of conventional imaging systems.
It is also an object of the present invention to provide a system and method for detecting, imaging, and determining the location of objects in a turbid medium such as smoke, fog, living tissue, etc. using light as a probe, the objects including, tumors (e.g., benign or cancerous) in living tissue (e.g., an organ, flesh, etc.), an individual, a building, or a vehicle such as an aircraft, a missile, etc. located in an obscuring atmosphere such as dense smoke, fog, hail, rain, snow, and vehicles and objects such as submarines and mines located in shallow and/or murky water using independent component analysis (ICA).
The present invention to uses a technique known as OPtical Tomography using Independent Component Analysis (OPTICA) to detect and localize targets in turbid media that and can overcome limitations of conventional inverse reconstruction methods and can provide millimeter resolution.
Accordingly, it is an object of the present invention to provide a method for detecting the presence of one or more objects in a turbid medium, the method including: illuminating at least a portion of the turbid medium with incident light having at least one predetermined wavelength which interacts with the one or more objects differently than the light interacts with the turbid medium; capturing and measuring light that emerges from the turbid medium; and detecting and locating the one or more objects using Independent Component Analysis (ICA) of light emergent from the turbid medium.
It is a further object of the present invention to provide a method wherein, the light emerging from the turbid medium has the same wavelength as the incident light; the emergent light is detected using a light detector comprising one of a CCD camera, a near-infrared area camera, a one-dimensional array of detectors, photodiodes, photomultiplier tubes, and a streak camera; the detected light is analyzed using Independent Component Analysis (ICA) to determine independent components; and the location of the one or more objects is obtained based on the independent components.
It is also an object of the present invention to provide a method whereby the emergent light includes a plurality of wavelengths at least one of the wavelengths being different from the at least one wavelength of the incident light, signal at different wavelengths are compared using comparisons (such as addition, subtraction, division) which are thereafter used to obtain diagnostic information for indicating whether a target is a tumor and can be further used to determine whether the tumor is benign or cancerous.
It is yet a further object of the present invention to provide a method, wherein the illuminating light includes at least one of a light pulse, continuous-wave light, and amplitude modulated light, laser light having a wavelength between 750 and 950 nm, 950 and 1150 nm, 700 and 1500 nm, and/or 1150 and 1500 nm range. The illuminating light can include light generated by a laser such as a Ti:sapphire laser, a Nd:YAG laser, a dye laser, a semiconductor laser, a solid-state laser, a Cr4+-based laser, a semiconductor laser, and a color-center laser. It is also an object of the present invention to produce light having a variable wavelength using a variable-wavelength laser.
It is also an object of the present invention to provide a system and a method for detecting one or more objects including an absorptive target having an absorption coefficient different from the turbid medium, a scattering target having have a scattering coefficient different from the turbid medium, and/or an emissive target emitting light having at least one wavelength which is different than the wavelength of the incident light. It is also an object of the present invention to detect the emissive targets using extrinsic and/or intrinsic fluorophores.
It is a further object of the presenting invention to provide a system and a method for attenuating noise due to at least one of multiple scattered light and ambient background by using a gating method which can include space gating, Fourier gating, time gating, polarization gating, confocal gating, nonlinear optical gating, and coherence gating. The time gating being optionally provided by an electronically controlled timed gate which can be used for the time gating. The electronically controlled time gate further including one of an ultrafast gated intensified camera system (UGICS) having a gated image intensifier coupled to a charge-coupled-device (CCD) camera, or other suitable device. Furthermore, the duration and position of the time gate can be variably controlled. In yet other embodiments, the time gating is provided by gates which can include an optical Kerr gate, a second harmonic generation cross correlation gate, a four-wave mixing gate, and an upconversion gate.
Accordingly, it is an object of the present invention to provide a system for detecting the presence of one or more objects in a turbid medium, the system including a light source for illuminating at least a portion of the turbid medium with incident light having at least one predetermined wavelength which interacts with the one or more objects differently than the light interacts with the turbid medium; an image capture device for capturing and measuring light that emerges from the turbid medium; and a processor for detecting the presence and determining the location of the one or more objects using Independent Component Analysis (ICA) of the emergent light from the turbid medium, wherein the light emerging from the turbid medium can have at least one wavelength which is the same as, or different from, a wavelength of the incident light and the emergent light is detected using a light detector (or other image capturing device such as a CCD camera, a near-infrared area camera, a one-dimensional array of detectors, photodiodes, photomultiplier tubes, and a streak camera); the processor being further used for analyzed the detected light using Independent Component Analysis (ICA) to determine independent components, and determining the location of the one or more objects is obtained using knowledge of the independent components.
It is yet another object of the present invention to provide a system for detecting the presence of a tumor in a body organ formed of another type of tissue, the system including: a light source for illuminating at least a portion of the body organ with incident light having at least one predetermined wavelength which interacts with the tumor differently than the way it interacts with the tissue in the body organ; an image capture device for capturing and measuring light that emerges from the turbid medium, the turbid medium at least partially surrounding the tumor; and a processor for detecting the presence and determining the location of the tumor using Independent Component Analysis (ICA) of the emergent light from the turbid medium.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the present invention will be more apparent from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a diagram of the experimental arrangement according to an embodiment of the present invention for imaging objects embedded in a turbid medium including a 2-D array in the input plane that is scanned across the incident laser beam;
FIG. 2 . is a diagram of a first specimen including an Intralipid-10% suspension in water and two long cylindrical absorbing objects having an absorption coefficient 0.23 mm −1 according to an embodiment of the present invention;
FIG. 3 is a diagram of a second specimen including a solid block formed from a scattering material in which four scattering cylindrical targets having their centers on the central plane are embedded;
FIG. 4 shows light intensity patterns and graphs illustrating normalized independent spatial intensity distributions as a function of the lateral position x at the input (or source) plane (first row) and the exit (or detector) plane (the second row) generated by ICA and a horizontal profile of intensity distributions on the source plane (illustrated by diamonds) and on the detector plane (illustrated by circles) are displayed on the third row for the two absorbing cylinders of the first specimen;
FIG. 5 shows light intensity patterns and graphs respectively illustrating independent spatial intensity distributions at the exit (or detector) plane generated by ICA corresponding to objects with scattering coefficients of 4 times, 2 times, 1.5 times, and 1.1 times of that of the material of the slab of the second specimen;
FIG. 6 shows graphs illustrating independent intensity distributions of the fluorescence from the target generated by ICA at the detector plane and at the source plane;
FIG. 7 shows graphs illustrating fitting of the independent intensity distribution of fluorescence from a sphere of diameter 9 mm embedded in Intralipid-10% solution to the model Green's function;
FIG. 8 shows are graphs illustrating fitting of the independent intensity distribution of fluorescence from a sphere of diameter 4 mm embedded in 26 mm thick human breast tissue to the model Green's function;
FIG. 9 is a block diagram illustrating a control system for controlling the experimental arrangement shown in FIG. 1 ; and
FIG. 10 is a flow chart illustrating the operation of an embodiment of the present invention for locating a target location.
DESCRIPTION OF THE PREFERRED EMBODIMENT
According to the present invention, optical tomographic imaging of objects in a highly scattered turbid media is provided using an Optical Imaging (OPT) technique and an Independent Component Analysis (ICA) technique to provide a technique known as OPTICA which can provide for the optical tomographic imaging of objects in a highly scattering turbid medium. According to the present invention, an object located in a highly scattered turbid medium, such as a tumor in a human breast tissue, can be determined with an accuracy of 1 mm. The OPTICA technique can use a multiple-source illumination and multiple detector data acquisition scheme as will be explained below.
According to the present invention, a multi-source illumination is used to scan a sample in the xy plane across the incident beam propagating in the z-direction and multiple detectors, for example a charge-coupled device (CCD) camera wherein each pixel of the CCD may be viewed as a detector, are used to locate the objects. The resulting spatial diversity and multiple angular observations provide robust data for extracting three-dimensional location information about the embedded targets (i.e., inhomogeneities) in the medium with a millimeter scale accuracy. The data can be analyzed using an Independent Component Analysis (ICA) of information theory. ICA of the light intensity distribution at the detection plane identifies the major components (which represent the embedded targets) contributing to the intensity distribution data. Using this scheme, every target may be looked upon as a secondary light emitter.
A salient feature of OPTICA is that ICA provides independent components due to the targets, with minimal processing of the data and the ICA does not have to resort to any specific light propagation model for obtaining this information. Specific light propagation models are necessary only in a later stage to determine location (of the targets) by curve fitting of Green's functions as will be described below. OPTICA is also not model specific, since any appropriate model for light propagation including a diffusion approximation or a radiative transfer equation may be used. Another advantage is that OPTICA can be used with light scattering and/or absorbing targets, as well as with fluorescent targets where the fluorophore may be extrinsic or intrinsic.
An advantage of the OPTICA method is that it can be used with data acquired from objects of different types of geometric shapes, such as, slabs, cylinders, spheres, and/or arbitrary shaped boundaries. The OPTICA approach as taught by the present invention is fast, and amenable to near real-time detection and localization of objects in a turbid medium, which is a key consideration for in vivo medical imaging. The approach disclosed herein is remarkably sensitive, and can detect a 5-mm diameter and a 5-mm long cylindrical target, at least one of having a reduced scattering coefficient, which is only 10% higher than the surrounding medium, in a 166-mm long, 82-mm wide, and 55-mm thick slab made of materials having a reduced scattering coefficient μ s , ˜0.9 mm −1 (transport length, l t ˜1.1 mm), and an absorption coefficient, μ a ˜0006 mm − 1. Conventionally, such objects were considered improbable to be detected (e.g., see J. Hall et al., “Imaging Very-Low-Contrast Objects In Breastlike Scattering Media With A Time-Resolved Method”, Appl. Opt., vol. 36, pp. 7270-7276, 1997)).
OPTICA is suitable for imaging small targets. For example, OPTICA can be used to detect small objects (e.g., objects with a size of ˜1 mm) in a highly scattering medium. Given its ability to identify low-contrast small objects, the present invention is suitable for imaging and detecting early, as well as later, -stage tumors in living tissue and body organs, which can be especially beneficial when dealing with cancerous tumors.
Theoretical formalisms and algorithms of OPTICA taught by the present invention will now be provided. OPTICA is an information theory approach to detect and locate objects within a turbid medium. For the sake of clarity a detailed description of well known principles will not be given, when it may obscure the present invention.
An exploded perspective view block diagram illustrating an OPTICA scanning system including a sample according to the present invention is shown in FIG. 1 . OPTICA uses a multi-source illumination and multi-detector signal acquisition scheme providing a variety of spatial and angular views essential for three-dimensional (3-D) object localization. The multi-source illumination can be realized by scanning an input surface (or, a source plane) 110 across an incident beam 170 in a two-dimensional (2-D) array of points (e.g., x s k , y s k ; k=1, 2, . . . , n). Alternatively, the input surface may be kept fixed, and a beam of light may be scanned. Corresponding to illumination of the k-th grid point on the source plane 110 , a charge-coupled device (CCD) camera 120 records the spatial intensity distribution, I k (x d ,y d ), on the exit surface (or, detector plane) 130 . Thus, every pixel of the CCD camera 120 can function as a detector implementing the multi-detector measurement arrangement. The difference between the above-mentioned spatial intensity distribution, I k (x d ,y d ) and an estimated background (for example, an averaged intensity distribution obtained from different source scanning positions) provides the perturbation in the spatial intensity distribution in the detector plane for illumination at the k-th grid point, ΔI k (x d ,y d ). The different source and scanning positions can be created using a light emitting diode (LED) LASER array (not shown). Additionally, one or more lasers 180 , can be used with steering optics to guide an incident beam 170 to predetermined locations. A fiber optic guide 175 can also be used to channel the incident beam 170 .
A localization algorithm is based on the premise that each object (or, target 160 ) within the turbid medium 150 alters the propagation of light through the turbid medium 150 . Consequently, the spatial distribution of the light intensity at a detector plane of the turbid medium 150 is different with embedded targets or objects (e.g., target 160 ) than that without them. The influence of an object on the light intensity distribution ΔI k (x d ,y d ) involves propagation of light from the source to the object, and from the object to the detector, and can be described in terms of two Green's functions (propagators): the first G(r,r s ) describing light propagation from a source r s to an object r; and the second G(r d ,r) from the object r to the detector at r d . In order to correlate perturbations in the light intensity distributions ΔI k (x d ,y d ), with the objects embedded in the turbid medium, these objects illuminated by the incident wave are assumed to be “virtual sources”, and light intensity distribution ΔI k (x d ,y d ) assumed to be a weighted mixture of signals arriving from the virtual sources to the detector plane. ICA assumes these “virtual sources” to be independent, and based on this assumption provides the independent components of the virtual sources. The number of leading independent components is the same as the number of the embedded objects. The effective contributions of the independent components to the light intensity distribution on the source and detector planes are proportional to the projection of the Green's functions G(r,r s ) and G(r d ,r), on the source and detector planes, respectively. The location and characteristics of the objects are obtained from fitting either or both of the projections of the Green's functions to those of the model Green's function in a background medium.
In a linearized scheme of inversion, the perturbation of the detected light intensities on the boundaries of the medium, the scattered wave field, due to absorptive and scattering objects (i.e., inhomogeneities) can be defined by a diffusion approximation (DA) shown in Equation 1 below. Diffusion approximations are further defined in Xu, M. Lax and R. R. Alfano, “Time-Resolved Fourier Optical Diffuse Tomography,” J. Opt. Soc. Am. A, vol. 18, no. 7, pp. 1535-1542, (2001), the contents of which are incorporated herein by reference.
φ sca ( r d ,r s )=−∫ d 3 rG ( r d ,r )δμ a ( r ) cG ( r,r s )−∫ d 3 rδD ( r ) c∇ r G ( r d ,r )·∇ r G ( r,r s ) (1)
When illuminated by a unit point source, where r s , r, and r d are the positions of the source, the inhomogeneity or object, and the detector, respectively, δμ a =(μ a,obj −μ a ) and δD=(D obj −D) are the differences in an absorption coefficient and a diffusion coefficient, respectively, between the inhomogeneity and the background, c is the speed of light in the medium, and G(r,r′) is a Green's function describing light propagation from r′ to r inside the background turbid medium of absorption coefficient μ a and diffusion coefficient D. It is noted that the explicit dependence on the modulation frequency of the incident wave in the frequency domain in Equation 1 has been omitted for the sake of clarity. The following formalism can be applied to continuous wave, frequency-domain and time-domain measurements. The time domain measurement is first Fourier transformed over time to obtain data over many different frequencies. Although Equation 1 includes a DA, it should be emphasized that the invention is not limited to a DA, but can be used with other models of light propagation in a turbid media, such as, a cumulant approximation (e.g., see W. Cai, M. Lax and R. R. Alfano, “Analytical Solution Of The Elastic Boltzmann Transport Equation In An Infinite Uniform Medium Using Cumulant Expansion,” J. Phys. Chem. B, vol. 104, no. 16, pp. 3996-4000, (2000); and M. Xu, W. Cai, M. Lax and R. R. Alfano, “A Photon Transport Forward Model For Imaging In Turbid Media,” Opt. Lett., vol. 26, no. 14, pp. 1066-1068, (2001)), a random walk model (e.g., see H. Gandjbakhche et. al., “Photon Path-Length Distributions For Transmission Through Optically Turbid Slabs,” Phys. Rev. B, vol. 48, no. 2, pp. 810-818, (1993, the contents of each of which are incorporated herein by reference) and linearized radiative transfer models.
The Green's function G for a slab geometry in the diffusion approximation is given by
G ( r , r ′ ) ≡ G ( ρ , z , z ′ ) = 1 4 π D ∑ k = - ∞ ∞ [ exp ( - kr k + ) r k + - exp ( - kr k - ) r k - ] ;
where
r k ± = ρ 2 + ( z ∓ z ′ ± 2 kd ) ( 2 )
for an incident amplitude-modulated wave of modulation frequency ω, where k=0, ±1, ±2, . . . ,
ρ = ( x - x ′ ) 2 + ( y - y ′ ) 2
is the distance between the two points r=(x,y,z) and r′=(x′,y′,z′) projected onto the xy plane,
k = ( μ a - ⅈϖ / c ) / D
chosen to have a nonnegative real part, and extrapolated boundaries of the slab are located at z=0 and z=d=L Z +2z e , respectively, where L Z is a physical thickness of the slab and an extrapolation length z e should be determined from a boundary condition of the slab (e.g., see Lax et. al., “Classical Diffusion Photon Transport In A Slab, In Laser Optics Of Condensed Matter,” Plenum, New York, pp. 229-237, (1987); and R. C. Haskell, et al., “Boundary Conditions For The Diffusion Equation In Radiative Transfer,” J. Opt. Soc. Am. A, vol. 11, no. 10, pp. 2727-2741, (1994) the contents of each of which are incorporated herein by reference). Equation 2 serves as the model of Green's function in the uniform background medium of a slab geometry. The modulation frequency ω=0 for a continuous wave light. The Green's function for the slab in time domain is the inverse Fourier transform of Equation 2 in a frequency domain.
In practice, the projections of the Green's function on the source and detector planes, are determined from the measured perturbations in the light intensity distribution using ICA according to the present invention. The comparison to the prototype Green's function is then used to locate and characterize the inhomogeneities. The formalism given is for absorptive, scattering and fluorescent targets are detailed in the following subsections.
Under the assumption that absorptive targets are localized, the jth one is contained in volume V j centered at r j (where l j J), the scattered wave field φ sca (r d ,r s ) of Equation 1 can be rewritten as:
Error! Objects cannot be created from editing field codes (3)
where q j =δμ a (r j )cV j is the absorption strength of the jth target, and r j is the position of the jth target. The scattered wave may be interpreted as an instantaneous linear mixture (e.g., see J. F. Cardoso, “Blind Signal Separation: Statistical Principles,” Proceedings of the IEEE, vol. 9, no. 10, pp. 2009-2025, (1998) the contents of which is incorporated herein by reference).
x ( r s )= As ( r s ) (4)
In Equation 4 separated virtual sources s(r s )=(q 1 G(r l ,r s ), . . . , q j G(r j ,r s )) T represents the J virtual sources, i.e., the J targets illuminated by the incident wave. A is a mixing matrix given by Equation 5.
A = ( G ( r d 1 , r 1 ) G ( r d 1 , r 2 ) … G ( r d 1 , r j ) G ( r d 2 , r 1 ) G ( r d 2 , r 2 ) … G ( r d 2 , r j ) ⋮ ⋮ ⋱ ⋮ G ( r d m , r 1 ) G ( r d m , r 2 ) … G ( r d m , r j ) ) ( 5 )
whose jth column (which is a mixing vector) provides weight factors for the contributions from the jth absorbtive target to the detectors, and a multi-source multi-detector set x(r s )=((φ sca (r d 1 ,r s ), . . . , −φ sca (r d m ,r s )) T ) is an observed light intensity change where the superscript “T” denotes a transposition. The observation is made over m positions r d 1 , . . . , r d m . The incident light source scans a total of n positions r s 1 , . . . , r s n , sequentially, which can be regarded as “temporal” sampling points in the instantaneous linear mixture model of Equation 4. The multi-source multi-detector data set x(r) thus describes signals observed in m channels (i.e., m detectors) from J virtual sources (or J absorbtive targets) simultaneously over n discrete “temporal” points (n spatial scanning points). A single absorptive target is represented by a single virtual source q j G(r j ,r s ). The virtual source q j G(r j ,r s ) represents the individual absorbtive target illuminated by the incident wave and is similar to the concept of the secondary source in Huygen's principle (e.g., see M. V. Klein, “Optics,” John Wiley & Sons, (1970)). The role of detectors and sources can be interchanged due to the reciprocal property of light propagation.
The principal assumption of the above-stated formalism is that the jth absorptive target (treated as virtual source q j G(r j ,r s )) is independent of the virtual sources at other locations. Under this assumption, ICA can be used with the observations from the light source scanned at n>>J positions to separate out both virtual sources s(r s ) and the mixing matrix A (e.g., see P. Comon, “Independent Component Analysis—A New Concept?”, Signal Processing, vol. 36, pp. 287-314 (1994); and J. F. Cardoso, “Blind signal separation: Statistical Principles”, Proceedings of the IEEE, vol. 9, no. 10, pp. 2009-2025, (1998), the contents of each of which is incorporated herein by reference).
ICA is a statistical approach to separate independent sources from linear instantaneous or convolutive mixtures of independent signals without relying on any specific knowledge of the sources except that they are independent. The sources are recovered by a minimization of a measure of dependence, such as mutual information (e.g., see P. Comon, “Independent Component Analysis—A New Concept?”, Signal Processing, vol. 36, pp. 287-314 (1994); and A. J. Bell, “Information Theory, Independent Component Analysis, and Applications”, in Unsupervised Adaptive Filtering, Vol. 1, Wiley, pp. 237-264, (2000), the contents of each of which is incorporated herein by reference) between the reconstructed sources (e.g., see J. F. Cardoso, “Blind Signal Separation: Statistical Principles”, Proceedings of the IEEE, vol. 9, no. 10, pp. 2009-2025, (1998), the contents of which are incorporated herein by reference). The recovered virtual sources and mixing vectors from ICA are unique up to permutation and scaling.
The two Green's functions of light propagating from the source to the target (i.e., G(r,r s )) and from the target to the detector (i.e., G(r,r d )) are retrieved from the separated virtual sources s(r s ) and the mixing matrix A. The jth element s j (r s ) of the virtual source array and the jth column a j (mixing vector) of the mixing matrix A provide scaled projections of the Green's function on the source and detector planes, G(r j ,r s ) and G(r d ,r j ), respectively. s j (r s ) and a j can be defined as:
s j ( r s )=α j G ( r j ,r e ); and
a j =β j G ( r d ,r j ), (6)
where α j and β j are scaling constants for the jth target.
Both the location and strength of the jth target can be computed by a simple fitting procedure using Equation 6. For example, a least square fitting procedure given by Equation (7)
min r j , α j , β j { ∑ r s [ α j - 1 s j ( r s ) - G ( r j , r s ) ] 2 + ∑ r s [ β j - 1 a j - G ( r d , r j ) ] 2 } ( 7 )
can be used. The fitting procedure yields the location r j of, and the two scaling constants α j and β j for, the jth absorptive target whose absorption strength is then given by q j =α j β j .
For scattering targets, under the assumption that the targets are localized in a few regions, an analysis which is similar to the analysis of absorptive targets can be used. Up to three virtual sources may appear for a single scattering target corresponding to the x, y, and z components in the dot product ∇ r G(r d ,r)·∇ r G(r,r s )= x G(r d ,r) x G(r,r s )+ y G(r d ,r) y G(r,r s )+ z G(r d ,r) z G(r,r s ) shown in Equation 1.
By introducing two auxiliary functions as shown in Equations 8 and 9 below,
g ⊥ ( r , r ′ ) = 1 4 π D ∑ k = - ∞ + ∞ [ ( kr k + + 1 ) exp ( - kr k + ) ( r k + ) 3 - ( kr k - + 1 ) exp ( - kr k - ) ( r k - ) 3 ] ( 8 ) g z ( r , r ′ ) = 1 4 π D ∑ k = - ∞ + ∞ { ( z - z ′ + 2 kd ) ( kr k + + 1 ) exp ( - kr k + ) ( r k + ) 3 - ( z + z ′ - 2 kd ) ( kr k - + 1 ) exp ( - kr k - ) ( r k - ) 3 } , ( 9 )
the scattered wave due to scattering targets can be rewritten as:
φ sca ( r d ,r s )=− d 3 rδD ( r ) c {[( x−x d )( x−x s )+( y−y d )( y−x 5 )] g ( r,r d ) g ( r,r s )+ g z ( r,r d ) g z ( r,r s )}. (10)
By denoting the scattering targets as q j ′=δD(r j )cV j ′ where c is the speed of light in the medium, an V j ′ is the volume of the jth scattering target, the scattered wave field can be transformed to:
ϕ sca ( r d , r s ) = ∑ j = 1 n ′ g z ( r j , r d ) q j ′ g z ( r j , r s ) +
∑ j = 1 n ′ ρ dj cos θ ⊥ ( r j , r d ) q j ′ ρ sj cos θ s g ⊥ ( r j , r s ) +
∑ j = 1 n ′ ρ dj sin θ ⊥ ( r j , r d ) q j ′ ρ sj sin θ s g ⊥ ( r j , r s ) ( 11 )
where
ρ
dj
=
(
x
d
-
x
j
)
2
+
(
y
d
-
y
j
)
2
,
ρ sj = ( x s - x j ) 2 + ( y s - y j ) 2
and θ d and θ s are the azimuth angles of r d −r j and r s −r j , respectively. This scattered wave can be regarded as a mixture of contributions from (3J′) virtual sources:
q j ′g z (r j ,r s ),q j ′ρ sj cos θ s g(r j ,r s ), and, q j ′ρ sj sin θ s g(r j ,r s ), (12
with the respective mixing vectors
g z (r j ,r d ), ρ dj cos θ d g(r j ,r d ), and, ρ dj sin θ d g(r j ,r d ), (13)
where 1<j<J. Generally, there are three virtual sources of specific patterns (e.g., one centrosymmetric pattern and two dumbbell shaped patterns) associated with a single scattering target, whereas only one centrosymmetric virtual source is associated with a single absorptive target. This difference may be used to discriminate absorptive and scattering targets. However, for scattering target deep within a turbid media, only the q j ′g z (r j ,r s ) virtual source remains significant and the other two virtual sources (i.e., q j ′ρ sj cos θ s g(r j ,r s ), and, q j ′ρ sj sin θ s g(r j ,r s )) are substantially attenuated. In such a situation, other corroborative evidences such as multi-wavelength measurements are required to determine the nature of targets. Both the location and strength of the jth scattering object are computed by fitting the retrieved virtual sources and mixing vectors to Equations 12 and 13, respectively.
The light propagation in a highly scattering medium with embedded fluorescent targets (e.g., intrinsic and/or exogenous contrast agents) excited by an external light source can be described by coupled diffusion equations at the excitation and emission wavelengths (e.g., see M. S. Patterson and B. W. Pogue, “Mathematical Model For Time-Resolved and Frequency-Domain Fluorescence Spectroscopy In Biological Tssues”, Appl. Opt., vol. 33, no. 10, pp. 1963-1974, (1994); and Adam B. Milstein et. al. “Fluorescence Optical Diffusion Tomography”, Appl. Opt., vol. 42, no. 16, pp. 3081-3094, (2003), the contents of each of which are incorporated herein by reference). A fluorescence signal U m (r d ,r s ω) can be expressed in terms of the two Green's functions G x (r,r s ω) and G m (r d ,r,ω) describing the light propagation from the source r s to a fluorophore at r at an excitation wavelength λ x and the light propagation from the fluorophore to the detector at r d at a transmission wavelength λ m , respectively where ω is the angular modulation frequency of the light as shown in Equation 14 below (e.g., see X. D. Li et. al., “Fluorescent Diffuse Photon Density Waves In Homogeneous And Heterogeneous Turbid Media: Analytic Solutions and Applications”, Appl. Opt., vol. 35, no. 19, pp. 3746-3758, (1996) the contents of which are incorporated herein by reference).
Accordingly, a fluorescence signal can be defined by:
U
m
(
r
d
,
r
s
,
ω
)
=
∫
G
m
(
r
d
,
r
,
ω
)
γ
(
r
)
c
1
-
jωτ
(
r
)
G
x
(
r
,
r
s
,
ω
)
ⅆ
r
(
14
)
Assuming a unit point illumination source located at r s and a single exponent decay model of fluorescence with a lifetime of τ(r). The subscripts x and m denote the quantities associated with the excitation and emission wavelengths, respectively, and c is the speed of light in the medium. A fluorescent yield y(r)=ημ af (r) is a product of the fluorophore's quantum efficiency η (which depends upon the type of the fluorophore and chemical environment) and the flororphore's absorption coefficient μ af (r)=η(r)σ a , where η(r) is the fluorophore concentration and σ a is the known fluorophore absorption cross section at the excitation wavelength. The nonlinear effect due to multiple passages of light through fluorophores can be incorporated into Equation 14 using a nonlinear correction factor if necessary. In the case of multiple fluorescent targets within the medium, it is preferable to rewrite Equation 14 as a summation shown in Equation 15 below.
U m ( r d , r s , ω ) = ∑ i G m ( r d , r i , ω ) q i ( ω ) G x ( r i , r s , ω ) , ( 15 )
where the fluorescence strength q f (ω)=γ(r i )cV i /(1−jωT(r i )) and r i is the location of the ith fluorescent target of volume V i . Equation 15 casts again the fluorescence signal to a mixture of contributions from virtual sources where the virtual source is proportional to q i G x (r i ,r s ,ω) and the mixing matrix is proportional to G x (r d ,r i ,ω). The virtual sources are statistically independent. By seeking the maximal mutual independence, the virtual sources can be separated with independent component analysis of observations made from a multi-detector array outside the medium produced by an external scanning point source. Both the location and strength of the fluorophores can be obtained by comparing the virtual source and mixing matrix to the respective Green's functions, in the exactly same procedure outlined for absorptive targets.
An exemplary fluorescent target will now be used to illustrate how the size and shape of a target can be estimated according to an embodiment of the present invention. Once one fluorescent target is located and centered at r i the fluorescent target's contribution to the fluorescence signal is given by:
U m i ( r d , r s , ω ) = γ i ( c ) 1 - jωτ ∫ V i G m ( r d , r , ω ) G x ( r , r s , ω ) ⅆ r , ( 16 )
where the integration is performed within an ith fluorescent target assuming uniform fluorescent yield γ j and lifetime r i . To estimate the shape of the fluorescent target, the volume V i is further projected in the longitudinal direction to its transverse cross section S i and thickness of the fluorophore Δz i (ρ) is introduced. Accordingly, Equation 16 can be rewritten as shown in Equation 17 below.
U m i ( r d , r s , ω ) =
γ i c 1 - jωτ i ∫ S i G m ( ρ d - ρ , ω ) Δ z i ( ρ ) G x ( ρ - ρ s , ω ) ⅆ ρ ( 17 )
where ρ d , ρ, and ρ s , are transverse coordinates of a detector, the fluorescent target, and the source, respectively. The weighted convolution of Equation 17 in ρ can be further simplified as shown in Equation 18 below.
U m i ( q d , q s , ω ) = γ i c 1 - jωτ i G m ( q d , ω ) Δ z i ( q d + q s ) G x * ( q s , ω ) , ( 18 )
in the Fourier space where q d , q, and q s are conjugate variables of ρ d , ρ, and ρ s , respectively, and “*” denotes a complex conjugate. This yields a solution for Δz i (q) shown in Equation 19 below.
Δ
z
i
(
q
)
=
1
-
jωτ
i
γ
i
c
U
m
i
(
q
-
q
s
,
q
s
,
ω
)
G
m
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q
-
q
s
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)
G
x
*
(
q
s
,
ω
)
m
i
=
1
-
jωτ
i
γ
i
c
U
m
i
(
q
d
,
0
,
ω
)
γ
i
c
G
m
(
q
d
,
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)
G
x
*
(
0
,
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)
.
,
(
19
)
Please note, q s was chosen to be equal to 0, because usually there are much fewer sources than detectors (e.g., in the present embodiment where a CCD camera is used to detect the light emission at the surface illuminated by a single laser source 120 as shown in FIG. 1 ). An inverse Fourier transform of (Δz i (q) yields a thickness profile of the fluorescent target in the z direction. The FWHM (full width at half maximum value) and the contour of the thickness profile provide an estimation of size and shape of the ith target, respectively.
According to the present invention using OPTICA, virtual sources are assumed to be mutually independent and a specific light propagation model is not assumed. Appropriate light propagation models including the diffusion approximation, the cumulant approximation (e.g., see W. Cai, M. Lax and R. R. Alfano, “Analytical Solution Of the Elastic Boltzmann Transport Equation In An Infinite Uniform Medium Using Cumulant Expansion,” J. Phys. Chem. B, vol. 104, no. 16, pp. 3996-4000, (2000); and M. Xu, W. Cai, M. Lax and R. R. Alfano, “A photon transport forward model for imaging in turbid media,” Opt. Lett., vol. 26, no. 14, pp. 1066-1068, (2001), the contents of which are incorporated herein by reference), the random walk model (e.g., see A. H. Gandjbakhche et. al., “Photon Path-Length Distributions For Transmission Through Optically Turbid Slabs,” Phys. Rev. E, vol. 48, no. 2, pp. 810-818, (1993) the contents of which are incorporated herein by reference), and radiative transfer can also be used with the OPTICA method according to the present invention. The number of targets within a medium is determined by the number of the independent components presented in a multi-source multi-detector data set contained within a turbid medium. Analysis of retrieved independent components from ICA then localizes and characterizes absorptive and/or scattering targets inside the turbid medium where an appropriate model of the light propagator is adopted. When a noise level is high and/or systematic errors are present, extra independent components may appear in readings. Only the leading independent components according to the respective contribution need to be analyzed to detect and characterize targets of interest and other components can be discarded.
Provided herein are several experiments which illustrate actual embodiments of the present invention in which OPTICA enables the detection and location of targets whose light absorption, scattering, or emission characteristic are different from that of a surrounding turbid medium. Absorptive, scattering, or fluorescent targets embedded in turbid media were used for experimental demonstration. A description of samples (e.g., specimens) used in the demonstration, experimental arrangement and procedures as well as experimental results will now be provided below.
Three tissue-simulating phantoms with absorption and scattering coefficients within the reported range of values emulating healthy human breast tissues and a fourth sample of (ex vivo) human breast tissue was used for following experiments (e.g., see H. Heusmarin et. al., “Characterization Of Female Breasts In vivo By Time Resolved And Spectroscopic Measurements In Near Infrared Spectroscopy”, J. Biomed. Opt., vol. 1, pp. 425-434, (1996), the contents of which are incorporated herein by reference).
A diagram of illustrating a first specimen including an Intralipid-10% suspension in water with two cylindrical absorbing objects having an absorption coefficient of 0.23 mm −1 is shown in FIG. 2 .
The first specimen 200 includes a 250 mm×250 mm×50 mm transparent plastic container (for forming a slab) 210 (which is similar to the sample 410 shown in FIG. 1 ) filled with Intralipid-10% suspension in water (not shown) with two absorbing targets 220 and 230 , respectively, embedded in the container 210 . The concentration of Intralipid-10% was adjusted (e.g., see Hugo J. van Staveren et. al., “Light Scattering In Intralipid-10% In The Wavelength Range Of 400-1100 nm”, App. Opt., vol. 30, no. 31, PP. 4507-4514, (1991), the contents of which are incorporated herein by reference) to provide a transport length l t ˜1 mm at 785 nm.
The absorbing targets 220 and 230 each include an 8-mm diameter 250-mm long cylindrical glass tube filled with a Intralipid-10% suspension (to provide the same scattering coefficient as the Intralipid-10% suspension) and an absorbing-ink solution for changing the absorption coefficient to 0.23 mm −1 . The absorbing targets 220 and 230 were placed at different depths along the 50 mm path length (i.e., the depth corresponding to the z-axis) of the plastic container 210 .
A diagram illustrating a second specimen including a plurality of cylindrical scattering objects is shown in FIG. 3 . The second specimen 300 includes a 166-mm long, 82-mm wide, and 55-mm thick slab 310 formed from materials having a reduced scattering coefficient μ′ s ˜0.9 mm −1 (transport length, l t ˜1.1 mm), and an absorption coefficient, μ′ a ˜0.006 mm −1 . The slab 300 includes four 5-mm diameter by 5-mm long cylindrical scattering targets 320 , 330 , 340 , and 350 . The center of each cylindrical scattering object (i.e., 320 , 330 , 340 , and 350 ) is located in a plane 360 which is located halfway between a front side 310 F and a back side 310 F of the slab 310 . The absorption coefficient of each cylindrical scattering object 320 , 330 , 340 , and 350 , is 0.006 mm −1 , which is the same as that of the material of the slab 310 , but the scattering coefficient of each cylindrical scattering object 320 , 330 , 340 , and 350 is respectively 1.5, 2.0, 4.0, and 1.1 times greater than the scattering coefficient of the slab 310 . The first and the third cylinders, and the second and the fourth cylinders are on two horizontal lines about 22 mm apart. The distance between neighboring cylinders is 11 mm. Further details about similar slabs may be obtained in D. J. Hall, et al. “Imaging Very-Low-Contrast Objects in Breastlike Scattering Media With A Time-Resolved Method”, Appl. Opt., vol. 36, pp. 7270-7276, (1997), the contents of which are incorporated herein by reference.
A perspective view diagram illustrating a third specimen is shown in FIG. 3 . The third specimen is also shown in FIG. 1 The third specimen 400 includes a spherical fluorescent target 420 placed inside a slab 410 measuring 250 mm×250 mm×50 mm, which is similar to the size and the composition of the slab 210 and 310 shown in the first and second specimens, respectively. The slab 410 is filled with an Intralipid-10% aqueous suspension. The fluorescent target 400 includes a 9.0 mm diameter sphere filled with a solution in water and Indocyanine green (ICG) dye that can be ex cited in the 650 nm-800 nm spectral range.
A fourth specimen (not shown) includes a spherical fluorescent target placed inside an ex vivo human breast tissue sample. The tissue sample was assembled as a 26 mm thick, 50 mm long and 50 mm wide slab slightly compressed between two glass plates. The fluorescent target was a 4.0 mm-diameter glass sphere filled with ICG solution in water. The experimental setup is the similar to the setup used by the third specimen and will not be further discussed for the sake of clarity.
Referring back to FIG. 1 , an experimental setup for analyzing a slab (e.g., the third specimen 400 ) will now be discussed in further detail. An optical source (e.g., a laser) provides incident light beams having a wavelength of λ x =785 nm. Two (optional) long wavelength pass absorption filters 150 - 1 and 150 - 2 were placed between the Fluorescent target 410 and the CCD camera unit 120 to block the excitation wavelength and allow fluorescence light to pass. The wavelength of the peak fluorescence light adjusted by the filtering and the CCD camera 120 response efficiency is about λ m =870 nm. The Intralipid-10% suspension is diluted with pure water such that the transport mean free paths and absorption coefficients are l t x =1.01 mm and μ a x =0.0022 mm −1 at the excitation wavelength, and l t m =1.14 mm and μ a m =0.0054 mm −1 at the emission wavelength, respectively. Sample targets 180 are shown for illustration purposes only and are not included with the third sample slab 400 in actual embodiments.
The experimental arrangement shown in FIG. 1 can be used for imaging of specimens, including the first to fourth specimens, etc. For CW measurements a 200-μm fiber 170 delivers a beam of 784-nm light from a diode laser 180 (e.g., an Ocean Optics R-2000) illuminates an input surface (or source plane) 110 of the specimen 410 . A cooled CCD camera 120 set to an acquisition time of 150-ms records two-dimensional (2-D) intensity patterns of the light transmitted through the opposite side of the slab specimen 410 (i.e., the side adjacent to a detector plane 190 ). For time-resolved measurements a 1-mm diameter collimated beam of 785-nm, 150-fs, 1-kHz repetition rate light pulses from a Ti:sapphire laser and amplifier system (e.g., see Q. Fu et. al. “High-average-power kilohertz-repetition-rate sub-100-fs Ti-sapphire amplifier system”, Opt. Lett, vol. 22, pp. 712-714, (1997)) can be used to illuminate the sample (e.g., fluorescent sample 410 ). An ultrafast gated intensified camera system (UGICS) that provides an FWHM gate width variable from 80 ps to 6 ns can be used to record 2-D intensity patterns of the light transmitted through the opposite side of the slab.
Computer controlled xy translation stages were used for scanning the specimens in an array of points in the xy plane as displayed in FIG. 3 . The computer controlled xy translation stages is adjusted according to variables which can include the number of expected targets and the size, shape, and type of expected targets. For example, for the long cylindrical absorbing targets included in the first specimen, a line scan of 16 points with a step size of 2.5 mm along x-axis is used to obtain (x, z) locations of the absorbing cylinders. Using the second specimen, an array of 20×18 points with a step size of 2.5 mm across the lateral positions of the 4 scattering targets was used for scanning to obtain the locations of the 4 scattering targets. Using the third specimen, point source scans over a 10×10 grid system with spacing of 2.5 mm between consecutive grids, was used to establish the position the fluorescent target.
Using the previously described methods and targets, temporal profiles of the transmitted pulses were generated using the UGICS in the scan mode with an 80-ps gate width. Average optical properties of the turbid medium were estimated by fitting the temporal profiles to the diffusion approximation of the radiative transfer equation (RTE).
ICA of the perturbations in the spatial intensity distributions provided corresponding independent intensity distributions on the source and detector planes. ICA generated independent intensity distributions on the source and detector planes are shown in diagrams (a) and (b) of FIG. 4 respectively, for the two absorbing cylinders of the first specimen. Locations of the absorbing cylinders are obtained by fitting independent component intensity distributions to those of the diffusion approximation in a slab using Equation 6. In actual experiments, the first cylinder was determined to be located at x=24 mm, 29 mm away from the source plane and 21 mm away from the detector plane, and the location was determined to be second cylinder at x=47 mm, 33 mm away from the source plane and 17 mm away from the detector plane. The experimentally obtained (x and z) coordinates of both of the cylinders are within 0.5 mm of their actual known positions.
Independent intensity distributions at the detector plane corresponding to the four scattering targets of the second specimen are displayed in diagrams (a)-(d) of FIG. 5 . These independent intensity distribution components are then used to obtain projections of a target-detector Green's function, G(r d ,r j ), with j=1, 2, 3, 4, on the detector plane for the four small cylindrical scattering targets embedded in the second specimen. Locations of the targets are determined by fitting the projections to those of the model Green's function e.g., see diagrams (e)-(h) of FIG. 5 . Locations of all four targets were then experimentally determined. Even the weakest scatterer, with a scattering coefficient just 11.1 times the background and hence considered to be rather unlikely to be found e.g., see Davie J. Hall et. al., “Imaging Very-Low-Contrast Objects in Breastlike Scattering Media With a Time-Resolved Method”, Appl. Opt., vol. 36, pp. 7270-7276, 1997), were detected. The known and OPTICA estimated positions of the four objects are presented in Table 1 below. As shown in Table 1, positions along z-axis (depth) of the cylinders were experimentally determined to be located at 28.13 mm, 27.87 mm, 27.08 mm and 32.6 mm. Except for the experimental results for the last cylinder, the depth of other cylinders agree within 1 mm of their known center positions of 27.5 mm. The OPICA-estimated lateral positions of each of the other targets was within 2-3 mm of the actual lateral positions of each respective target.
TABLE 1
Target
Known Position
OPTICA Estimated
Target
Strength
(x, y, z) (mm)
Position (x, y, z) (mm)
#1
4
(60, 60, 27.5)
(62, 63, 28.13)
#2
2
(47, 30, 27.5)
(48, 33, 27.87)
#3
1.5
(33, 60, 27.5)
(33, 62, 27.08)
#4
1.1
(20, 30, 27.5)
(18, 33, 32.6)
Independent intensity distributions at the detector plane and the source plane obtained by ICA for the third specimen 3 is shown in FIG. 6 . The fluorescent target is found to be z=33 mm away from the input window by fitting independent intensity distributions at the detector plane and the source plane to the respective Green's functions (e.g., see diagrams (a) and (b) of FIG. 7 ). This agrees with the input value z=32 mm away from the input window. The thickness map is obtained using Equation 19 and presented in diagram (c) of FIG. 7 while the horizontal and vertical thickness profile of Δ z /Z max are also plotted in diagram (d) of FIG. 7 . The target is found to be centered at (x=11, z=9) mm and have a circular shape. The FWHM of the peak found to be d=11.5 mm. This value should be compared to the diameter of the fluorophore 9 mm.
The fluorescent target in the fourth sample is found to be z=11 mm away from the input window by fitting independent intensity distributions at the detector plane and the source plane to the respective Green's functions (see diagrams (a) and (b) of FIG. 8 ). This agrees well with the input value z˜10 mm away from the input window. The thickness map is obtained using Equation 19 and presented in diagram (c) of FIG. 8 while the horizontal and vertical thickness profile of Δ z / zmax are also plotted in diagram (d) of FIG. 8 . The target is found to be centered at (21, 33) mm and have a circular shape. The FWHM of the peak is found to be d=7.1 mm. This value should be compared to the diameter of the fluorophore 4 mm.
The experimental results demonstrate that the present invention using OPTICA, can successfully detect and obtain the location of absorbing, scattering, and/or fluorescent targets embedded inside a turbid medium. 4 mm targets located deep within a thick human breast tissue have been shown to be successfully located within an error of several millimeters and characterized in experiments. Accordingly, the present invention using OPTICA can be used to detect and obtain the location of absorbing, scattering, and/or fluorescent targets of 1 mm size embedded inside a turbid medium.
Graphs illustrating normalized independent spatial intensity distributions as a function of the lateral position x at the input (or source) plane (first row) and the exit (or detector) plane (the second row) generated by ICA and a horizontal profile of intensity distributions on the source plane (illustrating diamonds) and on the detector plane (illustrating using circles) are displayed on the third row for the two absorbing cylinders of the first specimen is shown in diagrams (a)-(f) of FIG. 4 . Solid lines illustrate the respective Green's function fit used for obtaining locations of objects.
Graphs illustrating independent spatial intensity distributions at the exit (or detector) plane generated by ICA corresponding to objects with scattering coefficients: (a) 4 times, (b) 2 times, (c) 1.5 times, and (d) 1.1 times of that of the material of the slab in the second specimen are shown in diagrams (a)-(h) of FIG. 5 . Horizontal profiles of intensity distributions shown in diagrams (a)-(d) of FIG. 5 are illustrated by circles in diagrams (e) and (f) of FIG. 5 , respectively, with solid lines representing the Green's function fit used for extracting object locations.
Graphs illustrating independent intensity distributions of the fluorescence from the target generated by ICA at the detector plane and the source plane, are illustrated in diagrams (a)-(b) of FIG. 6 , respectively.
Graphs illustrating fitting of the independent intensity distribution of fluorescence from a sphere of diameter 9 mm embedded in Intralipid-10% solution to the model Green's function are shown in diagrams (a)-(c) of FIG. 7 . The independent intensity distribution of fluorescence from a sphere of diameter 9 mm embedded in Intralipid-10% solution to the model Green's function are at the detector plane and at the source plane are illustrated in diagrams (a) and (b) of FIG. 7 , respectively. The thickness map of the target centered at (11, 9) mm and the thickness profiles along X and Y directions, are illustrated in diagrams (c) and (d) of FIG. 7 , respectively.
Graphs illustrating fitting of the independent intensity distribution of fluorescence from a sphere of diameter 4 mm embedded in human breast tissue to the model Green's function is illustrated in diagrams (a)-(c) of FIG. 8 . The independent intensity distribution of fluorescence from a sphere of diameter 4 mm embedded in human breast tissue to the model Green's function at the detector plane and at the source plane, are illustrated in diagrams (a) and (b) of FIG. 8 , respectively. A thickness map of the target centered at (21, 33) mm, and a thickness profiles along X and Y directions, are shown in diagrams (c) and (d) of FIG. 8 , respectively.
FIG. 9 is a block diagram illustrating a control system for controlling the experimental arrangement shown in FIG. 1 according to an embodiment of the present invention. The system 900 includes a controller 930 , a CCD control unit 940 , a CCD camera 950 , an display unit 960 , an input/output device 970 , an optical control unit 980 , a light source unit 990 , an source control unit 922 , and a memory unit (e.g., RAM, ROM, FLASH, etc.) 920 . The controller 930 controls the overall operation of the system 900 and stores data and retrieves necessary data (e.g., operating instructions, data generated during use, etc.) in the memory unit 920 . The CCD control unit 940 interacts with the controller 930 and controls the operation of the CCD camera 950 . The display 960 receives data from the controller (and/or other device such as a CCD camera, etc.) and displays the data. The input/output unit 970 can include a mouse, a keyboard, a touch-screen, etc. (not shown) for entering commands from a user, and other devices (e.g., a network connection for communicating with a LAN/WAN, the Internet, etc., and an optional external memory) for controlling the operation of the system 900 . The optical control unit 980 is controls the location of incident light relative to a source plane. For example, optical control unit 980 can be used to focus and/or locate incoming (incident) light as desired using lenses and mirrors, respectively, which are controlled by stepper motors, etc. The source control unit 922 is operated by the controller 930 and controls the light source 990 . The light source 990 can include a laser or other suitable device for producing a desired incident beam and can preferably produce an incident beam having a given wavelength and duration. The controller 930 (and/or other devices shown in FIG. 9 can be included within a Personal Computer (PC) 190 shown in FIG. 1 . In other embodiments, optical sources and detectors can be remotely located and operated by one or more controllers. In yet other embodiments, a plurality of light sources (e.g., a plurality of light-emitting-diode (LED) lasers can be used in which case the source an optical control system for locating an incident beam may not be necessary.
FIG. 10 is a flow chart illustrating the operation of an embodiment of the present invention for locating a target location. In Step 1000 a sample is illuminated by the light source. In Step 1020 , a camera (e.g., a CCD camera) captures an image of the illuminated sample. In Step 1030 resulting special diversity and multiple angle observations are obtained. In Step 1040 a target located within the sample is located and characterized using a comparison to a prototype Greens function. In Step 1050 generated data is displayed on a display.
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
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Disclosed is a system and a method for detecting the presence of one or more objects in a turbid medium, the method including: illuminating at least a portion of the turbid medium with incident light having at least one wavelength which interacts with the one or more objects contained in the turbid medium differently than the incident light interacts with the turbid medium; measuring light that emerges from the turbid medium; and detecting and locating the one or more objects using Independent Component Analysis (ICA) of the emergent light from the turbid medium. The present invention is useful for medical applications, such as for finding and locating, a tumor(s) in body organs, or excised tissues. Moreover, the present invention can be used to locate objects in obscuring medium, such as, mines in shallow coastal water, a plane in fog, military targets under fog, smoke or cloud cover.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims priority to jointly owned U.S. Provisional Application corresponding to application No. 61/186,190 entitled, “Laser Diode Driver Current Input Signal Processing System.” This provisional application was filed on Jun. 11, 2009. The present application also claims priority to jointly owned U.S. Provisional Application corresponding to application No. 61/186,226 entitled, “Over Current Protection Device.” This provisional application was filed on Jun. 11, 2009.
DESCRIPTION OF RELATED ART
[0002] With the evolution of electronic devices, there is a continual demand for enhanced speed, capacity and efficiency in various areas including electronic data storage. Motivators for this evolution may be the increasing interest in video (e.g., movies, family videos), audio (e.g., songs, books), and images (e.g., pictures). Optical disk drives have emerged as one viable solution for supplying removable high capacity storage. When these cloves include light sources, signals sent to these sources should be properly processed to reduce potential damage and maintain appropriate light emission.
BRIEF DESCRIPTION OF THE DRAWINGS
[0003] The input signal processing system may be better understood with reference to the following figures. The components within the figures are not necessarily to scale, emphasis instead being placed upon clearly illustrating the principles of the invention. Moreover, in the figures, like reference numerals designate corresponding parts or blocks throughout the different views.
[0004] FIG. 1A , is a system drawing illustrating components within an optical disk drive.
[0005] FIG. 1B is an enlarged view of the innovative laser driver, which may be a laser diode drive (MD).
[0006] FIG. 2 is a graph illustrating an output waveform for the laser diode driver of FIG. 1B .
[0007] FIG. 3 is a circuit diagram illustrating for the ISPS of FIG. 2 that includes an input stage, low pass filter (LPF) stage, and an output stage 350 .
[0008] FIG. 4 is a circuit diagram for one implementation of the input stage of FIG. 3 .
[0009] FIG. 5 is a circuit diagram for one implementation of the transconductance device of FIG. 3 .
[0010] FIG. 6 is a circuit diagram for one implementation of the output stage of FIG. 3 .
[0011] While the input signal processing system is susceptible to various modifications and alternative forms, specific embodiments have been shown by way of example in the drawings and subsequently are described in detail. It should be understood, however, that the description herein of specific embodiments is not intended to limit the input signal processing system to the particular forms disclosed. In contrast, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the input signal processing system as defined by this document.
DETAILED DESCRIPTION OF EMBODIMENTS
[0012] As used in the specification and the appended claim(s), the singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise. Similarly, “optional” or “optionally” means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event or circumstance occurs and instances where it does not.
[0013] Turning now to FIG. 1A , is a system drawing illustrating components within an optical disk drive 100 . A controller 102 monitors the output light power level of a laser diode 115 using a Monitor PD 104 , or monitor photodiode, and an RF, or radio frequency, preamplifier 106 . This controller can keep an expected power level by changing an input control current of a laser driver 110 through an APC, or auto power controlling, feedback loop, even if a light source 115 such as a laser diode, has many changes of the output power due to various condition changes, such as temperature etc.
[0014] Also, the controller 102 sets the enable signal for switching some current channels of the laser driver 110 , which arranges a data writing pulse. In die case of data reading, the controller 102 may only set the DC current by disabling the switching and applying the indicated input current. In the case of data writing, the controller 102 applies some adjustment signals, or enable-switching signals, to arrange the writing pulse waveform as a combination of switching timing, which also changes the power level by different indicated current of each channel. The controller 102 can arrange these indicated currents based on the Monitor PD 104 output with some detecting function in the RF preamplifier 106 . At the very least, this controller has two controlling levels for the reading power and the writing power. Sometimes the controller may get the top, bottom, or average level of a writing pulse and calculate to control some power levels independently.
[0015] As illustrated in this figure, the laser driver 110 sends a signal that prompts an associated light source 115 (e.g., laser diode) to emit light. The light source 115 may emit light at any of a number of wavelengths (e.g., 400 nm, 650 nm, 780 nm). Light from this source contacts an associated optical media 117 , such as a compact disc (CD), blue ray device (Blu-ray), or digital versatile disk (DVD). Light contacting the optical media can either facilitate data storage or data retrieval from the optical media 117 .
[0016] FIG. 1B is an enlarged view of the innovative laser driver 110 , which may be a laser diode drive (LDD). The LDD 110 is an integrated, fully programmable, multi-function product that controls and drives laser diodes (e.g., light source 115 ) within optical drives as described with reference to FIG. 1A . More specifically, the LDD 110 can apply the current for the read, write, and erase removable high capacity disks capacities greater than approximately 50 Gbytes/disk). The LDD 110 also has low noise (e.g., noise of approximately 0.5 nA/rt-Hz), high speed (e.g., 1 Gb/S, 0.850 Gb/s) and high current (e.g., approximately 1 amp). Any numbers included in this application are for illustrative purposes only and numerous alternative implementations may result from selecting different quantitative values.
[0017] At a high level, the LDD 110 may include a current generator 120 . Generally, the current generator 120 receives some input signals 123 associated with several input channels, which have an associated input current. This current generator 120 works in tandem with a current driver 141 ) and produces a gain for the input current. As a result, the current generator 120 and current driver 140 control the amount of current for each output channel 145 . For the input signals that the current generator 120 receives, it transmits output signals that a current switch 130 receives. The current switch 130 decides which of the input channels should be turned on or turned off. For the channels that should be turned on, the current switch 130 makes those channels active. Similarly, the current switch 130 inactivates the channels that should be turned off and transmits output signals reflecting this change. The current driver 140 receives these output signals from the current switch 130 as input signals. The current driver 140 is the last current gain stage and drives the laser diode directly. In other words, the output signals from the current driver 140 also serve as output signals for the LDD 110 , which are used in driving the lasers, or the light source 115 (see FIG. 1A ).
[0018] In addition to the above-mentioned devices, the LDD 110 includes additional components. A serial interface (I/F) 150 has several inputs 155 (e.g., serial data enable, serial data, serial clock) that may be used for an enable, feature selection, or setting the gain. Like the serial interface 150 , the timing generator 160 receives various channel enable inputs 165 . Though there are five channel enable inputs that are shown in FIG. 1B , the LDD 110 may have any number of channel enable inputs, such as two, six, or the like. The timing generator 160 determines the time at which a given input channel will be either turned on or turned off. The LDD 110 also includes a high frequency modulator (HFM) 170 and voltage/temperature monitor (V/Temp Monitor) 180 . The HFM 170 modulates the output current for reducing mode-hopping noise of the laser diodes. The voltage/temperature monitor 190 monitors the laser diode voltage drop and on-chip temperature. One skilled in the art will appreciate that numerous alternative implementations may result from removing any or several of the blocks within the LDD 110 .
[0019] A laser diode driver (LDD) 110 in an optical pick up applications can generate an output signal 200 as shown in FIG. 2 . For this signal, there are four current levels in this case: write power level 210 , erase power level 220 , biasing power level 230 and a cooling/read power level 240 . Each level may come from either the output of one channel or the combination of the outputs of several channels, like the output channels 145 (see FIG. 1A ). Depending on the applications, sometimes there may be even more power levels that the LDD 110 generates. The input current to each input channel in applications, input channels 123 (see FIG. 1A ) may be limited to a few milliamps (e.g., approximately 2 mA) and the total input current may vary from approximately 0 mA to approximately 4 mA.
[0020] As illustrated in FIG. 1B , the current generator 120 includes an overprotection device 125 and a laser diode driver input signal processing system (ISPS) 127 used with input current signal received on input channels 123 . Transmitting a high current output signal directly to a laser diode can easily destroy this device. The LDD 110 protects an associated laser diode by including an over current protection device (OCPD) 125 within the current generator 120 . The OCPD 125 closely monitors the input current associated with the input signal. When the input current exceeds a predetermined limit level, this OCPD can either shut down all of the input channels or switch the over-current channel's output to the predetermined limit level.
[0021] FIG. 3 is a circuit diagram 300 for the ISPS 127 that includes an input stage 310 , low pass filter (LPF) stage 330 , and an output stage 350 . Numerous implementations may result by varying the types and number of devices included within each stage. An alternative implementation may not include all three stages. For example, one implementation may include simply the input stage 310 and the LPF stage 330 .
[0022] As shown in FIG. 3 , the input current associated with an input current signal that enters the input stage 310 will first be sinked by a resistor 301 (R in ) to be converted to a voltage V 1 associated with a voltage signal. The capacitor 302 (C in ) provides limited filtering function for very high frequency noise and smoothes out the input voltage to the transconducting device 304 (Gm 1 ). This voltage V 1 may be used for over-current protection detection with threshold level trimmable depending on the application. In other words, this voltage may be used with the over current protection device 125 . If the incoming current is larger than a certain pre-set threshold value, this device will either limit the current to the threshold level or essentially shut down the driver. Coupling noise from an actuator (e.g., a servo chip's track actuator) will be filtered out by an on-chip LPF with corner frequency adjustable from approximately 3 KHz to approximately 675 KHz that is described with reference to the LPF stage 330 . In order to filter out this coupling noise, the voltage V 1 is converted to a current signal through the transconducting device 304 (Gm 1 ), active device 306 (MN 1 ), active device 307 (Q 1 ), passive device 308 (R 1 ), and a capacitor 309 (CM 1 ). Therefore, the LPF stage 330 receives a second voltage signal corresponding to the voltage V 2 . The values associated with these devices may vary. For example, R 1 may have a resistance of approximately 2 KOhms, CM 1 may have a capacitance of approximately 3 pF, device MN 1 may have a threshold voltage of approximately 0.7V, while device Q 1 may have a threshold voltage of approximately 0.7V.
[0023] The input stage 310 shown in FIG. 3 is merely one of many possible implementations. An alternative implementation may result by removing the capacitor 302 , capacitor 309 , or both the capacitor 302 and the capacitor 309 . In addition, another implementation may occur by replacing the bipolar active device 307 with other type of devices such as a Metal-Oxide-Silicon (MOS) device, resistor, or the like. Yet, another implementation may occur by replacing MOS active device 306 with other type of devices, such as a bipolar active device. Another implementation may occur by using any one of several types of circuits for over-current protection. In other words, the over current protection device 125 may include a plurality of input channels for receiving an input signal; a plurality of low pass filters coupled to a first group of the plurality of input channels, wherein each low pass filter is associated with one input channel within the first group of input channels, the plurality of low pass filters operative for removing spikes in associated with the input signal; and a plurality of digital to analog converters coupled to a second group of the plurality of input channels, wherein each digital to analog converter is associated with one low pass filter in the second group of input channels, the digital to analog converters operative for triggering over current protection when a signal received from the associated low pass filter is beyond a preset level, wherein the over current protection device is on chip with the laser diode driver.
[0024] FIG. 4 is a circuit diagram 400 for one implementation of the input stage 310 described with reference to FIG. 3 . As mentioned above, similar devices have the same reference numerals. In this implementation, the passive device 401 is shown as two resistors in parallel, which may have resistances of approximately 1 KOhms. There is also a passive device 408 shown as a four resistors in series, though the numer of resistors in series may be 2, 3, 6 or the like. In addition, the resistances of these devices may range from approximately 1 KOhms to approximately 10 KOhms. The circuit diagram 400 may also include an inverter 420 , active device 422 , and active device 424 . Together, inverter 420 and active device 422 serve as pullup devices to save power in sleep mode. In an alternative implemenatio, the active device 424 may not be included. When it is, it can help in some cases to reduce the voltage headroom at the drain of MN 1 device and also serve as current mirror input devices to ship out the current through MN 1 /Q 1 /R 1 devices if needed.
[0025] The transconducting device 404 may have many implementations by varying the devices that make of this device. Turning now to FIG. 5 , this is a circuit diagram 500 for one implementation the transconducting device 404 . In this implementation there are four active devices 502 - 505 (Q 2 ˜Q 5 ) function as emitter followers to shift up the input voltage level by approximately 1.5 V. The circuit diagram 500 also includes an input differential pair made up of active devices 510 - 511 (Q 0 -Q 1 ) are the input differential pair. The passive devices 520 - 521 (R 0 -R 1 ) associated with the differential pair assist with degeneration that lowers gain and improves matching between active device 510 (Q 0 ) and active device 511 (Q 1 ). Finally, the circuit diagram 500 includes a current mirror formed by two active devices 530 - 531 (MN 0 -MN 1 ) that connect to a second gain stage formed by 540 (MP 0 ). An alternative implementation may result from including other devices in the second gain stage.
[0026] Returning to the LPF stage 330 shown in FIG. 3 , the voltage V 1 gets converted to a noisy, current signal. The LPF stage 330 substantially reduces the noise and produces a reduced noise voltage signal. In this implementation, die LPF stage 330 includes a LPF 335 with a corner frequency trimmable from approximately 3 KHz to approximately 675 KHz. In an alternative implementation, the LPF stage 330 may include more than one LPF. The reduced noise voltage signal V 3 biases the active device 352 (MN 2 ), active device 353 (Q 2 ), and the passive device 354 (R 2 ). In one implementation, the characteristics of these devices may be selected so that they are proportional to, or match, the devices 306 - 307 . Using the LPF stage 330 produces an essentially noiseless current signal for the output stage at the drain of the active device 332 (MN 2 ).
[0027] The output stage 350 includes additional components that improve accuracy and stability. More specifically, this output stage includes a current mirror formed from active devices 356 - 357 . The transconducting device 358 (Gm 2 ) reduces the voltage headroom requirements on active devices 356 - 357 , or the voltage drop from source to drain of active devices 356 - 357 and improves the current mirror's accuracy. An active device 359 (CM 2 ) is a miller compensation capacitor that enhances the stability of the feedback loop around the transconducting device 358 (Gm 2 ). An alternative implementation may not include this miller compensation capacitor. Like this output stage, the input stage 310 also includes a miller compensation capacitor, or active device 309 (CM 1 ); it enhances the stability of the feedback loop around the transconducting device (Gm 1 ). In another alternative implementation of the output stage 350 , the output current from the drain of active device 357 (MP 2 ) may be further processed via a scaler, digital to analog converter (DAC), and an output driver, or the like. Alternatively, the over-current protection device 125 can also be placed after LPF, which means the current will be stable without much noise.
[0028] FIG. 6 is a circuit diagram 600 for an implementation of the output stage 350 of FIG. 3 . In this implementation, the passive device 610 (R 0 ) connects to the miller miller compensation capacitor and improves stability. Active device 613 (MP 3 ) through active device 616 (MP 6 ) provide a gate bias voltage for output current passing transistor MP 0 , or active device 620 , at the drain of active device 357 (MP 2 ). Active device 620 limits the positive feedback loop's gain to less than that of the negative feedback loop's gain, which enhances stability. An alternative implementation may result from removing either one of the miller capacitors that generally stabilize the associated feedback loop or from changing the transistor types. Even still, another implementation may result from using a low voltage compliance, but high precision current mirror in lieu of the active devices 356 - 357 that is configured differently.
[0029] While various embodiments of the signal processing system have been described, it may be apparent to those of ordinary skill in the art that many more embodiments and implementations are possible that are within the scope of this system. Although certain aspects of the input signal processing system may be described in relation to specific techniques or structures, the teachings and principles of the present system are not limited solely to such examples. All such Modifications are intended to be included within the scope of this disclosure and the present input signal processing system and protected by the following claim(s).
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An input signal processing system is described. It comprises a first transconductance device having a first input, second input, and an output, wherein the first input is coupled to receive the input signal; a first resistor coupled to a first input of the first transconductance device, wherein the first resistor converts the input current signal to an input voltage signal; a first voltage-current converter coupled to the output, the second input, the resistor, and a low voltage supply, wherein the first voltage-current converter is operative for converting the input voltage signal to a input current signal; and a low pass filter having an input coupled to the voltage converter for filtering noise from the input current signal.
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This application is a continuation of application Ser. No. 08/242/015, filed May 12, 1994, now abandoned, which is a continuation-in-part of U.S. application Ser. No. 08/087,171, filed Jul. 2, 1993, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to manhole cover support inserts or grate support inserts for placing over and raising the effective grade of an existing manhole cover or grate receiving structure, and more particularly, to anchors for anchoring manhole cover support inserts or grate support inserts to manhole cover or grate receiving structures.
2. Description of the Related Art
Ordinarily, a manhole cover support insert or grate support insert is used when a roadway is resurfaced with an added layer of paving material. A support insert raises the level of the manhole cover or grate to the new street level. Support inserts typically occupy a seat where a manhole cover or grate was intended to rest in a utility access frame. Support inserts are available in a wide variety of shapes and sizes to accommodate the wide variety of utility access openings. Some support inserts are formed by a plurality of connectable segments, while others are of fixed dimension construction for length and width. Frequently, support inserts are anchored to the receiving structure, which is a utility access frame or manhole frame. A typical prior art anchor is simply a strap of metal which is bolted to a threaded hole in the support insert at its upper end. The lower end is angled to reach beneath a rim or flange which is formed in the utility access frame. A bolt which is threaded through the lower end of this strap contacts the underside of the rim to tighten the anchor. In other words, when the bolt is rotated, the strap is tensioned to secure the support insert to the utility access frame. A worker must hold the strap in position with one hand and thread the upper screw into the support insert with the other. Once the upper end of the strap is secured, the worker must reach inside the utility access frame opening to tension the strap by tightening a downward-facing bolt against the frame.
Another anchor device was developed by the present inventor and disclosed in U.S. patent application Ser. No. 07/986,980 titled Anchor for Manhole Cover Support filed on Dec. 8, 1992. In this development, a strap is connected to the support insert with a dovetail connection permitting the anchor to be dropped into place. A bolt is located at the opposite end of the strap for engaging the utility access frame and for tensioning the strap. A worker must reach inside the utility access hole and below street level to tighten the anchor bolt. The head of the tensioning bolt faces in a downward direction and is difficult to see and reach.
Oftentimes, parts and tools are dropped and lost due to the difficulty of installing support insert anchoring straps. There is a need for a simple, speedy positive means of connecting the anchor straps with the support insert to simplify and speed up installation and reduce the frequency of dropping parts.
SUMMARY OF THE INVENTION
Basically, the invention is an apparatus for securing a support insert to a rim of a utility access frame opening. The apparatus includes a rotatable locking member having a threaded portion, a toe portion for engaging said rim and a stop member opposite the toe portion. The apparatus includes a lock housing connected to and projecting inwardly and downwardly of the support insert. The housing has an opening for receiving the threaded portion of the lock member and for receiving a threaded shaft which is adapted to be threaded to the threaded portion. The housing also has a stop surface for engaging the stop member to stop rotation of the locking member at a predetermined position. The locking member is connected to the housing by the threaded shaft. The shaft has a head portion for permitting the shaft to be rotated. Rotation of the head portion and the shaft causes the locking member to rotate until the toe portion extends outside the perimeter of the utility access opening (as defined by the rim) to a stopping point. At the stopping point, the stop member engages the stop surface and further rotation of the shaft causes tension in the shaft thereby driving the locking member toward the rim to damp the insert to the frame.
In the preferred and illustrated embodiments the threaded shaft is the shaft of a threaded bolt and the head portion is the head of the bolt and the head of the bolt is located substantially near the rim of the utility access frame.
In the preferred and illustrated embodiments, a spring member is located between the head portion and the housing.
In the preferred and illustrated embodiments, nylon material is provided between the threads of the threaded shaft and the threaded portion of the locking member to create a resistance to rotation between the shaft and the threaded portion.
In one preferred embodiment, the locking apparatus is an integral part of a casting of a segment of a support insert.
In another preferred embodiment, the locking apparatus is a unit which is adapted to be welded to an inner surface of a support insert.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred embodiment of the invention is shown in the accompanying drawings in which:
FIG. 1 is a top plan view of a manhole cover support insert and an anchoring system;
FIG. 2 is a cross-sectional view as seen approximately from the plane indicated by the line 2--2 in FIG. 1;
FIG. 3 is a partial bottom plan view of a single anchoring device;
FIG. 4 is a partial cross sectional view as seen approximately from the plane as indicated by the line 4--4 of FIG. 3;
FIG. 5 is a partial cross sectional view as seen approximately from the plane indicated by the line 5--5 of FIG. 1;
FIG. 6 is a top fragmentary, plan view of an adjustable and a fixed grate support insert including the anchoring system;
FIG. 7 is a cross sectional view as seen approximately from the plane indicated by the line 7--7 of FIG. 6;
FIG. 8A is a side elevational view of an assembly including a locking member and a bolt with part of the locking member cut away;
FIG. 8B is a cross sectional view of the assembly of FIG. 8A as seen approximately from the plane indicated by the line 8B--8B of FIG. 8A;
FIG. 9 is a top plan view of an alternative embodiment showing a unitary member;
FIG. 10 is an elevational view of the member of FIG. 9 as seen approximately from the plane indicated by the line 10--10 of FIG. 9;
FIG. 11 is a side elevational view of the lock housing of FIG. 8 as seen approximately from the plane indicated by the line 11--11 of FIG. 10;
FIG. 12 is a bottom plan view of the lock housing of FIG. 8 as seen approximately from the plane indicated by line 12--12 of FIG. 10;
FIG. 13 is a top plan view of another lock housing embodiment;
FIG. 14 is a side elevational view of the lock housing of FIG. 13 as seen approximately from the plane indicated by the line 14--14 of FIG. 13;
FIG. 15 is a front elevational view of the lock housing of FIG. 13 as seen approximately from the plane indicated by the line 15--15 of FIG. 13; and
FIG. 16 is a bottom plan view of the lock housing of FIG. 13 as seen approximately from the plane indicated by the line 16--16 of FIG. 15.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1 and 2, a segmented manhole cover support insert 10 is shown. The cover support insert 10 has an upper annular cover seat 12 which receives a manhole cover (not shown). The annular seat 12 is connected to a segmented base member 14. The diameter of the base member 14 may be adjusted with turnbuckles 16 which join the segments of the base member 14. The base member 14 and the annular seat 12 are joined by the interconnection of dovetail members 18 formed in their confronting surfaces. The base member 14 engages a utility access frame or manhole frame 19 as shown in FIG. 2.
Referring to FIGS. 3-5, integrally formed on each segment of the base member 14 is a locking device 20. Each locking device 20 includes a housing 22 projecting from the base member 14. A vertical bore 23 is formed in each housing 22. A threaded bolt 24 is fitted into each bore with sufficient clearance to permit the bolt 24 to rotate. A recess 25 is formed at the top of each housing 22 to accommodate the heads of the bolts 24. A lock washer or Belleville-type spring disk 26 is placed between the head of the bolt 24 and the bottom of the recess 25 to resist loosening of the bolt 24 once it is tightened. To the end of each bolt 24 is threaded a locking member 28. The top of each housing 22 is low enough on the insert 10 to avoid interference with a manhole cover.
Each locking member 28 has a threaded portion 29 and a toe member 30 extending radially outward from the sleeve 29. The sleeve has a threaded bore sized to fit the threaded shaft of the bolt 24. A projection 32 extends from the locking member 28 opposite to the toe member 30. The toe member 30 is shaped to engage and cooperate with a rim 34 formed about a utility access openings or manhole 36 as seen in FIG. 2.
Each housing 22 includes an opening 29 coaxial with the bore 23 for receiving the threaded shaft of one of the bolts 24 and a portion of one of the locking members 28. The projection 32 of the locking member 28 is arranged to engage a stop surface 38 which is the edge of a slot 39 extending vertically through the wall of the housing 22 as best seen in FIGS. 2, 4 and 5. The housings 22 not only provide stop surfaces for the locking members 28, but also serve to protect the threads of the bolts 24 and the locking members 28 themselves from damage caused by pry bars and other tools used around manholes. The housing 22 also includes a second stop surface 31 for stopping the clockwise rotation of the locking member 28 (as viewed in FIG. 3) in a neutral position. When the lock members 28 are in their neutral position as seen in broken lines in FIG. 3, the insert 10 may be placed inside the manhole frame 19 without interference.
Referring to FIGS. 8A and 8B, a patch of nylon material 33 is applied to the threaded portion of each bolt 24 to increase the friction between the bolt threads and the locking member 28. The nylon material 33, which is commercially available from a company called ND Industries, is preferably sprayed on the bolt threads as a liquid which later dries to a solid. The nylon material 33 helps ensure that rotation of the bolt 24 will rotate the locking member 28 until it is in the proper position to be tightened against the rim 34. Too little friction between these parts could result in the tightening of the locking members 28 before they are outwardly rotated beneath the rim 34.
If a locking member 28 is in its inner neutral position, which is inside the perimeter of the access hole 36 as shown in broken lines in FIG. 3, rotation of the bolt 24 in a counterclockwise direction (as viewed in the direction of FIG. 3) will cause the me member 28 to rotate counterclockwise into its outer locking position where the toe portion 30 extends outside the perimeter of the access hole 36 (as seen in solid lines in FIG. 3). The rotation of the locking member 28 will stop when the projection 32 engages the stop member 38. Further rotation of the bolt 24 will cause the locking member 28 to move axially along the bolt 24 due to the relative motion of the threads formed on the outside of the bolt 24 and the inside of the sleeve 29. Tightening of the bolt 24 eventually causes the toe member 30 to engage the lower surface of the rim 34 which locks the support insert 10 to the frame 19. Rotation of the bolt 24 in the opposite direction when the cover support insert 10 is locked to the frame 19 causes the locking member 28 to move downward until it is free from the rim 34. Without the frictional drag of engagement with the rim 34, the locking member 28 will rotate inward (clockwise as viewed in FIG. 3) until it has again reached the neutral position inside the perimeter of the manhole 36 as shown in FIG. 3 in broken lines.
To install the manhole cover support insert 10, the locking members 28 are first rotated inward to the broken-line position of FIG. 3. Then, the cover support insert 10 is aligned with the manhole 36 and rested on the frame 19 such that the base 14 engages the edges of the access hole 36 as shown in FIG. 2. Then, a worker rotates the heads of the bolts 24 clockwise (as viewed in FIG. 1) to move the locking members 28 into locking position. The bolts 24 are further rotated to raise each locking member 28 into engagement with the underside of the rim 34 and to compress each Belleville spring 26. The rotation of the bolts 24 is done with full visibility of the head of the bolts 24 and without having to reach inside the utility access hole.
In another preferred embodiment shown in FIGS. 6-15, an adjustable insert 40 for raising the grade of a rectangular grating (not shown) that resides in a catch basin frame 42 or in a similar utility access frame includes a similar locking arrangement. The insert 40 is similar to that disclosed in U.S. Pat. No. 5,039,248 titled Support for Catch Basin Cover, which is incorporated herein by reference.
As shown best in FIG. 7, the catch basin frame 42 is anchored by material P from which the roadway is constructed, i.e., concrete, asphalt, etc. A typical catch basin frame 42 that is installed during initial construction of the roadway, includes an outwardly extending radial flange 42a and an upwardly extending vertical wall 42b. Extending radially inwardly from the vertical wall 42b is a ledge 42c which defines a seating or rim support surface 43 upon which the original grade cover (not shown) sits. An end wall 45 defines the access opening for the catch basin. The original catch basin frame may include gussets 47 for providing added structural strength or rigidity.
When a roadway is resurfaced, a layer of additional paving material P' is laid atop the original roadway. As a result, the overall level or grade of the roadway is raised. In order for the original catch basin cover (not shown) to be flush with the new roadway level, either a new catch basin frame must be installed or the searing or rim support surface for the catch basin frame must be raised.
The insert 40 illustrated in FIGS. 6 and 7 provides a means for effectively raising the seat for the original catch basin cover. As seen best in FIG. 6, the insert 40 includes interconnected side bars 50 and end bars 52. Referring also to FIG. 7, extending upwardly from the side bars and end bars are thin walled keepers 50a, 52b.
Extending radially outwardly from an upper part of the thin wall keepers 50a, 52a are respective reinforcing sections 50b, 52i which, for purposes of explanation are termed "wales". For an in depth discussion of the purposes and advantages of using wales as part of thin wall keepers, reference should be made to reissue Patent No. RE 34,550 which is hereby incorporated by reference.
The outside of the keeper walls which extend above the original roadway material P, are contained and supported by the new roadway material P'. With the disclosed insert, the original catch basin frame need not be modified or re-worked and the original catch basin cover may be utilized to cap the opening after the new roadway is completed.
In the preferred and illustrated embodiment, the insert 40 includes locking apparatus similar to that described above to mount and lock the insert to the ledge 42c of the original catch basin cover. Specifically, a housing 46 of a locking apparatus like that described in connection with FIGS. 1-5 is integrally cast into corner members 48 which, are welded to the side bars 50 and/or end bars 52 to form the insert 40.
Additionally, lock housings 54 are designed to be integrally cast into unitary members 56, which are adapted to be welded to the inside surfaces of the side bars 50 forming the insert 40. Each corner member 48 has an L-shaped portion 65 for receiving a squared end of a bar 52. Each bar 52 is welded to the L-shaped portion 65 as shown in FIG. 6. Each unitary member 56 has a flat surface 67 for abutting against the side bars 50 and for forming a welded connection with one of the bars 50 as shown in FIG. 6. The unitary members 56 are positioned at a predetermined location on the bars 52 such that the top of the housing 54 will not interfere with a grate or cover (not shown) resting on the insert 40.
Both the lock housing 46 of the corner members 48 and the lock housing 54 of the unitary members 56 are adapted to receive the bolt 24, spring 26, and locking member 28 described above to form locking assemblies for locking the insert 40 to the frame 42. The housings 46, 54 of the corner and unitary members 48, 56 are essentially the same as the housing 22 previously described. The housing 46 includes a stop surface 58, a recess 60, an opening 62, and a bore 64. Similarly, the housing 54 includes a stop surface 66, a recess 68, an opening 70 and a bore 72. Though not illustrated, a lock housing may also be integrally cast into an end support 74.
A portion of FIG. 6 illustrates another slightly modified embodiment of the invention. The upper right corner of the insert shown in FIG. 6 illustrates a non-adjustable version 40' of the insert. In this embodiment, fixed non-adjustable corner members 48' are used. The corner member 48' is welded to both the side bars 50 and the end bars 52. The lock housing 46' and associated components, however, are substantially identical to the components shown in FIGS. 8-15 and described above.
While preferred embodiments of this invention have been described in detail, it will be apparent that certain modifications or alterations can be made without departing from the spirit and scope of the invention set forth in the appended claims.
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A locking device for securing a manhole cover support insert or a grate cover support insert to a utility access frame is disclosed. The locking device includes a plurality of rotatable locking members which are connected to the support insert. The locking members are rotatable between a position where they rest inside the perimeter of the utility access hole and a locking position outside the perimeter of the utility access hole. The locking members may be rotated from an easy to reach position above the utility access hole by turning the exposed head of a bolt. The locking members are stopped from rotating at their locking position by engagement with a stop. From their locking position, the locking members may be axially moved by further rotation of the bolt to lock the support to the frame.
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BACKGROUND
[0001] 1. Technical Field
[0002] The disclosure generally relates to key structures, and more particularly relates, to a key structure used in an electronic device.
[0003] 2. Description of the Related Art
[0004] Different kinds of keys are generally assembled to circuit boards of mobile phones, personal digital assistants (PDAs), or other electronic devices by surface mount technology (SMT) or other welding method. However, mounting the keys on the circuit board may increase overall thickness of the electronic devices.
[0005] In addition, the SMT assembly process is complicated and requires such high processing precision, that even minor errors may result in defective products. Moreover, during the SMT process, the welding materials used may release gases.
[0006] Therefore, there is room for improvement within the art.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] Many aspects of a key structure and an electronic device employing the same can be better understood with reference to the following drawings. The components in the drawings are not necessarily drawn to scale, the emphasis instead being placed upon clearly illustrating the principles of the exemplary key structure and electronic device employing the same. Moreover, in the drawings, like reference numerals designate corresponding parts throughout the several views. Wherever possible, the same reference numbers are used throughout the drawings to refer to the same or like elements of an embodiment.
[0008] FIG. 1 is an exploded view of a key structure, according to an exemplary embodiment.
[0009] FIG. 2 is similar to FIG. 1 but viewed from the other aspect.
[0010] FIG. 3 is an enlarged view of a key body of the key structure shown in FIG. 2 .
[0011] FIG. 4 is an assembled view of the key structure shown in FIG. 1 .
[0012] FIG. 5 is an assembled cross-sectional view taken along line V-V of FIG. 4 .
[0013] FIG. 6 is an assembled cross-sectional view taken along line VI-VI of FIG. 4 .
DETAILED DESCRIPTION
[0014] FIGS. 1 and 2 show an exemplary embodiment of a key structure 100 used in an electronic device 2 , which may be a mobile phone, or a PDA. The electronic device 2 includes a key structure 100 and a circuit board 20 , and the key structure 100 includes a housing member 10 and a key body 30 . The key body 30 is mounted between the housing member 10 and the circuit board 20 , and is mounted within the housing member 10 .
[0015] The housing member 10 can be a part of the housing of the electronic device 2 and defines a receiving space 12 and an opening 14 communicating with the receiving space 12 . The receiving space 12 is capable of receiving the key body 30 . The receiving space 12 includes a bottom surface 122 and side surfaces 124 . The bottom surface 122 defines two substantially circular positioning holes 126 that extend through the bottom surface 122 .
[0016] The side surfaces 124 are perpendicularly connected to the bottom surface 122 , and two side surfaces 124 face each other, while the other side surface 124 is perpendicularly connected between the two parallel side surfaces 124 . The housing member 10 includes two first locking sections 128 respectively protruding from opposite side surfaces 124 . The two first locking sections 128 face each other, and each first locking section 128 includes a mounting surface 1282 .
[0017] The circuit board 20 can be a printed circuit board (PCB) of the electronic device 2 . The circuit board 20 defines a through hole 22 passing through the circuit board 20 . The circuit board 20 further defines assembling holes 24 symmetrically arranged at opposite sides of the through hole 22 , respectively. The assembling holes 24 pass through the circuit board 20 . The circuit board 20 includes a plurality of contacting sections (not shown), and the key body 30 is electrically connected to the circuit board 20 by the contacting sections.
[0018] Further referring to FIG. 3 , the key body 30 includes a main body 32 , an operation body 34 , and a frame body 36 . The main body 32 is substantially a rectangular block and includes two opposite first surfaces 32 a , two opposite second surfaces 32 b , and two opposite third surfaces 32 c . The main body 32 further includes two positioning columns 321 protruding from one first surface 32 a and a fixing column 323 protruding from the other first surface 32 a . The shape and the size of the positioning columns 321 substantially match the shape and the size of the positioning holes 126 . Thus, the positioning columns 321 can move in and out of the corresponding positioning holes 126 to releasably assemble the key body 30 to the housing member 10 . The shape and the size of the fixing column 323 substantially match the shape and the size of the through hole 22 to position the key body 30 on the circuit board 20 .
[0019] The main body 32 further includes engaging sections 325 , conducting sections 327 , and two second locking sections 328 . The engaging sections 325 , the conducting sections 327 , and the second locking sections 328 are symmetrically arranged at the two opposite second surfaces 32 b . Each engaging section 325 includes a connecting piece 3252 and a fixing piece 3254 . The connecting piece 3252 is substantially a rectangular flat sheet and is connected to the second surface 32 b , and each connecting piece 3252 defines a matching hole 3256 . Each fixing piece 3254 is substantially rectangular sheet and is perpendicularly connected to the distal end of the corresponding connecting piece 3252 .
[0020] The shape and the size of the fixing pieces 3254 substantially match the shape and size of the assembling holes 24 of the circuit board 20 . Thus, the fixing pieces 3245 can move in and out of the corresponding assembling holes 24 to assemble the key body 30 to the circuit board 20 in cooperation with the fixing column 323 . The conducting sections 327 may be made from copper, steel, or other metal and formed by punching and/or cutting a piece of metal. An end of the conducting section 327 elastically resists against and electrically connects to an existing switch (not shown); the other end passes through the matching hole 3256 to electrically connect to the circuit board 20 . Thus, the key body 30 is electrically connected to the circuit board 20 through the conducting sections 327 . The second locking section 328 is made from elastic material and defines a slope 3282 . The slope 3282 is located at the distal end of the second locking section 328 and faces the housing member 10 .
[0021] The main body 32 further includes hinging blocks 329 protruding from the opposite third surfaces 32 c , and two hinging blocks 329 are respectively located at opposite sides of each third surface 32 c . The operation body 34 is positioned on one of the third surfaces 32 c and is located between the two hinging blocks 329 . The operation body 34 can reliably move in and out of the main body 32 and is capable of forcing the switch of the main body 32 to turn on and off.
[0022] The frame body 36 covers the main body 32 and includes a clasp portion 362 and latching portions 364 . The clasp portion 362 is substantially a rectangular sheet and covers one of the first surfaces 32 a . The clasp portion 362 defines two notches 366 located at opposite ends of the clasp portion 362 . The notches 366 are substantially semicircular and correspond to the positioning blocks 321 , so the positioning blocks 321 can be releasably received within and partially exposed from the notches 366 . The latching portions 364 are perpendicularly connected to the clasp portion 362 and are capable of clasping the hinging blocks 329 to cooperatively mount the frame body 36 to the main body 32 .
[0023] Further referring to FIGS. 4 , 5 , and 6 , in assembly, the fixing column 323 of the main body 32 is aligned with the through hole 22 of the circuit board 20 , and the fixing pieces 3254 of the engaging sections 325 are respectively aligned with the corresponding assembling holes 24 . The fixing column 323 and the fixing pieces 3254 are detachably mounted into the through hole 22 and the assembling holes 24 , respectively, by pressing the main body 32 toward the circuit board 20 . Thus, the conducting sections 327 resist against and electrically connect to the circuit board 20 to establish electrical connections. The positioning holes 126 are respectively aligned with the positioning columns 321 of the key body 30 , and the first locking sections 128 are aligned with the second locking sections 328 . The mounting surfaces 1282 of the first locking sections 128 then slide along the slopes 3282 of the second locking sections 328 by pressing the housing member 10 toward the key body 30 . Thus, the second locking sections 328 are removably secured to the first locking sections 328 , the operation body 34 is partially exposed from the opening 14 , and the key body 30 is mounted between the housing member 10 and the circuit board 20 . By operating the operation body 34 , the switch of the key body 30 is turned on or off.
[0024] In addition, to further miniaturize and simplify the key structure 100 , the frame body 36 can be omitted.
[0025] In summary, in the key structure 100 and the electronic device 2 employing the same of the exemplary embodiment, the positioning columns 321 are removably mounted in the positioning holes 126 of the housing member 10 , and the engaging sections 325 are removably mounted in the corresponding assembling holes 24 . Therefore, the key body 30 is mounted between the housing member 10 and the circuit board 20 , which allow easy and efficient assembly. Furthermore, the key structure 100 has a simple structure and is easy to manufacture, which can effectively reduce production costs.
[0026] It is to be understood, however, that even though numerous characteristics and advantages of the exemplary disclosure have been set forth in the foregoing description, together with details of the structure and function of the exemplary disclosure, the disclosure is illustrative only, and changes may be made in detail, especially in matters of shape, size, and arrangement of parts within the principles of exemplary disclosure to the full extent indicated by the broad general meaning of the terms in which the appended claims are expressed.
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A key structure, and an electronic device employing the key structure, includes a housing member and a key body, and the key body is mounted within the housing member for electrically connection to a circuit board. The housing member defines at least one positioning hole; the positioning holes extend through the housing member. The key body includes at least one positioning column. Each at least one positioning column corresponds to a respective positioning hole, and each positioning column is removably received within its corresponding positioning hole to assemble the key body to the housing member.
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BACKGROUND OF THE INVENTION
The present invention relates to equipment for handling eggs and more particularly to a combined egg lifter or transfer device and an egg puncturing system.
Increasing use is being made of machinery for soft or hard cooking eggs. This machinery uses a variety of conveyor devices for carrying the eggs into and through the heating or cooking elements. It is necessary to provide for an efficient transfer device to load these egg feeding means rapidly and efficiently. One such device now in wide spread use is a vacuum egg lifter where an array of individual vacuum lifting egg cups are used to transfer the eggs from the supply trays or cartons to the heating or cooking means.
In the present invention, an improved egg lifter or transfer means is disclosed wherein the engagement or transfer of the eggs is accompanied by a simultaneous piercing or puncturing the eggs. This additional puncturing operation improves the heating or cooking operation by reducing the splitting of egg shells during the cooking to an insignificant amount, by reducing the tendency of eggs to float in a boiling liquid, and by providing more uniformly rounded eggs. While the advantages of punching prior to cooking are known, previous applications of the method have been done on an individual egg basis or by piercing devices performing the piercing operation as a separate step involving cumbersome inefficient and expensive separate egg handling and piercing operations.
Accordingly, an object of the present invention is to provide an improved egg lifter or transfer device.
Another object of the present invention is to provide an improved vacuum egg lifter for an egg transfer device incorporating an integral egg piercing means.
Another object of the present invention is to provide a combined egg transferring and piercing device.
Another object of the present invention is to provide an improved method of simultaneously transferring and piercing eggs.
Other and further objects of the invention will be obvious upon an understanding of the illustrative embodiment about to be described or will be indicated in the appended claims, and various advantages not referred to herein will occur to one skilled in the art upon employment of the invention in practice.
BRIEF DESCRIPTION OF THE DRAWING
A preferred embodiment of the invention has been chosen for purposes of illustration and description and is shown in the accompanying drawing, forming a part of the specification, wherein:
FIG. 1 is a perspective view of a preferred embodiment of an egg lifter in accordance with the present invention.
FIG. 2 is a side elevational view of the egg lifter and pricker of FIG. 1 in position above an egg tray as the pricker is moved to its egg lifting and pricking position.
FIG. 3 is a side elevational view corresponding to FIG. 2 illustrating the egg lifter depositing the transferred and pricked eggs into a row-type carrier.
FIG. 4 is a front elevational view illustrating the transferred and pricked eggs being heated.
FIG. 5 is an enlarged fragmentary view, partially in section, illustrating the vacuum cup and egg pricker.
FIG. 6 is an enlarged fragmentary front elevational view, partially in section, illustrating a heated egg in a cooking medium.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The combined vacuum lifter and egg punching device will now be described in connection with a hand manipulated egg lifter. It is clear that a combination of vacuum lifter and pricker device is equally useful in a machine driven egg transfer mechanism of the automatic or semi-automatic type.
The egg lifter 1 includes a plurality of flexible hollow egg lifting cups 2. The cups 2 are shaped to receive and to form an air tight seal with the end of eggs 3. A preferred style of egg cup 2 has a bellows shape as illustrated, for example, in FIG. 5 to facilitate the seal. The egg cups 2 are arranged with the desired spacing in one or more rows with the interior of each egg cup 2 coupled to a source of vacuum through a suitable vacuum control.
The vacuum coupling or manifold system, as illustrated in the preferred embodiment, comprises a hollow rod 4 having a central vacuum conduit 5 connected through a hollow handle 6 to a pump or other source of vacuum by a convenient coupling. A gripping handle 7 is provided including a hand grip 8. A control device, which applies and releases the vacuum, comprises a control switch 9 whose operating button 10 opens an air outlet when depressed to release the vacuum force from the egg cup manifold by admitting air to the pump and to the vacuum manifold. In its normal raised position under the force of the coil spring 11, the air outlet 12 is closed coupling the pump or other vacuum source to the egg cup manifold causing the vacuum forces to be applied to the egg cups 2 so that the eggs 3 are forced into and held by the individual egg cups 2 during the punching and/or transfer. Each of the individual egg cups 2 is connected to a support rod 4 by a suitable coupling stud 14, as illustrated in FIG. 5, which also acts as a mounting for the cups 2 by engaging the mounting collar 15 on each egg cup 2.
Each of the studs 14 has a needle-like prick or punch 16 mounted on it in position to engage the shell 17 of an egg 3 held in an egg cup 2. The vacuum forces, as exerted on the eggs 3, are sufficient to force the eggs 3 upwardly against a punch 16 and to force the punch 16 through the egg shell 17 in the manner illustrated in FIG. 5. The punches 16 are proportioned to insure complete penetration of the egg shells 17 for the range of egg sizes being handled and a punch 16 which will penetrate the average egg about 3/32 inches will insure an adequate punching operation for a normal range of sizes of the eggs being handled. The vacuum for a particular lifter 1 is readily adjustable to obtain the necessary combination of lifting force and punching force. For a six egg lifter 1 of the general type illustrated, a vacuum force of ten inches has been found to be sufficient to punch the eggs without additional downward force being exerted by an operator. A lesser vacuum may be used which will be adequate for the egg support function. Where a minimal vacuum force is used, the punching operation may be completed by a slight downward pressure on the lifter 1 by the operator.
Unexpectedly, no loss of egg content has been found to occur even at the higher vacuum lifting forces, such as ten inches of vacuum. This result, although unexpected, may be explained by the face that the presence of a single pin-size puncture 18 only in the egg shell 17 prevents a loss of the egg contents such as would occur were a second aperture present in the egg shell 17. The single puncture hole 18 filled by a punch 16 during the transfer provides only a very limited means for an entry of air which necessarily must accompany a loss of egg contents.
FIGS. 4 and 6 illustrate the punctured eggs 3 after their transfer to a heating medium 19, such as a boiler. The expansion of the egg contents generates no shell splitting forces as the egg contents expand into the natural egg air cell space 20 during an escape of air through the shell puncture 18. The escape of air from the egg shell 17 reduces the tendency of the eggs to float in the cooker water and also permits the eggs to expand to a desirable rounded shape.
The above described pricking operation is effective regardless of the exact position of the eggs in the trays or carriers. A preferred position, however, is that illustrated where the large ends of the eggs are uppermost with the natural air cell space 20 presented to the punches 16. This arrangement of eggs is conveniently obtained in the transfer operation as eggs are conventionally arranged in this manner by loading devices when placed into the supply cartons or trays.
The combination of the vacuum egg holding forces with the egg punching needles provides an effective means for assuring a precise punching of a number of eggs in a row since the vacuum force will assure a firm seating or gripping of each egg against its own egg cup regardless of minor variations in the exact attitude or positioning of the lifter pricker device. The vacuum pricker device thus provides for an improved egg punching operation independently of the egg transfer step.
It will be seen that an improved combined vacuum egg lifting and punching operation and device has been described where a vacuum egg lifting force is combined with a punching action. This results in the elimination of a separate punching apparatus and a separate punching operation and also provides a more effective and efficient punching operation.
As various changes may be made in the form, construction and arrangement of the parts herein without departing from the spirit and scope of the invention and without sacrificing any of its advantages, it is to be understood that all matter herein is to be interpreted as illustrative and not in a limiting sense.
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An improved egg handling device is disclosed in which a number of egg lifting vacuum cups, mounted on a convenient support, are used both to transfer eggs and to punch the egg shells. The egg piercing system is incorporated with the transfer cups to provide for a simultaneous piercing and lifting of the eggs. A piercing needle is mounted within each vacuum cup in a position to pierce or puncture each egg shell while it is held within the cup by the vacuum lifting force.
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RELATED APPLICATIONS
[0001] This application is a division of co-pending U.S. patent application Ser. No. 11/038,803, filed Jan. 19, 2005, which is a division of U.S. patent application Ser. No. 10/699,999, filed Nov. 3, 2003 (now U.S. Pat. No. 6,875,236), which is a division of U.S. patent application Ser. No. 09/935,479, filed Aug. 23, 2001 (now U.S. Pat. No. 6,673,116), which is a continuation-in-part of U.S. patent application Ser. No. 09/694,100, filed Oct. 20, 2000 (now U.S. Pat. No. 6,663,669), which claims the benefit of U.S. Provisional Patent Application Ser. No. 60/160,892, filed Oct. 22, 1999, all of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The invention relates to ankle replacement prostheses, systems, and associated surgical procedures.
BACKGROUND OF THE INVENTION
[0003] Until the early to mid 1970's, patients with injured or diseased ankle joints commonly resulting from osteoarthritis (age-related wear of the joints), or rheumatoid arthritis (generalized joint inflammation causing destructive changes), or traumatic arthritis (damage to a joint from a direct injury), had few satisfactory options when their ankle joints failed. Non-surgical options included weight loss, activity modification, medication, injections, braces and therapeutic shoes. The available surgical techniques included ankle arthroscopy (endoscopic examination of the joint), ankle arthrotomy (cutting into the joint to expose the interior) and debridement (opening the joint and removing bone spurs), osteotomy (cutting the bone to realign the joint), ankle fusion (removing the joint and making it stiff), and total ankle arthroplasty (removing the ankle joint and replacing it with an artificial substitute).
[0004] Many of the prior art surgical procedures were riddled with problems for the patient. While early success was realized, there was a high long-term term failure rate due to complications such as infection, loosening, and collapse, which lead to additional extensive surgical procedures.
[0005] Previous ankle replacement systems typically include a talar member, fixed to the talus, as one of their main functioning components. The talus, however, is relatively small, providing a small area of bone for fixation. Also, in most of these ankle replacement systems, the talar component is cemented to the talus. The combination of fixation with bone cement to a small fixation area allows for erosion of the cement from the fixation area and an increase in compliance due to formation of a soft tissue capsule over time. This contributes to aseptic loosening and migration of the device.
[0006] Previous ankle replacement systems are typically installed through incisions made at or near the ankle and make use of extramedullary alignment and guidance techniques. Such surgical procedures require making large incisions at the ankle, moving the tendons and other soft tissue aside; and separating the tibia and fibula from the talus—essentially detaching the foot from the leg—to install the device. Such procedures subsequently require complicated extramedullary realignment and reattachment of the foot. These procedures commonly result in infection and extended healing time with possible replacement failure from improper extramedullary realignment. The surgery also has increased risks associated with cutting or damaging neighboring nerves and tendons which may lead to further complications.
[0007] There remains a need for a total ankle replacement system that reduces the occurrence of subsidence and aseptic loosening while retaining the majority of the foot's natural motion.
SUMMARY OF THE INVENTION
[0008] The invention provides an implant for use in ankle arthroplasty which overcomes the problems and disadvantages associated with current strategies and systems in total ankle replacement (TAR).
[0009] The present invention may include a first member anchored to the tibia and a second member anchored to the talus and operable associated with the first member. The invention may also include a third member which is rigidly removably connected to the second member. The third member may include a portion for attachment to the calcaneous. The third member may be adapted to be in a first position in the calcaneous when the third member is in a first relative position with respect to the second member, and to provide for a second position in the calcaneous when the third member is in a second relative position with respect to the second member.
[0010] The present invention may also include a fourth member which is rigidly removably connected to the second member. The fourth member may have at least one dimension which is different than a dimension of the third member, such that the fourth and third members are interchangeable.
[0011] Another object of the invention is to provide a method or providing ankle arthroplasty. The method may include providing a prosthesis kit including a tibial component, a bearing component, a talar articulating component, a first talar mounting component, and a second talar mounting component. The second talar mounting component has at least one dimension different than the first talar mounting component. The method may further include preparing the talar cavity and the tibia cavity. The method may further include implanting the tibial component into the tibial cavity. The method may further include selecting either the first talar mounting component or the second talar mounting component and implanting the selected talar mounting component into the talar cavity. The method may further include positioning the bearing component between the tibial component and the selected talar mounting component.
[0012] Other objects, advantages, and embodiments of the invention are set forth in part in the description which follows, and in part, will be obvious from this description, or may be learned from the practice of the invention.
DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a view of the lower leg and foot skeleton.
[0014] FIG. 2 is a lateral view of a human foot and lower leg skeleton with the fibula shown in an assembly format and having a planarly resected tibia and talus.
[0015] FIG. 2 a is a posterior view of a human foot and lower leg skeleton with the fibula not shown and planar cuts of the tibia and talus are depicted.
[0016] FIG. 3 shows an intramedullary guidance system for providing intramedullary alignment of the tibial and/or talar cuts, one end of the system being oriented toward the tibia and the other end oriented toward the talus.
[0017] FIG. 4 is a lateral view of a lower leg and foot demonstrating the intramedullary insertion of a guide pin through the superior part of the tibia and terminating in the talus.
[0018] FIG. 5 is a lateral view of a lower leg and foot demonstrating the intramedullary insertion of a guide pin through the plantar surface of the calcaneus, passing through the talus and terminating in the tibia at variable lengths.
[0019] FIG. 5 a is a sectional view of a foot and depicts the insertion and removal of a guide pin through the plantar surface of the calcaneus, passing through the talus and terminating in the tibia, to produce an intramedullary channel, which may be made of various dimensions by using the guide pin to also direct the course of intramedullary reamers.
[0020] FIG. 6 is a lateral sectional view of the lower leg and foot showing the guide pin surrounded by the reaming instrument creating the intramedullary passage.
[0021] FIG. 7 is a lateral view and partial cross section of the human lower leg and foot showing the intramedullary channel and a resected portion of the anterior lower tibia to allow easier insertion of an intramedullary cutting guide.
[0022] FIG. 8 is a posterior section of the lower leg and foot with the fibula not shown and depicting the insertion of the intramedullary cutting guide between the tibia and the talus.
[0023] FIG. 9 is a perspective view of a talo-calcaneal reaming jig.
[0024] FIG. 9 a is a lateral/partial sectional view depicting the insertion of the reaming tool in the talo-calcaneal reaming jig for the posteriorly directed inferior stem to help support the talar component (the drill hole and stem can be only in the talus or extend into the calcaneus for increased stability, and the anterior-posterior position of the talar support stem can be variable).
[0025] FIG. 9 b is a cross-sectional view of the talo calcaneal jig and channel as positioned on the talus.
[0026] FIG. 9 c is a sectional view of resultant channel after the jig is removed, also showing the talar support stem.
[0027] FIG. 10 is a lateral cross-sectional view of the upper prosthetic body, showing the tibial stem and tibial component.
[0028] FIG. 10 a is a side view of an alternative embodiment of an upper prosthetic body with a shorter tibial stem than shown in FIG. 10 .
[0029] FIG. 11 shows the insertion of a tibial stem through the calcaneus and talus, and (if needed) through an anti-rotational sleeve.
[0030] FIG. 12 is a perspective view of the optional anti-rotational sleeve for the tibial stem.
[0031] FIG. 13 is a lateral cross sectional view of the tibial stem in the lower tibia and fixed with screws and (optionally) with the anti-rotational sleeve.
[0032] FIG. 14 shows a lateral cross sectional view of a lower prosthetic body in the foot, including the talar component with posterior fixation blade (if needed), talar fixation stem (extending into the calcaneus), and anterior talo-calcaneal fixation screws.
[0033] FIG. 15 shows both the upper and lower prosthetic bodies.
[0034] FIG. 16 shows an alternative lower prosthetic unit, with talar fixation stem at various angles.
[0035] FIG. 17 shows another alternative lower prosthetic unit, with talar fixation stem at various angles.
DESCRIPTION OF THE INVENTION
I. Anatomy of the Ankle
[0036] Referring to FIG. 1 , the foot comprises fourteen phalanges or toe bones 11 connected to the metatarsus bones 13 . There are also seven tarsal bones 14 , of which the talus 15 supports the tibia 16 and the fibula 18 , and the heel bone or calcaneus 17 . Of the tarsal bones, the talus 15 and the calcaneus 17 are the largest and are adjacent to each other. The other tarsal bones include the navicular 19 , three cuneiforms 21 , and the cuboid 23 .
II. Intramedullary Guidance System
[0037] In performing a total ankle replacement procedure, it is desirable to cut away bone on the inferior end of the tibia 16 and/or the superior end of the talus 15 , to thereby form a planar surface or surfaces 25 , as FIG. 2 and FIG. 2 a shows (in FIG. 2 a , the tibia 16 and talus 15 have been resected with the removed portions shown in phantom lines, leaving two planar surfaces 25 ).
[0038] A planar surface increases the amount of bone available for the fixation of a selected prosthetic base. This provides greater stability and less stress absorption. This also decreases the probability of prosthesis loosening and subsidence.
[0039] FIG. 3 shows the components of an intramedullary guidance system 10 for providing a desired alignment of the tibia and talar before and while the tibial and/or talar cuts shown in FIG. 2 are made.
[0040] As shown in FIG. 3 , the system 10 includes an intramedullary guide pin 27 . The intramedullary guide pin is made, e.g., of an inert material used in the surgical arts, such as surgical steel. The guide pin 27 may possess a range of desired diameters 29 , depending upon the function or functions it is intended to perform.
[0041] For example, the diameter 29 may be relatively small, e.g., about 2 mm to 4 mm, if the pin 27 is to be used principally to form an intramedullary void, as will be described later. The diameter 29 can be made larger, e.g., upwards to about 10 mm, if the pin 27 is to be used to guide passage of a surgical instrument, such as an intramedullary reamer or drill, to form an enlarged intramedullary void, as will also be described later.
[0042] In use, the guide pin 27 may be introduced through the tibia (as FIG. 4 shows) or through the calcaneus (as FIG. 5 shows). Before the guide pin 27 is introduced, the foot and ankle are first aligned in an acceptable position. One skilled in the art will recognize that this may require surgically opening the ankle joint to loosen contractures (permanent contraction of muscles, ligaments, tendons) and scarring.
[0043] When introduced through the tibia (see FIG. 4 ), a minimal exposure 200 is made at the tibial tubercle with an awl. Once the exposure has been made, the exposure may be kept open under distraction, pulling of the skin, or any other method common in the surgical arts. Non invasive visualization of the procedure can be accomplished through fluoroscopy or real time MRI, as well as through other means well known to those skilled in the art. Alternatively, or in conjunction with such less invasive means of visualization, open visualization may be used for part and/or all of the procedure.
[0044] In this approach, the guide pin 27 passed through the tibia 16 , the tibial plafond, and enters the talus.
[0045] When introduced through the calcaneus (see FIG. 5 ), the guide pin 27 is placed retrograde through a minimal exposure in the calcaneus 17 . The exposure may be kept open under any method common in the surgical arts and previously discussed. As with the tibial approach, non invasive visualization of the calcaneus approach can be accomplished through fluoroscopy or real time MRI, as well as through other means well known to those skilled in the art. Alternatively, or in conjunction with such less invasive means of visualization, open visualization may be used for part and/or all of the procedure.
[0046] In this approach, the guide pin 27 passes through the calcaneus, through the talus 15 , through the tibial plafond, and into the tibial shaft.
[0047] As FIG. 5 a shows, upon removal, the guide pin 27 leaves behind an intramedullary guide void or passage 28 through the region where the tibia adjoins the talus. The passage 28 is sized according to the diameter 29 of the guide pin 27 , or with a reamer to an appropriate size consistent with the size of the bones (the calcaneus, the talus, and the tibia).
[0048] As FIG. 7 shows, once the passage 28 is formed, an anterior section S of the tibia 16 can be removed by cutting, to expose the anterior portion of the ankle joint and the guide passage 28 .
[0049] As shown in FIG. 3 , the system 10 also includes an intramedullary cutting guide 31 , which is introduced into the ankle through an anterior surgical approach. In use, the intramedullary cutting guide 31 functions to guide the saw blade used to create the planar surfaces 25 on the tibia and/or talus, as shown in FIG. 2 . For this purpose, the cutting guide includes one or more cutting slots 33 , through which the saw blade passes. As shown in FIG. 3 , the cutting guide 31 also includes an intramedullary locating feature, which in the illustrated embodiment takes the form of an intramedullary locating post 35 (see FIG. 3 ).
[0050] In use (see FIG. 8 ), the intramedullary cutting guide 31 may be inserted anteriorly into the ankle joint after the resection of a small amount of bone from the anterior “lip” of the tibia. The alignment post 35 fits into the intramedullary guide passage 28 in both the talus and tibia. The intramedullary post 35 aligns the cutting guide 31 in the desired orientation with the talus 15 and tibia 16 . Intramedullary guidance enables the surgeon to produce bony cuts that more closely approximate the mechanical axis of the leg, which extramedullary guides, cannot do.
[0051] Oriented by the intramedullary post 35 , the upper slot 33 of the cutting guide 31 is aligned with the tibial shaft. The lower slot 33 is aligned in the same direction into the dome of the talus. The intramedullary post 35 maintains alignment as a bone saw is passed through the slots 33 , across the end regions of talus and tibia. The aligned planar surfaces 25 are thereby formed with intramedullary guidance. Removal of the cutting guide 31 exposes these planar surfaces 25 , as FIG. 2 and FIG. 2 a show. With intramedullary guidance, the cuts are superior to cuts using extramedullary guidance. Extramedullary guidance systems rely on surface bony prominences and visualization of the anterior ankle joint. These landmarks are inconsistent and can misdirect bony cuts by the surgeon.
[0052] The intramedullary guidance system 10 can be conveniently used with various surgical instruments or prosthetic parts. Because extramedullary alignment is avoided, more precise alignment can be made.
[0053] For example, as shown in FIG. 6 , prior to removal of the guide pin 27 and the use of the cutting guide 31 to form the tibial and talar cuts, the guide pin 27 can serve an additional function, namely, to guide the passage of an intramedullary reaming device or a cannulated drill 30 . In this arrangement, the guide pin 27 is used to direct the reaming device 30 over it. A minimally larger exposure will be required on the bottom of the foot to allow the passage of the reaming device or drill bit over the guide pin 27 .
[0054] Depending upon the manner in which the guide pin 27 is inserted, the reaming device 30 can be guided by the intramedullary guide pin 27 , either along a superior path, through the tibia and into the talus (as FIG. 4 shows), or along an inferior path, through the calcaneus and talus and into the tibia (as FIG. 5 shows). Guided by the pin 27 , the reaming device 30 leaves behind an enlarged intramedullary void or passage 28 .
[0055] Alternatively, the guide pin 27 and reaming device 30 may be placed through the tibia or calcaneus simultaneously, or a reaming rod may be placed through the tibia or calcaneus without a guide pin 27 , although it is preferable to use a guide pin. The reamer device 30 is preferably 5, 6, 7, 8, 9, or 10 mm wide, depending on the size of the patient's tibia 16 .
[0056] In this arrangement, the alignment post 35 of the cutting guide 31 is sized to fit into the enlarged reamed intramedullary passage 28 . As before described, the post 35 aligns the cutting guide 31 in the desired orientation with the talus and tibia for forming the end cuts, as well maintain the alignment of the reamed intramedullary passage 28 .
[0057] The size of the alignment post 35 of the cutting guide 31 depends upon how the intramedullary channel is formed. For example, if just a guide pin is used to form the channel, the post 35 will be sized smaller than if an intramedullary reamer is used in forming the channel. If just the guide pin is used to form the channel, straightforward, minimally invasive percutaneous access can be used to insert the guide pin into the calcaneus, into the talus and tibia, thereby forming the relatively small diameter intramedullary channel.
[0058] An upper prosthesis body may be fixed directly to planar cut of the tibia with or without a tibial stem. A lower prosthesis body of the talus may likewise be fixed directly to the planar cut of the talus, or with a fixation stem into the talus or into both the talus and the calcaneus. The upper and lower prosthesis bodies may be used in combination or singly. As will now be described in greater detail later, stemmed upper or lower prostheses may be located on the planar cuts, either individually or in combination.
III. Stemmed Upper Prosthetic Device
[0059] The reamed intramedullary passage 28 formed in the tibia using the intramedullary guidance system 10 can, e.g., serve to accept a stemmed upper prosthetic body 170 , as FIG. 10 shows. The stemmed upper prosthetic body can take various forms. Certain representative embodiments are found in U.S. patent application Ser. No. 09/694,100, now U.S. Pat. No. 6,663,669, filed Oct. 20, 2000, entitled “Ankle Replacement System,” which is incorporated herein by reference.
[0060] In one embodiment ( FIG. 10 ), the upper prosthetic body 170 comprises an elongated tibial stem 150 . The tibial stem 150 may be made of any total joint material or materials commonly used in the prosthetic arts, including, but not limited to, metals, ceramics, titanium, titanium alloys, tantalum, chrome cobalt, surgical steel, or any other total joint replacement metal and/or ceramic, bony in-growth surface, sintered glass, artificial bone, any uncemented metal or ceramic surface, or a combination thereof. The tibial stem 150 may further be covered with one or more coatings such as antimicrobial, antithrombotic, and osteoinductive agents, or a combination thereof. These agents may further be carried in a biodegradable carrier material with which the pores of tibial stem 150 may be impregnated. See U.S. Pat. No. 5,947,893.
[0061] The tibial stem 150 may be variable lengths, e.g., from 2 cm to 30 cm and variable widths, e.g., from 6 to 12 mm. In the preferred embodiment, the tibial stem 150 is preferably approximately 6 inches in length. Of course, it should be understood that the disclosed tibial stem could be of virtually any length, depending upon the size of the patient, his or her bone dimensions, and the anticipated future mobility of the patient. For example, as FIG. 10 a shows, the upper prosthetic body 170 ′ can comprises a shorter tibial stem 150 ′ having a diameter generally the same size (or slightly larger) than the guide pin that forms the passage 28 . The body 170 ′ can also include several short, spaced apart derotation pegs 171 .
[0062] The tibial stem 150 may be inserted into the reamed intramedullary passage 28 either superiorly (through the tibia), or inferiorly (through the calcaneus and talus and into the tibia), depending upon the path along which the guide pin 27 and reaming device 30 have followed.
[0063] For example, as depicted in FIG. 4 , when the passage 28 is made by the pin 27 and reaming device 30 superiorly through the tibia, the tibial stem 150 is inserted in a superior path through the tibia. Alternately, as depicted in FIGS. 11 to 13 , when the passage 28 is made by the pin 27 and reaming device 30 retrograde through the calcaneus, the tibial stem 150 may be introduced inferiorly through the retrograde passage 28 through the calcaneus and talus into the tibia ( FIG. 11 ).
[0064] The stem 150 is fixed in the lower tibia ( FIG. 13 ). The tibial stem 150 may be fixed in the tibia 16 with poly(methylmethacrylate) bone cement, hydroxyapatite, a ground bone composition, screws, or a combination thereof, or any other fixation materials common to one of skill in the art of prosthetic surgery. An anti-rotational sleeve 406 (see FIG. 12 ) can also be used alone or in combination with other fixation devices.
[0065] In a preferred embodiment, the tibial stem 150 is fixed to the tibia 16 with screws 125 a and 125 b. If screws are used, they can extend anteriorly, posteriorly, medially, laterally and/or at oblique angles, or any combination thereof.
[0066] Optionally, a sleeve 406 (see FIGS. 11 and 12 ) may be placed about the stem 150 , e.g., as the stem is passed between the talus and tibia. The sleeve 406 engages bone along the passage 28 . The sleeve 406 imparts an anti-rotational feature, including, e.g., outwardly extending fins. The sleeve 406 may be used in combination with the screws or alone without the screws.
[0067] The distal end of the tibial stem 150 may additionally have interlocking components, common to those of skill in the art, at its lower surface to allow other components of the upper prosthesis body to lock into the tibial stem. In a preferred embodiment, the tibial stem 150 has a Morse Taper 115 b at its lower surface to which a concave dome 155 is attached. The dome 155 can be made of a plastic, ceramic, or metal. The dome 115 articulates with the lower ankle joint surface, which can be the talus bone itself or a lower prosthetic body fixed to the talus, as will now be described.
IV. Stemmed Lower Prosthesis Body
[0068] A lower prosthetic body can be supported on the talus, either alone or in association with an upper prosthetic body mounted in the tibia. The upper prosthetic body may be stemmed, as just described, or affixed directly to the tibia without use of a stem. Likewise, the lower prosthetic body may be stemmed or affixed directed to the talus. Certain representative embodiments are found in U.S. patent application Ser. No. 09/694,100, now U.S. Pat. No. 6,663,669, filed Oct. 20, 2000, entitled “Ankle Replacement System,” which is incorporated herein by reference.
[0069] In one embodiment, the stem for the talar component does not extend beyond the inferior surface of the talar. In another embodiment, a subtalar joint (i.e., the joint formed between talus and calcaneus) is fused to allow fixation of the lower prosthesis body to both the talus and calcaneus. The subtalar joint may be fused using any method common to those of skill in the surgical arts including, but not limited to, fusion with, for example, poly (methylmethacrylate) bone cement, hydroxyapatite, ground bone and marrow composition, plates, and screws, or a combination thereof.
[0070] FIG. 14 shows one method of fusing the talus 15 to the calcaneus 17 using a stem 110 , a plate 130 , and screws 133 a, 133 b. The talo-calcaneal stem 110 is shown with a Morse Taper 115 a protruding from the stem 110 and extending beyond the proximal (top) surface of the talus 15 . In another embodiment, the Morse Taper could extend down from the talar component into the stem. FIG. 14 also shows an arrangement in which the lower end of the tibia has not been cut and does not carry a prosthesis.
[0071] The talo-calcaneal stem 110 may be made of various materials commonly used in the prosthetic arts including, but not limited to, titanium, titanium alloys, tantalum, chrome cobalt, surgical steel, or any other total joint replacement metal and/or ceramic, bony in-growth surface, sintered glass, artificial bone, any uncemented metal or ceramic surface, or a combination thereof. The talo-calcaneal stem 110 may further be covered with various coatings such as antimicrobial, antithrombotic, and osteoinductive agents, or a combination thereof. These agents may further be carried in a biodegradable carrier material with which the pores of the surface of the talo-calcaneal stem 110 may be impregnated. See U.S. Pat. No. 5,947,893, which is incorporated herein by reference. If desired, the talo-calcaneal stem may be coated and/or formed from a material allowing bony in-growth, such as a porous mesh, hydroxyapetite, or other porous surface.
[0072] The talo-calcaneal stem 110 may be any size or shape deemed appropriate to fuse the subtalar joint of a patient and is desirably selected by the physician taking into account the morphology and geometry of the site to be treated. For example, the stem 110 may be of variable lengths, from 2 cm to 12 cm, and variable widths, from 4 to 14 mm. In a preferred embodiment, the talo-calcaneal stem 110 is approximately 65 to 75 mm in length and approximately 7 to 10 mm wide. While in the disclosed embodiment the stem 110 has a circular cross-section, it should be understood that the stem could formed in various other cross-sectional geometries, including, but not limited to, elliptical, polygonal, irregular, or some combination thereof. In addition, the stem could be arced to reduce and/or prevent rotation, and could be of constant or varying cross-sectional widths.
[0073] The physician is desirably able to select the desired size and/or shape based upon prior analysis of the morphology of the target bone(s) using, for example, plain film x-ray, fluoroscopic x-ray, or MRI or CT scanning. The size and/or shape is selected to optimize support and/or bonding of the stem to the surrounding bone(s).
[0074] As FIGS. 9 a to 9 c show, the talo-calcaneal stem 110 can be passed from the top of the talus 15 into the distal calcaneus 17 through a cavity 601 that is drilled through the talus 15 and calcaneus 17 . The cavity 601 is preferably drilled after the surface of the talus 15 has cut and flattened, and after the location of the upper prosthesis body.
[0075] A suitable jig 600 (see FIG. 9 ) may be placed in the joint to assist with locating and placing the cavity 601 . Certain representative embodiments are found in U.S. patent application Ser. No. 09/694,100, now U.S. Pat. No. 6,663,669, filed Oct. 20, 2000, entitled “Ankle Replacement System,” which is incorporated herein by reference. The jig 600 includes a drill guide 620 and a post 610 that, in use, rests in the intramedullary passage 28 (see FIGS. 9 a and 9 b ). The drill guide 620 can extend from posterior to anterior (as FIG. 9 shows), or alternatively, from anterior to posterior.
[0076] The drill bit 603 for the jig 600 (see FIG. 9 a ) is preferably about ½ mm wider than the width of the talo-calcaneal stem 110 . The talo-calcaneal stem 110 may be further adapted so that the talo-calcaneal stem 110 is inserted as the cavity is being drilled or so that the talo-calcaneal stem itself is used to drill the hole.
[0077] Once the cavity 601 is formed, any easily accessed cartilage from the talo-calcaneal joint may be scraped, e.g., using a small angled curet or any other instrument commonly used in the surgical arts. The subtalar joint can then be fused by passing a talo-calcaneal stem 110 down the cavity 601 . The cavity 601 may be partially filled with a bone cement prior to the installation of the talo-calcaneal stem 110 to help fix the talo-calcaneal stem 110 to the subtalar joint. Desirably, the stem 110 incorporates screw holes or other openings to accommodate interlocking hardware, such as screws, to increase fixation and minimize rotation.
[0078] The stem 110 desirably includes a Morse Taper 115 a. A cap 160 a fits on the Morse Taper 115 a to form an articulating joint surface with the upper prosthesis. The upper surface of the cap 160 can be designed to fit the particular needs and walking requirements anticipated by the physician and patient. For example, a low demand surface, such as for an individual of advanced years having a less-active lifestyle, could comprise a simple smooth arc, without the “peaks and valleys” of the talus 15 that run from anterior to posterior. In addition, a low demand surface may not require a difference in the anterior to posterior talar width, which in an adult male can be approximately 4 to 5 mm wider in its anterior portion than its posterior portion. A higher demand surface, for a more active individual, may incorporate the trochlea (valley) in the talus as well as various other anatomical features found on the talus.
[0079] Desirably, as best seen in FIG. 16 , the stem 110 a extends downward from the cap 160 a, forming an angle α 0 relative to the vertical axis—taken relative to the longitudinal axis of cap 160 a (front to rear of the foot). In one embodiment, the angle α 0 will range from 105° to 205°, depending upon the size and orientation of the calcaneus 17 as well as the position of the lower prosthesis body. Moreover, as best seen in FIG. 17 , the stem may form an angle β 0 relative to the vertical axis—taken relative to the transverse axis of the cap 160 b (medial to lateral side of the foot). In a preferred embodiment, the angle β 0 will range from 155° (on the medial side of the foot) to 240° (on the lateral side of the foot), depending upon the size and orientation of the calcaneus 17 as well as the position of the lower prosthesis body. Desirably, the lower portion of the stem of the implant will not extend outside of the calcaneus.
[0080] As shown in FIG. 14 , a plate 130 may be fixed to the top of the talus 15 . The plate 130 can have an overhang portion 131 which allows the plate 130 to overlap both the talus 15 and part of the calcaneus 17 . The plate 130 and overhang portion 131 may be made of various materials commonly used in the prosthetic arts including, but not limited to, polyethylene, biologic type polymers, hydroxyapetite, rubber, titanium, titanium alloys, tantalum, chrome cobalt, surgical steel, or any other total joint replacement metal and/or ceramic, bony in-growth surface, sintered glass, artificial bone, any porous metal coat, metal meshes and trabeculations, metal screens, uncemented metal or ceramic surface, other bio-compatible materials, or any combination thereof. The plate 130 and overhang portion 131 may further be covered with various coatings such as antimicrobial, antithrombogenic, and osteoinductive agents, or a combination thereof. See U.S. Pat. No. 5,866,113 to Hendriks, et al, incorporated herein by reference. These agents may further be carried in a biodegradable carrier material with which the pores of the plate 130 and overhang portion 131 may be impregnated. In one preferred embodiment, the tray comprises a metal-backed polyethylene component.
[0081] The plate 130 and/or the overhang portion 131 may be fixed to the subtalar joint 90 with poly(methylmethacrylate) bone cement, hydroxyapatite, a ground bone and marrow composition, screws, or a combination thereof, or any other fixation materials common to one of skill in the art of joint replacement surgery. In a preferred embodiment, the plate 130 and overhang portion 131 are fitted over the Morse Taper 115 a of the talo-calcaneal stem 110 and fixed to the talus 15 and calcaneus 17 with screws 133 a and 133 b. In another embodiment, the posterior overhang portion 131 can be eliminated.
[0082] The lower prosthesis body may be formed in a single unit or, as illustrated, as a multi-component prosthesis.
[0083] In other embodiments, the upper prosthesis body may additionally comprise a fibular prosthesis of any variety known in the art of joint replacement. The fibular prosthesis would replace the inferior end of the fibula, especially when this prosthesis is used to revise a total ankle replacement system that has removed the distal end of the fibula. In still further embodiments, either the lower prosthesis body, upper prosthesis body, or both, as described above, may be fixed into strengthened or fortified bone. The bones of the subtalar joint, tibia, or fibula may be strengthened prior to or during fixation of the prosthesis using the methods described in U.S. Pat. No. 5,827,289 to Reiley. This type of bone strengthening procedure is particularly suggested for osteoporotic patients who wish to have a total ankle replacement.
[0084] It should be appreciated that installed prosthetic system need not include a calcaneal stem. Thus, the system would only include the tibial stem, the tibial component and the talar component. In this case there would be not Morse Taper holes or stems on the under surface of the talar component, just a flat or minimally stem component with or without screw holes for screw fixation.
[0085] Likewise, the installed prosthetic system need not include a tibial stem component. In this case, the system would include the tibial component without the Morse Taper attachments on its superior surface, the talar component, and the calcaneal stem component.
[0086] Furthermore, the installed prosthetic system need not include any stemmed component being utilized. However, the intramedullary guidance system 10 , deployed either superiorly from the tibia, or inferiorly from the calcaneus, would still provide intramedullary alignment of the tibial and talar cuts. In this arrangement, the tibial component and the talar component would be utilized, without Morse Taper stems or holes on either implant, but the intramedullary guidance system would still be used to insure properly aligned cuts in the talus and tibia.
[0087] It should be understood that the devices and methods of the present invention could be used as an index (initial) total ankle replacement, as well as a revision ankle replacement. If used as a revision device, only a portion of the disclosed methods and devices may be necessary in conjunction with such a procedure.
[0088] Other embodiments and uses of the inventions described herein will be apparent to those skilled in the art from consideration of the specification and practice of the inventions disclosed. All documents referenced herein are specifically and entirely incorporated by reference. The specification should be considered exemplary only with the true scope and spirit of the invention indicated by the following claims. As will be easily understood by those of ordinary skill in the art, variations and modifications of each of the disclosed embodiments can be easily made within the scope of this invention as defined by the following claims.
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An ankle implant for use in ankle arthroplasty in total ankle replacement is provided. The implant includes an upper prosthesis anchored to the tibia and a lower prosthesis anchored to the talus. The lower prosthesis is operable associated with the upper prosthesis. The implant also includes a stem which is rigidly removably connected to the second member. The stem includes a portion for attachment to the calcaneous. The stem is be adapted to be in a first position in the calcaneous when the stem is in a first relative position with respect to the lower prosthesis, and to provide for a second position in the calcaneous when the stem is in a second relative position with respect to the lower prosthesis.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an improved process for preparing epoxides, in particular alkylene oxides, from, corresponding starting compounds, in particular from the corresponding olefins, by means of aromatic peroxycarboxylic acids.
2. Description of the Background
The epoxidation of olefins with peroxycarboxylic acids, in particular with m-chloroperoxybenzoic acid, is a well established laboratory method for the synthesis of epoxides.
The method is extensively described in the chemical literature, for example by Y. Sawaki in S. Patai (ed.), Chem. Hydroxyl, Ether Peroxide Groups, p. 590-593 (1993) (1).
However, the method is less suitable for preparing epoxides on a larger scale, since the peroxycarboxylic acid is used in stoichiometric amounts and the resulting carboxylic acid has to be expensively regenerated by reaction with hydrogen peroxide.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a process for preparing alkylene oxides by epoxidation of olefins with aromatic peroxycarboxylic acids which permits a simple, safe and economical recycle of the resulting carboxylic acid into peroxycarboxylic acid without use of hydrogen peroxide.
We have found that this object is achieved by a process for preparing an epoxide from the corresponding olefin by means of an aromatic peroxycarboxylic acid, which comprises a step A of epoxidizing the olefin and removing the resulting aromatic carboxylic acid from the epoxide, a step B of catalytically hydrogenating the removed aromatic carboxylic acid to the corresponding aromatic aldehyde, and a step C of oxidizing this aldehyde with oxygen or an oxygen-containing gas mixture back to the aromatic peroxycarboxylic acid for re-use for preparing an epoxide.
DETAILED DESCRIPTION OF THE INVENTION
In principle, any olefin can be epoxidized in step A. Preference is given to olefins which carry not more than one electron-attracting substituent directly on the double bond. Particular preference is given to olefins without electron-attracting substituents on the double bond. Examples of useful olefins are linear or branched C 2 -C 40 -olefins, in particular C 3 -C 24 -olefins, or cyclic olefins, such as ethylene, propene, 1-butene, 2-butene, isobutene, 1-pentene, 2-pentene, 1-hexene, 1-heptene, 1-octene, 2,4,4-trimethyl-1-pentene, 2,4,4-trimethyl-2-pentene, 1-nonene, 1-decene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene, C 20 -olefin, C 22 -olefin, C 24 -olefin, C 28 -olefin or C 30 -olefin, cyclopropene, cyclobutene, cyclopentene, cyclohexene, cyclooctene, vinyl alkyl ethers such as vinyl methyl ether, vinyl ethyl ether or vinyl butyl ether, allyl chloride, allyl alcohol, vinyl acetate, vinyl propionate, styrene and also compounds having a plurality of olefinic double bonds such as 1,3-butadiene, isoprene, cyclopentadiene or cyclooctadiene. It is also possible to use olefin mixtures.
The process of the present invention is particularly highly suitable for epoxidizing propene to propylene oxide.
Suitable aromatic peroxycarboxylic acids are in particular compounds of the general formula I ##STR1## where R 1 to R 3 are independently of one another hydrogen, C 1 -C 6 -alkyl, C 3 -C 8 -cycloalkyl, C 6 -C 14 -aryl, C 7 -C 12 -phenylalkyl, halogen, C 1 -C 6 -alkoxy, C 3 -C 8 -cycloalkoxy, C 6 -C 14 -aryloxy or C 7 -C 12 -phenylalkoxy and one of R 1 to R 3 can also be a further peroxycarboxyl group or a carboxyl group.
More particularly, the substituents R 1 to R 3 have independently the following meanings:
hydrogen;
C 1 -C 6 -alkyl, preferably C 1 -C 4 -alkyl such as methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl or n-hexyl, in particular methyl or tert-butyl;
C 3 -C 8 -cycloalkyl such as cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl or cyclooctyl, in particular cyclopentyl or cyclohexyl or substituted C 3 -C 8 -cycloalkyl, in particular 1-methylcyclopentyl or 1-methylcyclohexyl;
C 6 -C 14 -aryl such as phenyl, 1-naphthyl, 2-naphthyl, 1-anthryl, 2-anthryl or 9-anthryl, in particular phenyl;
C 7 -C 12 -phenylalkyl such as 1-methyl-1-phenylethyl, benzyl, 1-phenylethyl, 2-phenylethyl, 1-phenylpropyl, 2-phenylpropyl, 3-phenylpropyl, 1-phenylbutyl, 2-phenylbutyl, 3-phenylbutyl or 4-phenylbutyl, in particular 1-methyl-1-phenylethyl;
halogen such as fluorine, chlorine or bromine;
C 1 -C 6 -alkoxy, C 3 -C 8 -cycloalkoxy, C 6 -C 14 -aryloxy or C 7 -C 12 -phenylalkoxy, in which case the radicals on the oxygen atom have the above-innumerated meanings of R 1 to R 3 (with the exception of hydrogen);
peroxycarboxyl or carboxyl for one of R 1 to R 3 .
Preference is further given to those aromatic peroxycarboxylic acids I which have one, two or three methyl groups as substituents R 1 to R 3 .
Examples of useful aromatic peroxycarboxylic acids are in particular peroxybenzoic acid, 2-methylperoxybenzoic acid (o-peroxytoluic acid), 3-methylperoxybenzoic acid (m-peroxytoluic acid), 4-methylperoxybenzoic acid (p-peroxytoluic acid), 2,4- and 3,5-dimethylperoxybenzoic acid, 2,4,6-trimethylperoxybenzoic acid, 4-tert-butylperoxybenzoic acid, 2-methyl-4-tert-butylperoxybenzoic acid, 2,6-dimethyl-4-tert-butylperoxybenzoic acid, 2-, 3- or 4-ethylperoxybenzoic acid, 4-(1-methylcyclohexyl)peroxybenzoic acid, 4-(1-methylcyclopentyl)peroxybenzoic acid, 4-phenylperoxybenzoic acid, 3-chloroperoxybenzoic acid, 4-methoxy- or 4-ethoxy-peroxybenzoic acid, 4-methoxy- or 4-ethoxy-2,6-dimethylperoxybenzoic acid, bisperoxyphthalic acid, monoperoxyphthalic acid, bisperoxyterephthalic acid and monoperoxyterephthalic acid. It is also possible to use mixtures of the aromatic peroxycarboxylic acids mentioned. o-Peroxytoluic acid is particularly preferred.
Step A of the process of the present invention is described in the literature as regards the epoxidation of olefins. The epoxidation is typically carried out as follows:
The aromatic peroxycarboxylic acid, dissolved in a suitable solvent, is made to react with an olefin. The molar ratio of olefin to peroxycarboxylic acid is within the range from 0.8:1 to 100:1, in particular from 1:1 to 20:1, especially from 1.5:1 to 5:1.
The peroxycarboxylic acid solution used can be an isolated peroxycarboxylic acid dissolved in a solvent. It is preferable, however, to use directly the solution prepared in oxidation step C (with or without a prior purification step during which the peroxycarboxylic acid remains in solution).
Suitable organic solvents for the peroxycarboxylic acids in the epoxidation are ketones (e.g., acetone, butanone or tert-butyl methyl ketone), esters (e.g., methyl or ethyl acetate or methyl benzoate), nitro compounds (e.g., nitromethane or nitrobenzene), halogenated hydrocarbons (e.g., di- or trichloromethane, 1,1,1-trichloroethane or chlorobenzene), carbonates (e.g., dimethyl carbonate), urea derivatives (e.g., tetramethylurea), inorganic esters or amides (e.g., trimethyl phosphate or hexamethylphosphoramide), hydrocarbons (e.g., hexane or heptane), or alkylaromatics (e.g., benzene, toluene or xylene). However, it is particularly preferable to use the same solvent as in the oxidation of step C. Particularly preferred solvents for both steps are acetone, methyl acetate and ethyl acetate.
The epoxidation can be carried out at from -20° to 100° C., depending on solvent and olefin. If acetone is used as solvent and terminal olefins (e.g., 1-octene or propene) as substrate, temperatures from 25° to 80° C. are preferred. Temperatures from 45° to 65° C. are particularly preferred.
Surprisingly, at the relatively high temperature of 45° C. or higher, the olefin is converted much more rapidly to the epoxide than any aromatic aldehyde still present from stage B is converted to carboxylic acid.
The aromatic carboxylic acids formed in step A from the aromatic peroxycarboxylic acids I are separated from the oxidation products, in particular the alkylene oxides, by customary methods, for example by filtration, extraction or distillation.
The catalytic hydrogenation of the aromatic carboxylic acids in step B is preferably effected with hydrogen in the gas phase in the presence of a lanthanide/zirconia catalyst. Such catalysts are known for use as hydrogenation catalysts for converting aromatic carboxylic acids into the corresponding aldehydes from German Patent Application P 44 28 994.4 (2).
Step B of the process of the present invention is advantageously carried out as follows:
The hydrogenation of the aromatic carboxylic acid with hydrogen is carried out in the presence of a catalyst whose catalytically active material comprises from 60 to 99.9, in particular from 80 to 99.9, % by weight of zirconium oxide (ZrO 2 ) and from 0.1 to 40, in particular from 0.1 to 20, % by weight of one or more elements of the lanthanides, is generally carried out at temperatures from 200° to 450° C., preferably from 250° to 400° C., in particular from 300° to 380° C., and pressures from 0.1 to 20 bar, preferably from 0.7 to 5 bar, in particular at atmospheric pressure. The temperature and pressure required are dependent on the catalyst activity and the thermal stability of precursor and product.
Suitable catalysts include supported catalysts, preferably solid catalysts of zirconium oxide in cubic, tetragonal or monoclinic phase, preferably in monoclinic phase, which have been doped with one or more elements of the lanthanide series. The catalytically active mass comprises preferably from 90 to 99.9% by weight, in particular from 92 to 99% by weight, of zirconium oxide and from 0.1 to 10% by weight, in particular from 1 to 8% by weight, of one or more elements of the lanthanides, in particular lanthanum, cerium, praseodymium, neodymium, samarium, europium or mixtures thereof, especially lanthanum as lanthanum(III) oxide. The doping is generally effected by saturating the zirconium oxide with salt solutions (aqueous or alcoholic) of the lanthanides.
The catalyst may additionally include further dopants (e.g., chromium, iron, yttrium, hafnium, manganese) in amounts from 0.001 to 10% by weight. Preference is given to catalysts without such further additions.
The BET surface area of the zirconium oxide can vary within wide limits and is generally from 5 to 150 m 2 /g, preferably from 20 to 150 m 2 /g, in particular from 40 to 120 m 2 /g.
Catalysts of this type are produced in a conventional manner, for example by saturating preformed carrier elements such as pellets, balls or extrudates, drying and calcining.
The preferred supported catalysts are very active over a prolonged period. Deactivated catalysts can be regenerated by treatment with gases containing molecular oxygen, e.g., air, at temperatures from 350° to 500° C.
The weight hourly space velocity over the catalyst is held in general within the range from 0.01 to 10, preferably from 0.01 to 3, kg of aromatic carboxylic acid per kg of catalyst per hour.
The hydrogen concentration in the feed gas depends on the carboxylic acid concentration. The molar ratio of hydrogen to aromatic carboxylic acid is in general within the range from 2:1 to 100:1, preferably within the range from 10:1 to 70:1. The hydrogen can also come from formic acid used as source.
It can also be advantageous to add an inert diluent. Typically, nitrogen, water or gaseous reaction-inert compounds such as hydrocarbons, aromatics or ethers are employed.
The reaction can be carried out in the gas phase, continuously as a fixed bed reaction with a fixed bed catalyst, for example in an upflow or downflow process, or as a fluidized bed reaction with the catalyst in the fluidized state. Preference is given to the use of a fixed bed.
To increase the selectivity, by-products of the hydrogenation, for example alcohols, can be recycled into the synthesis.
The step B exit mixture, containing the aromatic aldehyde, passes with or without prior purification into step C where it is advantageously taken up in a suitable solvent and oxidized in the liquid phase with oxygen or an oxygen-containing gas mixture to the corresponding aromatic percarboxylic acid. This is preferably done at temperatures from -10° C. to 100° C. and oxygen partial pressures from 0.001 to 100 bar.
DE-A-25 15 033 (3) discloses that p-tolualdehyde can be oxidized in acetone solution with air at 28° C. and 30 bar without catalyst to form p-peroxytoluic acid in a yield of about 80%. However, such high yields are only achieved with highly pure p-tolualdehyde and anhydrous acetone.
Step C of the process of the present invention is normally carried out as follows:
The concentration of the aromatic aldehyde in the solvent can be from 1 to 75% by weight. Preferably it is from 5 to 35% by weight, in particular from 8 to 20% by weight.
Oxygen or the oxygen-containing gas mixture can be made to react with the aromatic aldehyde either in gas form or as a solution, under atmospheric or superatmospheric pressure. The oxygen partial pressure is preferably from 0.01 to 30 bar, in particular from 0.05 to 5 bar.
The oxidation can be carried out mono- or diphasicly. Suitable reactors for the monophasic process are ones in which a solution of the aromatic aldehyde can be reacted with a solution of oxygen, under atmospheric or superatmospheric pressure, for example tubular reactors or flooded stirred tanks. Suitable reactors for the diphasic process ensure thorough gas-liquid mixing, such as bubble columns (with or without dividing walls or packing elements), stirred tanks (optionally equipped with sparging agitators and optionally arranged as a cascade) or trickle downflow reactors.
The reaction temperature is preferably from 0° to 60° C., in particular from 15° to 40° C.
The reaction time is chosen so as to produce an aldehyde conversion within the range from 40 to 100%. Preference is given to reaction times producing an aldehyde conversion within the range from 60 to 99%. Particular preference is given to reaction times producing an aldehyde conversion within the range from 75 to 95%.
The oxidation may additionally comprise a step of adding a stabilizer for the peroxycarboxylic acid product, e.g., 8-hydroxyquinoline, dipicolinic acid or 2,6-dihydroxymethylpyridine.
Suitable organic solvents for step C are ketones (e.g., acetone, butanone or tert-butyl methyl ketone), esters (e.g., methyl or ethyl acetate or methyl benzoate), nitro compounds (e.g., nitromethane or nitrobenzene), halogenated hydrocarbons (e.g., di- or trichloromethane, 1,1,1-trichloroethane or chlorobenzene), carbonates (e.g., dimethyl carbonate), urea derivatives (e.g., tetramethylurea), inorganic esters or amides (e.g., trimethyl phosphate or hexamethylphosphoramide) or alkylaromatics (e.g., benzene, toluene or xylene). Preference is given to ketones, in particular acetone and tert-butyl methyl ketone, and esters, in particular methyl acetate, ethyl acetate and methyl benzoate.
The aromatic peroxycarboxylic acid can either by isolated (by precipitation, for example), or else be re-used directly in step A without isolation (i.e., in solution).
It is surprising that o-tolualdehyde is faster and more selectively oxidizable than the isomeric m- and p-tolualdehydes.
The process of the present invention has the advantage that the aromatic peroxycarboxylic acid is regenerated without use of hydrogen peroxide after the oxidation/epoxidation. The aromatic peroxycarboxylic acid acts only as an oxygen transfer agent and is not consumed to any practical extent. The stoichiometry of the overall process is:
olefin+O.sub.2 +H.sub.2 →alkylene oxide+H.sub.2 O.
A reaction scheme for the epoxidation using an aromatic peroxycarboxylic acid I may be illustrated as follows: ##STR2##
EXAMPLES
Example 1
Epoxidation of 1-octene with p-peroxytoluic Acid in Acetone
50 g of an 8.3% strength by weight solution of p-peroxytoluic acid in acetone were admixed with 4.6 g (1.5 equivalents) of 1-octene and stirred at 40° C. for 5 hours, when the conversion of the peroxyacid was about 90%. The octene oxide selectivity was about 80%, based on the peroxyacid, and >95%, based on 1-octene. The reaction temperature was raisable without significantly reducing the selectivity. At a reaction temperature of 60° C. the peroxyacid conversion after 2 hours was about 90%. The octene oxide selectivity was unchanged compared with the run at 40° C.
Example 2
Epoxidation of Propene with p-peroxytoluic Acid in Acetone
35 g of an 8.4% strength by weight solution of p-peroxytoluic acid in acetone were charged initially to a 50 ml glass autoclave, 2.4 g of propene (3 equivalents) were injected, and the contents were stirred at 60° C. for 4.5 hours. The peroxyacid conversion was 94%. The propylene oxide selectivity based on the peroxyacid was >95%.
Example 3
Epoxidation of 1-octene with o-peroxytoluic Acid in Acetone
100 g of an 11.3% strength by weight solution of o-peroxytoluic acid in acetone were admixed with 16.8 g of 1-octene (2 equivalents) and stirred at 60° C. After 1 hour the peroxyacid conversion was 92%. The octene oxide selectivity was 97%, based on o-peroxytoluic acid.
Example 4
Preparation of the Catalyst for the Hydrogenation in Step B
Monoclinic ZrO 2 (BET surface area: 40-85 m 2 /g) in the form of tablets (catalysts A and E) or extrudates (catalysts B, C and D) was saturated with an aqueous solution of the lanthanide element nitrate (or lanthanide element nitrates) by thorough mixing and the mixture was held at room temperature for 2 hours. The catalyst was then dried at 120° C. for 15 hours and then heat-treated at from 400° to 500° C. for from 2 to 4 hours.
The catalysts thus prepared had the following lanthanide contents:
Catalyst A (surface area: 67 m 2 /g): 3% by weight of lanthanum;
Catalyst B (surface area: 46 m 2 /g): 3% by weight of praseodymium;
Catalyst C (surface area: 46 m 2 /g): 3% by weight of cerium;
Catalyst D (surface area: 46 m 2 /g): 3% by weight of lanthanides (distribution: 48.2% by weight of CeO 2 , 26.4% by weight of La 2 O 3 , 5.7% by weight of Pr 2 O 3 and 19.7% by weight of Nd 2 O 3 );
Catalyst E (surface area: 53 m 2 /g): 3% by weight of lanthanum.
Examples 5a to 5i
Hydrogenation of 4-substituted Aromatic Carboxylic Acids
Per hour, from 4 to 8 g of aromatic carboxylic acid, without a solvent or dissolved in tetrahydrofuran (THF), were passed into a vaporizer (<300° C.) and carried from there by 100 l/h of hydrogen through 100 g of catalyst in a trickle downflow. The gaseous reaction effluent was condensed in cold traps and analyzed by gas chromatography. The carboxylic acids used and the results are summarized in Table 1.
TABLE 1__________________________________________________________________________ Conc. of Yield Carboxylic carboxylic Reactor of Con-Ex. acid acid temp. aldehyde version SelectivityNo. Catalyst R.sup.1) wt. %!.sup.2) °C.! %! %! %!__________________________________________________________________________5a A H 100 340 98 100 985b A H 20 350 98 100 985c A methyl 100 340 96 99 975d A t-butyl 100 340 90 94 965e A t-butyl 20 340 93 97 965f A methyl 10 350 77 99 785g B H 100 360 95 100 955h C H 100 360 96 100 965i D H 100 360 97 99 98__________________________________________________________________________ .sup.1) substituent in position 4 of the carboxylic acid: ##STR3## .sup.2) in solvent (THF); 100% by weight indicates pure carboxylic acid, without solvent
Example 6
Hydrogenation of 3-methylbenzoic Acid
Hydrogen at 100 l/h was used to vaporize 8 g/h of 3-methylbenzoic acid (as melt) and pass it at 360° C. in the downflow direction through 100 g of catalyst E. The gaseous reaction effluent was condensed in cold traps and analyzed by gas chromatography. The yield of 3-methylbenzaldehyde was 92% (conversion 99%).
Example 7
Hydrogenation of 2-methylbenzoic Acid
Hydrogen at 200 l/h was used to vaporize 8 g/h of 2-methylbenzoic acid (as melt) and pass it at 350° C. in the downflow direction through 100 g of catalyst E. The gaseous reaction effluent was condensed in cold traps and analyzed by gas chromatography. The yield of 2-methylbenzaldehyde was 93% (conversion 99%).
Examples 8a to 8e
Oxidation of Aromatic Aldehydes with Air to Peroxycarboxylic Acids in Acetone
A solution of aromatic aldehyde (10% strength by weight in acetone) was oxidized with air at 30° C. in a four-neck flask equipped with gas inlet tube, high-speed Hoesch stirrer, a thermometer and a reflux condenser. The peroxyacid concentration was determined by iodometry. Other components can be determined by gas chromatography (after reduction of the peroxyacid with tributyl phosphite). The aldehydes used and the results are summarized in Table 2.
TABLE 2______________________________________ Conversion of PeroxyacidEx. Reaction time aldehyde selectivityNo. Aldehyde h! %! %!______________________________________8a benzaldehyde 2 34 778b p-tolualdehyde 7 84 838c m-tolualdehyde 6 90 828d o-tolualdehyde 4 80 938e p-methoxy- 1 37 72 benzaldehyde______________________________________
Example 9
Oxidation of p-tolualdehyde in Methyl Acetate
Example 8b was repeated with methyl acetate instead of acetone as solvent. After 7 hours of reaction the aldehyde conversion was 62%. The p-peroxytoluic acid selectivity was 69%.
Example 10
Oxidation of o-tolualdehyde with Oxygen under Superatmospheric Pressure
A 10% strength by weight solution of o-tolualdehyde in acetone was oxidized at 5 bar and 30° C. with pure oxygen in a magnetically stirred 10 ml glass autoclave. After 1.5 hours the aldehyde conversion was about 80%. o-Peroxytoluic acid had been formed with a selectivity of >90%. The rest was chiefly o-toluic acid. By-products such as phthalide, toluene, o-cresol and o-cresol formate were formed with a selectivity of only about 0.2%.
The oxidation could also be carried out in more concentrated solutions. The oxidation of a 20% strength by weight solution of o-tolualdehyde (30° C., 5 bar oxygen, 3 hours reaction time) yielded the corresponding peroxyacid with a selectivity of about 93% (aldehyde conversion: 90%).
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Preparation of epoxides from olefins by means of aromatic peroxycarboxylic acids comprises a step A of epoxidizing the olefin and removing the resulting aromatic carboxylic acid from the epoxide, a step B of catalytically hydrogenating the removed aromatic carboxylic acid to the corresponding aromatic aldehyde, and a step C of oxidizing this aldehyde with oxygen or an oxygen-containing gas mixture back to the aromatic peroxycarboxylic acid for re-use for epoxidizing an olefin.
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CROSS-REFERENCE TO RELATED PATENT APPLICATIONS
This application is related to co-pending U.S. patent application Ser. No. 09/573,805, filed May 18, 2000.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to color inkjet recording films, and, more particularly, to water-resistant color-receptive films coated with lightly crosslinked copolymers of vinyl pyrrolidone (VP) and dimethylaminopropyl methacrylamide (DMAPMA).
2. Description of the Prior Art
The advent of color inkjet printing has been instrumental in fueling the print-on-demand revolution and has also created a number of challenges. Often, the surface of the desired media does not possess the necessary properties for accepting the ink-jet ink. This results in long dry times and/or a poor ink-jet image. It has long been recognized that a surface treatment or media coating plays a critical role in the final print quality. Numerous media coatings are known in the art. They may contain any number of components and often consist of more than one layer. These ink-receptive coatings generally contain at least one hydrophilic polymer; often poly(vinylpyrrolidone) (PVP). PVP brings many benefits to properly formulated media coatings including rapid ink dry time, excellent print quality, highly resolved circular dots, and high, uniform optical density. Furthermore, copolymers of vinylpyrrolidone (VP) along with other suitable comonomers, such as dimethylaminoethyl methacrylamide (DMAPMA), acrylic acid, or vinyl acetate, have been used separately or in conjunction with PVP, to further optimize performance. However, it is desired also to provide long-term, excellent water-resistant qualities for such films.
SUMMARY OF THE INVENTION
What is described herein is a process for preparing a lightly-crosslinked copolymer of (a) vinyl pyrrolidone (VP) and (b) dimethylaminopropyl methacrylamide (DMAPMA) under more reproducible conditions. Suitably the weight ratio of (a):(b) is 50-90:50-5, preferably 80:20. The copolymer has a Brookfield viscosity of 5,000 to 45,000 cps; preferably 10,000 to 30,000 cps, and a haze of <100 NTU; it includes about 0.1 to 0.5 wt. %, preferably 0.2 to 0.4 wt. %, of a cross-linking agent based upon the total weight of monomers in the copolymer.
Preferably the crosslinking agent is pentaerythritol triallyl ether (PETE), and the polymerization initiator is an azo-type initiator.
The ink-receptive film of the invention is capable of being printed from a color inkjet printer to form superior water-resistant color images thereon.
DETAILED DESCRIPTION OF THE INVENTION
EXAMPLES 1-3
Process Examples
Example 1
1. To a 2-l kettle fitted with a nitrogen inlet tube, thermocouple, agitator, and feed lines is added 87.15 g of vinyl pyrrolidone HPVP, 697 g DI water of 0.275 g (0.25% based upon monomer) pentaerythritol triallyl ether.
2. Purge with nitrogen subsurface for 30 minutes.
3. Heat to 70° C.
4. In a separate container weigh out 22.69 g DMAPMA.
5. When kettle temperature is at 70° C., stop subsurface nitrogen purge and purge above surface. Precharge 1.1 g DMAPMA from container.
6. Start continuous addition of the remaining DMAPMA (21.86 g) over 210 minutes. Flow rate 0.1 ml/minute. Once DMAPMA flow started initiate with first shot of Vazo® 67 in isopropanol IPA (Time 0).
7. Initiator is added in 5 shots at 0, 30, 60, 150, and 210 minutes. 0.2 grams of Vazo® 67 in 1.0 g IPA is added for each shot and two 0.5 g IPA washes are made.
8. Hold the reaction temperature overnight at 70° C.
9. When VP is below 400 ppm dilute the batch with 266.7 g DI water.
10. Cool batch to 50° C.
11. Neutralize the batch with conc. HCl to pH of 6.2 to 6.8 at 50° C. Room temperature pH will be 6.8 to 7.2. Requires approximately 14 g of conc. HCl.
12. Add 0.15 to 0.19% of preservative.
Example 2
1. To a 2-l kettle fitted with a nitrogen inlet tube, thermocouple, agitator, and feed lines is added 87.15 g of HPVP, 697 g DI water and 0.275 g (0.25% based upon monomer) pentaerythritol triallyl ether.
2. Purge with nitrogen subsurface for 30 minutes.
3. Heat to 70° C.
4. In a separate container weigh out 22.69 g DMAPMA.
5. When kettle temperature is at 70° C., stop subsurface nitrogen purge and purge above surface. Precharge 1.1 g DMAPMA from container.
6. Start continuous addition of the remaining DMAPMA (21.86 g) over 210 minutes. Flow rate 0.1.1 ml/minute. Once DMAPMA flow started initiate with first shot of Vazo® 67 in IPA (Time 0).
7. Initiator is added in 5 shots at 0, 30, 60, 150, and 210 minutes. 0.3 grams of Vazo® 67 in 1.0 g IPA is added for each shot and two 0.5 g IPA washes are made.
8. Hold the reaction temperature overnight at 70° C.
9. When VP is below 400 ppm dilute the batch with 266.7 g DI water.
10. Cool batch to 50° C.
11. Neutralize the batch with conc. HCl to pH of 6.2 to 6.8 at 50° C. Room temperature pH will be 6.8 to 7.2. Requires approximately 14 g of conc. HCl.
12. Add 0.15 to 0.19% of preservative.
Example 3
1. To a 2-l kettle fitted with a nitrogen inlet tube, thermocouple, agitator, and feed lines is added 87.15 g of HPVP, 630 g DI water and 0.33 g (0.3% based upon monomer) pentaerythritol triallyl ether.
2. Purge with nitrogen subsurface for 30 minutes.
3. Heat to 70° C.
4. In a separate container weigh out 22.69 g DMAPMA and 67 g DI water. Purge with nitrogen 30 minutes. Continue nitrogen purge while feeding.
5. When kettle temperature is at 70° C., stop subsurface nitrogen purge and purge above surface. Precharge 4.23 g DMAPMA/water from container.
6. Start continuous addition of the remaining DMAPMA water (85.46 g) over 210 minutes. Flow rate 0.40 ml/minute. Once DMAPMA/water flow started initiate with first shot of Vazo® 67 in IPA (Time 0).
7. Initiator is added in 5 shots at 0, 30, 60, 150, and 210 minutes. 0.4 grams of Vazo® 67 in 1.0 g IPA is added for each shot and two 0.5 g IPA washes are made.
8. Hold the reaction temperature overnight at 70° C.
9. When VP is below 400 ppm dilute the batch with 266.7 g DI water.
10. Cool batch to 50° C.
11. Neutralize the batch with conc. HCl to pH of 6.2 to 6.8 at 50° C. Room temperature pH will be 6.8 to 7.2. Requires approximately 14 g of conc. HCl.
12. Add 0.15 to 0.19% of preservative.
Test Methods
Drawdowns from a 10% aqueous solution of the polymer were cast onto a polyester substrate using a #38 Mayer bar and allowed to dry in an oven at 100° C. to give a dry coating thickness of ˜9 micron.
Coated samples were then printed using a HP 832C printer at 600 DPI in “HP Premium Photo Paper” mode. Individual blocks of cyan(C), magenta(M), yellow(Y), and black(K), approximately 1″×1.75″ in size, were printed side by side. Small blocks of C, M, Y, and K, approximately ⅛″×¼″, are printed repeatedly down one edge of the page to provide a built-in time-line for measuring off-set time as described below.
Off-set time is the minimum time required for no ink to transfer to a cover sheet placed on top of the print when contacted with a 4-lb roller immediately after printing. Ink transfer is determined at the point where the OD after testing dropped by a value of 0.2 units. For off-set times are most desirable.
Water-resistance was measured by the standard test procedure set forth below*.
* Water resistance was tested by placing the printed sheet at a 45° angle and dripping 10 ml of water at a constant rate (2 ml/min) over the surface for a maximum of 5 minutes. The samples were then judged by following rating system:
Poor—All ink removed in less than 1 minute.
Fair—Most or all ink removed between 1 and 5 minutes.
Moderate—Some (<50%) loss of ink after 5 minutes.
Good—Very slight (<10%) loss of ink with minimal running.
Very Good—100% water resistance with no change in appearance.
Results
The results of these tests, shown in Table 1 below, establish that the lightly-crosslinked VP/DMAPMA copolymer exhibits an advantageous water-resistant property as well as desired viscosity and haze properties.
The crosslinker suitably is a di-, tri- or poly-functional crosslinking agent, such as pentaerythritol triallyl ether (PETE); diethylene glycol di(meth)acrylate; triethylene glycol di(meth)acrylate; or polyethyleneglycol di(meth)acrylate.
The polymerization initiators suitably is an azo type such as Vazo® 52, 64 or 67.
TABLE 1
WATER-
Ex.
X-Linker*
Initiator**
VP
Haze
VISC
PROOF
No.
(%)
(g/shot)
(ppm)
(NTU)***
(cps)
(min)
1
0.25
0.2
139
28200
10
2
0.25
0.3
151
25.2
13000
11
3
0.3
0.4
173
45.7
12800
7.12
*Based on total monomers
**A total of 5 shots
***NTU = nephelometric turbidity unit
The offset times of Examples 1-3 were <1 minute.
While the invention has been described with particular reference to certain embodiments thereof, it will be understood that changes and modifications may be made which are within the skill of the art. Accordingly, it is intended to be bound only by the following claims, in which:
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What is described herein is a process for preparing a lightly-crosslinked copolymer of (a) vinyl pyrrolidone (VP) and (b) dimethylaminopropyl methacrylamide (DMAPMA) under more reproducible conditions. Suitably the weight ratio of (a):(b) is 50-95:50-5, preferably 80:20. The copolymer has a Brookfield viscosity of 5,000 to 45,000 cps; preferably 10,000 to 30,000 cps, and a haze of <100 NTU; it includes about 0.1 to 0.5 wt. %, preferably 0.2 to 0.4 wt. %, of a cross-linking agent based upon the total weight of the monomers in the copolymer.
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CROSS REFERENCE TO RELATED APPLICATION
This application is a standard utility based upon provisional patent application Ser. No. 60/484,621, filed Jul. 2, 2003, the contents of which are incorporated herein.
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates in general to methods for return shipping of goods. Specifically, the present invention relates to methods of doing business that optimize the return of goods under warranty claims, when the good is damaged, the wrong size, or not the good the customer expected, etc. More particularly, the present invention relates to methods of doing business that optimize the return of goods to one or a few sources from a significant number of customers.
2. Background Information
The current global economy is based upon numerous sellers who provide a vast array of goods. Advancements in technological resources and in global marketing have enabled sellers to reach customers throughout the world. Clearly, these sellers require logistical support to deliver their goods to their customers worldwide. The term seller (“Seller”) broadly includes any individual or entity that provides goods, which may include the manufacturer, a wholesaler, a distributor, a dealer or a retailer, and the term customer (“Customer”) broadly includes any individual or entity that receives goods, which may include an intermediate manufacturer, a wholesaler, a distributor, a dealer, a retailer, or any other end customer. Goods include tangible property in any shape, form, or size (“Goods”). The process of “forward logistics” captures the systematic transfer of goods from the seller to the customer. This process may contain a series of steps from one end of the transaction to the other.
For purposes of describing the forward logistics process, the seller is considered the party who currently has the goods, and the customer is the party who will be receiving the goods. These parties may or may not be the “initial” manufacturer or the “end” customer. Rather, the terminology refers to two parties who directly abut one another in the chain of distribution. Any participant in this chain of distribution will employ the services of a transportation company (“carrier”) to deliver the goods from them to the next party in the chain. The chain includes, but is not limited to, manufacturers, wholesalers, distributors, dealers, retailers, and end customers.
The seller is generally a well-established company that employs the services of one or more carriers to move the goods from them to the next participant in the chain. This process is repeated as the goods move through the chain of commerce. The seller and customer have a well defined relationship and the forward logistics process in its most simplistic form takes the following methodology: a seller receives an order from an end customer, packages the order, prepares shipping documentation known as a “bill of lading,” and contacts its preferred carrier who picks up the goods during its scheduled daily coverage of the region where the seller is located. In many instances, this process is automated and software readily tracks the shipment. The current information systems sufficiently track the movement of goods given the limited number of carriers and the close relationships between sellers and their carriers. These current information systems are very desirable to the sellers, carriers and customers as they are generally efficient, accurate, convenient, affective and provide real-time information, and as a result most sellers, carriers and customers would agree that this “forward logistics” system works efficiently and effectively. The seller who is typically paying the freight invoice optimizes the time, size, cost, etc. of the shipment. The seller readily understands the most cost effective, timely and efficient manner of shipping its goods based upon a variety of factors, including: shipment destination, timing, urgency, size of order, etc. In addition, the seller chooses the best shipping method, which may range from a small box to an entire truck and the best shipping mode, which may involve transportation by ground or by air.
However, in some cases the good shipped is the wrong good, size, shape, color, type, kind, etc., the customer merely does not like the good now that the customer has received it, or initially likes and begins using the good but then has a warranty claim, etc. Basically, the customer did not get what they wanted or the customer needs to make a warranty claim, or for any other reason the customer wants to return the good. In any case, the good may have to be returned to the seller. The good must be returned from the customer via some carrier to the seller. This return process is known as “reverse logistics”, and is performed by a reverse logistics provider (“provider”).
The most common “reverse logistics” scenario involves the last participant in the chain that takes part in manufacturing the good or its distributor is the seller, and a dealer or store is the customer. Given the shear volume of “forward logistics” transactions that take place daily, it is common that a small but still material percentage of these shipments will have to be returned by utilizing the “reverse logistics” process.
In a typical reverse logistics process, a customer calls the seller to request a return or reverse shipment. The carrier has no information on the good (unlike the forward logistics movement where the seller and the carrier perform numerous transactions and create a close working relationship), and must obtain the specifics regarding the good to be returned such as size, shape, weight, priority, etc. The provider creates a bill of lading that is typically faxed to the customer (who has already received the good and will be the “shipper” when returning it) and entered into the provider's electronic database who notifies the carrier of the pick up need. Carrier picks up the good during either its scheduled daily coverage of the region where the customer is located or when it is next geographically near the customer (except where an express or priority shipment is requested), and takes it to the provider's warehouse. At the warehouse, the provider will typically (1) validate the good as being the good identified on the bill of lading, and may even compare it to a predetermined good value list the provider has for the seller, (2) inspect the returned good, and (3) enter pertinent information including value of the good and inspection into a warehouse application that is then transmitted to the provider's main office. Information is typically gathered together at the main office and electronically delivered to the seller, who then credits the customer's account.
The “reverse logistics process,” as described thus far, suffers from a number of defects and inefficiencies. First, the verification that the good picked up is the good noted on the bill of lading often does not occur until the good is delivered to the provider's warehouse. Second, verification that the good picked up matches a model number that the seller actually delivered to the customer often does not occur until the good is delivered to the provider's warehouse. Third, a serial number or other form of identification cannot be compared against a master seller list, which is necessary to verify the warranty claim or return, until the good is delivered to the provider's warehouse. Finally, the quantity of that particular good sold to that particular customer in comparison to the quantity of that particular good returned by that particular customer, does not occur until the good is delivered to the provider's warehouse. These examples are merely a sampling of the inherent deficiencies in the current “reverse logistics” process. Clearly, a better solution is needed.
BRIEF SUMMARY OF THE INVENTION
A reverse logistics process is invented for automating and optimizing the return of goods such as, goods under warranty claims or where the good is damaged, the wrong size or other parameter, or not the good the customer expected, etc. The reverse logistics process includes: the customer inputting information on a website regarding the good they wish to return, the provider verifying whether the good may be returned by comparing the information the customer provided with its own database information, and upon verification, the provider determining the most efficient shipping method for returning the good based upon the seller's needs.
The foregoing advantages, construction and operation of the present invention will become more readily apparent from the following description and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiment of the invention, illustrative of the best mode in which applicant has contemplated applying the principles, are set forth in the following description and are shown in the drawings and are particularly and distinctly pointed out and set forth in the appended claims.
FIG. 1 is a diagram of the process.
Similar numerals refer to similar parts throughout the drawings.
DETAILED DESCRIPTION OF THE INVENTION
The reverse logistics process of the present invention is generally defined below and assumes that a seller, who might be a manufacturer, distributor or other party hereinafter referred to as the seller, has shipped goods via a carrier to a customer, who might be a distributor, dealer, retailer, or end consumer hereinafter referred to as the customer. This customer desires for any of a variety of reasons to return one or more of the goods. There are a number of reasons why a good is returned including, the wrong good was shipped, the good is of the wrong size or other characteristic such as shape, color, type, kind, etc., the customer does not like the good, the good is defective and is under warranty, the good has been recalled, or any other reason that a good could be returned. This good must now be returned from the customer via some provider or carrier to the seller. This return process in general is known as the “reverse logistics process.”
The present invention is a unique, non-obvious and novel reverse logistics process or method that optimizes the returning of a good to a seller that is one of many goods distributed to many customers. In the forward logistics process of distributing the goods, the seller controls the distribution through one or more carriers controlled and hired by the seller, and the seller knows the details about every shipment including which good is in each shipment, what model and/or serial numbers, what sizes, what colors, etc. The present invention optimizes the far more difficult reverse logistics process where one or more of the many customers who received one or more of the many goods the seller sells needs to return a good from the many sold by the seller. In this reverse logistics case, the customer, not the seller, has the goods to be returned and thus many difficulties arise as noted above in the background including lack of or difficulty in: 1.) acquiring information on the good, 2.) centralized control of the carrier and shipment, 3.) assuring the correct good is returned to proper location, 4.) verifying that the good being returned is eligible for return, 5.) verifying that the customer is eligible to return the good, 6.) avoiding fraud in the returns process such as where a customer returns more of the good than they ever ordered, etc.
In general, one embodiment of the reverse logistics process of the present invention involves the following steps: (1) information input via a website or other electronic communication channel on the good to be returned, known hereinafter as information input step, (2) comparison of information inputted in the information input step against a provider database, known hereinafter as verification step which may include one or more of several sub-steps such as verifying the good is a seller good, verifying the good is eligible for warranty, verifying serial number, and approval of return, (3) provider database provides critical characteristics on good to be returned known hereinafter as critical characteristic definition step, (4) queuing of return, known hereinafter as queuing step, (5) shipping instructions created including such sub-steps as the creation of a of packing slip and other necessary shipping and warranty paperwork, known hereinafter as shipping instructions step, (6) shipping request is made to carrier, known hereinafter as shipping request step, and (7) return shipping occurs under a typical shipping process as known in the art including (a) carrier picks up the good to be returned, and (b) carrier takes the good to be returned to one or more provider warehouses and eventually returns the good to seller whereby provider has less good validation to perform. The reason for less good validation is that most of the validation occurred in steps (2) to (6) between the customer and provider prior to the carrier becoming involved.
In detail, one example of the first embodiment of the process begins with the customer, who desires to return a good, logging into a provider web site which contains an administrative database. This web site may be encrypted and/or password protected, and is a web site that the provider provides for the seller. The customer will perform the information input step by inputting data using one or more of a keyboard, mouse, scanner, optical reader, voice recognition input, or the like. The provider web site requires the inputting of certain data as desired or required by the provider and/or seller. Such information may include description of the good, the name of the good, the model number of the good, the serial number of the good, the color of the good, the size of the good, the date the good was ordered, order number associated with original shipment of the good, the delivery date of the good, customer name, customer code, etc. In addition, the provider database is a “smart” database containing seller provided information such as, seller information on all types of goods, model numbers, serial numbers, customers shipped to, etc. and therefore requires accurate information input from the customer desiring the return.
Once this information is inputted into the provider database, the database performs the verification step. In this step, the seller sets forth verification parameters that are desirable to the seller such as, verification that the good is seller's good versus a competitors which may be done by comparison of model or serial numbers. Other verifications that may be performed include: verification that the good is under warranty, by perhaps reviewing the delivery date, verification that the customer has actually purchased that type of good from seller in the past and that the quantity of returns does not exceed the number of purchases, verification that the original manufacturer (“OEM”) of the good desires or allows returns via a middle-man versus directly to the OEM where the seller is not the OEM, etc. The provider database will deny any request with inaccurate, fraudulent or incomplete information thereby assuring only proper authorized returns, i.e., returns of seller's goods within the return or warranty period from a customer certified to make returns, etc. The provider database may also be programmed to perform statistical analysis on specific good types, specific customers, etc. to allow the seller to identify specific good or customers with abnormal rates of returns, etc. that may be investigated by the seller prior to, during or after a return shipment. This would allow the seller to more readily identify at an earlier time repetitive issues such as any carriers that are repeatedly damaging goods, any customers that have an unusually high return rate, etc.
For example, a customer cannot enter the serial number of a transmission to be returned where the serial number corresponds to a brand X transmission when the return is being attempted with a brand Y transmission on provider's database. A second example of the smart characteristics of such a database is as follows: a customer who only originally ordered three widgets from a seller will be denied any attempt to return a fourth widget, under warranty thereby prohibiting excessive fraud where parts are returned that are purchased in the salvage market, etc. A third example of the smart characteristics of such a database is as follows: the customer purchased one widget from seller three years ago with a one year warranty and another of the same type widget six months ago with a one year warranty whereby the provider's database requests serial numbers thereby assuring the older good no longer under warranty is not returned as if it were under warranty. These and many other examples show the characteristics of the database at this point in the reverse logistics process and how the seller saves significant money by never wrongly agreeing to return these goods.
Once all programmed verifications have occurred, the database provides either an approval or denial of the return. This approval is the approval verification sub-step of the verification step.
Critical characteristics are then provided by the provider database to optimize shipping. These may include shipping parameters such as return delivery speed for perishable items, packing requirements for fragile goods, as well as size and weight parameters to assist in optimization of the truck size or number of trucks needed. The size and weight parameters are critical in allowing the provider to choose the proper mode of carriage. Shipping rates vary amongst motor carriers whereby certain companies rates and timing to ship a small package may be optimal while their ability to ship a partial or full truck may not be optimal, or they may not even offer such a large shipment option. In other cases, a certain carrier may be optimal for the larger returns. Distances for the shipment may also be a factor in motor carrier choice as certain carriers may not provide shipping to all locations, or may be more expensive or not timely for certain pick-ups or destinations. The provider database may include the rates, tariffs and limitations of the approved carriers and optimizes the return shipment parameters to provide the optimized cost and timing for the return shipment. The critical characteristics step produces two outputs that optimize the reverse logistics process including, size and weight parameters that the customer uses to determine the optimal carrier or an instruction on which carrier to use based upon the size, weight and distance parameters.
The shipment is queued after a carrier is determined. This determination is based upon the critical characteristics. The queuing step involves both (a) placing the shipment in a standard carrier's queue such that the carrier will pick up the return shipment either on its usual daily or routine rounds or on a more urgent basis if needed, and (b) verifying the return shipment meets standard return shipment parameters between that particular customer and the seller. Such standard return shipping parameters may be any queuing rules between the parties including no more than a set number of return shipments per period unless customer pays for extra return shipments. The queue is typically maintained by the provider with information thereon transmitted via the web or a database to seller and customer.
Once the return shipment is queued, optimized shipping instructions are transmitted to the customer. In this shipping instructions step, shipping instructions are created, which include a packing slip, bill of lading, and other necessary shipping and warranty paperwork. This paperwork is typically created by the web site and printable at the customer's location.
The shipping request is made to carrier by transmitting the shipping instructions to the carrier. At the proper time based upon the queuing, the carrier arrives at the customer location for return shipping. The carrier picks up the return good, transports it to a designated provider warehouse, and returns it to seller. The customer's account is then credited.
In sum, the process involves the following steps: (1) information input step, (2) verification step, (3) critical characteristic definition step, (4) queuing step, (5) shipping instructions step, (6) shipping request step, and (7) return shipping occurs under a typical shipping process as known in the art including (a) carrier picks up good to be returned, and (b) carrier takes good to be returned to a designated provider warehouse and eventually returns good to seller.
The above process is one embodiment of the reverse logistics method of the current invention. Many other embodiments are contemplated. These include embodiment with the following features or variations.
The information input step is any form of inputting general information on the customer and the good to be returned to the seller. Such step may involve use of the internet or other common worldwide publicly-available network, or alternatively a secure private seller or carrier network that the customer accesses via a telephonic, cable-modem, modem, DSL, T-1 or other high speed connection. The software may be downloaded or otherwise provided to the customer, or most preferably is a web-site with software that is maintained by the provider on its network whereby the customer logs in and uses its interface and database in a select and secure manner. Preferably, the software and/or user interface guides the customer through the questions that need to be answered and only allows the customer to proceed if all questions are answered with accurate and correct information.
This involves the verification step where many pieces of information may be verified including that the good is a seller good rather than a competitor good, that the good is eligible for warranty, that the good is eligible for return versus an “all sales final” or other clearance sale good, that the customer knows the serial number and such serial number is one of the seller's goods, that the customer is a customer of the seller, that the customer is current on its account with seller, and if these and any other verifications the seller or provider requires are sufficiently answered in an acceptable manner, then approval of return is given. This verification step is performed on a computer housing a provider database containing critical information on the seller goods, customers, etc. The database interacts with the customer inputted information from the input step to perform this verification. The database may be any form of an electronic database that has “smart” capabilities allowing for it to be searched, prioritized, categorized or otherwise able to manipulate and sort data. The database also in various embodiments provides critical characteristics on good to be returned. These characteristics may be any information known about a good, a customer, a carrier, etc. The database is capable of storing many characteristics on each good, and such useful information may be used for a return good to optimize the return process including speed, type and manner of return.
The customer, provider and seller all use the common reverse logistics database. This assures that all parties have up-to-date information as each thus always has information on the good in question, assurance that the correct good is returned to proper location, verification that the good being returned is eligible for return, verification that the customer is eligible to return the good, assurance that common fraud in the returns process such as where a customer returns more of the good than they ever ordered is avoided.
Accordingly, the invention as described above and understood by one of skill in the art simplifies the reverse logistics process by providing an optimized, effective, and efficient system and process, which eliminates difficulties encountered with prior systems and processes, solves problems, and obtains new results in the art.
In the foregoing description, certain terms have been used for brevity, clearness and understanding; but no unnecessary limitations are to be implied therefrom beyond the requirement of the prior art, because such terms are used for descriptive purposes and are intended to be broadly construed.
Moreover, the invention's description and illustration is by way of example, and the invention's scope is not limited to the exact details shown or described.
Having now described the features, discoveries and principles of the invention, the manner in which it is constructed and used, the characteristics of the construction, and the advantageous, new and useful results obtained; the new and useful structures, devices, elements, arrangements, parts and combinations, are set forth in the appended claims.
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A reverse logistics process or business method that optimizes the return of goods such as the return of goods under warranty claims or where the good is damaged, the wrong size, not the good the customer expected, etc. The system design accounts for the return of goods to one or a few sources after delivery to a significant number of customers.
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BACKGROUND OF THE INVENTION
The present invention relates generally to automatically-controlled marking devices and, more specifically, to devices for spray marking lumber boards at predetermined locations while they are conveyed past the apparatus.
Lumber for use in the manufacture of furniture must be free from defects such as checks, loose knots, or planar skips. Because of the high cost of clear boards of matched lengths, it has become customary to process boards containing imperfections to remove the defects and use the boards so processed to make glued-up stock. In the past, such processing of defective boards has entailed manually severing the boards to cut out the imperfect parts. These operations have been labor intensive, and as a result of their reliance on human judgment to determine how and where boards should be cut, the lumber has not always been processed with maximum efficiency.
Consequently, computer-controlled sawing systems have been developed to process lumber to be used in the manufacture of glued-up stock. These operations normally involve several processing steps, including visually inspecting the lumber and marking any defects with luminous paint, scanning the boards to detect and record the relative positions of the marked defects, automatically computing the most efficient way to cut the boards, and then ripping and crosscutting the boards to remove the defects.
Before the boards are ripped, those parts of the boards which will comprise strips after the ripping operation are marked at the points at which they are to be crosscut. Crosscutting is then later automatically accomplished after ripping in a separate operation based on the position of the points marked on each strip. In order to provide for the continuous operation of the machinery, the lumber should be marked while it is in the process of being conveyed. Spray marking has been found to be the only reliable method of applying marks to the rough surfaces of lumber boards while they are moving relative to the marking device. The spray marks must, however, be accurately located on the surfaces of the boards and be sufficiently well-defined so as to be easily detectable. Furthermore, the spray marks must be applied at high speed so as not to impede the progress of the processing operation.
Accordingly, it is a principle object of the present invention to provide a lumber board making apparatus capable of reliably spray marking moving lumber boards at predetermined locations.
It is another object of the present invention to provide a board marking apparatus capable of accurately applying marks to lumber boards with sufficient speed so as not to impede the progress of associated processing operations.
It is a further object of the present invention to provide a lumber board marking apparatus capable of applying well-defined and easily detected marks to moving boards and to provide a marking apparatus otherwise well suited to the purposes for which the same is intended.
SUMMARY OF THE INVENTION
An apparatus for spray marking boards moving on a conveyor comprising a tachometer and photoelectric unit, a solenoid operated paint sprayer, and corresponding circuitry for processing of electric signals from the tachometer and photoelectric unit and control of the paint sprayer. The tachometer and photoelectric unit measure the speed and define the location of boards on the conveyor. The paint sprayer applies marks to the board by use of a straight line flow path atomizing air nozzle. The timing of the application of the marks to the boards and, therefore, the location of the marks is controlled by special circuitry associated with the tachometer, photoelectric unit, and paint sprayer. This circuitry acts to provide correction information to the controlling computer and to process instructions from the computer to the sprayer so the paint marks may be applied accurately to the boards under all conditions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially broken away pictorial view of the present invention and overall system in which it operates.
FIG. 2 is a detailed side view of one of the paint sprayers of the present invention.
FIG. 3 is a circuit diagram of certain electronic components associated with the tachometer and photoelectric unit of the present invention.
FIG. 4 is a circuit diagram of the signal processing electronic components which direct the activation of the paint sprayer.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the figures wherein like reference characters designate like or corresponding parts throughout the several views, FIG. 1 shows the components of the present invention disposed in the overall system in which they operate. Boards 10 are inspected by scanner 11 which detects the location of any defects on the boards which are marked with fluorescent paint and delivers this information to computer 12. Computer 12 registers the position of the defects on the boards 10 and calculates the optimum positions at which the boards should be ripped and crosscut to remove the defects. Boards 10 are transferred to the spray marking apparatus 13 where in response to instructions from the computer 12 the boards are marked at the positions at which they will be later crosscut by paint sprayer 20 as they are transported on conveyor 14. After being marked, the boards are automatically ripped into strips 28 by saws 25. The crosscut position marks on these strips 28 are then detected by scanner 26, and these strips are automatically crosscut at these positions by saws 27.
Examining the operation of the spray marking apparatus 13 in greater detail, tachometer generator 17 is attached to the conveyor 14 and produces digital pulses at a rate proportional to the speed of the conveyor. The photoelectric unit comprises sending component 18 and receiver 19 disposed on opposite sides of conveyor 14 which produce a step-down function output when the light path between the two components is interrupted. The output of tachometer generator 17 and the photoelectric unit is coupled to electronic processor 23 which, in turn, communicates with computer 12. As illustrated in FIG. 3, the output of the photoelectric unit is connected to a monostable multivibrator 30 such as a Digital Equipment Corporation K323 circuit board. This multivibrator 30 is coupled to resistor 31 and capacitor 32 which complete the multivibrator circuitry and set the output pulse width. In the instant case, a 2 mfd. capacitor and a 50K resistor may be employed to obtain 8 millisecond wide output pulses from the multivibrator 30 upon activation of the component by a step function input from the photoelectric unit. The output of the multivibrator 30 and of the tachometer 17 are connected to an AND gate 33 such as a Texas Instruments 7400 integrated circuit. The AND gate 33 is connected to the computer 12 and produces a signal output to the computer only when it simultaneously is receiving high-level logic signals from both the multivibrator 30 and the tachometer 17. The output signal is generated when a board interrupts the light path maintained by the photoelectric unit across the conveyor and consists of a series of pulses corresponding in number to the relative speed of the board on the conveyor 14. This signal informs the computer of the location and speed of boards 10 on the conveyor 14.
During its transit across marking apparatus 13, boards 10 are kept transversely positioned by a retaining means 16 which presses them against fence 15. A set of paint sprayers 20 are suspended over the conveyor 14, and over the path of any boards thereon, by a support structure 22 including a set of ball screws 21 by which the transverse position of any of the paint sprayers may be adjusted. In operation, the computer 12 tracks the location of boards on the conveyor 14 and consistent with its computations of where the boards 10 should be optimumly ripped and crosscut positions the paint sprayers 24 relative to the fence 15 and signals the paint sprayers to mark the boards at the desired positions as they pass underneath.
Referring now to FIG. 2, paint sprayer 20 is supplied with pressurized air by line 51 leading to paint reservoir 52 and by line 53 leading to air valve 54. Reservoir 52 is, in turn, connected by line 55 to paint valve 56. Air valve 54 and paint valve 56 are operated by solenoids 57 and 58 respectively. Solenoid 57 is connected to electronic processor 23 through junction box 59 by line 60; solenoid 58 is connected to the processor through junction box 59 by line 61. Electronic processor 23 receives input from computer 12, which input comprises signals directing the activation of the paint sprayer. Processor 23 coordinates these signals with the mechanical operation of the paint sprayer properly sequencing the activation of the air and paint valves so the paint marks may be efficiently applied to the boards. Air valve 54 and paint valve 56 are connected to nozzle 64 by line 63 and coupling plug 65 respectively. Nozzle 64 is an atomizing air nozzle having a straight line flow path to minimize plugging problems and is equipped with a fan-patterned atomizing air nozzle tip 66.
On account of the position of the valves relative to the nozzles and the properties of the fluids being employed, the air valve 54 must be activated prior to activating the paint valve 56 in order to provide well-defined marks with paint sprayer 20; and for optimum results, the air valve should be operated for 4-8 milliseconds and then after a 2-4 millisecond delay, the paint valve should be operated for 2-3 milliseconds. The circuit illustrated in FIG. 4 provides this sequencing of valve operations by controlling the activation of solenoids 57 and 58 on receipt pulse signals from the computer 12 directing operation of the paint sprayer 20.
The output signal from computer 12 is coupled to monostable multivibrator 70 which is adjusted to provide a low-level logic output pulse of 4-8 milliseconds duration in response to any pulse inputs from the computer. Multivibrator 70 has one output coupled to monostable multivibrator 71 which is adjusted to provide a high-level logic output pulse of 2-4 milliseconds duration when triggered by the voltage step-up at the trailing edge of pulses from multivibrator 70. The output of multivibrator 71 is, in turn, coupled to monostable multivibrator 72 which is adjusted to provide a low-level logic output pulse of 2-3 milliseconds duration when triggered by the voltage step-down at the trailing edge of the pulses from multivibrator 72. Multivibrators 70, 71, and 72 may be any standard monostable multivibrators such as the type supplied on a Digital Equipment Corporation K-323 circuit board. The resulting coordinated outputs on lines 73 and 74 are a 4-8 millisecond pulse on line 73 followed after a 2-4 millisecond interval by a 2-3 millisecond pulse on line 74. These pulses are coupled through buffers 75 and 76 which are connected to a 5 volt source through pull-up resistors 78 and 79 and function to increase the voltage level and power of the pulses. Buffers 75 and 76 may be any two input positive NAND buffers such as Texas Instruments SN7438 integrated circuits. The output of buffers 75 and 76 is coupled to the bases of power transistors 80 and 81, such as RCA 2N6533 Darlington transistors. The emitters of power transistors 80 and 81 are connected to ground, and their collectors are connected to a 50 volt power source through solenoids 57 and 58 respectively. Resistors 83, 84, 85, and 86 are employed to pull up the output of the buffers 75 and 76 and to provide biasing to the transistors 80 and 81. Zener diodes 87 and 88 and capacitors 89 and 90 are employed to protect the circuit components against voltage spikes, caused by the switching action of the transistors and the action of the solenoids, and to protect the circuit against noise, respectively. When coupled through buffers 75 and 76 and output transistors 80 and 81 to solenoids 57 and 58, the pulses from lines 73 and 74 provide for the operation of solenoids 57 and 58 with proper valve action sequence timing; namely, the operation of the air valve for 4-8 milliseconds and then the operation of the paint valve for 2-3 milliseconds after a 2-4 millisecond delay.
Since many changes could be made in the above construction and many apparently widely different embodiments of this invention could be made without departing from the scope thereof, it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense.
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An apparatus for spray marking lumber boards with paint at predetermined locations while they are being conveyed past the device for further processing. A tachometer and a photoelectric unit are employed for determining the location and speed of the board. A solenoid-operated paint sprayer is used to deliver the paint to the boards. Electronic control circuitry is provided to activate the paint sprayer and properly coordinate the operation of paint sprayer with the location and speed of the board so the board is marked at the desired locations.
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FIELD OF THE INVENTION
The present invention relates generally to circuit breakers. More specifically, the present invention relates to an auxiliary switch for a circuit breaker which is capable of switching substantially the rated interrupt current of the circuit breaker.
BACKGROUND OF THE INVENTION
Control panel systems, having a variety of panel mounted circuit breakers mounted thereon, are often sold in both the United States and Europe to provide branch circuit protection or supplementary (equipment) protection. By way of example, circuit breakers are often mounted in theater lighting control panel systems to provide protection for branch circuits which supply electrical power to the various lights of a theater. Alternatively, circuit breakers can also be mounted in control panels to provide dedicated supplementary protection to equipment such as computers, power supplies or copying machines.
Circuit protection standards vary between the United States and Europe, and impose different performance requirements on the circuit breakers involved. For example, U.S. standards rarely allow the provision of a disconnect to the neutral (return) side of a circuit load, while European standards often require it. European standards for a neutral disconnect effectively requires the addition of another switch, capable of handling the rated interrupt current capacity of the circuit breaker, when connected in series with the circuit breaker and the load. Rated interrupt current, i.e., interrupting rating, is defined in article 100 of the 1996 edition of the National Electric Code, published by the National Fire Protection Association, Quincy, Mass., as: “the highest current at rated voltage that a device is intended to interrupt under standard test conditions”. The interrupt current and the standard test conditions for a device, such as a circuit breaker, would typically be specified in an industry excepted standard, e.g., UL 1077, titled Standard For Supplementary Protectors For Use In Electrical Equipment, or UL489, titled Standard For Molded Case Circuit Breakers And Circuit Breaker Enclosures. Prior art attempts to modify existing U.S. circuit breakers to provide neutral side disconnects involved stacking a second pole up against the single pole circuit breaker, effectively doubling the width and size of such an assembly.
However, space is a premium in control panel systems. In the telecommunication industry, for example, telecommunication equipment designers can earn bonuses of up to $1000 for every square inch of panel space saved. Consequently, there is often very little panel space to accommodate the additional second pole for the circuit breakers without an expensive redesign of the system. This is especially critical when the additional requirements increase the overall package width, since the circuit breakers are often stacked side by side, leaving very little space in between for growth.
Auxiliary switches are often mounted to the bottom portions of circuit breakers to provide an extra set of switching contacts without a significant increase in overall package size or width. However, auxiliary switches are primarily used to indicate status of the circuit breaker, e.g., whether the circuit breaker is open or closed, and typically have current switching capacities which are much lower than the interrupt current capacity rating of the main breaker. The low power auxiliary switches are constructed of much smaller components and require much less space to actuate than the main contacts of the circuit breaker.
To construct an auxiliary switch capable of switching the rated interrupt current capacity of its associated circuit breaker with a minimum impact in overall package width is problematic for several reasons. For example, the contact gap spaces and spring forces for the auxiliary switch must increase, tending to increase the package size and width. Also, since the auxiliary contacts are mechanically actuated by the main breaker contacts, the increased spring forces from the auxiliary switch actuator acting on the main breaker contacts may significantly change the main breaker contact pressure. This can result in excessive arcing and premature circuit breaker contact wear.
Another significant factor which tends to make the auxiliary switch package grow is that the higher power requirements can result in greater arcing during make (make contact) or break (break contact) of the auxiliary contacts. This increases the possibility of welding the contacts together or leaving debris and carbon deposits on the contacts. This problem is often minimized in the main circuit breaker with a lateral wiping action designed between the movable and stationary contacts of the main breaker. The wiping action is used to clean the contacts and shear away any welds as the contacts make or break. That is, the moveable contacts of the main circuit breaker pivots on a moveable contact lever to make contact with the stationary contact. A generally kidney shaped slot at the pivot point of the movable contact lever is fundamental to this arcuate motion. This slot is easily elongated to provide for over travel in the lateral directions of the contacts relative to each other, which results in the wiping action.
However, auxiliary switch contacts are typically designed to have a substantially linear motion when bridging the contact gaps (bridge contacts), rather than the arcuate motion described above for the main breaker contacts. Problematically, the bridge contacts are not conducive to providing a wiping action in the lateral direction. The arcing problem can be compensated for by increasing the size of the auxiliary contacts and their associated contact gaps, but this tends to unduly increase the overall package size and width.
Accordingly, there is a need for an improved auxiliary switch for a circuit breaker, which is capable of switching the rated interrupt current capacity of the associated circuit breaker.
SUMMARY OF THE INVENTION
The present invention offers advantages and alternative over the prior art by providing an auxiliary switch for a circuit breaker capable of switching the rated interrupt current capacity of the breaker. The auxiliary switch/circuit breaker assembly can be used to provide neutral disconnects to an existing control panel system to meet European standards.
These and other advantages are accomplished in an exemplary embodiment of the invention by providing a circuit breaker assembly comprising a circuit breaker and an auxiliary switch. The circuit breaker has a predetermined rated interrupt current capacity, and includes a movable contact lever having a circuit breaker moveable contact disposed thereon. The contact lever has an open position and a closed position. The auxiliary switch includes a switch housing mounted in an opening defined by the circuit breaker. An auxiliary actuator is movably mounted within the switch housing and has an upper portion of the auxiliary actuator protruding into the opening of the circuit breaker from the switch housing. An auxiliary moveable contact member has an auxiliary moveable contact disposed thereon, the member is moveably mounted to the auxiliary actuator. A contact spring acts between the auxiliary actuator and the auxiliary moveable contact member. An auxiliary stationary contact is arranged in the switch housing for engagement with the auxiliary moveable contact. A return spring is disposed between the switch housing and auxiliary actuator urging the auxiliary stationary and moveable contacts apart. The auxiliary switch is adapted to switch substantially the rated interrupt current of the circuit breaker through the moveable and stationary auxiliary contacts when the moveable contact lever of the circuit breaker moves from the open position to the close position, thereby depressing the auxiliary actuator to have the auxiliary moveable contact make contact with the auxiliary stationary contact.
In an alternative embodiment of the invention the overall width of the auxiliary switch is substantially equal to or less than the overall width of the circuit breaker.
Several embodiments of the auxiliary switch disclose various features which contribute to increasing the interrupt current rating and/or down sizing the width of the auxiliary switch. Among them are:
an early make, late break of the auxiliary contacts compared to the circuit breaker contacts;
an inertia dampening fly wheel attached to the actuator of the switch to enhance the early make/late break feature;
a wiping action between the moveable and stationary contacts of the auxiliary switch to clean off welding and debris deposited from arcing;
dual auxiliary contacts to enhance the contact area with little impact on package size and width; and
a positioning of the auxiliary actuator on the contact lever of the circuit breaker to prevent the spring forces acting on the actuator from affecting circuit breaker contact pressure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a circuit breaker assembly in accordance with the present invention;
FIG. 2 is a side view of FIG. 1;
FIG. 3 is a perspective view of the interior of the circuit breaker assembly with the circuit breaker moveable contact lever in the open position;
FIG. 4 is a perspective view of the interior of the circuit breaker assembly with the circuit breaker moveable contact lever in the closed position;
FIG. 5 is a perspective view of an embodiment of the auxiliary switch showing an inertia dampening fly wheel in accordance with the present invention;
FIG. 6 is a perspective view of an embodiment of the auxiliary switch showing a canted moveable contact member in accordance with the present invention;
FIG. 7 is a side view of the actuator of the switch in FIG. 6;
FIG. 8 is an enlarged view of the moveable and stationary contact of the auxiliary switch of FIG. 6 with their centerlines offset;
FIG. 9 is an enlarged view of the moveable and stationary contact of the auxiliary switch of FIG. 6 with their centerlines aligned;
FIG. 10 is a force balance diagram on the moveable contact lever of the circuit breaker of FIG. 4 in the closed position;
FIG. 11 is a schematic diagram of the auxiliary switch contacts having a single pole, single throw, double break arrangement;
FIG. 12 is a schematic diagram of the auxiliary switch contacts having a single pole, double throw, double break arrangement;
FIG. 13 is a wiring diagram of the auxiliary switch used as a neutral disconnect with the circuit breaker; and
FIG. 14 is a wiring diagram of the auxiliary switch wired in series with the circuit breaker to increase interrupt capability of the circuit breaker in a DC circuit.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIGS. 1 and 2, front and side views respectively, of an exemplary embodiment of a circuit breaker assembly in accordance with the present invention is shown generally at 10 . The circuit breaker assembly 10 includes a circuit breaker 12 with an auxiliary switch 14 mounted thereon. Half shells 16 and 18 form a split case enclosure 20 which encloses the interior components of the circuit breaker 12 . Toggle handle 22 , extending out of the top of circuit breaker 12 , is pivotally mounted to the interior of the split case 20 to provide manual actuation of the circuit breaker 12 , and circuit breaker terminals 24 and 26 , extending through the bottom of circuit breaker 20 , provide electrical connection to load and source lines (not shown). The auxiliary switch 14 includes a switch housing 28 mounted in an opening defined by the circuit breaker 12 , and has a pair of auxiliary terminals 30 and 32 extending straight through the bottom of switch housing 28 . The auxiliary terminals include a center hole 33 through which a wire, e.g., a source line or load line, can be attached.
As will be discussed in greater detail hereinafter, the auxiliary switch 14 is adapted to switch substantially the rated interrupt current of circuit breaker 12 without substantially changing the overall package width of the circuit breaker assembly 10 . That is the overall width of the auxiliary switch 14 is substantially equal to or less than the overall width of the circuit breaker 12 .
Typically, the auxiliary switch 14 and circuit breaker 12 fall into a general industry classification of “Low Voltage” circuit protection devices, which have normal operation ratings that range up to 100 amps at 300 volts AC or 100 amps at 80 volts DC. In addition to the normal operation ratings, circuit protection devices are required to be rated for the maximum current they can safely interrupt under standard test conditions at their rated voltage. This rating is known as the interrupt current capacity of the circuit protection device. The auxiliary switch 14 is typically rated for use, in series with the circuit breaker, with an interrupt current capacity of 5000 amps at 120 volts AC, 3000 amps at 240 volts AC, and 5000 amps at 80 volts DC.
Comparatively, prior art auxiliary switches in these voltage ranges are not rated for handling substantially higher interrupt currents than the normal operation current ratings and are therefore limited to use for indicating circuit breaker status, e.g., on/off or make/break.
Though this embodiment describes a split case circuit breaker, the circuit beaker can be any switch that automatically interrupts an electric circuit under an infrequent abnormal condition, e.g., current overload.
Referring to FIGS. 3 and 4, the circuit breaker 12 includes a collapsible linkage assembly 34 engaged between a moveable contact lever 36 and the handle 22 which is pivotally mounted to the circuit breaker enclosure 20 . The moveable contact lever 36 includes a circuit breaker moveable contact 38 disposed thereon which traverses from an open position 40 to a closed position 42 across a predetermined first distance 43 , to make electrical contact (make) with circuit breaker stationary contact 44 . Typically, when the contact lever 36 is in the closed position, a source current will conduct through terminal 26 to the stationary contact 44 . The current is conducted through the stationary contact 44 , through the movable contact 38 , to the movable contact lever 36 . The movable contact lever 36 is connected to the current sensing electromagnetic coil 48 through lead 52 . The coil 48 is connected through lead 50 to the terminal 24 and out to a load. When the current in the coil exceeds a predetermined rated current capacity, e.g. rated operational current or rated interrupt current, the coil will cause the circuit breaker to trip, thereby collapsing the linkage assemble 34 , pivoting the moveable contact lever 36 from the closed position 42 to the open position 40 and breaking contact (break) between the moveable and stationary contacts 38 and 44 to open the circuit. An auxiliary coil 45 may be provided for allowing remote or relay opening of the contacts 42 / 44 . The auxiliary coil 45 is preferably on a separate bobbin from the main coil 48 rather than simply supplied as an alternative to the usual circuit breaker configuration with a single main coil. See U.S. Pat. No. 4,982,174 for such an arrangement. In FIGS. 3 and 4, the auxiliary coil bobbin is made in two parts so as to surround the coil 45 completely. The arrangement assures that failure of the coil 45 will not interfere with normal circuit breaker operation.
The auxiliary switch housing 28 , of the auxiliary switch 14 , includes flanges 54 which slidably engages circuit breaker mounting grooves 56 to mount the housing 28 into opening 58 defined by the circuit breaker enclosure 20 . The auxiliary switch 14 also includes an auxiliary actuator 60 slidably mounted within the switch housing 28 . An upper portion 62 of the auxiliary actuator 60 protrudes into the opening 58 of the circuit breaker 12 from the switch housing 28 . An auxiliary moveable contact member 64 extends laterally out of opposing sides of a hollow lower portion 66 of the auxiliary actuator 60 and has a pair of auxiliary moveable contacts 68 disposed thereon. The moveable contact member 64 is moveably mounted and retained by the hollow lower portion 66 of the auxiliary actuator 60 . A contact spring 70 (shown in dotted lines) acts between the auxiliary actuator 60 and the auxiliary moveable contact member 64 to urge the moveable contact member 64 against the bottom of the auxiliary actuator 60 . A return spring 72 is disposed between the switch housing 28 and the auxiliary actuator 60 urging the upper portion 62 of the auxiliary actuator 60 into engagement against the movable contact lever 36 of the circuit breaker 12 . A pair of auxiliary stationary contacts 74 are arranged in the switch housing 28 for engagement with the auxiliary moveable contacts 68 and are spaced a second predetermined distance 76 therefrom. When the moveable contact lever 36 of the circuit breaker 12 moves from the open position 40 to the close position 42 , the contact lever 36 depresses the auxiliary actuator 60 to have the auxiliary moveable contact 68 traverse the second predetermined distance 76 and make contact with the auxiliary stationary contact 74 .
Typically, when the auxiliary switch 14 is used as a neutral disconnect for a protected load, the auxiliary contacts 68 and 74 of the auxiliary switch 14 will be wired on the neutral side of the load in series with the load and the circuit breaker contacts 38 and 44 of the circuit breaker 12 . In this case, when the auxiliary contacts 68 and 74 are closed, load current will conduct from terminal 30 , through one of the moveable and stationary contacts 68 and 74 , across the moveable contact member 64 , through the other moveable and stationary contacts 68 and 74 , and out terminal 32 to the source. Since the auxiliary actuator 60 of the auxiliary switch 14 is mechanically actuated by circuit breaker contact lever 36 , when the circuit breaker 12 trips the actuator switch 14 will also trip, thereby causing the auxiliary contacts 68 and 74 to separate and disconnect the neutral line from the load.
By utilizing the dual pair of moveable and stationary auxiliary contacts 68 and 74 rather than a single set of contacts, the contact surface area and gap size are effectively doubled without significantly affecting the overall width of the auxiliary switch 14 . The dual contacts are therefor a contributing factor to the increased current capacity of the auxiliary switch 14 .
Another factor that reduces arcing in the auxiliary switch 14 and enables the auxiliary switch 14 to switch substantially the rated interrupt current of the circuit breaker 12 , is a late break, early make feature. That is, the predetermined second distance 76 through which the auxiliary moveable contacts 68 must traverse is designed to be less than the predetermined first distance 43 through which the circuit breaker moveable contact 38 must traverse. Consequently, the moveable and stationary contacts 68 and 74 of the auxiliary switch 14 will make earlier and break later, than the moveable and stationary contacts 38 and 44 of the circuit breaker 12 . Therefore, most of the arcing occurs across the larger circuit breaker contacts when they make or break first, enabling the smaller auxiliary contacts to be reduced in size for the same interrupt current rating.
Though the circuit breaker moveable contact lever 36 is shown as a pivotally mounted moveable contact arm, other moveable contact lever embodiments are also considered within the scope of this invention. By way of example, the lever 36 may have a dual contact bridge configuration similar to that of the moveable contact member 64 .
Though the auxiliary actuator 60 is shown in this embodiment as being slidably mounted within the switch housing 28 , one skilled in the art would recognize that the auxiliary actuator 60 may be moveably mounted in other ways, e.g., pivotally mounted. Additionally, though the auxiliary actuator 60 is shown in this embodiment as making contact with the moveable contact lever 36 when it is in the open position 40 , a gap may exist between the auxiliary actuator 60 and the moveable contact lever 36 when it is in this position 40 . In that case, the gap will be closed as the moveable contact lever 36 moves from the open position 40 to the closed position 41 to contact and depress the auxiliary actuator 60 .
Referring to FIG. 5, another embodiment of the auxiliary actuator switch 14 shows an enhancement to the early make, late break feature whereby an inertia dampening flywheel 73 is pivotally attached to the switch housing 28 via flywheel pivot axis 75 . The flywheel has an engagement slot 77 slidably engaged to a mounting pin 79 located on the lower portion 66 of the auxiliary actuator 60 .
The fly wheel 73 engaged with the auxiliary switch actuator 60 provides inertia dampening to the auxiliary switch 14 such that the moveable and stationary contacts 68 and 74 of the auxiliary switch 14 break later than the moveable and stationary contacts 38 and 44 of the circuit breaker 12 . When the inertia dampening of the flywheel is combined with the early make, late break design discussed previously, the arcing across the auxiliary contacts 68 and 74 is further reduced, allowing the auxiliary switch 14 to be further down sized.
Referring to FIGS. 6 and 7, an alternative embodiment of the auxiliary switch 14 is shown where case 28 further includes an upper portion 78 removeably attached to a lower portion 80 . The lower portion 80 covers and protects right angle terminals 82 and has lower portion hooks 84 extending upwardly to removably engage with upper portion hooks 86 extending downwardly from the bottom of the upper portion 78 of case 28 .
This embodiment also shows the auxiliary moveable contact member 64 canted (tilted) relative to the substantially horizontal stationary contacts 74 which enables a contact wiping action when the moveable and stationary contacts 68 and 74 make and break. The lower portion 66 of the auxiliary actuator 60 has a hollow section 88 with a canted bottom surface 89 which slidably retains the contact spring 70 and contact member 64 . The contact spring 70 urges the contact member 64 flush against the canted surface 89 when the actuator 60 is fully extended, i.e., when the moveable contact lever 38 is in the open position 40 .
Referring to FIGS. 8 and 9, a convex surface 90 is disposed on the auxiliary moveable contacts 68 having a centerline 92 substantially normal to the surface 90 . Additionally, a convex surface 94 is disposed on the auxiliary stationary contacts 74 having a centerline 96 substantially normal to the surface 94 , and facing the convex surface 90 of the auxiliary moveable contacts 68 . When the moveable contact lever 36 pivots from the open position 40 to the closed position 42 , the actuator 60 is depressed. The moveable and stationary contacts 68 and 74 move linearly toward each other until their convex surfaces 90 and 94 make contact with their centerlines 92 and 96 being offset. The pair of stationary contacts 74 then lift the moveable contact member 64 off of the canted surface 89 of the actuator 60 such that the contact spring 70 generates a force along the centerline 92 of the moveable contacts 68 . Consequently, a reactionary force is generated along the centerline 96 of the stationary contact 74 . This misalignment of forces creates a moment that rotates the moveable contact member 64 . Since the contact member 64 is retained by the hollow section 88 of actuator 60 , it is forced to pivot about a pivot point 98 urging the centerlines 92 and 96 of the contacts 68 and 74 substantially into alignment. This rotation causes a relative lateral motion between the moveable and stationary contacts 68 and 74 , wiping the surfaces 90 and 94 clean of welds and debris caused by arcing on break. On break, the slanted surface 89 of the actuator 60 contacts one side of the moveable contact member 64 first, generating a twisting moment that will shear any contact welds caused by arcing on make. The wiping action enables the spring forces and contact surface areas to be downsized, and therefore is an additional factor in enabling the switch to keep a small package size and a high interrupt current rating.
Referring to FIG. 10, a force balance diagram on the moveable contact lever 36 in the closed position 42 is shown. A toggle compression force F T is generated by the collapsible linkage assembly 34 on the contact lever 36 . The toggle compression force F T has a line of direction which passes through toggle attachment point 100 and fulcrum point 101 which is located on the moveable contact 38 side of the moveable contact lever 36 . A main spring force F MS through the main spring pin 102 reacts to the toggle compression force F T to generate a moment M MS defined by the equation M MS =F MS (A), where “A” is the distance between the line of direction of F MS and the fulcrum point 101 . This moment M MS is reacted to by the moveable contact 38 on the stationary contact 44 to generate a predetermined contact pressure force F C and an equal and opposite contact pressure moment M C . The contact pressure moment M C is defined by the equation M C =F C (B) where “B” is the distance between the line of direction of F C and the fulcrum point 101 . The upper portion 62 of the auxiliary actuator 60 is positioned at the fulcrum point 101 and generates an auxiliary actuator force F AUX which is substantially in line with the direction of the opposing toggle compression force F T .
It is important to maintain the predetermined contact pressure F C between the moveable and stationary contacts 38 and 44 to insure proper circuit breaker 12 performance and to prevent premature wear on the contacts 38 and 44 . By positioning the actuator 60 at the fulcrum point 101 , the larger springs required to enable the auxiliary switch 14 to handle the higher interrupt current ratings of the circuit breaker 12 can be utilized without affecting the contact pressure F C or the performance of the circuit breaker 12 .
Referring to FIG. 11, as is well known, the auxiliary switch contacts are discussed above as having a single pole, single throw, double break arrangement. However, it is also considered within the scope of this invention to have other contact arrangements as well. By way of example, a single pole, double throw, double break embodiment is shown in FIG. 12 .
Referring to FIG. 12, the contact lever 64 of the auxiliary switch 14 has an additional pair of moveable contacts 104 disposed on its opposing side. An additional pair of terminals 106 and 108 are connected to an additional pair of stationary contacts 110 . The terminals 30 and 32 could be connected in one circuit, and the terminals 106 and 108 could be connected to a separate circuit. Alternatively, terminals 30 and 106 or terminals 32 and 108 could be tied together in the same circuit.
Referring to FIG. 13, a wiring diagram of the auxiliary switch used as a neutral disconnect is shown. The line side of the source 112 is connected to terminal 26 which is in series with the circuit breaker contacts 38 and 44 , current sensing coil 48 and terminal 24 of the circuit breaker. The load line is connected in series to load 114 . The return side of the load is connected to auxiliary terminal 32 which is in series with auxiliary contacts 74 and 68 , and auxiliary terminal 30 . Auxiliary terminal 30 is in turn connected to the return side of the source 112 to complete the circuit. The full load current must conduct through both the circuit breaker contacts 38 and 44 on the line side of the circuit, and the auxiliary contacts 68 and 74 on the load side of the circuit. Since the auxiliary contacts 68 and 74 are mechanically tied to the circuit breaker contacts 38 and 44 , when the circuit breaker 12 disconnects the line side, the auxiliary switch 14 will disconnect the neutral side.
Referring to FIG. 14, a wiring diagram of the auxiliary switch 14 used in series with the circuit breaker 12 in a DC circuit is shown. In this embodiment the circuit breaker contacts 38 and 44 are in series connection with the auxiliary contacts 68 and 74 on the high side of a DC circuit between a DC source 116 and a load 118 . By connecting the auxiliary switch in this fashion, the DC interrupt capacity of the circuit breaker can be increased.
While preferred embodiments have been shown and described, various modifications and substitutions may be made thereto without departing from the spirit and scope of the invention. Accordingly, it is to be understood that the present invention has been described by way of illustration and not limitation.
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An auxiliary switch for a circuit breaker of the split case type. The switch is capable of switching the rated interrupt current capacity of the breaker and is fitted in to the circuit breaker case so that the overall width is substantially equal to or less than the overall width of the circuit breaker. Several embodiments of the auxiliary switch disclose various features which contribute to increasing the interrupt current rating and/or down sizing the width of the auxiliary switch. Among them are: an early make, late break of the auxiliary contacts compared to the circuit breaker contacts; an inertia dampening fly wheel attached to the actuator of the switch to enhance the early make/late break feature; a wiping action between the moveable and stationary contacts of the auxiliary switch to clean off welding and debris deposited from arcing; dual auxiliary contacts to enhance the contact area with little impact on package size and width; and a positioning of the auxiliary actuator on the contact lever of the circuit breaker to prevent the spring forces acting on the actuator from affecting circuit breaker contact pressure.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention relates to a rare earth magnet constituted by a polycrystal having nanosize crystal grain size and to a manufacturing method therefor.
[0003] 2. Description of the Related Art
[0004] Rare earth magnets such as a neodymium magnet (Nd 2 Fe 14 B) have been used for various applications as very powerful permanent magnets with a high magnetic flux density. A nanosize crystal grain size should be ensured to obtain even better magnetic properties.
[0005] A technique by which a melt of a magnet composition is rapidly cooled by a single roll method or a twin roll method to obtain a thin strip has been used to realize a nanosize crystal grain size. Where the cooling rate during rapid cooling is too high, an amorphous structure is obtained in the entire magnet or part thereof. The amorphous structure can be crystallized by appropriate annealing, but the grain size in this case becomes larger than that of the crystal structure directly formed by rapid cooling.
[0006] In sintered magnets using multi-domain Nd 2 Fe 14 B particles with a size of about several micron, a grain boundary phase should be present as a barrier preventing the movement or appearance of magnetic walls in order to realize a high coercive force.
[0007] For example, Japanese Patent Application Publication No. 2007-251037 (JP-A-2007-251037) and Japanese Patent Application Publication No. 2008-069444 (JP-A-2008-069444) disclose a method including the steps of feeding an alloy melt containing praseodymium (Pr), neodymium (Nd), iron (Fe), cobalt (Co), niobium (Nb), yttrium (Y), and boron (B) to a rotating cooling roll, rapidly cooling, obtaining a thin strip, and crystallizing the thin strip by heat treating at a temperature rise rate of 150 to 250° C./min. As a result, a thin alloy strip for a rare earth magnet constituted by a polycrystal and including the aforementioned constituent element can be obtained.
[0008] However, no consideration is given to a graph boundary phase and there is room for increasing a coercive force.
[0009] A coercive force of the aforementioned magnet at room temperature has been evaluated, but for a motor of a hybrid vehicle the evaluation should be conducted for a coercive force at a temperature close to 160° C. which is in the usage temperature range of the motor.
SUMMARY OF INVENTION
[0010] The invention provides a rare earth magnet in which the refinement of crystal grains to a nanometer size is enhanced and a coercive force is increased due to the presence of a grain boundary phase and also provides a method for manufacturing such a magnet.
[0011] The first aspect of the invention relates to a rare earth magnet having a composition represented by the compositional formula R a H b Fe c Co d B e M f , where:
[0012] R is at least one rare earth element including Y;
[0013] H is at least one heavy rare earth element from among Dy and Tb;
[0014] M is at least one element from among Ga, Zn, Si, Al, Nb, Zr, Ni, Cu, Cr, Hf, Mo, P, C, Mg, and V;
[0015] 13≦a≦20;
[0016] 0≦b≦4;
[0017] c=100−a−b−d−e−f;
[0018] 0≦d≦30;
[0019] 4≦e≦20;
[0020] 0≦f≦3, and having a structure constituted by a main phase: a (RH) 2 (FeCo) 14 B phase, and a grain boundary phase: a (RH)(FeCo) 4 B 4 phase and a RH phase, with a crystal grain size of the main phase of 10 nm to 200 nm.
[0021] The second aspect of the invention relates to a method for manufacturing a rare earth magnet, including:
[0022] rapidly cooling and solidifying an alloy melt having a composition represented by the compositional formula R a H b Fe c Co d B e M f , where:
[0023] R is at least one rare earth element including Y;
[0024] H is at least one heavy rare earth element from among Dy and Tb;
[0025] M is at least one element from among Ga, Zn, Si, Al, Nb, Zr, Ni, Cu, Cr, Hf, Mo, P, C, Mg, and V;
[0026] 13≦a≦20;
[0027] 0≦b≦4;
[0028] c=100−a−b−d−e−f;
[0029] 0≦d≦30;
[0030] 4≦e≦20;
[0031] 0≦f≦3, thereby creating a structure constituted by a main phase: a (RH) 2 (FeCo) 14 B phase, and a grain boundary phase: a (RH)(FeCo) 4 B 4 phase and a RH phase, with a crystal grain size of the main phase of 10 nm to 200 nm.
[0032] The rare earth magnet in accordance with the invention is constituted by a main phase: a (RH) 2 (FeCo) 14 B phase, and a grain boundary phase: a (RH)(FeCo) 4 B 4 phase and a RH phase, and has a crystal grain size of the main phase of 10 nm to 200 nm. As a result, a high coercive force can be obtained.
[0033] With the method for manufacturing a rare earth magnet in accordance with the invention, a rare earth magnet with a high coercive force can be manufactured by performing rapid cooling and solidification at a cooling rate at which the above-described crystal structure is generated.
[0034] When an amorphous phase is produced during rapid cooling and solidification, this phase can be crystallized by annealing.
[0035] When, b, d, and f are zero in the above-described rare earth magnet and manufacturing method therefor, it means that the respective elements are not contained in the compositional formula. For example, when b=d=f=0, the compositional formula is R a Fe c B e .
BRIEF DESCRIPTION OF DRAWINGS
[0036] The foregoing and further objects, features and advantages of the invention will become apparent from the following description of exemplary embodiments with reference to the accompanying drawings, wherein like numerals are used to represent like elements and wherein:
[0037] FIG. 1 is a schematic diagram illustrating a single roll used in the fabrication of a rapidly cooled ribbon of a nano-polycrystalline rare earth magnet in accordance with the invention;
[0038] FIG. 2 is a graph illustrating results obtained in measuring magnetic properties of the rapidly cooled ribbon fabricated in Example 1;
[0039] FIG. 3 is a graph illustrating the relationship between a coercive force and a NdFe 4 B 4 phase ratio in the grain boundary phase of the rapidly cooled ribbon fabricated in Example 1;
[0040] FIG. 4 is a graph illustrating a X-Ray Diffraction (XRD) chart of the rapidly cooled ribbon fabricated in Example 1;
[0041] FIG. 5 is a graph illustrating the relationship between a coercive force and a NdFe 4 B 4 phase ratio in the grain boundary phase of the rapidly cooled ribbons with various volume ratio of grain boundary phase that were fabricated in Example 1;
[0042] FIG. 6 is a graph illustrating results obtained in measuring magnetic properties of the rapidly cooled ribbon fabricated in Example 2;
[0043] FIG. 7 is a graph illustrating the relationship between a coercive force and an amount of Ga added to the rapidly cooled ribbon fabricated in Example 2;
[0044] FIG. 8 is a graph illustrating the effect produced by addition of Dy on magnetic properties of the rapidly cooled ribbon fabricated in Example 2;
[0045] FIG. 9 is a graph illustrating results obtained in measuring magnetic properties of the rapidly cooled ribbon fabricated in Example 3;
[0046] FIGS. 10A to 10C are photos illustrating Scanning Electron Microscope (SEM) images of fracture surfaces of the rapidly cooled ribbon fabricated in Example 3;
[0047] FIG. 11 is a graph illustrating the relationship between a crystal grain diameter and a coercive force of the rapidly cooled ribbon fabricated in Example 3;
[0048] FIG. 12 is a graph illustrating results obtained in measuring magnetic properties of the rapidly cooled ribbon fabricated in Example 4;
[0049] FIG. 13 is a graph illustrating results obtained in measuring magnetic properties of another rapidly cooled ribbon fabricated in Example 4;
[0050] FIG. 14 is a graph illustrating the relationship between a temperature rise rate of the rapidly cooled ribbon fabricated in Example 5 during annealing and a coercive force of the rapidly cooled ribbon fabricated in Example 5;
[0051] FIG. 15 is a schematic diagram illustrating structural changes during annealing in Example 5;
[0052] FIG. 16 is a graph illustrating the relationship between a coercive force of the rapidly cooled ribbon fabricated in Example 6 and a measurement temperature;
[0053] FIGS. 17A and 17B are photos showing Transmission Electron Microscope (TEM) images of the rapidly cooled ribbon fabricated in Example 6;
[0054] FIG. 18 is a graph illustrating the relationship between a coercive force of another rapidly cooled ribbon fabricated in Example 6 and a measurement temperature; and
[0055] FIG. 19 is a schematic diagram illustrating the relationship between variations in a grain boundary phase of the rapidly cooled ribbon fabricated in Example 6 and a coercive force decrease rate with temperature.
DETAILED DESCRIPTION OF EMBODIMENTS
[0056] The nanosize crystal grain size in the embodiments of the invention is preferably equal to or less than a single domain particle diameter, that is 10 to 200 nm, more preferably 10 to 50 nm.
[0057] A representative rare earth magnet of an embodiment of the invention is represented by the compositional formula Nd a Fe c B e with 13≦a≦20; 4≦c≦20; e=100−a−c, and has a structure constituted by a main phase: a Nd 2 Fe 14 B phase, and a grain boundary phase: a NdFe 4 B 4 phase and a Nd phase.
[0058] A phase ratio (volume ratio) of the NdFe 4 B 4 phase and the Nd phase constituting the graph boundary phase is preferably (NdFe 4 B 4 phase):(Nd phase)=20:80 to 80:20.
[0059] In the rare earth magnets of the embodiments of the invention, in the case of a pure three-component NdFeB system containing no additional element M, a coercive force at normal temperature in a state immediately after rapid cooling and solidification is equal to or higher than 15 kOe and in the case of a system including an additional element M, a coercive force of equal to or higher than 20 kOe can be obtained.
[0060] A reduction ratio of the coercive force with temperature in the rare earth magnets of the embodiments of the invention is equal to or less than 0.42%/° C., preferably equal to or less than 0.40%/° C.
[0061] A ratio (volume) of a crystalline phase in the structure is preferably equal to or higher than 95%.
[0062] In the method for manufacturing the rare earth magnet of the embodiment of the invention, the production of an amorphous structure is inhibited and a nanosize crystalline structure is readily produced by conducting rapid cooling at a cooling rate equal to or higher than 5×10 5 K/s, preferably equal to or lower than 2×10 6 K/s. When the cooling rate during rapid cooling is too high (for example, higher than 2×10 6 K/s), an amorphous phase is generated. A single roll method and a twin roll method can be used for rapid cooling, but these methods are not limiting. In the below-described Examples 1 to 4 and 6, rare earth magnet ribbons were manufactured by conducting rapid cooling and solidification at a cooling rate of 5×10 5 K/s to 2×10 6 K/s.
[0063] When an amorphous phase has appeared during rapid cooling and solidification, this phase may be crystallized by annealing.
[0064] In the manufacturing method in accordance with the invention, the process from a molten state of the alloy to completion of solidification is preferably performed in a nonoxidizing atmosphere.
Example 1
[0065] Ingots of NdFeBGa alloys with compositions a to e shown in table 1 were produced by arc melting. The compositions a to e were selected on a NdFeB ternary equilibrium state diagram such as to obtain a volume fraction of a grain boundary phase (NdFe 4 B 4 phase+Nd phase) of 18% (constant). Table 1 also shows the NdFe 4 B 4 phase:Nd phase ratio in the grain boundary phase. This ratio was determined by calculations on the NdFeB ternary equilibrium state diagram.
[0000]
TABLE 1
NdFe 4 B 4
Nd
a. Nd 20 Fe 73.5 B 5.5 Ga
15%
85%
b. Nd 17.5 Fe 74 B 7.5 Ga
39%
61%
c. Nd 16 Fe 74 B 9 Ga
56%
44%
d. Nd 14 Fe 74.5 B 10.5 Ga
76%
24%
e. Nd 13 Fe 74.5 B 11.5 Ga
87%
13%
[0066] Ribbons were fabricated from the ingots by using the single roll furnace shown in FIG. 1 and conducting rapid cooling and solidification under the conditions shown in Table 2. A ribbon 4 (referred to hereinbelow as “rapidly cooled ribbon”) is obtained by ejecting the alloy melt from a nozzle 3 on the outer peripheral surface of a single roll 2 rotating in the direction shown by arrow 1 , thereby causing rapid cooling and solidification.
[0000]
TABLE 2
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
2350
rpm
Melting temperature
1450°
C.
[0067] Magnetic properties of the obtained rapidly cooled ribbon were measured with a Vibrating Sample Magnetometer (VSM) (manufactured by Lake Shore Co., model 7410). A crystal structure of the ribbon was analyzed with a XRD (manufactured by Rigaku Co., RINT-2000).
[0068] FIG. 2 shows the results obtained in measuring magnetic properties. A coercive force increased with the increase in the NdFe 4 B 4 phase ratio in the grain boundary phase in the order of a→c, assumed a maximum value in the c composition of Nd 16 Fe 74 B 9 Ga 1 and then decreased in the order of c→e with the increase in the NdFe 4 B 4 phase ratio. Since the Mr/Mr at27kOe value is constant, there is no difference in exchange coupling ability between the crystal grains, and the difference in grain size of the main phase Nd 2 Fe 14 B apparently became the difference in coercive force. In FIG. 3 , a coercive force is plotted against a NdFe 4 B 4 phase ratio in the grain boundary phase.
[0069] It is considered that the main phase grain size varied depending on the phase ratio in the grain boundary phase apparently because the main phase coarsening was inhibited as the ratio (volume ratio) of the NdFe 4 B 4 phase that was in a peritectic relationship with the main phase increased from that of the composition a to that of the composition c and the coercive force increased due to crystal grain refinement. However, where the ratio (volume ratio) of the NdFe 4 B 4 phase increased in excess of that of the composition c, the nucleation frequency of the main phase decreased, crystal grains of the main phase were coarsened, and the coercive force decreased.
[0070] FIG. 4 is diffraction chart of XRD. In the composition a, the diffraction intensity of NdGa is high and a clear peak is observed. Therefore, it is obvious that Ga used as the additional element M formed a compound with Nd contained in the grain boundary phase.
[0071] In the composition b and compositions with a lower content ratio of neodymium, a NdGa peak was eliminated and a peak intensity of the NdFe 4 B 4 phase increased. In the composition b and compositions with a lower content ratio of neodymium, the NdFe 4 B 4 phase contained in the grain boundary phase was a crystalline phase, but the Nd phase (NdGa phase) apparently became amorphous. In the composition a, a volume fraction of the Nd phase in the finally solidified portion was high, the Nd phase that has locally aggregated was slowly cooled and crystallized, whereas in the composition b and compositions with a lower content ratio of neodymium, the volume fraction of the Nd phase was low and the uniformly dispersed Nd phase was rapidly cooled and amorphousized.
[0072] In the composition e, the peak intensity of the NdFe 4 B 4 phase increased abruptly. Therefore, the reaction path was different from that of the compositions a to d and it is possible than the initial crystals were not of the Nd 2 Fe 14 B phase. This is apparently why the coarsening of the Nd 2 Fe 14 B phase could not be prevented by the peritectic reaction of the NdFe 4 B 4 phase and the coercive force decreased.
[0073] As a result, the highest coercive force was obtained in the composition c in which the Nd phase was uniformly dispersed and the peritectic reaction of the NdFe 4 B 4 phase could be used.
[0074] <Effect of Volume Fraction of Grain Boundary Phase>
[0075] The above-described results were obtained in the case in which the volume fraction of grain boundary phase was 18% (constant). Rapidly cooled ribbons were also fabricated in the same manner as described above and magnetic properties thereof were measured with the VSM in the cases in which the volume fraction of grain boundary phase was 28% (constant) and 12% (constant).
[0076] In FIG. 5 , a coercive force is plotted against the NdFe 4 B 4 phase ratio in the grain boundary phase for volume fractions of 12%, 18%, and 28%.
[0077] As shown in FIG. 5 , the maximum value of coercive force and the phase ratio of the NdFe 4 B 4 phase at which the coercive force becomes maximum increase with the increase in the volume fraction of the grain boundary phase. Thus, a peak position of a curve representing a coercive force with respect to a phase ratio of the NdFe 4 B 4 phase shifts up and to the right as shown by a broken line in the figure. From this standpoint, the preferred phase ratios of the NdFe 4 B 4 phase can be generally classified in the following manner.
[0078] When the volume fraction of the grain boundary phase is <15%, the phase ratio of the NdFe 4 B 4 phase is <50%.
[0079] When the volume fraction of the grain boundary phase is 15% to 23%, the phase ratio of the NdFe 4 B 4 phase is 15 to 80%.
[0080] When the volume fraction of the grain boundary phase is >23%, the phase ratio of the NdFe 4 B 4 phase is 30 to 80%.
Example 2
[0081] <Effect of Additional Element>
[0082] Arc ingots were prepared of compositions obtained by adding 2 at. % of Ga, Cr, Si, V, or Ni as an element other than a heavy rare earth element, to Nf 16 Fe 47 B 10 according to the example 2 of the invention. A rapidly cooled ribbon was fabricated from each ingot under the conditions shown in Table 3 by using a single roll furnace shown in FIG. 1 .
[0000]
TABLE 3
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
2350
rpm
Melting temperature
1450°
C.
[0083] Magnetic properties of the obtained rapidly cooled ribbon were measured with the VSM.
[0084] FIG. 6 shows the results obtained in measuring magnetic properties. The addition of the elements increased the coercive force by comparison with that of the composition Nd 16 Fe 47 B 10 containing no additional elements. This is apparently because the additional elements produce a compound or a solid solution with the grain boundary phase, thereby inhibiting the growth of crystal grains of the main phase.
[0085] <Effect of the Amount Added>
[0086] FIG. 7 shows a coercive force obtained when Ga was added within a range of up to 2 at. % to Nd 16 Fe 47 B 10 . The coercive force increased with the increase in the amount of Ga added. However, no significant changes in the coercive force were observed after the amount added was higher than 1 at. %. Since magnetization decreases with the increase in the amount added, the amount of 2-3 at. % can be considered as an upper limit.
[0087] <Effect of Addition of Heavy Rare Earth Element>
[0088] FIG. 8 shows magnetization curves obtained when Dy was added at a ratio of 0.5 at. % to Nd 16 Fe 47 B 10 and when no addition was made. The coercive force could be increased without decreasing the magnetization with respect to the composition Nd 16 Fe 47 B 10 by adding merely 0.5 at. % of Dy. When Dy was added at 2 at. %, the coercive force exceeded 30 kOe and thus exceeded the measurement limit of the VSM. As a result, the measurements could not be conducted.
Example 3
[0089] <Effect of Crystal Grain Size>
[0090] Rapidly cooled ribbons of compositions (1) to (5) shown in Table S were fabricated in the same manner as in Example 1 under the conditions shown in Table 4 by using a single roll.
[0000]
TABLE 4
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
2350
rpm
Melting temperature
1450°
C.
[0000]
TABLE 5
Grain size
Grain size
Coercive
(nm)/number
(nm)/volume
Composition
force (kOe)
calculation
calculation
(1)
Nd 14 Fe 76 B 8 GaCu
20.5
65
93
(2)
Nd 14 Fe 75 B 10 Ga
22.8
60.5
87
(3)
Nd 15 Fe 70 B 14 Ga
23.9
51
64.5
(4)
Nd 15 Fe 65 B 19 Ga
26.7
32
44
(5)
Nd 15 Fe 65 B 19 Ga
28.1
24.5
40
[0091] Magnetic properties of the obtained rapidly cooled ribbon were measured with the VSM.
[0092] Fracture surfaces of the rapidly cooled ribbons were observed with a SEM and a crystal grain size was calculated.
[0093] FIG. 9 shows magnetic properties, and FIGS. 10A to 10C show SEM images.
[0094] The coercive force obtained increased with the decrease in the crystal grain diameter. Since the ribbon used had compositions obtained by adding Ga or GaCu to the NdFeB base composition, crystal period anisotropy of the main phase Nd 2 Fe 14 B did not vary among the ribbons. Therefore, the increase in the coercive force can be attributed to crystal grain refinement of the main phase.
[0095] In a region of a single domain (SD) crystal grain size, the volume-recalculated grain size was found to lay on a line with a constant inclination. In a rapidly cooled ribbon of composition (1) that had a coercive force of 20.5 kOe, because the grain size distribution was large ( FIG. 10A ), the effect of coarse crystal grains with a small coercive force increased and the calculated coercive force could be below the coercive force predicted on the basis of the average grain size. Experimental results suggest that when an anisotropic magnetic field of Nd 2 Fe 14 B is 67 kOe, a crystal grain size of about 10 nm is necessary to realize 33.5 kOe (67 kOe×½), which is a theoretical value for an isotropic system.
[0096] FIG. 11 shows a relationship between a crystal grain size and a coercive force for compositions (1) to (5). In this case, a black rhombic mark shows a grain size and coercive force after the rapidly cooled ribbon of composition (3) has been annealed (575° C.×1 min). The coercive force decreased as the crystal grains coarsened and the result laid almost on the extension of a line connecting points of five other plots. It is clear that within this range of composition variations, there is a strong correlation between the coercive force and the crystal grain size.
Example 4
[0097] <Fabrication of Rapidly Cooled Ribbon of Pure Ternary NdFeB>
[0098] Rapidly cooled ribbons a to d of pure ternary NdFeB obtained by changing x in a succession of 11.8, 14, 15, and 17 (at. %) in Nd x Fe 100-3x/2 B x/2 were fabricated under the conditions shown in Table 6 by using a single roll, and magnetic properties were measured by using the VSM. The phase ratio Nd:NdFe 4 B 4 of the grain boundary phase was fixed at 59:41.
[0000]
TABLE 6
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
2350
rpm
Melting temperature
1450°
C.
[0099] Rapidly cooled ribbons were also fabricated by using a Nd-rich composition e (Nd 15 Fe 70 B 15 , phase ratio Nd:NdFe 4 B 4 of the grain boundary phase was 22:78) and a B-rich composition f (Nd 20 Fe 65 B 15 , phase ratio Nd:NdFe 4 B 4 of the grain boundary phase was 41:59), and magnetic properties of the ribbons were measured.
[0100] FIGS. 12 and 13 show the results obtained in measuring magnetic properties.
[0101] As shown in FIG. 12 , when the Nd amount was increased in compositions a to d, the coercive force reached saturation at 22 kOe. This is apparently because even when the Nd amount was increased, crystal grains of the Nd 2 Fe 14 B phase of the main phase could not be refined when the amount of neodymium was equal to or higher than a predetermined value.
[0102] As shown in FIG. 13 , in the Nd-rich and B-rich compositions e and f, the volume fraction of the grain boundary phase NdFe 4 B 4 increased and magnetization decreased, but the coercive force increased and a coercive force with a maximum of 24.5 kOe was realized in the Nd 20 Fe 65 B 15 composition. Therefore, it was shown that by optimizing the composition, it was possible to refine crystal grains and fabricate rapidly cooled ribbons with high magnetization and high coercive force that are nano-polycrystalline magnets.
Example 5
[0103] A rapidly cooled ribbon of a Nd 20 Fe 65 B 15 composition was fabricated by using a single roll under the conditions shown in Table 7. When the cooling rate during rapid cooling and solidification was equal to or higher than 2×10 6 K/s, a rapidly cooled ribbon that was mostly amorphous was fabricated. The obtained amorphous phase was crystallized by annealing, thereby making it possible to obtain a coercive force close to that of the rapidly solidified ribbon produced at a cooling rate of 5×10 5 K/s to 2×10 6 K/s.
[0000]
TABLE 7
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
3500
rpm
Melting temperature
1450°
C.
[0104] In the present example, the rapidly solidified ribbon was crystallized by annealing with am infrared lamp (575° C.×1 min). Magnetic properties were then measured with the VSM.
[0105] FIG. 14 shows the relationship between a temperature rise rate during annealing and a coercive force. The higher was the temperature rise rate, the higher was the coercive force. This is apparently because the final crystal grain size and coercive force are determined by the nucleation frequency and grain growth of the main phase, as shown by a schematic diagram in FIG. 15 .
[0106] The general annealing conditions for crystallization were as follows: inactive atmosphere, temperature of 550 to 650° C., holding time 0.1 to 10 min, temperature rise rate equal to or higher than 20° C./min, preferably equal to or higher than 120° C./min.
Example 6
[0107] <Dependence of Coercive Force on Temperature>
[0108] Rapidly cooled ribbons of compositions (1) Nd 15 Fe 70 B 15 and (2) Nd 15 Fe 77 B 8 in accordance with the example 6 of the invention were fabricated by using a single roll under the conditions shown in Table 8. Magnetic properties were measured at various temperature with the VSM.
[0000]
TABLE 8
Nozzle diameter
0.6
mm
Clearance
0.7
mm
Ejection pressure
0.4
kg/cm 3
Roll speed
2350
rpm
Melting temperature
1450°
C.
[0109] FIG. 16 shows the relationship between a coercive force and a measurement temperature for various samples. For comparison, the figure also shows properties of (3) Dy-added sintered magnet Nd 11 Dy 2 Fe 80 B 6.5 and (4) Dy-free sintered magnet Nd 13.5 Fe 80 B 6.5 .
[0110] The coercive force at room temperature of the Dy-added sintered magnet (3) is higher than that of the nano-polycrystalline magnets (1) and (2) of the examples, but at a high temperature of 160° C., the relationship is inverted, and the nano-polycrystalline magnets (1) and (2) show a higher coercive force. This is because the reduction ratio of coercive force with respect to temperature of the nano-polycrystalline magnets (1) and (2) is 0.35%/° C. and 0.39%/° C. respectively, and lower than that of Comparative Example (3) (0.48%/° C.).
[0111] Further, where the nano-polycrystalline magnets (1) and (2) are compared to each other, the coercive force of the nano-polycrystalline magnet (1) is higher and the reduction ratio of the coercive force is lower than those of the nano-polycrystalline magnet (2). This is apparently because the volume fraction of the grain boundary phase of the nano-polycrystalline magnet (1) increased over than of the nano-polycrystalline magnet (2) and, therefore, isolation between Nd 2 Fe 14 B phases of the main phase increased.
[0112] A grain boundary phase can be observed with a TEM, typically as shown in FIGS. 17A and 17B .
[0113] <When Additional Elements are Present>
[0114] FIGS. 18 and 19 show variations in the coercive force caused by a volume fraction of the grain boundary phase and increase in a B content in the case in which Ga was added.
[0115] As the volume fraction of the grain boundary phase increased and the ratio of the NdFe 4 B 4 phase in the grain boundary phase also increased, grain refinement of the main phase and isolation between the main phases increased, the coercive force increased, and the reduction ratio of coercive force caused by temperature simultaneously decreased.
[0116] The invention provides a rare earth magnet in which formation of nanosize crystal grains is enhanced and a coercive force is increased due to the presence of a grain boundary phase and also a manufacturing method for such a magnet.
|
A rare earth magnet of the invention has a composition represented by the compositional formula R a H b Fe c Co d B e M f , where:
R is at least one rare earth element including Y; H is at least one heavy rare earth element from among Dy and Tb; M is at least one element from among Ga, Zn, Si, Al, Nb, Zr, Ni, Cu, Cr, Hf, Mo, P, C, Mg, and V; 13≦a≦20; 0≦b≦4; c=100−a−b−d−e−f; 0≦d≦30; 4≦e≦20; 0≦f≦3, and has a structure constituted by a main phase: a (RH) 2 (FeCo) 14 B phase, and a grain boundary phase: a (RH)(FeCo) 4 B 4 phase and a RH phase, with a crystal grain size of the main phase of 10 nm to 200 nm.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to software configuration and, more specifically, to providing a visual preview of the intermediate steps of software configuration before the software configuration is actually performed.
2. Description of the Related Art
Software products, such as complex operating systems, are often comprised of many interdependent configurable subsystems, and the relationship between these subsystems or components is not always obvious to the untrained eye. Graphical user interfaces can enhance an end-user's understanding of complex software by modeling the system and its components visually. However, graphical user interfaces themselves can be complex to understand without accompanying documentation or prior experience. Explanatory text that explains the software configuration process, while it may be helpful, is often too brief to provide the necessary context and detail to facilitate an adequate understanding of the software configuration process for the users. Furthermore, such supplemental text is typically not presented in a manner integrated to the graphical user interface. As a result, users of complex software have to configure software without the background information necessary to evaluate the outcome of a variety of selections that they make during the software configuration process.
Conventional software configuration tools, if they include a graphical user interface at all, typically utilize a simple series of steps or a “wizard” to accept the user's selection of a variety of configuration options or parameters to configure the software. Each step of the wizard, even though it may depend upon preceding steps, is usually presented in isolation in order to simplify its appearance. The conventional software configuration wizards do not provide a step-by-step visual representation of the progress of the software configuration as various selections are made by the user in each step of the software configuration process. In fact, conventional software configuration wizards are often designed to hide many of the steps and complexity of the software configuration process to simplify presentation to the user. Thus, such conventional software configuration wizards cannot guide the user effectively by illustrating the consequences of the user's selection of a variety of options, step by step during the software configuration process.
In addition, although some conventional software configuration wizards, such as the disk management tool provided by Microsoft Corporation, include graphical representations of the software, they only show the initial state of the software prior to the software configuration and the final state of the software after the software configuration is complete. Conventional software configuration wizards do not show a preview of the software state that reflects the user's selections of the parameters modifying the initial state of the software before the software configuration is actually performed. Thus, there is no way for users to preview the consequences of their selection of the various parameters during the software configuration process without actually committing the software configuration.
Therefore, there is a need for a software configuration tool that provides a visual, step-by-step illustration of a software configuration process and how the software configuration changes in response to the selection of various software configuration options. There is also a need for a software configuration tool that shows previews of the software state reflecting the selection of the various software configuration options before the software configuration is actually performed.
SUMMARY OF THE INVENTION
The present invention provides a step-by-step visual preview into a guided software configuration process, where the preview is updated in real time as users specify the parameters of the software during the software configuration process, thereby providing a visual explanation of the various components of the software and their relationship to one another. Before the newly assembled software configuration is committed, the complete graphical representation of the software configuration is displayed for approval.
Embodiments of the present invention include a method, a computer program product, and a system for providing the step-by-step visual preview of the software configuration process. In one embodiment, a plurality of parameters for configuring the software are displayed, and a selection of one or more of the parameters is received to configure the software. One or more previews of the software are displayed before the software configuration is actually performed, where the preview is representative of an intermediate state of the software configuration modifying an initial state of the software configuration in response to the selection of said one or more of the parameters. In other words, the preview graphically represents the intermediate state of the software configuration that would result from the selected parameters if the software configuration is actually performed with the selected parameters. Each of the previews corresponds to a different step of the software configuration and to a different selected parameter for the software configuration. Then, the software configuration is actually performed based on the selected parameters.
The present invention has the advantage that the users are graphically guided throughout the software configuration process such that they easily understand the consequences of their selection of various software configuration parameters during the software configuration process before they make a final commitment completing the software configuration process. In addition, constant visual feedback illustrating the change in the software configuration in response to their selection of the various software configuration parameters helps the users familiarize themselves with the software system gradually as it is configured, resulting in a graphical representation of the software that can be useful during on-going maintenance, monitoring and control of the software after the software configuration is performed.
The features and advantages described in the specification are not all inclusive and, in particular, many additional features and advantages will be apparent to one of ordinary skill in the art in view of the drawings, specification, and claims. Moreover, it should be noted that the language used in the specification has been principally selected for readability and instructional purposes, and may not have been selected to delineate or circumscribe the inventive subject matter.
BRIEF DESCRIPTION OF THE DRAWINGS
The teachings of the embodiments of the present invention can be readily understood by considering the following detailed description in conjunction with the accompanying drawings.
FIG. 1 illustrates a general purpose computer system upon which the method of providing a visual preview of intermediate steps of software configuration can be implemented, according to one embodiment of the present invention.
FIG. 2 is a flow diagram illustrating the method of providing one or more visual previews of intermediate steps of software configuration, according to one embodiment of the present invention.
FIGS. 3A-3F illustrate examples of user interfaces through which the visual previews of intermediate steps of software configuration are provided, according to one embodiment of the present invention.
DETAILED DESCRIPTION OF EMBODIMENTS
The Figures (FIG.) and the following description relate to preferred embodiments of the present invention by way of illustration only. It should be noted that from the following discussion, alternative embodiments of the structures and methods disclosed herein will be readily recognized as viable alternatives that may be employed without departing from the principles of the claimed invention.
Reference will now be made in detail to several embodiments of the present invention(s), examples of which are illustrated in the accompanying figures. It is noted that wherever practicable similar or like reference numbers may be used in the figures and may indicate similar or like functionality. The figures depict embodiments of the present invention for purposes of illustration only. One skilled in the art will readily recognize from the following description that alternative embodiments of the structures and methods illustrated herein may be employed without departing from the principles of the invention described herein.
FIG. 1 illustrates a general purpose computer system upon which the method of providing a visual preview of intermediate steps of software configuration can be implemented, according to one embodiment of the present invention. The computer 100 can be one on which a software is to be installed, where the software itself also includes the functionalities of providing a step-by-step visual preview of intermediate steps of configuring the software itself. For example, the software may be computer virtualization software such as those offered by VMware, Inc. of Palo Alto, Calif., where the virtualization software is installed on the computer 100 . Such software is capable of configuring a variety of software components and functionalities based on the user's selection of various parameters during the software configuration process. The example of configuring a virtual Ethernet switch will be used herein to illustrate the present invention, although the present invention may be used in any type of software configuration process. The computer 100 includes one or more processors 102 , a memory 103 , a storage module (e.g., hard disk drive) 104 , an input device (e.g., keyboard, mouse, and the like) 106 , a display device 107 , and a network interface 105 , exchanging data with one another through a bus 101 .
The network interface 105 may include a NIC (network interface card) or other standard network interfaces to communicate with other network interface devices coupled to a network (not shown). The storage module 104 stores the software that is to be installed and configured in the computer 100 , which software itself also includes the functionalities of providing the step-by-step visual preview of intermediate steps of configuring the software itself. Such software is loaded to the memory 103 and run by the processor 102 . The display device 107 can be a standard liquid crystal display or any other type of display device, and displays the graphical representations of the various software configuration states, step-by-step, during the software configuration process. Note that not all components of the computer 100 are shown in FIG. 1 and that certain components not necessary for illustration of the present invention are omitted herein.
FIG. 2 is a flow diagram illustrating the method of providing a visual preview of intermediate steps of software configuration according to one embodiment of the present invention, and FIGS. 3A-3F illustrate examples of user interfaces displayed on the computer 100 through which the visual preview of intermediate steps of software configuration are provided, according to one embodiment of the present invention. The examples shown in FIGS. 3A-3F are screenshots of the graphical user interface for configuring a virtual Ethernet switch. FIG. 2 will be explained together with FIGS. 3A-3F .
Referring to FIG. 2 , as the software configuration process is started, a plurality of options (or parameters) for software configuration are displayed 202 on the display device 107 of the computer 100 for selection by the user. For example, referring to FIG. 3A , options are provided to the user to select the connection type 302 for the virtual Ethernet switch, i.e., Virtual Machines 304 , VMotion and IP storage 306 , and Service Console 308 . The user's selection of one or more of the options is received 204 ( FIG. 2 ). For example, as shown in FIG. 3A , Virtual Machines 304 was selected as the connection type 302 . The user can proceed to the next step of the software configuration process by clicking the “Next” button 309 .
Referring back to FIG. 2 , a graphical preview of the intermediate configuration of the software with the selected option is displayed 206 to the user on the display device 107 of the computer 100 in real time as the option is selected. For example, referring to FIG. 3B , a preview 316 graphically represents the configuration state of the software that would result from the user's selection of Virtual Machines in FIG. 3A if the software configuration is actually executed. Specifically, in the example of FIG. 3B , “VM Network 1 ” 317 (VM for virtual machine) is shown selected in response to the selection of “Virtual Machines” 304 in FIG. 3A . In order to display the previews in real time, the software may include pre-stored graphical representations of all possible combinations of the software configurations corresponding to each step and each combination of parameters of the software configuration process, and display the one corresponding to the parameters selected in that software configuration step. Although FIG. 3A illustrates that the selection of the options or parameters is made by selecting an icon separate from the preview 316 , in other embodiments, the selection of the parameters can be made by directly modifying or selecting the parameters in the preview 316 itself, either in addition to, or instead of, the method illustrated in FIG. 3A .
Then, it is determined 208 whether the software configuration is complete. If it is complete, then the final state of the software configuration is displayed 209 on the display device 107 of the computer 100 before the software configuration is actually performed. Then, the software configuration is actually performed 210 according to the parameters as selected by the user in the various steps of the software configuration process. If the software configuration is not complete in step 208 , the process returns to step 202 for the next step of the software configuration.
For example, in the example of FIG. 3B , the software configuration process is still not complete, so the process returns to step 202 . This time, a selection of network access adaptors 312 , 314 is requested in the display (step 202 ). In FIG. 3C , it is shown that Adaptor 2 318 is selected (step 204 ), and a preview 316 includes the Adaptor 2 320 shown as the selected network adaptor.
Referring to FIG. 3D , the software configuration is still not complete, this time requesting the user to define the Port Group Properties 322 , specifically the Network Label 324 (step 202 ). Referring to FIG. 3E , as the user selects “Blue” 326 as the network label 324 (step 204 ), the preview 316 also reflects that the network label has changed to “Blue” 326 (step 206 ).
Referring to FIG. 3F , now that the software configuration is complete (i.e., all selections of the software configuration parameters have been made), the final software configuration that reflects all the previous steps of the software configuration is graphically displayed in the preview 316 before the user finally commits to this software configuration (step 209 ). The software will be configured (step 310 ) according to the parameters selected in the preceding steps as shown in FIG. 3F once the user clicks the “Finish” button 330 .
The present invention has the advantage that the users are graphically guided throughout the software configuration process such that they easily understand the consequences of their selection of various software configuration parameters during the software configuration process before they make a final commitment completing the software configuration. In addition, constant visual feedback illustrating the change in the software configuration in response to their selection of various software configuration parameters helps the users familiarize themselves with the software system gradually as it is configured, resulting in a graphical representation of the software that can be useful during on-going maintenance, monitoring and control of the software after the software configuration.
Upon reading this disclosure, those of ordinary skill in the art will appreciate still additional alternative processes for providing a visual, step-by-step preview of the software configuration process. For example, although the present invention was described in the context of configuring a virtual Ethernet switch, the present invention can be applied to the configuration of any type of software running on any type of computer. The present invention can be used for configuring new software as well as modifying the configuration of software that has been previously configured. For another example, although visual previews 316 were provided to illustrate the various intermediate software configuration states, audible messages describing the intermediate configuration states can also be provided as the previews. Various graphical techniques such as zooming and panning operations may be used with the present invention in order to more effectively present the previews to the user.
Thus, while particular embodiments and applications of the present invention have been illustrated and described, it is to be understood that the invention is not limited to the precise construction and components disclosed herein. Various modifications, changes and variations which will be apparent to those skilled in the art may be made in the arrangement, operation and details of the method and apparatus of the present invention disclosed herein without departing from the spirit and scope of the invention as defined in the appended claims.
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A step-by-step visual preview into a guided software configuration process is provided, where the preview is updated in real time as users specify the parameters of the software during the software configuration process, thereby providing a visual explanation of the various components of the software and their relationship to one another. Before the newly assembled software configuration is actually performed, the complete graphical representation of the software configuration is displayed for approval.
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This application is a continuation-in-part of application Ser. No. 853,466, filed Apr. 18, 1986, now abandoned.
BACKGROUND OF THE INVENTION
The invention relates to an automatic attack angle adjusting bracket for a concrete finishing float, of the type generally known as a bull float, and more particularly relates to a device which causes the leading edge of a concrete float to automatically lift in response to the pushing or pulling force routinely applied by the worker to the handle of the float to maneuver the float over the surface being smoothed.
A concrete bull float includes a generally rectangular finishing blade or float and an elongated pole handle attached to the center of the float. A worker uses the pole handle to push the float forward and pull the float backward across the work surface in order to smooth the concrete. The handle of the float may be formed from several pole sections that are interconnected by couplings of the threaded, telescoping/spring-pin locked or similar type.
As the worker manipulates the currently typical long handled float, he tilts the leading edge of the finishing face slightly upwards away from the concrete surface as he pulls or pushes the float. The tilting of the float pushes the concrete in the direction that the float is being moved and prevents the leading edge of the trowel from digging into the concrete being smoothed. As the concrete begins to dry, the wetness of the concrete changes. With drier concrete, the workers must tilt the leading edge of the float higher to provide more action to smooth the concrete. With wet concrete, the worker puts less tilt in the leading edge of the float to prevent the blade from plowing the concrete. Thus, the worker must be able to manipulate the face of the float at various angular positions while maneuvering the trowel over the concrete.
Where the float face is fixed in a rigid relationship to the handle, the adjustment in the angle of the face is made by the worker raising and lowering the handle to tilt the face. Where the concrete surface covers a wide area, the handle of the trowel may be up to twenty-four feet long. With such a long handle, the worker must repetitively straighten up, raise hands and arms above the head, then bend downward and drop arms in order to manipulate the trowel. Clearly, adjustment of the trowel angle relative to the concrete is difficult and exhausting to the worker.
In order to avoid putting the worker through this series of calisthenics, the angle of the float blade relative to the handle is made adjustable by the worker. Heretofore, this angle adjustment has been accomplished in a number of different ways.
For example, L. L. Bennett in U.S. Pat. No. 2,934,937 issued on May 3, 1960 and L. H. Ferrell, Jr., et al. in U.S. Pat. No. 3,090,066, issued May 21, 1963, disclose cement slab finishing trowels in which the worker rotates the pole for adjusting the angle of the float. Other patents showing other means for tilting the float relative to the handle, include U.S. Pat. No. 3,146,481 issued to E. Chiuchiarelli on Sept. 1, 1964 and U.S. Pat. No. 3,798,701 issued to W. Irwin et al. on Mar. 26, 1974. Such devices utilize complicated connection structure for performing the tilting of the float as the operator rotates the elongated pole. Further, with such devices, the operator must remember which way to rotate the pole depending on whether he is performing a pushing stroke or a pulling stroke. Also, the worker must remember to rotate the pole so that the float lies flat at the completion of each stroke to avoid marking the surface. Because such devices utilize a rotational movement of the pole, the sections of the elongated handle must be secured together by means other than non-locking screw connections to avoid having the handle come apart.
It is one object of the present invention to provide a bull float which is easily manipulated without the need to learn or to become skilled at or to remember additional rotational manipulations of the pole handle.
It is another object of the present invention to provide a bull float which is compatible with existing types of handles and specifically non-locking pole handle sections.
It is a further object of the present invention to provide a bull float in which the handle may be kept at a comfortable work height because the leading edge of the float is automatically raised by the conventional pushing and pulling force exerted on the handle by the worker.
It is yet another object of the present invention to provide a float having automatic tilt adjustment in which the worker may selectively stop the automatic tilt adjustment to permit shearing of high spots in the concrete surface.
It is also an object of the present invention to provide a float bracket which automatically adjusts the tilt of the float in accordance with the wetness of the concrete being smoothed by the float.
SUMMARY OF THE INVENTION
These and other objects of the invention are achieved in a tilting mechanism for a concrete bull float which automatically tilts the float blade in response to the force on and the direction of movement of the handle of the float. In the preferred embodiment, the tilting mechanism includes a base member and cover member which are interconnected by a mechanical assembly which moves the base member relative to the cover member in accordance with the force and direction of movement of the pole. The base member pivots relative to the cover member as defined by a "pivotal point" lying below the concrete surface being finished.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing a workman using a bull float having a tilting mechanism of a preferred embodiment of the present invention;
FIG. 2 shows a cut-away perspective view of the tilting mechanism of the bull float of FIG. 1;
FIG. 3 shows a top view of the tilting mechanism of FIG. 2;
FIG. 4 shows a sectional side view of the tilting mechanism of FIG. 2 taken through line 4--4 of FIG. 3;
FIG. 5 shows a cross-sectional end view of the tilting mechanism of FIG. 2 taken through line 5--5 of FIG. 4;
FIG. 6 shows a cross-sectional view of a coupling mechanism of FIG. 4 during a pulling stroke on the float;
FIG. 7 shows a cross-sectional side view of the coupling mechanism of FIG. 4 during a pushing stroke on the float; and
FIG. 8 shows a cross-section view of a coupling mechanism of FIG. 4 during stop-engagement of the blade for shearing high spots in the concrete surface.
DETAILED DESCRIPTION OF INVENTION
Referring to FIG. 1, a concrete float 11 includes a finishing float or blade 13 for movement across concrete 15 to spread and smooth the concrete prior to hardening. Blade 13 is generally rectangular in shape and usually formed of wood, magnesium, aluminum or other light material, and preferably has a length of 40-54 inches and a width of approximately eight inches. A pole handle 17 is used by a worker from a remote position to reciprocally push and pull the blade across the concrete. Pole 17 is connected to blade 13 by a tilting bracket or mechanism 19.
As the worker pushes pole 17 forward to move blade 13 across the concrete, tilting mechanism 19 causes the forward edge 23 of the float to be lifted upwardly away from the concrete. This prevents the leading edge (forward edge 23) from digging into the concrete. Then as the worker pulls pole 17 toward him, tilting mechanism 19 causes the now leading edge, rear edge 25, of the float to be lifted upwardly away from the concrete. When the worker neither pushes nor pulls the pole handle 17, the float blade lies flat.
The extent of the angle of inclination of the blade 13 is automatically adjusted in accordance with the degree of wetness of the concrete. With dry concrete, the angle of tilt increases, pitching the leading edge higher than with wet concrete.
As shown in FIGS. 2-8, tilting mechanism 19 is formed of a base member 27, a pivotal or cover member 29 and a pair of pivotal links 31, 33. Base member 27 is secured to one or more longitudinal ribs 35 formed integral to the topside of blade 13 and extending upwardly therefrom, as shown, for supporting base member 27. Four screws 37 pass through washers 39, through holes (not shown) drilled in base member 27 and into ribs 35, to hold the base member fixed relative to blade 13. Alternatively, where blade 13 is formed with a single longitudinal rib, a channel 36 formed in the base member receives the top of the rib and holes 38 permit screw securement of the base member to the single rib. In the event that the float blade is of solid, unribbed construction (i.e., a plain wooden panel), suitable fasteners through holes 38 and/or 39 may be used to secure bracket 19 to the blade 13.
Base member 27 includes a pair of upstanding parallel walls 41, 43 (FIG. 5) disposed substantially orthogonal to the underside finishing face 45 of the blade. The lower ends of links 31, 33 are pivotally secured between walls 41, 43 by a pair of cylindrical bearing surfaces 47, 49 (FIG. 2). Bearing surfaces 47, 49 are supported by walls 41, 43 and are secured in a fixed relationship to base member 27. Links 31, 33 include respective cylindrical openings 51, 53 (FIG. 4) through which pass cylindrical bearing surfaces 47, 49 for permitting the links to pivot about the respective axes 55, 57 (FIG. 4) of the cylindrical bearing surfaces 47, 49. The two axes 55, 57 are disposed parallel to one another lying in a plane generally parallel to finishing surface 45.
Cover member 29 is a generally hollowed, cup-shaped member for covering links 31, 33 and a portion of base member 27 for protecting the area generally indicated at 59, 61 (FIG. 5) where the links pivot on bearing surfaces 47, 49. Concrete, dirt, or other debris is thus prevented from lodging in the pivotal area which might hamper pivoting.
As will suggest itself, cover member 29 need not perform the function of a cover but need only perform the function of providing a structure which is securable to the pole for receiving the pulling and pushing force applied to the pole handle by the worker, and providing a structure to be coupled to the base member for controlling the "pivotal" movement of the blade. Such a structure may be a pair of side walls 70, 72 (FIG. 5) of sufficient height to provide an area for bearing surfaces 67, 69 wherein the side walls are formed integral to a tail member 66, (FIG. 2) having a threaded sleeve 99 for receiving a threaded end of pole 17.
Cover member 29 establishes two pivotal axes 63, 65 (FIG. 4) about which pivot the upper ends of links 31, 33. A pair of cylindrical bearing surfaces 67, 69 (FIG. 4) are secured between the side walls 70, 72 (FIG. 5) of the cover member and have axes 63, 65 (FIG. 4) as their center axes. The bearing surfaces 67, 69 are held fixed relative to cover member 29. Links 31, 33 include respective cylindrical openings 71, 73 (FIG. 4) through which pass cylindrical bearing surfaces 67, 69 (FIG. 2) for permitting the links to pivot about respective axes 63, 65 (FIG. 4).
The two upper axes 63, 65 are disposed parallel to one another and parallel to lower axes 55, 57. As seen from FIG. 4, the plane formed from axes 63, 55 and the plane formed from axes 65, 57 intersect at a pivotal line 75 disposed below the finishing surface 45. Reference numeral 75 may also be referred to as the "pivotal point" in reference to the cross-sectional plane shown in FIG. 4.
The line or "point" of intersection of the two planes (defined by axes 63, 55 and 65, 57) takes on positions different than point 75 (as indicated, for example, by points 77, 79, 81, 83) as base member 27 is pivoted relative to cover member 29. A dotted line 78 represents the locus of points resulting from the intersection of the two planes during the pivotal movement of base member 27 relative to cover member 29. Thus, the "pivot point" of the base member relative to the cover member is a dynamic point, tracing out a curve 78. The pivot point must at all times lie below the finishing face 45 of the blade.
When the plane defined by axes 63, 65 is parallel to the plane defined by axes 55, 57 (as shown in FIG. 4) the pivot point takes the position identified by numeral 75. In this position, the pivot point 75 is about 4 inches beneath finishing surface 45. The coefficient of friction provided by the concrete affects the pivoting of the base member relative to the cover member, and therefore the distance of pivot point 75 below the finishing surface 45 is selected for compatibility with the frictional coefficient of the concrete.
Assume, for explanation purposes, that there is no frictional drag on blade 13 as the blade is pulled across the concrete, as though the blade was pulled along in mid air. The blade would not be tilted relative to the cover member but would occupy the relative position shown in FIG. 4 with the pivot point located at point 75. However, in reality, as the blade is moved across the concrete, a frictional force occurs which tilts the blade.
FIG. 4, pivot point 75 is below the finish surface 45. Pole handle 17 is pulled by the worker, the frictional drag on the surface 45 of the blade causes relative movement of the blade 13 with respect to base member 27. The friction force of the concrete serves to drag or pull the blade rearwardly relative to the cover member. The pivotal links 31, 33 define the path of the movement of the blade, referred to herein as a pivotal or rotational movement, as the blade is dragged rearwardly. This rotational movement of the blade raises its leading edge 91 (FIG. 6) and shifts the pivot point to location 76 on curve 78. This rotational movement becomes opposed by the gravitational weight of the concrete float 11 bearing upon the surface of the concrete. As the blade 13 and base member 27 rotate, the leading edge 91 is raised so that the float surface 45 is only in partial contact with the concrete surface (FIG. 6). The area 92 of the float surface 45, which is in contact with the concrete surface, supports the weight of the concrete float 11. The support area 92 has moved rearward (as compared to the float in its rest position, FIG. 4) and the distributed force on the support area is the equal of a force centered at the reaction force 104. The force 104 is rearward of the pivot point 76 which is the support center for the weight W1 of the cover 29, and portion of the pole handle 17. The force 104 is also rearward of the center of the weight W2 of the blade 13 and base member 27. The weights of the cover 29, pole handle 17, blade 13 and base 27 are reacting downward and the locations of their weights are laterally disposed forward from the upward force 104 to cause a rotational moment. This rotational moment balances a second rotational moment created by the frictional drag force F o and the pulling force P o on the handle.
The wetness of the concrete determines the frictional force F o and the area 92 which is in contact with the concrete surface. As area 92 moves rearward, so does force 104. As the concrete gets drier, the frictional force gets larger and the angle of tilt increases, pitching the leading edge higher. With wet concrete, the frictional force is lower and the angle of tilt decreases.
For example, with concrete at a wetness A 1 , the pivot point will occupy position 76 on curve 78 (see FIG. 4). With this wetness A 1 , the blade is at a small angle of tilt. With concrete at a wetness A 2 (drier than A 1 ), the pivot point will occupy position 79 of FIG. 4. With this wetness A 2 , the blade is at a greater angle of tilt than with concrete at wetness A 1 . With concrete at a wetness A 3 (drier than A 2 ), the pivot point will occupy position 82 of FIG. 4. With this wetness A 3 , the blade is at a greater angle of tilt than with concrete at wetness A 2 .
The change in the tilt of the blade is automatically adjusted by the wetness of the concrete itself. This discussion with respect to the frictional effect of the concrete on the extent of the tilt of the blade relative to the horizontal surface of the concrete assumes that the cover member 29 has a constant angular orientation with respect to the horizontal surface of the concrete. The angular orientation of the cover member with respect to the horizontal surface of the concrete may be defined by angle 87.
When the float is in a stationary rest position shown in FIG. 4, the angle between the axis of pole 17 and the finishing surface 45 is approximately 14 degrees. The angle 87 is the angle between the axis of the pole 17 and the horizontal, i.e., the concrete surface. During float operations, angle 87 may take on a value within a range of angles from 4 to 24 degrees.
Using the structure of the preferred embodiment, the angle 87 continuously changes as the blade moves closer and then farther from the worker. Assuming the worker holds the pole handle at waist height, a comfortable position, then when the blade is close to the worker, angle 87 will be greater than when the blade is far from the worker. The blade will pivot relative to the cover member depending on both handle angle and blade friction with the concrete.
Referring again to FIG. 6, the angular orientation of the cover member relative to the concrete (angle 87) varies the location of the pivot point along curve 78. Thus, both the frictional effect of the concrete and the angular orientation of cover member 29 determines the tilt position of the blade relative to the concrete.
As shown in FIG. 7, during a pushing stroke on pole 17, base member 27 pivots relative to cover member 29. The line of intersection between the plane formed by axes 63, 55 and the plane formed by axes 65, 57 is line or pivot point 80. The angle 87 between the axis of pole 17 and the horizontal is shown at approximately 14 degrees. As the blade is pushed away from the worker, angle 87 will decrease and the blade will automatically pivot relative to the cover member in accordance with the wetness of the concrete.
As pole 17 is pushed (FIG. 7), concrete drag on the face 45 of the float causes the leading edge 89 of the float to be pivoted upwardly away from the concrete. The amount of force which must be supplied to the pole is determined by the amount of frictional drag. The force applied to the pole automatically causes relative pivoting between the base member and the cover member. The same force and moment analysis can be applied to the pushing stroke as was made above with respect to the pulling stroke of FIG. 6.
Referring again to FIG. 4, axes 55, 57 of the lower ends of respective links 31, 33 follow respective arcuate paths 93, 95 during pivoting of the base member relative to the cover member. When links 31, 33 are pivoted to their forwardmost position on arcuate paths 93, 95, the relative position of cover member 29 and base member 27 is as shown in FIG. 8.
A stop member 97 (FIG. 8) is formed integral to cover member 29 for contacting float blade 13 at this forwardmost pivotal position. At this point, the blade no longer automatically adjusts its tilt. The worker may select this position of the float by lowering the handle until the blade contacts stop 97 (FIG. 6), when angle 87 becomes approximately 4 degrees. The worker may then use the float in this position for shearing off high spots on the concrete surface using leading edge 91 as the worker pulls the float toward him.
Referring again to FIG. 2, cover member 29 is formed with a threaded sleeve 99 at its rearward end for receiving the threaded end of pole handle 17. Sleeve 99 may be secured to the cover member by forming the sleeve integral with the cover member or may be secured to the cover member by other means. The side walls of cover member 29 depend downwardly about links 31, 33 to prevent dirt from entering the pivotal area, as best seen in FIG. 5. As shown in FIG. 5, the cover member may be formed to include depressions 101, 103 to provide a handle for carrying of the float separate from the pole by the workman. As will suggest itself, cover member 29 need not be configured to "cover" the pivotal links but may take on other shapes for establishing the upper pivoting axes 63, 65 of links 31, 33 and carrying the force applied through pole handle 17.
Also, one or more of links 31, 33 may be replaced by cam rollers and a cam track for pivoting the base member relative to the float blade. For example, the base member may carry a cam track and the cover member may carry rollers which follow the cam track.
It is to be understood, of course, that the foregoing describes different embodiments of the present invention and that modifications may be made therein without departing from the spirit or scope of the present invention as set forth in the appended claims.
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An automatic tilt adjusting bracket for connection between a pole handle and a concrete float blade. The bracket includes a base member, a cover member and mechanical linkage interconnecting the base and cover members. As the pole handle is pushed and pulled, a force is applied to the cover member pivoting the base member relative thereto for automatically lifting the leading edge of the float blade.
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CROSS REFERENCE TO RELATED APPLICATIONS
U.S. Provisional Application No. 60/603,480, filed Aug. 20, 2004 for “Group III-V Compound Semiconductor Based Heterojunction Bipolar Transistors with Various Collector Profiles on a Common Wafer” by Mary Chen and Marko Sokolich, the disclosure of which is incorporated herein by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
The present invention was made with support from the United States Government under Grant number F33615-02-C-1286 awarded by DARPA. The United States Government has certain rights in the invention.
FIELD
This invention relates to a new design with InP based Heterojunction Bipolar Transistors (HBTs) with emitter-down profiles, including those for high Ft HBTs, and emitter-up profiles, including those for high breakdown voltage (BVceo), on a common wafer and to a method of producing the same.
BACKGROUND AND PRIOR ART
InP based HBT Integrated Circuit (IC) technologies have demonstrated great potential in high-speed digital and mixed-signal applications because of superior speed and bandwidth properties over the SiGe based HBT technology. Although C. R. Bolognesi et al, “Non-blocking collector InP/GaAs 0.51 Sb 0.49 /InP double heterojunction bipolar transistor with a staggered lined up base-collector junction”, IEEE Electron Device Letters, Vol., 20, No. 4, April, 1999, pp. 155-157 suggests that a symmetry of InP/GaAsSb/InP DHBT band structure may have the potential for integration of collector-up and emitter-up devices, present invention implements selective ion implantation technology for integration of high Ft HBT (collector-up HBTs) and high BVceo HBT (emitter-up HBTs) on same chip.
SiGe based HBT technology of various collector concentrations available on the same chip has been described in the prior art. See, for example, G. Freeman et al, “Device scaling and application trends for over 200 GHz SiGe HBTs”, 2003 Topical Meetings on Silicon Monolithic Integrated Circuits in RF Systems, pp. 6-9, Digest of papers. The SiGe based HBT technology enables high F t to be traded for high BVceo on the same chip. However, IC designers up to now could not trade high F t for high BVceo or vice versa on the same InP.
The ability to provide high F t HBTs and high BVceo HBTs on the same chip is particularly useful in smart Power Amplifiers (PAs) in millimeter wave image radar. Increased power provides longer distance of operation. Smart PAs with digital electronics to control the PAs can be realized by high speed signal processes for regular logic and high BVceo (breakdown voltage) for large swing at output stage. However, presently, when high BVceo HBTs are used in logic circuits lower speed may occur as compensation due to inability to serve as high F t HBTs in logic circuits on the same chip.
The ability to provide high F t HBTs and high BVceo HBTs on a common chip substrate may also be useful in the front-end stage of an analog to digital (A/D) converter. Having high F t HBTs and high BVceo HBTs on common chip substrate may provide increased dynamic range and larger input to analog converter which may be advantageous for higher signal/noise (S/N) ratio and resolution. However, A/D technologies of today cannot provide significantly higher peak-to-peak input signal than 1V with good linearity. Better dynamic range may improve this technology.
Accordingly there is a need for fabricating and integrating high F t HBTs and high BVceo HBTs on the common non-silicon based wafer.
BRIEF DESCRIPTION OF THE FIGURES AND THE DRAWINGS
FIG. 1 depicts a side view of an emitter-up HBT;
FIG. 2 depicts a side view of an emitter-down HBT;
FIG. 3 depicts a wafer with HBTs on the wafer;
FIGS. 4-23 depict a process of forming HBTs based on an exemplary embodiment;
FIGS. 24-29 depict a process of forming HBTs based on another exemplary embodiment.
DETAILED DESCRIPTION
In the following description, like reference numbers are used to identify like elements. Furthermore, the drawings are intended to illustrate major features of exemplary embodiments in a diagrammatic manner. The drawings are not intended to depict every feature of every implementation nor relative dimensions of the depicted elements, and are not drawn to scale.
The present disclosure describes new designs with InP based HBTs with emitter-up (collector-down) and emitter-down (collector-up) profiles including those for high F t HBTs and high BVceo HBTs on a common wafer. Specially designed epi-taxial layer structures with selective area doping by ion implantation can integrate HBTs with emitter-up and emitter-down profiles, including those HBTs for high F t and HBTs for high BVceo on the same InP wafer without backside processing.
Referring to FIGS. 1 and 2 , in one exemplary embodiment, a cutaway side view is shown of two out of hundreds of thousands (for example) of HBTs 10 and 11 of the presently disclosed technology that may be grown as part of individual circuits 30 separated by streets 40 on a substrate of wafer 20 (See FIG. 3 ). For clarity reasons the HBTs 10 and 11 , individual circuits 30 and wafer 20 , as depicted in FIGS. 1 , 2 and 3 , are not to scale.
According to the presently disclosed technology, HBTs, as shown in FIGS. 1 and 2 , may be grown having either a high BVceo or a high F t by performing ion implantation in layer 90 or layer 70 , as shown in FIGS. 1 and 2 .
Referring to FIGS. 1-19 , individual HBTs 10 and 11 may be grown on the substrate 50 of the wafer 20 , wherein the substrate layer 50 may be a Semi-Insulating (S.I.) InP wafer. The thickness of the substrate layer 50 may be about 0.5 mm. For clarity and example purposes FIGS. 3-19 depict the process of forming at least one emitter-up HBT 10 and at least one emitter-down HBT 11 on the single wafer 20 , as shown in FIG. 3 .
Referring to FIG. 4 , layer 60 may be formed, for example by epitaxial growth, on top of the substrate 50 . The layer 60 may comprise, for example, N-type InGaAs (N+) material that is heavily doped with silicon or N-type InP (N+) material that is heavily doped with silicon. The thickness of the layer 60 can vary from about 100 Å to about 5000 Å. Layer 60 may function as a sub-collector layer for emitter-up HBT 10 or as a sub-emitter layer for emitter-down HBT 11 .
Referring to FIG. 5 , layer 70 may be formed, for example, by epitaxial growth, on top of the layer 60 . The layer 70 may comprise, for example, N-type InP (N−) undoped material. The thickness of the layer 70 may be determined by the emitter-up HBTs in the wafer 20 with the highest BVceo requirement. Layer 70 may be formed uniformly across layer 60 to a maximum thickness that is required to yield the emitter-up HBT with the highest BVceo requirement. The profile of the layer 70 for emitter-up HBTs may be varied as described in the U.S. Provisional Application No. 60/603,480, incorporated herein by reference. Layer 70 may function as a collector layer for emitter-up HBT 10 or as an emitter layer for emitter-down HBT 11 .
Referring to FIGS. 2 and 6 - 11 , to form an emitter layer for emitter-down HBT 11 , an ion implantation may be performed on layer 70 to create N-type doped (N) regions 75 and isolated regions 78 . Isolation regions 78 may prevent parasitic current injection through the extrinsic base-emitter junction area under forward bias. The ion implantation of region 75 in the individual emitter-down HBTs 11 may be performed by: 1) applying and forming an implant mask 71 on top of the layer 70 so as to expose only the portion of the layer 70 for one or more of the emitter-down HBTs, as shown in FIG. 6 ; 2) performing ion implantation until region 75 is formed, as shown in FIG. 7 ; 3) removing implant mask 71 and annealing the structure in FIG. 8 for implant activation and damage removal wherein N region 75 is formed.
This disclosure is not limited to a shape of implant region 75 as depicted in FIGS. 2 and 6 - 8 . There may be single or multiple implants forming individual region 75 depending on the performance requirements for the emitter-down HBTs 11 . The thickness and doping level of region 75 may be formed by varying the energy and dose of the ion implantation process.
Referring to FIGS. 2 and 9 - 11 , the ion implantation of regions 78 for isolation in the individual emitter-down HBTs 11 may be performed by: 1) applying and forming an implant mask 72 on top of the layer 70 so as to expose only the portions of the layer 70 for one or more of the emitter-down HBTs, as shown in FIG. 9 ; 2) performing ion implantation until regions 78 are formed, as shown in FIG. 10 ; 3) removing implant mask 72 , as shown in FIG. 11 . This disclosure is not limited to shape of implant isolation regions 78 as depicted in FIGS. 2 and 9 - 11 .
The ion implantation of regions 75 may follow ion implantation of regions 78 . If regions 78 are implanted before regions 75 , regions 75 may be subjected to rapid thermal annealing to avoid possible thermal instability in regions 78 .
The ion implantation of regions 75 and 78 may be performed by regular masked implantation or by stencil mask ion implantation technology. See for example Takeshi Shibata et al, “Stencil mask ion implantation technology”, IEEE Transactions on semiconductor manufacturing, Vol, 15, No. 2, May 2002, pp. 183-188.
Upon completion of the ion implantation, an optional smoothing layer (not shown) may be formed by epitaxial growth on top of the layer 70 . The smoothing layer may enable smoothing of the epitaxial growth surface prior to deposition of the base-collector interface and emitter-base interface. The smoothing layer may comprise, for example, N-type InP (N−) material. The thickness of the smoothing layer may, for example, be about 200 Å.
Referring to FIG. 12 , a base layer 80 may be formed, for example, by epitaxial growth, on top of the layer 70 or on top of the optional layer referred to above. The base layer 80 may comprise, for example, P-type GaAsSb (P+) material. The thickness of the base layer 80 may, for example, be about 400 Å.
Referring to FIG. 13 , a layer 90 may be formed, for example by epitaxial growth, on top of the base layer 80 . The layer 90 may comprise, for example, N-type InP (N) material doped with silicon. The thickness of the layer 90 may, for example, be about 1500 Å. Layer 90 may function as an emitter layer for emitter-up HBT 10 or as a collector layer for emitter-down HBT 11 .
Referring to FIG. 14 , a layer 100 may be formed, for example by epitaxial growth. The emitter cap layer 9 may comprise, for example, N-type InGaAs (N+) material that is doped heavily with silicon. The thickness of the layer 100 may, for example, be about 1000 Å. Layer 100 may function as a collector cap for emitter-down HBT 11 or as an emitter cap for emitter-up HBT 10 .
Referring to FIG. 1 , an optional implantation of region 95 may be performed to increase doping of the emitter layer (layer 90 ) and lower emitter resistance Re for emitter-up HBTs 10 .
Referring to FIGS. 1 and 15 - 17 , to form an emitter layer for emitter-up HBT 10 , an ion implantation may be performed on layer 90 to create a heavily doped (N+) region 95 . The ion implantation of region 95 in the individual emitter-up HBTs 10 may be performed by: 1) applying and forming an implant mask 91 on top of the layer 100 so as to expose only the portions of the layers 90 and 100 for one or more of the emitter-up HBTs, as shown in FIG. 15 ; 2) performing ion implantation until region 95 may be formed, as shown in FIG. 16 ; 3) removing implant mask 91 and performing rapid thermal annealing of the structure in FIG. 17 for implant activation and damage removal wherein N+ region 95 may be formed.
Ion implantation of region 95 may be performed on layer 90 prior to formation of layer 100 .
This disclosure is not limited to a shape of implant region 95 as depicted in FIGS. 1 and 15 - 17 . There may be single or multiple implants forming individual region 95 depending on the performance requirement for emitter-up HBTs 10 . The thickness and doping level of region 95 may be formed by varying the energy and dose of the ion implantation process.
In one exemplary embodiment, the process of HBT fabrication may include: providing metal contacts 110 through lithography and metal deposition as shown in FIG. 18 ; etching emitter mesas 150 for emitter-up HBT 10 and collector mesas 160 for emitter-down HBT 11 , as shown in FIG. 19 ; providing base metal contacts 120 through lithography and metal deposition, as shown in FIG. 20 ; etching base mesas 170 , as shown in FIG. 21 ; providing metal contacts 130 through lithography and metal deposition, as shown in FIG. 22 ; and etching isolation mesas 180 , as shown in FIG. 23 . As shown in FIGS. 18-23 , the substrate 50 has the same thickness at locations under the emitter-up HBT 10 and the emitter-down HBT 11 . The substrate 50 may also have the same thickness at locations between the emitter-up HBT 10 and the emitter-down HBT 11 .
Metal contacts 110 may function as emitter contacts for emitter-up HBTs 10 or as a collector contact for emitter-down HBTs 11 . Metal contacts 130 may function as collector contacts for emitter-up HBTs 10 or as emitter contacts for emitter-down HBTs 11 . The electrically conducting metal contacts 110 , 120 , 130 may comprise, for example, Ti/Pt/Au, Pt/Ti/Pt/Au, AuGe or AuGe/Ni/Au.
Referring to FIGS. 24-29 , in another exemplary embodiment, the process of HBT fabrication may include formation of self-aligned base metal contacts 120 so as to lower base resistance. Referring to FIG. 24 , formation of self-aligned metal contacts 120 may include providing metal contacts 110 through lithography and metal deposition. Referring to FIG. 25 , emitter mesas 210 for emitter-up HBT 10 and collector mesas 220 for emitter-down HBT 11 may be etched. Using metal contacts 110 as a mask, etching of mesas 210 and 220 may be performed. Due to over etching, lateral overhang of the metal contacts 110 may be expected.
Referring to FIG. 26 , layer 200 may be formed to at least partially cover metal contacts 110 . Layer 200 may comprise, for example, positive tone photo definable polyimide (PDPI) or positive tone photo sensitive interlayer dielectric (ILD).
Referring to FIG. 27 , layer 200 may be soft baked, may be flood exposed (maskless) and may be developed so as to remove most of the exposed layer 200 material except for the portions 201 , 202 , 203 and 204 protected by the lateral overhang of the metal contacts 110 . Flooding of the layer 200 may be performed with g-line (436 nm) or l-line (365 nm) lithography tools. Portions 201 , 202 , 203 and 204 may further be cured so as to avoid damage from sequential solvents or other processes.
Referring to FIGS. 28-29 , formation of self-aligned metal contacts 120 may be performed by: providing a photoresist layer 205 (patterned for base contact metal) so as to expose portions of layer 80 , as shown in FIG. 28 ; depositing metal contacts 120 and removing photoresist layer 205 through lift off process, as shown in FIG. 29 ; removing any metal flaxes that may be deposited on portions 201 , 202 , 203 , 204 by performing slight Argon (Ar) ion milling etch process.
The process of HBT fabrication may further include: etching base mesas (not shown); providing metal contacts 130 through lithography and metal deposition; and etching isolation mesas (not shown).
The foregoing Detailed Description of exemplary and preferred embodiments is presented for purposes of illustration and disclosure in accordance with the requirements of the law. It is not intended to be exhaustive nor to limit the invention to the precise form(s) described, but only to enable others skilled in the art to understand how the invention may be suited for a particular use or implementation. The possibility of modifications and variations will be apparent to practitioners skilled in the art. No limitation is intended by the description of exemplary embodiments which may have included tolerances, feature dimensions, specific operating conditions, engineering specifications, or the like, and which may vary between implementations or with changes to the state of the art, and no limitation should be implied therefrom. Applicant has made this disclosure with respect to the current state of the art, but also contemplates advancements and that adaptations in the future may take into consideration those advancements, namely in accordance with the then current state of the art. It is intended that the scope of the invention be defined by the claims as written and equivalents as applicable. Reference to a claim element in the singular is not intended to mean “one and only one” unless explicitly so stated. Moreover, no element, component, nor method or process step in this disclosure is intended to be dedicated to the public regardless of whether the element, component, or step is explicitly recited in the claims. No claim element herein is to be construed under the provisions of 35 U.S.C. Sec. 112, sixth paragraph, unless the element is expressly recited using the phrase “means for . . . ” and no method or process step herein is to be construed under those provisions unless the step, or steps, are expressly recited using the phrase “comprising the step(s) of . . . .”
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A wafer comprising at least one emitter-up Heterojunction Bipolar Transistor (HBT) and at least one emitter-down HBT on a common InP based semiconductor wafer. Isolation and N-type implants into the device layers differentiate an emitter-down HBT from an emitter-up HBT. The method for preparing a device comprises forming identical layers for all HBTs and performing ion implantation to differentiate an emitter-down HBT from an emitter-up HBT.
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[0001] The entire disclosure of Japanese Patent Application No. 2007-305486, filed on Nov. 27, 2007, is expressly incorporated by reference herein.
BACKGROUND
[0002] 1. Technical Field
[0003] The present invention relates to a character processing device, character distinction method and computer program for converting input characters to extended Latin characters.
[0004] 2. Related Art
[0005] Character processing devices that are capable of converting input alphabetical characters (standard alphabetical characters) to corresponding extended Latin characters (nonstandard alphabetical characters) have been generally known. In such a character processing device, after an alphabetical character is input and a conversion button is pressed by a user, conversion candidates for extended Latin characters related (similar) thereto are displayed. From the conversion candidates, the user selects a desirable extended Latin character. As described in JP-A-11-203032, for example, with the conversion button pressed after the input of an alphabetical character “e,” extended Latin characters similar to “e” are displayed; and therefrom a desirable extended Latin character (e.g., “ë”) is selected.
[0006] In the conversion to extended Latin characters mentioned above, unlike in the kana-to-kanji conversion made using the Roman character input, not all input alphabetical characters are subject to conversion. In the above character processing device, however, both alphabetical characters convertible and inconvertible to extended Latin characters are displayed without distinction. Accordingly, users who are well acquainted with extended Latin characters have no difficulty using such a device (converting to extended Latin characters) because they know what alphabetical characters are convertible to extended Latin characters, but users who are not familiar with extended Latin characters have difficulty discerning whether an input alphabetical character is convertible to an extended Latin character.
SUMMARY
[0007] An advantage of some aspects of the invention is to provide a character processing device, character distinction method and computer program for making it easy to discern whether a character subject to editing is convertible to an extended Latin character.
[0008] According to one aspect of the invention, a character processing device that converts an input character formed of an input alphanumeric or symbol to an extended Latin character similar to the input character includes a display unit displaying as an editing character the input character with a cursor attached thereto, a conversion target distinction unit discerning whether or not the editing character is convertible to an extended Latin character, and a notification unit indicating that the editing character is convertible to an extended Latin character when the editing character is regarded as convertible.
[0009] According to another aspect of the invention, a character distinction method for converting an input character formed of an input alphanumeric or symbol to an extended Latin character similar to the input character includes displaying as an editing character the input character with a cursor attached thereto, discerning whether or not the editing character is convertible to an extended Latin character, and indicating that the editing character is convertible to an extended Latin character when the editing character is regarded as convertible.
[0010] With these configurations, it is discerned whether a character subject to editing (editing character) is convertible to an extended Latin character, and it is indicated that the editing character is convertible if it is. Accordingly, even users who are not familiar with extended Latin characters (users who are little acquainted with extended Latin characters) may easily discern whether an input character is convertible to an extended Latin character. Extended Latin characters mean accented alphabetical characters seen in French or other languages (e.g., alphabetical characters with diacritical marks) and special symbols.
[0011] In this case, it is preferable that the conversion target distinction unit discern that the editing character is convertible to an extended Latin character when being a character subject to conversion to an extended Latin character, and that the editing character is inconvertible to an extended Latin character when not being a character subject to conversion.
[0012] With this configuration, the editing character is regarded as convertible to an extended Latin character when being a character subject to conversion, and the editing character is regarded as inconvertible to an extended Latin character when not being a character subject to conversion. In other words, it is possible to discern whether the editing character is convertible based on whether the editing character has an extended Latin character corresponding thereto. Characters subject to conversion mean alphabetical characters (e.g., “e”) similar (corresponding) to extended Latin characters (e.g., “ë”).
[0013] In this case, it is preferable that the conversion target distinction unit discern that the editing character is inconvertible to an extended Latin character when the editing character is not a character subject to conversion or is a specified character, if the editing character that is subject to conversion to an extended Latin character is regarded as a specified character with the cursor moved therefrom or the character converted to an extended Latin character.
[0014] With this configuration, a character subject to conversion that has been off target for conversion (e.g., a character subject to conversion that has been converted to and specified as an extended Latin character, or a character subject to conversion from which the cursor has moved) is regarded as a specified character, and the editing character is regarded as inconvertible to an extended Latin character if it is not a character subject to conversion or is a specified character. Regarding such characters as characters inconvertible to extended Latin characters may enhance the convenience of users.
[0015] In these cases, it is preferable that the character processing device also include a converter that converts the editing character to an extended Latin character based on a conversion operation when the conversion target distinction unit discerns that the editing character is convertible.
[0016] With this configuration, the editing character is converted to an extended Latin character based on the conversion operation when the editing character is convertible. This prevents device malfunctions caused by user mishandling because the conversion operation is deactivated with the editing character inconvertible.
[0017] In these cases, it is preferable that the notification unit be formed of an indicator that is turned on when the editing character is convertible to an extended Latin character and is turned off when the editing character is inconvertible.
[0018] With this configuration, the indicator is turned on when the editing character is convertible, and the indicator is turned off when the editing character is inconvertible (off target for conversion). This allows users to visibly discern whether a target character is a character convertible to an extended Latin character, and facilitates the discernment of whether the character is convertible to an extended Latin character.
[0019] In these cases, it is preferable that the character processing device also include a conversion candidate display unit displaying one or more extended Latin characters that are conversion candidates of the character subject to conversion, wherein the conversion candidate display unit displays the extended Latin characters in both lower and upper cases for the conversion candidates corresponding to the character subject to conversion.
[0020] With this configuration, conversion candidates corresponding to the character subject to conversion are displayed in both upper and lower cases despite the attribute (uppercase or lowercase) of the character subject to conversion. This makes it possible to provide user-friendly environments.
[0021] In this case, it is preferable that the conversion candidate display unit gives preference to the conversion candidates in lower case over the conversion candidates in upper case on the display when the character subject to conversion is lowercase, and that the conversion candidate display unit gives preference to the conversion candidates in upper case over the conversion candidates in lower case on the display when the character subject to conversion is uppercase.
[0022] With this configuration, preference is given to the conversion candidates for extended Latin characters in lower case on the display when the character subject to conversion is lowercase, and preference is given to the conversion candidates for extended Latin characters in upper case on the display when the character subject to conversion is uppercase. In general, users psychologically expect that if a character subject to conversion to an extended Latin character is input in lower case, it will be converted to an extended Latin character in lower case, and that if a character subject to conversion to an extended Latin character is input in upper case, it will be converted to an extended Latin character in upper case. Accordingly, preference is given to conversion candidates for extended Latin characters with the same attribute (lowercase or uppercase) as that of the input character subject to conversion on the display, which makes it possible to provide user-friendly environments.
[0023] According to yet another aspect of the invention, a computer program features the capability of causing a computer to execute each process of the character distinction method described above.
[0024] Using the computer program makes it possible to indicate that an input character is convertible to an extended Latin character.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The invention will be described with reference to the accompanying drawings, wherein like numbers reference like elements.
[0026] FIG. 1 is a system configuration diagram of a tape printing device according to one embodiment of the invention.
[0027] FIG. 2 is a control block diagram for the tape printing device.
[0028] FIG. 3 is a diagram illustrating a sequence of operations that converts target characters to extended Latin characters.
[0029] FIG. 4 is a diagram illustrating a sequence of operations that converts target characters to extended Latin characters.
[0030] FIG. 5 is a diagram illustrating the status change (on/off) of an extended Latin character conversion indicator that results from the move of a cursor.
[0031] FIG. 6 is a diagram illustrating the status change of the extended Latin character conversion indicator with the tape printing device turned ON and OFF.
[0032] FIGS. 7A and 7B are diagrams illustrating an example of characters subject to conversion, characters exempt from conversion and extended Latin characters corresponding to characters subject to conversion.
DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0033] One embodiment of the invention will hereinafter be described in detail with reference to the accompanying drawings. A tape printing device that produces labels by printing on tape-shaped media will be taken for an example of a character processing device to describe the embodiment of the invention.
[0034] FIG. 1 is an external perspective view of a tape printing device 1 according to the embodiment of the invention with an opening/closing lid 4 open. As shown in FIG. 1 , the exterior of the tape printing device 1 is provided by a device case 2 ; arranged on the front top of the device case 2 is a keyboard 3 (input unit) incorporating various input keys; and disposed on the left-rear and right-rear top thereof are the opening/closing lid 4 and a display screen 5 (display unit) respectively. Inside the opening/closing lid 4 , a cartridge holder 6 to install a tape cartridge C in is provided so as to be a depression. With the opening/closing lid 4 open, a tape cartridge C is installed in the cartridge holder 6 so that it may be ejected and re-installed. On the opening/closing lid 4 , an observation window 7 is provided to allow for visual checks on tape cartridge C installation with the opening/closing lid 4 closed.
[0035] Arranged on the keyboard 3 are a character key group 3 a and a function key group 3 b used to set various operation modes or the like. The character key group 3 a has features common to a keyboard for a regular word processor or the like such as a full-keyboard structure based on the JIS keyboard layout and shift keys to restrain an increase in the number of keys. The function key group 3 b includes a Print key 11 to issue a command for printing, a Delete key 12 to delete characters, a Power key 13 to turn ON and OFF the power, an Extended Latin Character Conversion key 14 to convert characters (alphabetical characters) to extended Latin characters 73 described below, cursor keys (“↓”, “↑”, “←” and “→”) 15 to move a cursor and do scrolling, and a Select key 16 to select from a menu, specify a character, and perform other tasks.
[0036] The display screen 5 is a liquid crystal display, which is used when users input data with the keyboard 3 , create and edit printing data such as character strings (text data) and images, and check on the data result. Disposed at the bottom of the display screen 5 is an area showing an indicator (hereinafter called “extended Latin character conversion indicator 18 [notification unit]”) that makes it possible to discern whether a character subject to editing (editing character or character with a cursor K attached thereto) is convertible to an extended Latin character 73 . The extended Latin character conversion indicator 18 is turned on when the character is a character subject to conversion 71 that is convertible to an extended Latin character 73 ; and it is turned off when the character is a character exempt from conversion 72 that is inconvertible. (Characters subject to conversion 71 , characters exempt from conversion 72 and extended Latin characters 73 corresponding to characters subject to conversion 71 are detailed in FIGS. 7A and 7B .)
[0037] Provided in the left side of the device case 2 is a tape ejecting slot 21 that connects the cartridge holder 6 and outside. Attached to the tape ejecting slot 21 is a tape cutter 22 to cut a printing tape T (tape-shaped material) that is fed out. Fed out of the tape ejecting slot 21 is a given length of the printing tape T that has been printed. With feeding motion stopped briefly, the printing tape T that has been printed is cut by the tape cutter 22 and made into a label. Cutting processes may switch from automatic cutting to manual cutting and vice versa. A cutter motor 23 (see FIG. 2 ) is driven automatically (in auto mode) for printing in fixed lengths, and manually (in manual mode) by the operation of a Cut key included in the keyboard 3 for printing in random lengths.
[0038] The cartridge mounting section 6 includes a head unit 24 having a printhead 26 (printing unit) incorporated therein and formed of a thermal head inside a head cover 25 , a platen drive spindle 27 facing the printhead 26 , a takeup reel drive spindle 28 to reel in an ink ribbon R described below, and a positioning boss 29 that positions a tape reel 32 described below. Embedded under the cartridge mounting section 6 is a tape feeding motor 30 (see FIG. 2 ) that rotates the platen drive spindle 27 and takeup reel drive spindle 28 .
[0039] A tape cartridge C is formed so as to house a tape reel 32 with a printing tape T of a given width (approximately 4 . 5 to 48 mm) wound therearound in the upper central interior of a cartridge case 31 , and a ribbon reel 33 with an ink ribbon R wound therearound in the lower right interior of the cartridge case 31 . The printing tape T and ink ribbon R are formed so as to have the same width. A through aperture 34 for inserting to the head cover 25 covering the head unit 24 is formed at the bottom left of the tape reel 32 . Arranged according to where the printing tape T and ink ribbon R overlap is a platen roller 35 fitted and driven to rotate on the platen drive spindle 27 . Arranged adjacent to the ribbon reel 33 is a ribbon takeup reel 36 . The ink ribbon R fed out of the ribbon reel 33 is arranged so as to travel around the head cover 25 to be reeled in onto the ribbon takeup reel 36 .
[0040] The printing tape T is formed of a recording tape Ta (backing tape) with an adhesive layer on the back and a detachable tape Tb stuck on the recoding tape Ta with the adhesive layer (see FIG. 1 ). Wound into a roll with the recording tape Ta outside and the detachable tape Tb inside, the printing tape T is contained in the cartridge case 31 . The printing tape T comes in a plurality of different tape types (e.g., in different tape widths, tape colors and ink colors), and has in the back of the cartridge case 31 a plurality of holes (not shown) that allow for identification of such tape types. The cartridge holder 6 has a plurality of tape type recognition sensors (microswitches) 37 (see FIG. 2 ) corresponding to the plural number of holes. The tape type recognition sensors 37 enable identification of tape types by checking on the plural number of holes.
[0041] Referring to the control block diagram shown in FIG. 2 , the control configuration of the tape printing device 1 will be described hereinafter. The tape printing device 1 includes a central processing unit (CPU) 61 , a random access memory (RAM) 62 , a read only memory (ROM) 63 , the keyboard 3 , the display screen 5 , the extended Latin character conversion indicator 18 , the cutter motor 23 , the tape cutter 22 , the tape feeding motor 30 , the printhead 26 and the tape discriminating sensors 37 . Some of the above, i.e., the ROM 63 , keyboard 3 , display screen 5 , extended Latin character conversion indicator 18 , cutter motor 23 , tape feeding motor 30 and printhead 26 are connected with the CPU 61 via buses 64 . Connected directly to the RAM 62 , the CPU 61 uses the RAM 62 as a work area for exercising various controls.
[0042] The ROM 63 stores a control program used for various controls executed by the CPU 61 . The ROM 63 also has an extended Latin character storage area 65 storing extended Latin characters 73 corresponding to characters subject to conversion 71 that are convertible to extended Latin characters 73 . Included in the control program is an extended Latin character conversion program that discerns whether an editing character (character pointed to by a cursor K) is convertible to an extended Latin character 73 , and controls the extended Latin character conversion indicator 18 based on the discernment result.
[0043] The extended Latin character conversion indicator 18 indicates by brightening or darkening part of the display screen 5 whether an editing character is convertible. The extended Latin character conversion indicator 18 may use an independent display such as an LED instead of brightening part of the display screen 5 .
[0044] The cutter motor 23 , connected to the tape cutter 22 , functions as a cutting unit. The tape feeding motor 30 and printhead 26 function as a printing unit to print on a printing tape T. The printhead 26 and tape discriminating sensors 37 are disposed in the cartridge holder 6 as described above. The tape discriminating sensors 37 detect the type of a printing tape T contained in the tape cartridge C.
[0045] Referring to FIGS. 3 and 4 , a sequence of operations that converts target characters to extended Latin characters 73 (character distinction method) will be described hereinafter. In the figures, a white square used for the extended Latin character conversion indicator 18 means it is off, and a black square used therefor means it is on. This is also applicable to FIGS. 5 and 6 described below.
[0046] The extended Latin character conversion indicator 18 is turned on when the extended Latin character conversion program described above discerns that an editing character is a character subject to conversion 71 and is convertible to an extended Latin character 73 . On the other hand, the extended Latin character conversion indicator 18 is turned off when the extended Latin character conversion program discerns that the character is not a character subject to conversion to an extended Latin character 73 (a character exempt from conversion 72 ) or that a character subject to conversion 71 is a specified character (e.g., a character subject to conversion 71 that has been off target for editing as a result of the move of the cursor K, or a character subject to conversion 71 that has been converted to and specified as an extended Latin character 73 ). Accordingly, characters exempt from conversion 72 and characters subject to conversion 71 that have been off target for editing as specified characters are regarded as characters inconvertible to extended Latin characters 73 , which may enhance the convenience of users.
[0047] As shown in FIG. 3 , a character input screen 5 a (display screen 5 ) is displayed (D 01 ) when the tape printing device 1 is turned ON by a user. In this case, the extended Latin character conversion indicator 18 is off. When a character “T” is input (input character) under this situation (D 01 ), the tape printing device 1 displays on the character input screen 5 a a character “T” with a cursor K attached thereto (editing character) (D 02 ). In this case, the tape printing device 1 , based on the list of extended Latin characters 73 shown in FIG. 7B , discerns that the character “T” is a character exempt from conversion 72 (a character that is not a character subject to conversion 71 ) (conversion target distinction unit), and does not turn on the extended Latin character conversion indicator 18 .
[0048] When a character “e” is input next, the tape printing device 1 discerns that the character “e” is a character subject to conversion 71 , and turns on the extended Latin character conversion indicator 18 (D 03 ). Since the character “e” has never been converted to an extended Latin character 73 and the cursor K has never been moved away from the character “e,” the tape printing device 1 discerns that the character “e” is a character subject to conversion 71 that is convertible to an extended Latin character 73 (conversion target distinction unit).
[0049] When a character “l” is input without the Extended Latin Character Conversion key 14 pressed under this situation (D 03 ), the tape printing device 1 discerns that the character “e” is a specified character and that the character “l” that has been input is a character exempt from conversion 72 , and turns off the extended Latin character conversion indicator 18 (D 04 ). When another character “e” is input, the tape printing device 1 discerns that the character “e” is a character subject to conversion 71 (a character subject to conversion 71 that is convertible), and turns on the extended Latin character conversion indicator 18 (DOS).
[0050] With the Extended Latin Character Conversion key 14 pressed under this situation (D 05 ), the tape printing device 1 calls conversion candidates 81 related to the character “e” out of the extended Latin character storage area 65 , and displays them on a conversion candidate selection screen 5 b (display screen 5 ) (D 06 , conversion candidate display unit) Since the character “e” subject to conversion has been input in lower case, the tape printing device 1 gives preference to conversion candidates 81 in lower case on the display (displays conversion candidates 81 in lower case before conversion candidates 81 in upper case), and highlights the first conversion candidate 81 a. The extended Latin character conversion indicator 18 is kept on.
[0051] With a cursor key 15 (“→” or “↓”) or the Extended Latin Character Conversion key 14 several pressed under this situation (D 06 ), the tape printing device 1 displays one of the other conversion candidates 81 after another. At this moment, the conversion candidates 81 in lower case are followed by the conversion candidates 81 in upper case on the display (D 07 , D 08 ). In other words, conversion candidates 81 in both upper and lower cases corresponding to the character subject to conversion are displayed despite the attribute (uppercase or lowercase) of the character subject to conversion. At this moment, the extended Latin character conversion indicator 18 is also on. Accordingly, not only are conversion candidates 81 with the attribute identical with or different from that of a character subject to conversion (lowercase or uppercase) displayed, but preference is given to conversion candidates 81 for extended Latin characters 73 with the same attribute as that of the character subject to conversion on the display, which makes it possible to provide user-friendly environments.
[0052] With the above keystrokes used, a space SP (“_”) indicating the last conversion candidate 81 is highlighted (D 09 ) With the Select key 16 pressed under this situation, the tape printing device 1 gives an alert to a user by graying the screen out (D 10 ), and returns to the last screen D 09 . With the space SP (“_”) highlighted, the press of the cursor key 15 (“→” or “↓”) or Extended Latin Character Conversion key 14 results in the return to the first ( 81 a ) of the conversion candidates 81 (D 11 ).
[0053] With the Select key 16 pressed under this situation (D 11 ), the tape printing device 1 specifies the conversion candidate 81 a that has been selected (highlighted), and displays the character 82 replacing the character “e” on the character input screen 5 a (D 12 , converter). At this moment, the tape printing device 1 discerns that the character “e” is a specified character, and turns off the extended Latin character conversion indicator 18 . When the Extended Latin Character Conversion key 14 is pressed again with the screen D 12 displayed, the tape printing device 1 gives an alert by graying the screen out to notify a user that the target character 82 is off target for conversion (inconvertible) (D 13 ) because the target character 82 is regarded as a specified character, returning to the last screen D 12 .
[0054] When the Delete key 12 is pressed with the screen D 06 displayed, the tape printing device 1 cancels the display of conversion candidates 81 and returns to the last document input screen (D 05 ). When another character (e.g., a character “A”) is instead input without the Select key 16 pressed with the screen D 11 displayed, the tape printing device 1 displays the character 82 replacing the character “e” followed by a character “A” on the character input screen 5 a (D 14 ). In this case, the extended Latin character conversion indicator 18 is on because the character “A” is regarded as a character subject to conversion 71 that is convertible. When a character exempt from conversion 72 (e.g., a character “P”) is input instead of a character “A,” the extended Latin character conversion indicator 18 is turned off.
[0055] Referring to FIG. 5 , the status change (on/off) of the extended Latin character conversion indicator 18 that results from the move of the cursor K will be described hereinafter. When a character “e” is input with a user-input character string “Tel” displayed (D 21 ), the tape printing device 1 not only displays a character string “Tele” on the character input screen 5 a but discerns that the character “e” is a character subject to conversion 71 that is convertible, turning on the extended Latin character conversion indicator 18 (D 22 ). At this moment, the cursor K points to the character “e”.
[0056] When the left cursor key 15 (“←”) is pressed, the tape printing device 1 moves the cursor K one character to the left to point it to the character “l” (D 23 ). At this moment, the tape printing device 1 discerns that the character “l” is a character exempt from conversion 72 , and turns off the extended Latin character conversion indicator 18 .
[0057] When the right cursor key 15 (“→”) is pressed, the tape printing device 1 moves the cursor K one character to the right to point it to the character “e” (D 24 ). Since the character “e” has been off target for editing (conversion) as a result of the move of the cursor K in this case, the tape printing device 1 discerns that the character “e” is a specified character (a character subject to conversion 71 that has been off target for conversion). Accordingly, the tape printing device 1 does not turn on the extended Latin character conversion indicator 18 (keeps the extended Latin character conversion indicator 18 off).
[0058] Referring to FIG. 6 , the status change of the extended Latin character conversion indicator 18 with the tape printing device 1 turned OFF during character input processes will be described hereinafter. When a user inputs characters “T,” “e,” “l” and “e” in turn, the tape printing device 1 not only displays a character string “Tele” on the character input screen 5 a but discerns that the character “e” input at the end is a character subject to conversion 71 that is convertible, and turns on the extended Latin character conversion indicator 18 (D 31 ). When the tape printing device 1 is turned OFF with the Power key 13 pressed, the tape printing device 1 specifies the character “e” before turning OFF itself (D 32 ).
[0059] When the tape printing device 1 is turned ON with the Power key 13 pressed again, the tape printing device 1 displays the character input screen 5 a that had been displayed before the power was turned OFF (D 33 ). Since the character “e” has been specified at this moment, the tape printing device 1 discerns that the character “e” is off target for conversion, and turns off the extended Latin character conversion indicator 18 . Turned ON again after turned OFF during the display of conversion candidates 81 corresponding to the character “e” (with the extended Latin character conversion indicator 18 on), the tape printing device 1 discerns that the character “e” is off target for conversion, and turns off the extended Latin character conversion indicator 18 , as described above.
[0060] According to the embodiment of the invention as described above, when a character subject to editing (editing character) is convertible to an extended Latin character 73 , that is indicated with the extended Latin character conversion indicator 18 on, and the character is converted to an extended Latin character 73 based on the conversion operation. Accordingly, even users who are not familiar with extended Latin characters 73 (users who are little acquainted with extended Latin characters 73 ) may easily discern whether target characters are convertible to extended Latin characters 73 (whether target characters are characters that are convertible to extended Latin characters 73 ).
[0061] According to the embodiment of the invention, a target character that is a character subject to conversion 71 but has been off target for editing (has been a specified character) is no longer allowed to be converted to an extended Latin character 73 (when the character has been converted to and specified as an extended Latin character 73 or when the cursor K has left the character, for example). Instead, conversion to an extended Latin character 73 may be allowed to be carried out repeatedly if a target character is a character subject to conversion 71 . A target character that has been converted to and specified as an extended Latin character 73 may also be allowed to be converted to another extended Latin character 73 until the cursor K is moved. The extended Latin character conversion indicator 18 is turned on whenever a target character is convertible to an extended Latin character 73 .
[0062] According to the embodiment of the invention, conversion candidates 81 for extended Latin characters 73 are always displayed in the same order, beginning with the first of the conversion candidates 81 . However, with a learning function to learn results of conversion to extended Latin characters 73 incorporated, for example, conversion candidates 81 may be displayed based on the learning results.
[0063] According to the embodiment of the invention, visual notification of whether a target character is convertible to an extended Latin character 73 is provided with the extended Latin character conversion indicator 18 turned on or off. Instead, such notification may be provided with a target character decorated or aural notification may be provided with electronic sounds.
[0064] The characters subject to conversion 71 , characters exempt from conversion 72 and extended Latin characters 73 shown in FIGS. 7A and 7B are exemplary and do not limit the invention.
[0065] Each process of the character distinction method for the tape printing device 1 shown in the foregoing embodiment of the invention may be provided as a computer program that is executed by a computer. Such a computer program may be provided in a storage medium (not shown). As storage media, CD-ROM, flash ROM, memory cards (e.g., CompactFlash [registered trademark], SmartMedia, Memory Stick), Compact Discs, magneto-optical disks, digital versatile discs, flexible disks or other storage media may be used.
[0066] Despite the above embodiment of the invention, appropriate changes and modifications to the device configuration of the tape printing device 1 , the processes including the method of conversion to extended Latin characters and other part of the embodiment may be made without deviating from the scope of the invention.
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Provided herein is a character processing device that converts an input character formed of an input alphanumeric or symbol to an extended Latin character similar to the input character including: a display unit displaying as an editing character the input character with a cursor attached thereto; a conversion target distinction unit discerning whether or not the editing character is convertible to the extended Latin character; and a notification unit indicating that the editing character is convertible to the extended Latin character when the editing character is regarded as convertible.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 62/050,509, filed Sep. 15, 2014. This application is related to U.S. patent application Ser. No. ______, filed on ______. The entire contents of each of the above applications are hereby incorporated herein by reference.
TECHNICAL FIELD
[0002] The present disclosure relates to surgical devices, systems, and methods for performing prostatectomies, and, more particularly, to surgical devices, systems, and methods for coupling a urethra to a bladder after resecting a prostate.
BACKGROUND
[0003] Prostatectomy is the surgical removal of all or part of the prostate for men with early-stage disease or cancer that is confined to the prostate. In removing the prostate, the portion of the urethra that extends through the prostate becomes resected so that an anastomosis (e.g., stitching, stapling, etc.) is required to reconnect the urethra to the bladder. To effectuate a reliable anastomosis, the bladder neck is often pulled down into the pelvic cavity resulting in distortion of the bladder. Distortion of the bladder anatomy can lead to reduced bladder functionality or even incontinence. In cases of extensive prostate resection, the bladder neck may need to be removed entirely, making anastomosis to the bladder impossible.
[0004] After surgery, a catheter such as a Foley catheter is inserted through the urethra and anchored in the bladder by a balloon to maintain urine flow through the catheter while the surgical site of the anastomosis heals. Even if the anastomosis procedure is successful, post-operative complications such as anastomotic failure and/or infections can occur at the anastomotic site, necessitating further procedures or prolonged catheterization. When an anastomosis fails or otherwise cannot be performed, the patient may be subject to permanent catheterization.
SUMMARY
[0005] Accordingly, new devices, systems, and methods that improve prostatectomy procedures would be desirable. For instance, eliminating the anastomosis step in a prostatectomy would reduce operative time, post-operative complications, and infections. As a result, patient recovery time is shortened and patient comfort is maximized.
[0006] In one aspect, the present disclosure relates to a catheter assembly for coupling a body conduit to tissue. For example, in a prostatectomy procedure, a catheter and an implant of the catheter assembly are positionable in vivo to enable the implant to permanently act as a bridge between a patient's urethra and bladder after a resection of the patient's prostate.
[0007] The catheter assembly may include an elongated member such as a catheter, a balloon, first and second ports, and an implant. In some embodiments, the catheter assembly may include first and second balloons. The elongated member has an outer surface and an inner surface. The outer surface defines a distal opening. The balloon is supported on the outer surface of the elongated member adjacent to the distal opening. The first port is defined in a proximal end of the elongated member and is in fluid communication with the distal opening. The second port is defined in the proximal end of the elongated member and is in fluid communication with the balloon.
[0008] The implant is selectively positionable about the outer surface of the elongated member and is configured to receive a bioactive agent having tissue growth properties. The implant is configured to act as a bridge between the body conduit and the tissue and is separable from the catheter assembly. The implant may be at least partially formed from a collagen or a collagen copolymer. In certain embodiments, the implant may include a biologic derived from a decellularized tissue source. In some embodiments, the implant may have a tubular or planar configuration that engages the outer surface of the elongated member. In certain embodiments, the bioactive agent has bacteriostatic properties. In some embodiments, the implant may be at least partially formed from a decellularized biologic material. It is also recognized that the catheter may be useful for urethral reconstruction often associated strictures occurring from any number of causes but usually reconstructed with buccal mucosa where supporting an autologous graph and maintaining strain to the diameter of the urethra is important.
[0009] The bioactive agent may include one or more of epithelial cells, stem cells, epidermal growth factors, and fibroblast growth factors. In certain embodiments, the bioactive agent is impregnated within the implant.
[0010] The outer surface of the elongated member may be configured to receive the bioactive agent and the implant may be positionable over the outer surface of the elongated member so that at least a portion of an inner surface of the implant engages the bioactive agent.
[0011] In some embodiments, a distal portion of the implant is positioned over a proximal portion of the balloon and a proximal portion of the implant is positioned over the outer surface of the elongated member. The balloon may be configured to expand the implant in response to inflation of the balloon to anchor the distal portion of the implant against tissue. The implant may define a plurality of slits configured to facilitate expansion of the implant. It is appreciated that positioning the implant in close proximity to surrounding vascularized tissue is essential to growth of the implant and prevention of necrosis of the implant.
[0012] In certain embodiments, the implant is seeded with extracted cells from a patient prior to implantation. The seeded implant may be incubated prior to implantation.
[0013] According to one aspect, the present disclosure relates to a method for coupling a body conduit to tissue. The method includes engaging an implant about an outer surface of a catheter, the implant configured to receive a bioactive agent having tissue growth properties; inserting the catheter through the body conduit and into a tissue opening across a resected area; positioning the implant in the resected area; inflating a balloon to anchor the catheter within the tissue opening such that the implant bridges the body conduit and the tissue opening across the resected area; and maintaining the catheter and the implant in vivo to enable the bioactive agent to secure the implant in the resected area and to permanently bridge the body conduit and the tissue opening.
[0014] The method may involve deflating the balloon to remove the catheter after the implant is permanently secured in vivo. The method may include sliding the implant over the outer surface of the catheter to position the implant on the outer surface of the catheter, temporarily fixing it to the catheter such as with an un-knotted stay suture, wherein the catheter includes a Foley catheter. The method may involve impregnating the outer surface of the catheter with the bioactive agent and positioning the implant over an impregnated portion of the outer surface of the catheter. Inserting the catheter may include advancing the catheter through an unresected portion of a resected urethra and into a bladder such that the implant bridges a resected area defined between the unresected portion of the resected urethra and the bladder.
[0015] The method may involve inflating a second balloon to engage the implant with surrounding tissue. The method may include inflating a second balloon in a pulsatile manner. The method may include exchanging fluid through a conduit in communication with the implant.
[0016] In another aspect, the present disclosure relates to a method for implanting a xenograft in a human body. The method includes decellularizing a xenograft to form a collagen-based scaffold, seeding the collagen-based scaffold with human stem cells, changing a morphology of the human stem cells to render the collagen-based scaffold suitable for implantation within the human body, mounting the collagen-based scaffold on a catheter, and implanting the collagen-based scaffold within the human body to provide a bridge between tissues of the human body.
[0017] The method may involve harvesting the xenograft from porcine tissue. The porcine tissue may be a porcine urethra. In some embodiments, changing a morphology of the human stem cells includes differentiating of the human stem cells. Morphology changes can be effectuated via the use of pulsatile stress, growth factors, and/or signaling proteins. Scaffold structure and/or material elasticity may also effect morphology changes. Differentiating of the human stem cells may be conducted ex vivo.
[0018] In yet another aspect of the present disclosure, a catheter system includes a catheter, a biologic implant supported on the catheter, and a fluid conduit defined in the catheter and configured to exchange fluid between the catheter and the biologic implant. In some embodiments, the catheter supports an inflatable balloon having a porous membrane mounted thereon. The porous membrane may be in fluid communication with the fluid conduit.
[0019] According to still another aspect of the present disclosure, a catheter includes a body member having an inner surface and an outer surface, a first port defined in the body member, a balloon disposed about the outer surface of the body member, and a porous membrane supported on the balloon. The balloon may be configured to position an implant in close proximity to surrounding tissue. The porous membrane may be in communication with the first port to transport fluids and bioactive agents from the first port through the porous membrane.
[0020] In aspects, the catheter may further include a second port defined in the catheter and in communication with the balloon to communicate inflation fluid between the second port and the balloon.
[0021] In aspects, the balloon is configured to be inflated in a pulsatile manner.
[0022] In aspects, the catheter may further include a second balloon supported on the body member and configured to anchor a distal end of the body member within a conduit or an organ.
[0023] The body member may include a proximal end and a distal end. The distal end of the body member may define a distal opening in communication with the proximal end of the body member to enable transportation of fluids through the distal opening.
[0024] An implant may be supported on the balloon. The implant may be configured to act as a tissue scaffold in a repair or replacement of a natural anatomical conduit.
[0025] Other aspects, features, and advantages will be apparent from the description, the drawings, and the claims that follow.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and, together with a general description of the disclosure given above, and the detailed description of the embodiment(s) given below, serve to explain the principles of the disclosure, wherein:
[0027] FIG. 1A is a perspective view of one embodiment of a catheter assembly in accordance with the principles of the present disclosure;
[0028] FIG. 1B is a cross-sectional view of the catheter assembly of FIG. 1A as taken along line segment 1 B- 1 B;
[0029] FIG. 1C is an enlarged view, in partial cross-section, of the indicated area of detail shown in FIG. 1A ;
[0030] FIG. 2 is a cross-sectional view of an implant of the catheter assembly of FIG. 1A ;
[0031] FIGS. 3A-3D are progressive views of a prostatectomy procedure in accordance with the principles of the present disclosure;
[0032] FIG. 4 is a perspective view of another embodiment of a catheter assembly in accordance with the principles of the present disclosure;
[0033] FIG. 5 is a partial, cross-sectional view showing the catheter assembly of FIG. 4 positioned in vivo;
[0034] FIG. 6 is a side view of another embodiment of an implant;
[0035] FIG. 7 is a side view illustrating the implant of FIG. 6 as positioned on a catheter of the catheter assembly of FIG. 1A ;
[0036] FIG. 8 is a perspective view, with parts separated, of another embodiment of a catheter assembly with an implant thereof shown in cross-section;
[0037] FIG. 9 is an enlarged perspective view of a distal portion of the catheter assembly of FIGS. 8 ; and
[0038] FIG. 10 is a schematic illustration of a medical work station and operating console in accordance with the present disclosure.
DETAILED DESCRIPTION
[0039] Particular embodiments of the present disclosure are described hereinbelow with reference to the accompanying drawings in which like reference numerals designate identical or corresponding elements in each of the several views. As used herein the term “distal” refers to that portion of the system, apparatus and/or device, or component thereof, that are farther from the user, while the term “proximal” refers to that portion of the system, apparatus and/or device, or component thereof, that are closer to the user. In the following description, well-known functions or constructions are not described in detail to avoid obscuring the present disclosure in unnecessary detail.
[0040] Turning now to FIGS. 1A-1C , one embodiment of a catheter assembly 10 includes a catheter 100 (e.g., a Foley catheter) and an implant 200 supported thereon. Catheter 100 defines a longitudinal axis “A” and includes a manifold 110 and an elongated member 112 that extends distally from manifold 110 . Manifold 110 includes a first port 110 a and a second port 110 b that extend proximally therefrom. Elongated member 112 defines a first lumen 112 a having a proximal end in fluid communication with first port 110 a of manifold 110 and a distal end in communication with a distal opening 114 defined by elongated member 112 . Elongated member 112 defines a second lumen 112 b having a proximal end in fluid communication with second port 110 b of manifold 110 and a distal end in fluid communication with a distal balloon 116 supported on an outer surface of elongated member 112 . Elongated member 112 further defines a third lumen 112 c having a proximal end in communication with a third port 110 c and a distal end in fluid communication with a proximal balloon 118 supported on an outer surface of elongated member 112 at a location proximal to distal balloon 116 . Proximal balloon 118 is configured to at least partially overlap a gap in urethra length (e.g., resected area “RA” shown in FIG. 3B ), which may be surgically or otherwise created. Proximal balloon 118 and distal balloon 116 may be adjacent or at any space needed to achieve the urethral repair specific to the patient's anatomy. A porous membrane 120 is supported on proximal balloon 118 between an outer surface of the proximal balloon 118 and an inner surface of the implant 200 .
[0041] Elongated member 112 also defines a fourth lumen 112 d in communication with a port 110 d at a proximal end thereof and a fluid passage 122 at a distal end thereof. Fluid passage 122 is defined between the outer surface of proximal balloon 118 and the inner surface of implant 200 . The fluid passage 122 is arranged to facilitate drainage of fluids from, and/or transfer of fluids and/or nutrients “N” to, implant 200 . The porous membrane 120 is configured to enable these fluids and/or nutrients “N” therethrough.
[0042] As seen in FIG. 2 , implant 200 has a tubular configuration and may be at least partially formed of a fiber of collagen, a collagen copolymer, chitosan, polyvinyl alcohol (PVA), poly(acrylic acid) (PAA) and β-glycerol phosphate, poly(L-lactic acid) (PLLA), polycaprolactone (PCL), poly (d, 1-lactide-co-glycolide) (PLGA) and/or the like material. Implant 200 may be a tubular biomaterial or tube rolled from a biomaterial derived from porcine (e.g., urethra, skin, bowel, pericardium, etc.) and/or may be related to previous art known in commercial Medtronic Permacol products. Permacol derived materials have the advantage of being decellularized, but retain extracellular matrix and important growth factors. Durability of the Permacol processed material may enable crosslinking of tissue matrix to provide durability if ingrowth is delayed by insufficient blood supply.
[0043] Implant 200 extends between proximal and distal ends 202 , 204 and includes an outer surface 200 a and an inner surface 200 b that defines a lumen 200 c. Inner surface 200 b supports one or more bioactive agents 206 having tissue growth properties such as, for example: epithelial cells, stem cells, epidermal growth factors, and/or fibroblast growth factors. Inner surface 200 b may also support one or more bioactive agents 208 having bacteriostatic properties, (e.g., chitosan) to prevent infection (e.g., urinary tract infection). As can be appreciated, one or more of these bioactive agents 206 , 208 may have both tissue growth and bacteriostatic properties. In some embodiments, one or more of these bioactive agents are layered on inner surface 200 b. In certain embodiments, one or more of these bioactive agents are impregnated within implant 200 . The bioactive agents of any of the presently described catheter assemblies may be any substance or mixture of substances that have clinical use. The bioactive agents may invoke a biological action, exert a biological effect, or play a role in one or more biological processes. The type and amount of bioactive agent(s) used will depend, among other factors, on the particular site and condition to be treated.
[0044] Examples of classes of bioactive agents which may be utilized in accordance with the present disclosure include anti-adhesives, antimicrobials, analgesics, antipyretics, anesthetics, antiepileptics, antihistamines, anti-inflammatories, cardiovascular drugs, diagnostic agents, sympathomimetics, cholinomimetics, antimuscarinics, antispasmodics, hormones, muscle relaxants, adrenergic neuron blockers, antineoplastics, immunogenic agents, immunosuppressants, gastrointestinal drugs, diuretics, steroids, lipids, lipopolysaccharides, polysaccharides, platelet activating drugs, clotting factors, and enzymes.
[0045] In some embodiments, the bioactive agent may be a growth factor, such as transforming growth factors (TGFs), fibroblast growth factors (FGFs), platelet derived growth factors (PDGFs), epidermal growth factors (EGFs), connective tissue activated peptides (CTAPs), osteogenic factors, and biologically active analogs, fragments, and derivatives of such growth factors. In some embodiments, members of the transforming growth factor (TGF) supergene family, which are multifunctional regulatory proteins, are utilized. Members of the TGF supergene family include the beta transforming growth factors (for example, TGF-β1, TGF-β 2 , TGF-β3); bone morphogenetic proteins (for example, BMP-1, BMP-2, BMP-3MP-4, BMP-5, BMP-6, BMP-7, BMP-8, BMP-9); heparin-binding growth factors (for example, fibroblast growth factor (FGF), epidermal growth factor (EGF), platelet-derived growth factor (PDGF), insulin-like growth factor (IGF)); Inhibins (for example, Inhibin A, Inhibin B); growth differentiating factors (for example, GDF-1); and Activins (for example, Activin A, Activin B, Activin AB). Vascular growth factor (VGF) can be important to reestablishing blood supply to a graft and/or surrounding tissue, the absence of which is a leading cause of biological graft failure.
[0046] In some embodiments, the bioactive agent is a biologic or cell specific ligand capable of attracting or recruiting specific cell types, such as smooth muscle cells, stem cells, immune cells, and the like.
[0047] Suitable antimicrobial agents which may be included as a bioactive agent include triclosan, also known as 2,4,4′-trichloro-2′-hydroxydiphenyl ether; chlorhexidine and its salts, including chlorhexidine acetate, chlorhexidine gluconate, chlorhexidine hydrochloride, and chlorhexidine sulfate; silver and its salts, including silver acetate, silver benzoate, silver carbonate, silver citrate, silver iodate, silver iodide, silver lactate, silver laurate, silver nitrate, silver oxide, silver palmitate, silver protein, and silver sulfadiazine; polymyxin; tetracycline; aminoglycosides such as tobramycin and gentamicin; rifampicin; bacitracin; neomycin; chloramphenicol; miconazole; quinolones such as oxolinic acid, norfloxacin, nalidixic acid, pefloxacin, enoxacin and ciprofloxacin; penicillins such as oxacillin and pipracil; nonoxynol 9 ; fusidic acid; cephalosporins; and combinations thereof. In addition, antimicrobial proteins and peptides such as bovine lactoferrin and lactoferricin B may be included as a bioactive agent in the present disclosure.
[0048] Other bioactive agents include: local anesthetics; non-steroidal antifertility agents; parasympathomimetic agents; psychotherapeutic agents; tranquilizers; decongestants; sedative hypnotics; steroids; sulfonamides; sympathomimetic agents; vaccines; vitamins; antimalarials; anti-migraine agents; anti-parkinson agents such as L-dopa; anti-spasmodics; anticholinergic agents (e.g., oxybutynin); antitussives; bronchodilators; cardiovascular agents such as coronary vasodilators and nitroglycerin; alkaloids; analgesics; narcotics such as codeine, dihydrocodeinone, meperidine, morphine and the like; non-narcotics such as salicylates, aspirin, acetaminophen, d-propoxyphene and the like; opioid receptor antagonists such as naltrexone and naloxone; anti-cancer agents (i.e., to limit uncontrolled growth); anti-convulsants; anti-emetics; antihistamines; anti-inflammatory agents such as hormonal agents, hydrocortisone, prednisolone, prednisone, non-hormonal agents, allopurinol, indomethacin, phenylbutazone and the like; prostaglandins and cytotoxic drugs; chemotherapeutics (i.e., to limit uncontrolled growth); estrogens; antibacterials; antibiotics; anti-fungals; anti-virals; anticoagulants; anticonvulsants; antidepressants; antihistamines; and immunological agents.
[0049] Other examples of suitable bioactive agents include viruses and cells; peptides; polypeptides and proteins, as well as analogs, muteins, and active fragments thereof; immunoglobulins; antibodies; cytokines (e.g., lymphokines, monokines, chemokines); blood clotting factors; hemopoietic factors; interleukins (IL-2, IL-3, IL-4, IL-6); interferons (β-IFN, α-IFN and γ-IFN); erythropoietin; nucleases; tumor necrosis factor; colony stimulating factors (e.g., GCSF, GM-CSF, MCSF); insulin; anti-tumor agents and tumor suppressors; blood proteins such as fibrin, thrombin, fibrinogen, synthetic thrombin, synthetic fibrin, synthetic fibrinogen; gonadotropins (e.g., FSH, LH, CG, etc.); hormones and hormone analogs (e.g., growth hormone); vaccines (e.g., tumoral, bacterial and viral antigens); somatostatin; antigens; blood coagulation factors; growth factors (e.g., nerve growth factor, insulin-like growth factor); protein inhibitors; protein antagonists; protein agonists; nucleic acids such as antisense molecules, DNA, and RNA; oligonucleotides; polynucleotides; ribozymes; naturally occurring polymers including proteins such as collagen and derivatives of various naturally occurring polysaccharides such as glycosaminoglycans; peptide hydrolases such as elastase, cathepsin G, cathepsin E, cathepsin B, cathepsin H, cathepsin L, trypsin, pepsin, chymotrypsin, γ-glutamyltransferase (γ-GTP) and the like; sugar chain hydrolases such as phosphorylase, neuraminidase, dextranase, amylase, lysozyme, oligosaccharase and the like; oligonucleotide hydrolases such as alkaline phosphatase, endoribonuclease, endodeoxyribonuclease and the like.
[0050] In some embodiments, the bioactive agent may include an imaging agent such as iodine or barium sulfate, or fluorine, to allow visualization of the fluid at the time of application or thereafter through the use of imaging equipment, including X-ray, MRI, and CAT scan equipment. Other imaging agents which may be included are within the purview of those skilled in the art and include, but are not limited to, substances suitable for use in medical implantable medical devices, such as FD&C dyes 3 and 6, eosin, methylene blue, indocyanine green, or colored dyes normally found in synthetic surgical sutures. Suitable colors include green and/or blue because such colors may have better visibility in the presence of blood or on a pink or white tissue background.
[0051] In use such as in a prostatectomy procedure, as illustrated in FIGS. 3A-3C , tissue such as a prostate “P” or portions thereof, and portions of a body conduit such as a urethra “U,” are surgically removed from a resected area “RA.” Prior to insertion in urethra “U,” one or more bioactive agents 208 (e.g., epithelial cells obtained from the patient's body) may be placed on one or more surfaces of implant 200 such as inner surface 200 b. For example, a cytology brush or the like may be used to scrap the patient's body for removing epithelial cells from urethra “U” and for depositing the removed epithelial cells onto at least portions of implant 200 . The epithelial cells (or any other suitable bioactive agent) may be arranged on implant 200 so as to limit undesirable tissue adhesion. Implant 200 may then be slid over catheter 100 for insertion within urethra “U.” With implant 200 positioned on catheter 100 , catheter assembly 10 is advanced through urethra “U,” across resected area “RA,” and into a tissue opening “TO” of bladder “B.” Once in vivo, catheter 100 and implant 200 are positioned so that implant 200 acts as a bridge between urethra “U” and bladder “B.” Once catheter assembly 10 is disposed in the desired position, inflation fluid (not shown) can be delivered through catheter 100 via second port 110 b and second lumen 112 b (see FIGS. 1A and 1B ) to balloon 116 for inflation thereof. Inflation of balloon 116 within bladder “B” anchors catheter 100 so that implant 200 remains fixed in resected area “RA.”
[0052] Proximal balloon 118 is then inflated to engage implant 200 with the abdominal tissue surrounding the target anastomosis or graph location. Inflation may be pulsed to facilitate the conditioning of cells implanted and/or entering the implant 200 in vivo. Fluid accumulation surrounding implant 200 may be selectively drained through implant 200 via the fluid passage 122 between the proximal balloon 118 and the implant 200 . Alternately, the fluid passage 122 may pass nutrients or biologic agents “N” by injection through fluid passage 122 . By virtue of pulsation of proximal balloon 118 and control of fluids through fluid passage 122 , the catheter system is configured to form an in vivo bio reactor typical of industry applications.
[0053] Fluid “F,” such as urine (or blood) that pools within bladder “B,” can be drained from bladder “B” through distal opening 114 of catheter 100 and discharged through first port 110 a via first lumen 112 a (see FIGS. 1A and 1B ). Some fluid “F” collected within the bladder “B” may seep around catheter 100 and gather in resected area “RA” between implant 200 and catheter 100 . Suitable bioactive agents 206 positioned on implant 200 that have bacteriostatic properties protect against infection that could form in resected area “RA” as a result of the gathered fluid “F.”
[0054] While catheter assembly 10 is fixed in vivo, and with the properties of the one or more bioactive agents 206 , 208 , tissue growth “TG” is formed on and/or around at least portions of implant 200 (e.g., inner surface 200 b, distal and/or proximal portions of outer surface 220 a, etc.) to reconnect urethra “U” to bladder “B.” Tissue growth “TG” helps reform epithelial mucosal surfaces on inner surface 200 b of implant 200 , for example.
[0055] Tissue growth “TG” can occur along inner and/or outer surfaces 200 a, 200 b of implant 200 so that a proximal portion of implant 200 becomes fixed to the urethra “U” and a distal portion of implant 200 becomes fixed to the bladder “B.” As can be appreciated, distal and/or proximal ends 202 , 204 of implant 200 may be secured to urethra “U” using known fastening techniques such as stitching, stapling, and/or adhesive to facilitate securement of implant 200 thereto.
[0056] With reference to FIG. 3D , once implant 200 is fixedly secured in the patient's body across resected area “RA,” balloon 116 can be deflated and catheter 100 can be separated from implant 200 for withdrawal from the patient's body. With catheter 100 withdrawn, implant 200 remains in the patient's body and acts as a permanent bridge between urethra “U” and bladder “B.”
[0057] Turning now to FIG. 4 , one embodiment of a catheter assembly 10 ′ is illustrated. Catheter assembly 10 ′ includes catheter 100 and an implant 200 ′ supported thereon. Implant 200 ′ defines a plurality of slits 210 that enable implant 200 ′ to expand and facilitate tissue ingrowth. With implant 200 ′ in a contracted condition as shown in FIG. 4 , a distal portion 204 of implant 200 ′ is positioned on a proximal portion 116 a of balloon 116 of catheter 100 and a proximal portion 202 of implant 200 ′ is positioned on outer surface 112 c of catheter 100 .
[0058] As seen in FIG. 5 , once catheter assembly 10 ′ is inserted into bladder “B,” distal balloon 116 of catheter 100 is inflated, expanding implant 200 to contact surrounding abdominal tissue. Inflation of the distal balloon 116 and expansion of the implant 200 may be further facilitated by a plurality of slits 210 of implant 200 ′ so that implant 200 ′ can be positioned in an expanded condition with distal portion 204 of implant 200 ′ anchored to bladder “B” as depicted in FIG. 5 . Distal portion 204 may be flared outwardly relative to a remainder of implant 200 ′ to facilitate anchoring to bladder “B.” In particular, distal portion 204 of implant 200 ′ is anchored between proximal portion 116 a of balloon 116 and inner surfaces of bladder “B.” Proximal end 202 of implant 200 ′ can be secured to urethra “U” by appropriate application of suitable bioactive agents and/or using known fastening techniques such as stitching, stapling, adhesive, and/or the like as described herein. Notably, distal end 204 of implant 200 ′ can also be further secured to bladder “B” by appropriate application of suitable bioactive agents and/or using known fastening techniques such as stitching, stapling, adhesive, and/or the like as described herein. Once implant 200 ′ is fixedly secured in patient's body across resected area “RA,” balloon 116 can be deflated and catheter 100 can be separated from implant 200 ′ for withdrawal from the patient's body similar to that described above with respect to catheter assembly 10 . Also similar to implant 200 , implant 200 ′ acts as a permanent bridge in the patient's body between a body conduit such as urethra “U” and tissue such as bladder “B” (see FIG. 3D ).
[0059] With reference to FIG. 6 , one embodiment of an implant 300 has a planar configuration and includes an outer surface 302 a and an inner surface 302 b. Inner surface 302 b supports one or more bioactive agents 304 , 306 which maybe be layered thereon. As depicted in FIG. 7 , implant 300 can be wrapped around outer surface 112 c of elongated member 112 of catheter 100 , (e.g., in a spiral fashion as illustrated by arrow “Z”), to arrange the planar configuration of implant 300 into a tubular configuration with inner surface 302 b of implant 300 engaged with outer surface 112 c of catheter 100 . In use, catheter 100 and implant 300 are positioned in vivo so that when catheter 100 is withdrawn from the patient's body, implant 300 remains in the patient's body and acts as a permanent bridge similar to that described above with respect to implants 200 and 200 ′.
[0060] Turning now to FIGS. 8 and 9 , one embodiment of a catheter assembly 10 ″ having a catheter 400 and an implant 200 ″ is illustrated. Catheter 400 includes manifold 110 having an elongated shaft 412 extending distally therefrom. Elongated shaft 412 supports balloon 416 and defines distal opening 414 . Elongated shaft 412 includes an outer surface having an impregnated portion 412 a that supports one or more bioactive agents 208 as described herein. Implant 200 ″ includes an outer surface 200 a and an inner surface 200 b that supports one or more bioactive agents 206 . As illustrated by arrow “C,” implant 200 ″ is positionable over impregnated portion 412 a of catheter 400 so that inner surface 200 b and/or bioactive agent 206 of implant 200 ″ engages and/or contacts impregnated portion 412 a. In this regard, the one or more bioactive agents 208 of impregnated portion 412 a can migrate/transfer to inner surface 200 b of implant 200 ″. In use, catheter 400 and implant 200 ″ are positioned in vivo so that when catheter 400 is withdrawn from the patient's body, implant 200 ″ remains in the patient's body and acts as a permanent bridge similar to that described above with respect to implants 200 , 200 ′, and 300 .
[0061] Although described herein with regard to prostatectomies, the presently described devices, systems, and methods can be applied to any tissue and/or body conduit.
[0062] In some embodiments, any of the presently described implants can be formed ex vivo and implanted using the devices, systems, and/or methods presently described herein. In one example, body tissue can be a xenograft harvested from any suitable animal (e.g., porcine, bovine, etc.). For instance, a porcine urethra is harvested and decellularized to create a collagen-based scaffold (e.g., proteins, lipids, etc. are removed until only collagen or mostly collagen remains). The collagen-based scaffold may include elastin. The porcine urethra can be decellularized using any known physical treatments (e.g., temperature, force/pressure, and/or electrical disruption) and/or chemical treatments (e.g., acids, alkaline treatments, ionic/nonionic/zwitterionic detergents, etc). Once decellularized, the collagen-based scaffold can be seeded with human cells (e.g., stem cells), which may be stem cells. While the collagen-based scaffold is in a sterile environment (e.g., a sterile cell culture bag), a bioreactor can be coupled to the sterile environment to feed the collagen-based scaffold with an appropriate media including any required nutrients to sustain viability and/or growth. As the collagen-based scaffold becomes populated over time, the morphology of the human cells can be changed.
[0063] For example, the human cells can be proliferated and dedifferentiated as necessary to rebuild/regrow the human cells on the collagen-based scaffold into an epithelized urethra. Preferably, the tissue implant is configured to enable rapid ingress of the patients tissue (e.g., by fibroblast in the bulk and by spreading epithelial cells along the inner lumen of the implant). The ability to provide growth media through the membrane of the implant, as well as the ability to pulse the balloon of the implant will help in differentiating the cells in the implant and in accelerating the production of extracellular matrix (ECM)
[0064] In the hospital, cells may be harvested and proliferated to populate the implant structure prior to implantation, or through the porous membrane after implantation. Preferably, mesenchymal stem cells will be harvested and may be provided from a donor or from the patient's adipose or bone marrow. Proliferating and differentiation of these cells is well understood along with the potency of the cells often associated with patient age. In the case of an elderly patient, it may be preferred to have a donor source or a donor bank. It also possible to proliferate the patient's differentiated (adult) cells for the epithelium and the nonstriated muscle fibers in addition to the ECM extruded by fibroblasts and forming the wall of the implant or neourethral structure. The catheter system may be used to facilitate growth of the neourethra in a bioreactor vessel ex vivo or in the preferred in vivo process described.
[0065] The collagen-based scaffold may be attached to, and/or grown into and/or around tissue of the human body. The collagen-based scaffold may be implanted with a catheter similar to the process described above. For instance, a first end of the collagen-based scaffold can be secured to a body conduit such as the urethra and a second end of the collagen-based scaffold can be secured to tissue such as a bladder. However, with the collagen-based scaffold rebuilt/regrown ex vivo with the human cells prior to an implantation procure, the implantation procedure will be expedited.
[0066] The robotic arms of the surgical system are typically coupled to a pair of master handles by a controller. The handles can be moved by the surgeon to produce a corresponding movement of the working ends of any type of surgical instrument (e.g., end effectors, graspers, knifes, scissors, etc.) which may complement the use of one or more of the embodiments described herein. The movement of the master handles may be scaled so that the working ends have a corresponding movement that is different, smaller or larger, than the movement performed by the operating hands of the surgeon. The scale factor or gearing ratio may be adjustable so that the operator can control the resolution of the working ends of the surgical instrument(s).
[0067] The master handles may include various sensors to provide feedback to the surgeon relating to various tissue parameters or conditions, e.g., tissue resistance due to manipulation, cutting or otherwise treating, pressure by the instrument onto the tissue, tissue temperature, tissue impedance, etc. As can be appreciated, such sensors provide the surgeon with enhanced tactile feedback simulating actual operating conditions. The master handles may also include a variety of different actuators for delicate tissue manipulation or treatment further enhancing the surgeon's ability to mimic actual operating conditions.
[0068] Referring also to FIG. 10 , a medical work station is shown generally as work station 1000 and generally may include a plurality of robot arms 1002 , 1003 ; a control device 1004 ; and an operating console 1005 coupled with the control device 1004 . The operating console 1005 may include a display device 1006 , which may be set up in particular to display three-dimensional images; and manual input devices 1007 , 1008 , by means of which a person (not shown), for example a clinician, may be able to telemanipulate the robot arms 1002 , 1003 in a first operating mode.
[0069] Each of the robot arms 1002 , 1003 may include a plurality of members, which are connected through joints, and an attaching device 1009 , 1011 , to which may be attached, for example, a surgical tool “ST” supporting an end effector 1100 (e.g., a pair of jaw members), in accordance with any one of several embodiments disclosed herein, as will be described in greater detail below.
[0070] The robot arms 1002 , 1003 may be driven by electric drives (not shown) that are connected to the control device 1004 . The control device 1004 (e.g., a computer) may be set up to activate the drives, in particular by means of a computer program, in such a way that the robot arms 1002 , 1003 , their attaching devices 1009 , 1011 and thus the surgical tool (including the end effector 1100 ) execute a desired movement according to a movement defined by means of the manual input devices 1007 , 1008 . The control device 1004 may also be set up in such a way that it regulates the movement of the robot arms 1002 , 1003 and/or of the drives.
[0071] The medical work station 1000 may be configured for use on a patient “P” lying on a patient table 1012 to be treated in a minimally invasive manner by means of the end effector 1100 . The medical work station 1000 may also include more than two robot arms 1002 , 1003 , the additional robot arms likewise connected to the control device 1004 and telemanipulatable by means of the operating console 1005 . A medical instrument or surgical tool (including an end effector 1100 ) may also be attached to the additional robot arm. The medical work station 1000 may include a database 1014 coupled with the control device 1004 . In some embodiments, pre-operative data from patient/living being “P” and/or anatomical atlases may be stored in the database 1014 .
[0072] Persons skilled in the art will understand that the structures and methods specifically described herein and shown in the accompanying figures are non-limiting exemplary embodiments, and that the description, disclosure, and figures should be construed merely as exemplary of particular embodiments. It is to be understood, therefore, that the present disclosure is not limited to the precise embodiments described, and that various other changes and modifications may be effected by one skilled in the art without departing from the scope or spirit of the disclosure. Additionally, the elements and features shown or described in connection with certain embodiments may be combined with the elements and features of certain other embodiments without departing from the scope of the present disclosure, and that such modifications and variations are also included within the scope of the present disclosure. Accordingly, the subject matter of the present disclosure is not limited by what has been particularly shown and described.
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A method for coupling a body conduit to tissue is provided. The method includes engaging an implant about an outer surface of a catheter. The implant receives a bioactive agent having tissue growth properties. The method involves inserting the catheter through the body conduit and into a tissue opening across a resected area, positioning the implant in the resected area, inflating a balloon to anchor the catheter within the tissue opening such that the implant bridges the body conduit and the tissue opening across the resected area, and maintaining the catheter and the implant in vivo to enable the bioactive agent to secure the implant in the resected area to permanently bridge the body conduit and the tissue opening.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Applicant hereby claims the benefit of PCT application, Application No. PCT/US2010/046165, filed Aug. 20, 2010, which claims priority to an earlier filed provisional application, Application No. 61/235,587, filed Aug. 20, 2009, incorporated herein by reference.
TECHNICAL FIELD
[0002] This disclosure relates generally to cryogenic pressurization systems. More particularly, the present disclosure relates to a system and method for accumulating pressurized liquefied gases for downstream use.
BACKGROUND
[0003] Cryogenic fluids and liquefied gases (referred to collectively throughout this disclosure as liquefied gases), that is, fluids having a boiling point generally below −150° F. at atmospheric pressure, are used in a variety of applications. As an example, laboratories and industrial plants use nitrogen in both liquid and gas form for various processes.
[0004] Liquefied gases are typically stored as liquids that require pressurization and sometimes heating prior to usage. The liquid nitrogen stored by laboratories and industrial plants typically must be pressurized prior to use as a gas or liquid.
[0005] In other systems, the liquefied gas is converted to the gaseous phase and stored at a high pressure before the end-use application. Because the gas phase is less dense, the volume of these tanks had to be larger to store the necessary amount of gas phase liquefied gas to meet the pressure and volume requirements of the end-use application. Storing large amounts of high-pressure gas phase material required specialized and often expensive equipment. In addition, such storage poses a safety concern as the large gas accumulators store gas phase liquefied gas at relatively high pressures often around 3000 psig (pounds per square inch gauge) to accommodate the end-use application. There are a number of disadvantages of such systems. Storage tanks for pressurized gaseous phase liquefied gas are often bulky and have a large footprint. This is due in part to the increased volume of the gaseous phase as opposed to the liquids phase. In addition, such storage tanks are often expensive. In view of these disadvantages, it would be desirous for a system to accommodate the pressure and volume needs of an end-use application as well as reducing the expense, bulk, and danger of the system that provides the vaporized liquefied gas for the end-use application.
SUMMARY OF THE INVENTION
[0006] In accordance with one aspect of the invention, a system is provided that includes a supply of liquefied gas or cryogenic liquid. The liquid is supplied to a pump which builds pressure in the fluid stream. A liquid accumulator vessel collects liquid from the pump and is pressurized by vaporized fluid from a vaporizer that is also supplied by the pump. The vaporized fluid is added to the headspace of the accumulator to pressurize the liquid contents in the accumulator. A control system controls the parameters of the system to produce the desired pressure and flow of the output of the pressurized liquid, which is vaporized in a second vaporizer for use in an end-use application.
[0007] A method of the present invention comprising a supply source of a liquefied gas or cryogenic liquid in substantially a liquid state. A pump is fluidly connected to the supply source which in turn is fluidly connected to a liquid accumulator, a first vaporizer, and a second vaporizer. Liquid from the pump can be vaporized in the first vaporizer and fed into the headspace of the liquid accumulator to pressurize the liquid in the accumulator. Liquid from the pump may also be fed directly to the liquid accumulator or may bypass both the first vaporizer and the liquid accumulator and be supplied directly to the second vaporizer. Pressurized liquid from the liquid accumulator may also be supplied to the second vaporizer to produce pressurized vaporized liquefied gas or cryogenic liquid to an end-use application. A control system controls the operation and flow of the liquefied gas or cryogenic fluid and the vaporization of the same.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a schematic overview of a system for accumulating pressurized liquefied gases according to one embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0009] FIG. 1 shows one embodiment of the present invention which is a system for accumulating pressurized liquefied gases. System 10 includes a bulk storage tank 12 but can include any other supply means of storing liquefied gas in either bulk or otherwise. The pressure of such stored liquefied gases is usually between 30-600 psig. Storage tank 12 includes vents 13 which may be controlled by control system 14 for venting the storage tank 12 under preprogrammed or preset conditions such as temperature or pressure settings as is commonly known in the art. Such preprogrammed or preset conditions are usually determined by the construction of the vessel and/or the properties of the liquefied gas. Storage tank 12 is in fluid connection with a pump 16 via a valve 18 which is commonly known in the art and which may be replaced with any suitable means to supply liquefied gas from the storage tank 12 to the pump 16 . Pump 16 can be any type of pump commonly used in the art, including a positive displacement pump. The operation of pump 16 is controlled by control system 14 which may include a programmable logic controller (PLC) and a variable frequency drive (VFD). Sensors in the system (not shown) provide feedback to the control system 14 to ensure that the proper quality of liquefied gas remains in the pump 16 to prevent cavitation of the pump 16 which would be detrimental to the process. Pump 16 also may be used to increase the pressure of the liquefied gas. Generally, pump 16 will increase the pressure of the liquefied gas to a pressure of 400 to 3000 psig, though other pressures are contemplated by this invention. Pump 16 is fluidly connected to both the liquid accumulator 28 and a pressure building process vaporizer 20 via supply line 21 which diverges into two supply lines 22 , 24 . Liquefied gas exiting the pump 16 will most often have at least some gaseous phase liquefied gas included from the exposure to ambient air or the temperature increase that occurs during pumping and/or transmittal. The composite mixture of liquid and gas phase liquefied gas enters supply line 21 and is directed to supply lines 22 , 24 by the control system 14 . Control system 14 uses end-use application requirements as well as system feedback to determine the flow path of the composite fluid exiting the outlet side 17 of the pump 16 . A portion of such composite fluid may be directed to both supply lines 22 and 24 , or the composite fluid may be directed to only one of the supply lines. Supply line 22 is fluidly connected to the liquid accumulator 28 via a regulator or valve 30 as is commonly known in the art. Any suitable regulator or valve may be used and may be controlled by control system 14 or other suitable means including manually. Liquefied gas (or the composite fluid) can be supplied from bulk storage tank 12 through the pump 16 to the liquid accumulator 28 . Supply line 24 supplies liquefied gas (or the composite fluid) from the outlet side 17 of the pump 16 to a pressure building process vaporizer 20 . The pressure building process vaporizer 20 may be of any kind that is suitable for vaporizing liquefied gas or cryogenic fluid and such vaporizers are commonly known in the art. One type of vaporizer that is used is a fin-type heat exchanger that uses only ambient air to vaporize the liquefied gas. However, other suitable vaporizers are contemplated by this invention. The liquefied gas that is directed to the pressure building process vaporizer 20 by the control system 14 through the operation of valve 30 is thus heated thereby changing the phase of the material from liquid to gas or at least a portion of the fluid undergoes a phase change from liquid to gas. The pressure building process vaporizer 20 is fluidly connected to the headspace 32 of the liquid accumulator 28 . The vaporized liquid passes through a control valve 34 or other suitable means of controlling flow, which can be controlled by the control system 14 . The vaporized liquefied gas is then fed into the headspace 32 of the liquid accumulator 28 thereby exerting pressure on the liquid portion of the contents of the liquid accumulator 28 . The pump 16 is also in fluid connection with the liquid accumulator 28 . Liquefied gas, or the composite mixture exiting the outlet side 17 of the pump 16 can be directed into the liquid accumulator 28 by the control system 14 to ensure a proper volume of liquid in the accumulator 28 .
[0010] For some end-use applications, the liquefied gas may bypass the liquid accumulator 28 through the use of a valve 44 and/or check valve 42 or any other suitable means that is commonly known in the art. In such applications, the liquid accumulator 28 may be used to manage and normalize flow from the pump 16 to an ambient air heat exchanger 36 . The ambient air heat exchanger 36 can be any type of vaporizer commonly known in the art and is not limited to an ambient air exchanger.
[0011] In one aspect of the invention, liquefied gas may be fed into the liquid accumulator 28 to a level detected and controlled by control system 14 . Vaporized liquefied gas may be fed into the headspace 32 of the liquid accumulator 28 which can also be measured and controlled by the control system 14 . The pressure exerted on the liquid phase of the contents of the liquid accumulator 28 will increase the pressure with which the liquid phase exits the liquid accumulator 28 . The pressure and volume requirements of the end-use application can be used by the control system 14 to control the various valves to adjust the ratio of vaporized liquefied gas to liquid phase liquefied gas in the liquid accumulator 28 . The liquid accumulator 28 is in fluid connection with ambient air heat exchanger 36 which is also fluidly connected to bypass line 38 . A valve 40 is disposed between the liquid accumulator 28 and the ambient air heat exchanger 36 . The bypass line 38 has a check valve 42 and a valve 44 to bypass the accumulator 28 under preset conditions as may be determined by the control system 14 or by the valve specifications. The ambient air heat exchanger 36 may be of any kind known in the art including the fin-type heat exchanger discussed above, and is used to convert the liquid phase liquefied gas into the gas phase before the end-use application which may be any of a number of applications including industrial applications. The liquid phase liquefied gas exiting the liquid accumulator 28 is under pressure from the pressure exerted on it from the vaporized liquefied gas in the headspace 32 of the liquid accumulator 28 . When the pressurized liquid phase liquefied gas exits the liquid accumulator 28 it is in turn vaporized in the ambient air heat exchanger 36 . After the liquefied gas is vaporized, the vaporized liquefied gas can be supplied to the end-use application via supply line 46 . Alternatively, the liquid phase liquefied gas from the liquid accumulator 28 may be supplied to the ambient air heat exchanger 36 and then used directly in the end-use application via supply line 46 . In yet another alternative, the liquefied gas from the outlet side 17 of the pump 16 can be supplied to the ambient air heat exchanger 36 and then used directly in the end-use application via supply line 46 .
[0012] It can be seen from one skilled in the art that the present system provides a number of advantages. The invention of the present disclosure eliminates the need for large volume gas phase accumulators by instead using a liquid accumulator 28 . The end-use application pressure requirements can still be met by vaporizing the liquid stored in the liquid accumulator 28 . Moreover, the control system 14 can adjust the system to accommodate the requirements of the end-use application. For example, if the application requires a higher pressure of the gas phase at the supply line 46 , then more of the liquefied gas from the outlet side 17 of the pump 16 is fed into the pressure building process vaporizer 20 which is then supplied to the headspace 32 of the liquid accumulator 28 . This in turn pressurizes the liquid phase present in the accumulator 28 . When that higher-pressure liquid phase is then vaporized in the ambient air heat exchanger 36 , it allows a supply of higher-pressure gaseous phase liquefied gas to be used by the end-use application via supply line 46 .
[0013] In previous systems, accumulating a pressurized liquefied gas was not feasible or suitable because pressurizing the liquefied gas would often lead to an increase in the temperature of the liquefied gas and vaporization thereof, In addition, many current systems use the liquefied gas stored in the accumulation tank, vaporize it, and return it to the tank to build pressure in the accumulator. The system of the present invention does not utilize the liquefied gas from the accumulator tank to build pressure, but rather, uses liquefied gas from the bulk tank to both maintain the liquid level and the pressure in the accumulator. This allows for the entirety of the contents of the liquid phase in the accumulator tank to be used for the end-use application rather than for building pressure, thereby increasing the efficiency of the system.
[0014] Those skilled in the art will recognize that numerous modifications can be made to the specific implementations described above. Therefore, the following claims are not to be limited to the specific embodiments illustrated and described above. The claims, as originally presented and as they may be amended, encompass variations, alternatives, modifications, improvements, equivalents, and substantial equivalents of the embodiments and teachings disclosed herein, including those that are presently unforeseen or unappreciated, and that, for example, may arise from applicants/patentees and others.
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A system and method for accumulating pressurized liquefied gas or cryogenic fluids in which a source supply of liquefied gas or cryogenic fluid is fed to a pump which pressurizes the fluid and feeds it to a liquid accumulator. The pump also feeds a first vaporizer which vaporizes the fluid and feeds it into the headspace of the liquid accumulator thereby building pressure in the liquid accumulator. The pressurized liquid is then fed to a second vaporizer where the pressurized liquid is vaporized before use.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application claims benefit under 35 U.S.C. 119(e) to U.S. Provisional Application No. 61/419,191, filed Dec. 2, 2010, which is incorporated by reference herein in its entirety.
BACKGROUND
1. Field of Invention
The invention generally relates to lithography, and more particularly to support structures and arrangements for patterning devices.
2. Related Art
Lithography is widely recognized as a key process in manufacturing integrated circuits (ICs) as well as other devices and/or structures. A lithographic apparatus is a machine, used during lithography, which applies a desired pattern onto a substrate, such as onto a target portion of the substrate. During manufacture of ICs with a lithographic apparatus, a patterning device, which is alternatively referred to as a mask or a reticle, is typically used to generate a circuit pattern to be formed on an individual layer in an IC. This pattern is transferred onto the target portion (for example, comprising part of one, or several dies) of the substrate (for example, a silicon wafer). Typically, the pattern is transferred to a layer of radiation-sensitive material (for example, resist) provided on the substrate by imaging the pattern onto the radiation-sensitive material. A typical substrate may contain many such target portions that are adjacent to one another and are successively patterned.
Known lithographic apparatus include steppers, in which each target portion is irradiated by exposing an entire pattern onto the target portion at one time, and scanners, in which each target portion is irradiated by scanning the pattern through a radiation beam in a given direction (the “scanning” direction) while synchronously scanning the substrate parallel or anti-parallel to this direction. It is also possible to transfer the pattern from the patterning device to the substrate by imprinting the pattern onto the substrate.
To increase production rate of scanned patterns, a patterning device, for example, a mask or reticle, is scanned at constant velocity, for example, 3 meters/second across a projection lens, back and forth along a scan direction. Therefore, starting from rest, the reticle quickly accelerates to reach the scan velocity, then at the end of the scan, it quickly decelerates to zero, reverses direction, and accelerates in the opposite direction to reach the scan velocity. The acceleration/deceleration rate is, for example, 15 times the acceleration of gravity. There is no inertial force on the patterning device during the constant velocity portion of the scan. However, the large inertial force encountered during the acceleration and deceleration portions of the scan, for example, approximately 60 Newtons (=0.4 kg of patterning device mass×150 m/sec2 of acceleration), can cause the patterning device to slip. Such slippage can result in a misaligned device pattern on a substrate.
Attempts to solve patterning device slippage include using a clamp, such as a vacuum system, to hold the patterning device in place and/or using a friction coating to increase friction between the patterning device and the clamp. However, ever increasing production rates demand ever faster direction reversals and, therefore, higher accelerations have reduced the benefits of these solutions. With clamps, the normal force between the patterning device and the clamp generates a friction force during the acceleration and deceleration portions of the scan. The friction force holds the patterning device in place during these portions. However, with vacuum clamps, the friction force is limited by the maximum differential pressure between atmosphere and the vacuum, which now is only about 1 bar. Further, the small surface area of patterning devices in contact with the clamps limits the normal force that can be generated by the clamps. Currently, the highest friction coefficient of suitable friction coatings is only approximately 0.25.
SUMMARY
Given the foregoing, improved methods and systems are needed that provide an anti-slip solution for patterning devices that can function under high acceleration with minimal additional mass or controls.
An embodiment of the invention provides a patterning device transport system comprising a holding system having a support device, a holding device, and magnetostrictive actuator, and a support transport device configured to move and coupled to the support device. The holding device is configured to releasably couple a patterning device to the support device, and the magnetostrictive actuator is configured to provide a force to the patterning device. The support transport device moves the support device concurrently with the magnetostrictive actuator providing the force to the patterning device such that patterning device slip during the movement of the support device is substantially eliminated.
Another embodiment of the invention provides a patterning device stage system for a lithographic apparatus, comprising a stage configured to releasably couple a patterning device to the stage, a stage control system configured to control movement of the stage, and a magnetostrictive control system configured to apply a force to the patterning device.
A further embodiment of the present invention provides a method for reducing patterning device slip during movement of a patterning device stage, comprising supporting a patterning device with a support device; concurrently holding the patterning device to the support device with a holding device; moving the support device using a first moving device; and applying a force to the patterning device using a magnetostrictive actuator concurrently with moving the support device using the first moving device.
Features and advantages of the invention, as well as the structure and operation of various embodiments of the invention, are described in detail below with reference to the accompanying drawings. The invention is not limited to the specific embodiments described herein. Such embodiments are presented herein for illustrative purposes only. Additional embodiments will be apparent to persons skilled in the relevant art(s) based on the teachings contained herein.
BRIEF DESCRIPTION OF DRAWINGS/FIGURES
The accompanying drawings, which are incorporated herein and form part of the specification, illustrate the present invention and, together with the description, farther serve to explain the principles of the invention and to enable a person skilled in the relevant art(s) to make and use the invention.
FIG. 1A is a schematic illustration of a reflective lithographic apparatus according to an embodiment of the invention.
FIG. 1B is a schematic illustration of a transmissive lithographic apparatus according to an embodiment of the invention.
FIG. 2 is a schematic illustration of a patterning device transport system with anti-slip control, according to an embodiment of the invention.
FIG. 3 is a schematic illustration of a top view of a patterning device transport system without anti-slip control according to an embodiment of the invention.
FIG. 4 is a schematic illustration of a partial side view of a patterning device transport system with anti-slip control according to an embodiment of the invention.
FIG. 5 is a schematic illustration of a stage system with anti-slip control according to an embodiment of the invention.
FIG. 6 is a flowchart illustrating a method for patterning device transport with anti-slip control according to an embodiment of the invention.
FIG. 7 is a flow chart illustrating a method for loading a patterning device on a transport system with anti-slip control according to an embodiment of the invention.
FIGS. 8A-8D are schematic illustrations of a partial side view of a patterning device transport system with anti-slip control at various steps of a method for loading a patterning device on a transport system according to an embodiment of the invention.
FIG. 9 is a schematic illustration of a stage system with anti-slip control according to an embodiment of the invention.
FIG. 10 is a schematic illustration of a partial side view of a patterning device transport system with anti-slip control according to an embodiment of the invention.
Various features and advantages of the invention will become more apparent from the detailed description set forth below, read in conjunction with the drawings, in which like reference characters identify corresponding elements throughout. In the drawings, like reference numbers generally indicate identical, functionally similar, and/or structurally similar elements. Generally, the drawing in which an element first appears is indicated by the leftmost digit(s) in the corresponding reference number.
DETAILED DESCRIPTION
Embodiments of the invention are directed to a patterning device transport system with anti-slip control. This specification discloses one or more embodiments that incorporate the features of the present invention. The disclosed embodiment(s) merely exemplify the invention. The scope of the invention is not limited to the disclosed embodiment(s). The invention is defined by the claims appended hereto.
The embodiment(s) described, and references in the specification to “one embodiment,” “an embodiment,” “an example embodiment,” etc., indicate that the embodiment(s) described can include a particular feature, structure, or characteristic, but every embodiment can not necessarily include the particular feature, structure, or characteristic. Moreover, such phrases are not necessarily referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with an embodiment, it is understood that it is within the knowledge of one skilled in the art to affect such feature, structure, or characteristic in connection with other embodiments whether or not explicitly described.
Embodiments of the invention may be implemented in hardware, firmware, software, or any combination thereof. Embodiments of the present invention can also be implemented as instructions stored on a machine-readable medium, which can be read and executed by one or more processors. A machine-readable medium can include any mechanism for storing or transmitting information in a form readable by a machine (for example, a computing device). For example, a machine-readable medium can include the following: read-only memory (ROM); random access memory (RAM); magnetic disk storage media; optical storage media; and, flash memory devices. Further, firmware, software, routines, instructions can be described herein as performing certain actions. However, it should be appreciated that such descriptions are merely for convenience and that such actions in fact result from computing devices, processors, controllers, or other devices executing the firmware, software, routines, instructions, etc.
FIG. 1A is a schematic illustration of a reflective lithographic apparatus 100 in which embodiments of the present invention may be implemented. FIG. 1B is a schematic illustration of a transmissive lithographic apparatus 100 ′ in which embodiments of the present invention may be implemented. Lithographic apparatus 100 and lithographic apparatus 100 ′ each include the following: an illumination system (illuminator) IL configured to condition a radiation beam B (for example, DUV or EUV radiation); a support structure (for example, a mask table) MT configured to support a patterning device (for example, a mask, a reticle, or a dynamic patterning device) MA and connected to a first positioner PM configured to accurately position the patterning device MA; and, a substrate table (for example, a wafer table) WT configured to hold a substrate (for example, a resist coated wafer) W and connected to a second positioner PW configured to accurately position the substrate W. Lithographic apparatuses 100 and 100 ′ also have a projection system PS configured to project, through a lens system L, a pattern imparted to the radiation beam B by patterning device MA onto a target portion (for example, comprising one or more dies) C of the substrate W. In lithographic apparatus 100 , the patterning device MA and the projection system PS are reflective. In lithographic apparatus 100 ′, the patterning device MA and the projection system PS are transmissive.
The illumination system. IL may include various types of optical components, such as refractive, reflective, magnetic, electromagnetic, electrostatic, or other types of optical components, or any combination thereof, for directing, shaping, or controlling the radiation B.
The support structure MT holds the patterning device MA in a manner that depends on the orientation of the patterning device MA, the design of the lithographic apparatuses 100 and 100 ′, and other conditions, such as whether or not the patterning device MA is held in a vacuum environment. The support structure MT may use mechanical, vacuum, electrostatic, or other clamping techniques to hold the patterning device MA. The support structure MT can be a frame or a table, for example, which can be fixed or movable, as required. The support structure MT can ensure that the patterning device is at a desired position, for example, with respect to the projection system PS.
The term “patterning device” MA should be broadly interpreted as referring to any device that can be used to impart a radiation beam B with a pattern in its cross-section, such as to create a pattern in the target portion C of the substrate W. The pattern imparted to the radiation beam B can correspond to a particular functional layer in a device being created in the target portion C, such as an integrated circuit.
The patterning device MA may be transmissive (as in lithographic apparatus 100 ′ of FIG. 1B ) or reflective (as in lithographic apparatus 100 of FIG. 1A ). Examples of patterning devices MA include reticles, masks, programmable mirror arrays, and programmable LCD panels. Masks are well known in lithography, and include mask types such as binary, alternating phase shift, and attenuated phase shift, as well as various hybrid mask types. An example of a programmable mirror array employs a matrix arrangement of small mirrors, each of which can be individually tilted so as to reflect an incoming radiation beam in different directions. The tilted mirrors impart a pattern in the radiation beam B which is reflected by the mirror matrix.
The term “projection system” PS can encompass any type of projection system, including refractive, reflective, catadioptric, magnetic, electromagnetic and electrostatic optical systems, or any combination thereof, as appropriate for the exposure radiation being used, or for other factors, such as the use of an immersion liquid or the use of a vacuum. A vacuum environment can be used for EUV or electron beam radiation since other gases can absorb too much radiation or electrons. A vacuum environment can therefore be provided to the whole beam path with the aid of a vacuum wall and vacuum pumps.
Lithographic apparatus 100 and/or lithographic apparatus 100 ′ can be of a type having two (dual stage) or more substrate tables (and/or two or more mask tables) WT. In such “multiple stage” machines, the additional substrate tables WT can be used in parallel, or preparatory steps can be carried out on one or more tables while one or more other substrate tables WT are being used for exposure.
Referring to FIGS. 1A and 1B , the illuminator IL receives a radiation beam from a radiation source SO. The source SO and the lithographic apparatuses 100 , 100 ′ can be separate entities, for example, when the source SO is an excimer laser. In such cases, the source SO is not considered to form part of the lithographic apparatuses 100 or 100 ′, and the radiation beam B passes from the source SO to the illuminator IL with the aid of a beam delivery system BD (in FIG. 1B ) including, for example, suitable directing mirrors and/or a beam expander. In other cases, the source SO can be an integral part of the lithographic apparatuses 100 , 100 ′—for example when the source SO is a mercury lamp. The source SO and the illuminator IL, together with the beam delivery system BD, if required, can be referred to as a radiation system.
The illuminator IL can include an adjuster AD (in FIG. 1B ) for adjusting the angular intensity distribution of the radiation beam. Generally, at least the outer and/or inner radial extent (commonly referred to as “σ-outer” and “σ-inner,” respectively) of the intensity distribution in a pupil plane of the illuminator can be adjusted. In addition, the illuminator IL can comprise various other components (in FIG. 1B ), such as an integrator IN and a condenser CO. The illuminator IL can be used to condition the radiation beam B to have a desired uniformity and intensity distribution in its cross section.
Referring to FIG. 1A , the radiation beam B is incident on the patterning device (for example, mask) MA, which is held on the support structure (for example, mask table) MT, and is patterned by the patterning device MA. In lithographic apparatus 100 , the radiation beam B is reflected from the patterning device (for example, mask) MA. After being reflected from the patterning device (for example, mask) MA, the radiation beam B passes through the projection system PS, which focuses, using lens system L, the radiation beam B onto a target portion C of the substrate W. With the aid of the second positioner PW and position sensor IF 2 (for example, an interferometric device, linear encoder, or capacitive sensor), the substrate table WT can be moved accurately (for example, so as to position different target portions C in the path of the radiation beam B). Similarly, the first positioner PM and another position sensor IF 1 can be used to accurately position the patterning device (for example, mask) MA with respect to the path of the radiation beam B. Patterning device (for example, mask) MA and substrate W can be aligned using mask alignment marks M 1 , M 2 and substrate alignment marks P 1 , P 2 .
Referring to FIG. 1B , the radiation beam B is incident on the patterning device (for example, mask MA), which is held on the support structure (for example, mask table MT), and is patterned by the patterning device. Having traversed the mask MA, the radiation beam B passes through the projection system PS, which focuses the beam onto a target portion C of the substrate W. With the aid of the second positioner PW and position sensor IF (fix example, an interferometric device, linear encoder, or capacitive sensor), the substrate table WT can be moved accurately (for example, so as to position different target portions C in the path of the radiation beam B). Similarly, the first positioner PM and another position sensor (not shown in FIG. 1B ) can be used to accurately position the mask MA with respect to the path of the radiation beam B (for example, after mechanical retrieval from a mask library or during a scan).
In general, movement of the mask table MT can be realized with the aid of a long-stroke module (coarse positioning) and a short-stroke module (fine positioning), which form part of the first positioner PM. Similarly, movement of the substrate table WT can be realized using a long-stroke module and a short-stroke module, which form part of the second positioner PW. In the case of a stepper (as opposed to a scanner), the mask table MT can be connected to a short-stroke actuator only or can be fixed. Mask MA and substrate W can be aligned using mask alignment marks M 1 , M 2 , and substrate alignment marks P 1 , P 2 . Although the substrate alignment marks (as illustrated) occupy dedicated target portions, they can be located in spaces between target portions (known as scribe-lane alignment marks). Similarly, in situations in which more than one die is provided on the mask MA, the mask alignment marks can be located between the dies.
The lithographic apparatuses 100 and 100 ′ can be used in at least one of the following modes:
1. In step mode, the support structure (for example, mask table) MT and the substrate table WT are kept essentially stationary, while an entire pattern imparted to the radiation beam B is projected onto a target portion C at one time (i.e., a single static exposure). The substrate table WT is then shifted in the X and/or Y direction so that a different target portion C can be exposed.
2. In scan mode, the support structure (for example, mask table) MT and the substrate table WT are scanned synchronously while a pattern imparted to the radiation beam B is projected onto a target portion C (i.e., a single dynamic exposure). The velocity and direction of the substrate table WT relative to the support structure (for example, mask table) MT can be determined by the (de-)magnification and image reversal characteristics of the projection system PS.
3. In another mode, the support structure (for example, mask table) MT is kept substantially stationary holding a programmable patterning device, and the substrate table WT is moved or scanned while a pattern imparted to the radiation beam B is projected onto a target portion C. A pulsed radiation source SO can be employed and the programmable patterning device is updated as required after each movement of the substrate table WT or in between successive radiation pulses during a scan. This mode of operation can be readily applied to maskless lithography that utilizes a programmable patterning device, such as a programmable mirror array of a type as referred to herein.
Combinations and/or variations on the described modes of use or entirely different modes of use can also be employed.
Although specific reference can be made in this text to the use of lithographic apparatus in the manufacture of ICs, it should be understood that the lithographic apparatus described herein can have other applications, such as the manufacture of integrated optical systems, guidance and detection patterns for magnetic domain memories, flat-panel displays, liquid-crystal displays (LCDs), and thin-film magnetic heads. The skilled artisan will appreciate that, in the context of such alternative applications, any use of the terms “wafer” or “die” herein can be considered as synonymous with the more general terms “substrate” or “target portion,” respectively. The substrate referred to herein can be processed, before or after exposure, in for example a track (a tool that typically applies a layer of resist to a substrate and develops the exposed resist), a metrology tool, and/or an inspection tool. Where applicable, the disclosure herein can be applied to such and other substrate processing tools. Further, the substrate can be processed more than once, for example, in order to create a multi-layer IC, so that the term substrate used herein can also refer to a substrate that already contains multiple processed layers.
In a further embodiment, lithographic apparatus 100 includes an extreme ultraviolet (EUV) source, which is configured to generate a beam of EUV radiation for EUV lithography. In general, the EUV source is configured in a radiation system (see below), and a corresponding illumination system is configured to condition the EUV radiation beam of the EUV source.
In the embodiments described herein, the terms “lens” and “lens element,” where the context allows, can refer to any one or combination of various types of optical components, including refractive, reflective, magnetic, electromagnetic, and electrostatic optical components.
Further, the terms “radiation” and “beam” used herein encompass all types of electromagnetic radiation, including ultraviolet (UV) radiation (for example, having a wavelength λ of 365, 248, 193, 157 or 126 nm), extreme ultraviolet (EUV or soft X-ray) radiation (for example, having a wavelength in the range of 5-20 nm such as, for example, 13.5 nm), or hard X-ray working at less than 5 nm, as well as particle beams, such as ion beams or electron beams. Generally, radiation having wavelengths between about 780-3000 nm (or larger) is considered IR radiation. UV refers to radiation with wavelengths of approximately 100-400 nm. Within lithography, the term “UV” also applies to the wavelengths that can be produced by a mercury discharge lamp: G-line 436 nm; H-line 405 nm; and/or, Mine 365 nm. Vacuum UV, or VUV (i.e., UV absorbed by air), refers to radiation having a wavelength of approximately 100-200 nm. Deep UV (DUV) generally refers to radiation having wavelengths ranging from 126 nm to 428 nm, and in an embodiment, an excimer laser can generate DUV radiation used within a lithographic apparatus. It should be appreciated that radiation having a wavelength in the range of, for example, 5-20 nm relates to radiation with a certain wavelength band, of which at least part is in the range of 5-20 nm.
FIG. 2 is a schematic illustration of a patterning device transport system 200 , according to an embodiment of the invention. Patterning device transport system 200 includes a support transport device 230 and a holding system having a support device 250 , a holding device 280 , and a magnetostrictive actuator 260 . Transport device 230 moves support device 250 . Support device 250 supports a patterning device 270 . Magnetostrictive actuator 260 applies a force to patterning device 270 during an accelerating portion of a scanning motion profile. Holding device 280 holds patterning device 270 , such that during a constant velocity portion of a scanning motion profile there is no displacement of the patterning device 270 relative to support device 250 .
In one example, patterning device 270 (for example, a mask, a reticle, or a dynamic patterning device) is releasably held to support device 250 by holding device 280 (for example, a vacuum system). Support device 250 can be configured to move in both an x-direction and a y-direction. Transport device 230 can be coupled to support device 250 , such that transport device 230 provides sufficient force to accelerate support device 250 during an acceleration portion of a scanning motion profile.
In one example, transport device 230 may move support device 250 , and the releasably held patterning device 270 , at a high rate of speed and acceleration. High acceleration can generate a shearing force between patterning device 270 and support device 250 . The shearing force can cause slippage of patterning device 270 , relative to holding device 280 and support device 250 . To substantially eliminate the shearing force, a magnetostrictive actuator 260 may be releasably coupled to patterning device 270 . Magnetostrictive actuator 260 can provide a sufficient force directly on patterning device 270 to reduce the shearing force between patterning device 270 and support device 250 . Given the coupling of magnetostrictive actuator 260 to patterning device 270 , holding device 280 can provide a sufficient holding force, such that there is substantially no relative movement between patterning device 270 and support device 250 .
In one example, the holding device 280 includes a releasable vacuum clamp system to hold patterning device 270 in a relatively stationary manner during movement. In another example, holding device 280 can use other suitable methods to hold patterning device 270 , such as a high friction coating, as known to one of ordinary skill in the art. A high friction coating can also be used to increase the shear force capacity of a vacuum clamp.
FIG. 3 is a schematic illustration of a patterning device transport system 300 without anti-slip control according to an embodiment of the invention.
In this example, patterning device transport system 300 includes a long stroke device 310 , a support frame 320 , a support transport device 330 (for example, coils 330 A- 330 D and magnets 340 A- 340 D), a support device 350 , and a holding device 380 that releasably couples a patterning device 370 to the support device 350 .
In an example, support device 350 can be magnetically levitated relative to support frame 320 by vertically oriented Lorentz type actuators (not shown). There can be no physical contact between support frame 320 and support device 350 .
In one example, a patterning device 370 (for example, a mask, a reticle, or a dynamic patterning device) may be releasably held to support device 350 by holding device 380 . In one example, holding device 380 may comprise a pair of vacuum clamps 380 A and 380 B that hold patterning device 370 to support device 350 through friction enhanced by a vacuum force. In one example, support device 350 can move in both the x-direction and y-direction. In one example, coils 330 A- 330 D can provide a force in the y-direction to produce a motion of support device 350 . Magnets 340 A- 340 D electromagnetically couple coils 330 A- 330 D without physical contact. Pairs of respective items 330 - 340 comprise Lorentz type electromagnetic actuators as known in the art as pure force couplings.
In one example, long stroke device 310 moves support frame 320 in the x direction (via X-oriented Lorentz actuators not shown) at a relatively slow speed that does not generate any shearing forces between patterning device 370 and support device 350 .
In one example, transport device 330 moves support device 350 and releasably held patterning device 370 in the +y and −y directions accelerating at a relatively high rate to a substantial scanning speed. In one example, transport device 330 allows for high Y-forces to be exerted by support frame 320 to support device 350 . In one example, transport device 330 includes coils 330 A- 330 D and magnets 340 A- 330 D. In one example, the coils 330 A- 330 D are mounted to support frame 320 and magnets 340 A- 340 D are coupled to support device 350 .
For example, to move support device 350 with the releasably coupled patterning device 370 , in a −y direction (for example, left to right in FIG. 3 ), coils 330 A and 330 C are energized to produce a repelling force against magnets 340 A and 340 C. When coils 330 A and 330 C are energized, the repelling force against magnets 340 A and 340 C propels support device 350 in the −y direction. To assist movement of support device 350 in the −y direction, coils 330 B and 330 D are energized, such that they substantially simultaneously produce a pulling force to magnets 340 B and 340 D. Therefore, coils 330 A and 330 C and magnets 340 A and 340 C push support device 350 in the −y direction, while coils 330 B and 330 D and magnets 340 B and 340 D substantially simultaneously pull support device 350 in the −y direction.
Similarly, movement of the support device 350 and patterning device 370 in the +y direction is performed in the same manner, except the forces are reversed. Device coils 330 A and 330 C and magnets 340 A and 340 C, when energized, pull support device 350 in the +y direction, while coils 330 B and 330 D and magnets 340 B and 340 D substantially simultaneously push support device 350 in the +y direction.
It is to be appreciated that the embodiment shown in FIG. 3 relies on the friction created by holding device 380 (for example, vacuum clamps and/or friction coating) between patterning device 370 and support device 350 to prevent slippage of patterning device 370 during movement.
FIG. 4 is a schematic illustration of a patterning device transport system 400 with anti-slip control according to an embodiment of the invention.
In this example, patterning device transport system 400 includes a support frame 420 coupled to a long-stroke device (not shown), a support device 450 coupled to a support transport device (not shown), a holding device 480 that releasably couples a patterning device 470 to support device 450 , and a magnetostrictive actuator 460 .
In one example, patterning device transport system 400 works in a similar manner to patterning device transport system 300 , but with the addition of magnetostrictive actuator 460 . Movement in the x direction is accomplished as in FIG. 3 through the use of a long stroke device (not shown), which moves support frame 420 on which support device 450 is coupled. Movement in the y direction is accomplished as in FIG. 3 through the use of a coupled support transport device (not shown). In one example, to move in the −y direction, the support transport device, for example, electromagnetically coupled coils and magnets, are energized to move support device 450 in the −y direction, while movement of the support device 450 and patterning device 470 in the +y direction is done in the same manner, except that the forces are reversed.
In another example, magnetostrictive actuator 460 is used in patterning device transport system 400 to supplement the frictional force created by holding device 480 (for example, vacuum clamps or friction coating) with a normal push force applied directly to patterning device 470 at the edge opposite to the direction of acceleration to substantially reduce or eliminate patterning device slip. In one example, magnetostrictive actuator 460 can include a magnetic field source 462 , a push rod 463 , a biasing device 464 , and a clamping device 465 . Magnetostrictive actuator 460 can farther include additional magnetic field sources, push rods, biasing devices, and clamping devices on either the same side or the opposite side of patterning device 470 , which operate in substantially the same manner.
In one example, push rod 463 comprises a magnetostrictive material that changes its shape or dimensions under a magnetic field. The push rod 463 can be electromagnetically coupled with magnetic field source 462 . When magnetic field source 462 creates a magnetic field, push rod 463 changes dimensions and releasably couples with patterning device 470 .
In one example, magnetic field source 462 is a coil, and push rod 463 passes through the coil. When the coil is energized, the resulting magnetic field increases the length of push rod 462 such that a distal end 466 of the push rod 463 contacts the patterning device 470 . The contact between distal end 466 of push rod 463 and patterning device 470 produces a force directly on patterning device 470 . The magnetostrictive material can be any suitable material that change dimensions under a magnetic field. The push rod's magnetostrictive material and dimensions, as well as the coil's turns per unit length of the push rod and current, can be modified or adjusted to achieve the desired change in length of the push rod 463 . Further, because the change in length of the push rod 463 caused by the magnetic field is substantially linear and repeatable, additional position and force sensors to control the push rod 463 in closed-loop operation are not necessary. Instead, the repeatable response of push rod 463 may be used during open-loop operation. Such sensors, however, may be used to calibrate the patterning device transport system 400 before manufacturing any ICs or other devices and/or structures.
In one example, the magnetostrictive material is Terfenol-D, and the push rod 463 is approximately 0.75 cm in diameter, and approximately 5 cm in length. In this example, the coil has approximately 500 turns over the length of the rod 463 and is driven by approximately a 1 A current. This example is provided merely to exemplify the invention, and the invention is not limited to these specific examples of rod material, rod dimensions, coil turns, and coil current.
In another example, the magnetostrictive actuator includes a biasing device 464 biases the push rod 463 towards the patterning device 470 . Although the biasing device 464 is illustrated as a spring in FIG. 4 , the biasing device 464 is not limited to springs. The biasing device 464 can be a spring, a pneumatic actuator, a hi-stable actuator, or any other suitable device for applying a biasing force to the push rod 463 . The biasing device 464 can apply a preload to set the initial gap 467 between the distal end 466 of the push rod 463 and the patterning device 470 as discussed below with reference to FIGS. 7 and 8 A- 8 D. The biasing device 464 can also allow the push rod 463 to retract away from the patterning device 470 during patterning device exchanges. In another example, biasing device 464 can be configured also to retract push rod 463 away from patterning device 470 .
In one example, the magnetostrictive actuator 460 can also include a clamping device 465 . Clamping device 465 is configured to releasably couple a proximal portion 468 of push rod 463 to support device 450 . When coupled, clamping device 465 prevents the proximal portion 468 from moving relative to the patterning device 470 . Clamping device 465 can, for example, include a vacuum system or any other suitable device for releasably coupling a portion of the push rod 463 .
In one example, a common control signal controls the transport device coupled to the support device 450 and the magnetostrictive actuator 460 . For example, the current used to drive the transport device, for example, electromagnetically coupled coils and magnets, can be used to control the magnetic field source 462 . Thus, the transport device moves the support device 450 substantially simultaneously with energizing the coil of the magnetic field source 462 to create a magnetic field. Also substantially simultaneously, the magnetic field causes the length of the push rod 463 to increase and contact patterning device 470 . This operation produces a force on both the patterning device 470 to supplement the friction force created by holding device 480 . In another example, the current that drives the long-stroke device coupled to support frame 420 can be used to control the magnetic field source 462 . Accordingly, the coil of magnetic field source 462 is energized and the length of push rod 463 is increased simultaneously with moving support frame 420 with the long-stoke device. These configurations eliminate the need for additional control signal processing devices, for example, signal amplifiers, for the signal that controls magnetostrictive actuator 460 .
In another example, however, the signal that controls the magnetostrictive actuator 460 is separate from the signal that controls the transport device or long-stroke device. In this example, additional control signal processing devices, for example, a signal amplifier, may be necessary for the magnetostrictive actuator 460 .
FIG. 5 is a schematic illustration of a stage system 500 for a lithographic apparatus according to an embodiment of the invention. Stage system 500 includes stage control system 530 , a stage 550 which is movable, and a magnetostrictive actuator 560 .
In one example, a patterning device 570 is releasably held to stage 550 (for example, using a vacuum). Stage control system 530 is coupled to stage 550 . Stage control system 530 can provide sufficient force to allow movement of stage 550 . Stage control system 530 can move stage 550 , and the releasably held patterning device 570 , at a high rate of speed with a corresponding high rate of acceleration. Such acceleration can generate a shearing force between patterning device 570 and stage 550 , such that patterning device 570 can slip relative to stage 550 . To substantially eliminate the shearing force, a magnetostrictive actuator 560 is releasably coupled to patterning device 570 . Magnetostrictive actuator 560 can provide a force directly to patterning device 570 to reduce the shearing force between patterning device 570 and stage 550 . The force between patterning device 570 and stage 550 is such that, given the coupling of magnetostrictive actuator 560 to patterning device 570 , there is sufficient holding force such that there is substantially no relative movement between patterning device 570 and stage 550 .
In another embodiment stage 550 can use other methods to hold patterning device 570 , such as a friction coating or other methods as known to one of ordinary skill in the art.
FIG. 6 is an illustration of a flowchart depicting a method 600 for moving a patterning device according to an embodiment of the present invention. For example, method 600 may be performed using one or more of the above devices depicted in FIGS. 1A , 1 B, and 2 - 5 . In this example, method 600 starts at step 602 , and proceeds to step 604 . In step 604 , a patterning device is supported with a support device. In step 606 , the patterning device is concurrently supported using a holding device, for example, a vacuum system. In step 608 , the support device is moved using a first moving device. In step 610 , a force is applied to the patterning device using a magnetostrictive actuator concurrently with moving the support device. The method then ends at step 612 .
FIG. 7 is an illustration of a flowchart depicting a method 700 for loading a patterning device on a patterning device transport system according to an embodiment of the present invention. The change in length of a magnetostrictive push rod under a magnetic field can be limited to tens of micrometers. Thus, the distal end of the push rod must be located in close proximity to the patterning device when not exposed to a magnetic field and in its non-extended state. Additionally, the push rod cannot be in constant contact with the patterning device during the scan interval because thermal expansion of the push rod can disturb the positioning of the patterning device. Thus, it is desirable to load a patterning device on a patterning device transport system according to method 700 to automatically create an initial gap between the distal end of the push rod and the patterning device.
In this example, method 700 starts at step 702 , and proceeds to step 704 . In step 704 , a patterning device is supported with a support device. In step 706 , a biasing device moves a magnetostrictive push rod against the patterning device on the support device. In step 708 , a magnetic field is created using a magnetic field source. In one example, the magnetic field is proportional to the desired no-field clearance or gap between the push rod and the patterning device. The magnetostrictive push rod, which is electromagnetically coupled with the magnetic field source, increases in length. Steps 706 and 708 are interchangeable and may be performed concurrently. In step 710 , a proximal portion of the magnetostrictive push rod is releasably coupled to the support device using a clamping device, for example a vacuum system. In step 712 , the magnetic field is removed, and the magnetostrictive push rod returns to its original length, creating a gap between the distal end of the push rod and the patterning device. The process ends at 714 .
FIGS. 8A-8D are schematic illustrations of a patterning device transport system 800 with anti-slip control at different steps of method 700 for loading a patterning device 870 on a patterning device transport system 800 including a support frame 820 . In each of these figures, a magnetorestrictive actuator 860 is biased by a biasing device 864 , pictured as a spring.
In FIG. 8A , while the coil of magnetic field source 862 is de-energized and not forcing magnetostrictive actuator 860 , the patterning device 870 is placed on support device 850 (step 704 ). Biasing device 866 moves magnetostrictive push rod 863 towards patterning device 870 such that the distal end 866 of push rod 863 contacts patterning device 870 (step 706 ). This contact creates a preload force against patterning device 870 . In FIG. 8B , the coil of magnetic field source 862 is energized to create a magnetic field (step 708 ). The length L of magnetostrictive push rod 863 , which is electromagnetically coupled to magnetic field source 862 , is increased.
In FIG. 8C , a proximal portion 868 is releasably coupled to the support device 850 using a clamping device 865 , for example, a vacuum system (step 710 ). When clamped, the proximal portion 868 is fixed relative to the patterning device 870 . In FIG. 8D , the coil of magnetic field source 862 is de-energized to remove the magnetic field. When the magnetic field is removed, the length L of magnetostrictive push rod 863 returns to its original length, as in step 704 . The decrease in length L creates a gap 867 between the distal end 866 of the push rod 863 and the patterning device 870 . In one example, gap 867 is approximately 2 micrometers.
In one example, method 800 is performed before for moving a patterning device 870 according to method 700 .
FIG. 9 is a schematic illustration of a stage system 900 with anti-slip control according to an embodiment of the invention. In this embodiment, the system includes a piezoelectric actuator 960 , instead of a magnetostrictive actuator as shown in prior embodiments. The system 900 can be configured in a similar fashion to the systems discussed above, and can be operated to reduce slippage of patterning device 970 during movement of a movable stage 950 controlled by a stage control system 930 in a similar manner as described above. For example, a voltage excitation can be used to create or manipulate an electric field, which changes the dimensions of a piezoelectric element of piezoelectric actuator 960 .
FIG. 10 is a schematic illustration of a partial side view of a patterning device transport system 1000 with anti-slip control according to an embodiment of the invention.
In this example, patterning device transport system 1000 includes a support frame 1020 coupled to a long-stroke device (not shown), a support device 1050 coupled to a support transport device (not shown), a holding device 1080 that releasably couples a patterning device 1070 to support device 1050 , and a piezoelectric actuator 1060 .
In one example, patterning device transport system 1000 works in a similar manner to the patterning device transport systems 400 , but with a piezoelectric actuator 1060 instead of a magnetostrictive actuator. Movement in the x direction is accomplished as in FIG. 4 through the use of a long stroke device (not shown), which moves support frame 1020 on which support device 1050 is coupled. Movement in the y direction is accomplished as in FIG. 4 through the use of a coupled support transport device (not shown). In one example, to move in the −y direction, the support transport device, for example, electromagnetically coupled coils and magnets, are energized to move support device 1050 in the −y direction, while movement of the support device 1050 and patterning device 1070 in the +y direction is done in the same manner, except that the forces are reversed.
In another example, piezoelectric actuator 1060 is used in patterning device transport system 1000 to supplement the frictional force created by holding device 1080 (for example, vacuum clamps or friction coating) with a normal push force applied directly to patterning device 1070 at the edge opposite to the direction of acceleration to substantially reduce or eliminate patterning device slippage.
In one example, piezoelectric actuator 1060 can include a piezoelectric element 1063 , a biasing device 1064 , and a clamping device 1065 configured to releasably couple a proximal portion 1068 of piezoelectric element 1063 to support device 1050 . Piezoelectric actuator 1060 can further include additional piezoelectric elements, biasing devices, and clamping devices on either the same side or the opposite side of patterning device 1070 , which operate in substantially the same manner.
In one example, piezoelectric element 1063 changes its dimensions under an electric field. The piezoelectric element 1063 can be electrically coupled to a voltage source via power terminals 1069 . When a voltage or charge is applied to piezoelectric element 1063 , the internal electric field of the piezoelectric element 1063 changes, which causes the piezoelectric element 1063 to change dimensions and releasably couple with patterning device 1070 . In one example, the resulting electric field increases the length of piezoelectric element 1062 such that a distal end of the piezoelectric element 1062 contacts the patterning device 1070 . The contact between the distal end of piezoelectric element 1062 and patterning device 1070 produces a force directly on patterning device 1070 . Piezoelectric actuator 1060 may be any suitable device that changes dimensions under an electric field, for example, piezoelectric stacks and tubes.
In another example, method 600 for moving a patterning device, as described above, may be performed using patterning device transport system 1000 . In this example, at step 610 , a force is applied to the patterning device using the piezoelectric actuator 1060 concurrently with moving the support device.
Further, method 700 for loading a patterning device, as described above, may be performed using patterning device transport system 1000 . In this example, at step 706 , a biasing device moves a piezoelectric element against the patterning device on the support device. In step 708 , an electric field is created by applying a voltage or charge to the piezoelectric element, which increases the length of the piezoelectric element. In step 710 , a proximal portion of the piezoelectric element is releasably coupled to the support device using a clamping device. In step 712 , the electric field is removed, and the piezoelectric element returns to its original length, creating a gap 1067 between the distal end of the piezoelectric element and the patterning device.
CONCLUSION
It is intended that the Detailed Description portion of this patent document, and not the Summary and Abstract sections, be used to interpret the claims. The Summary and Abstract portions may set forth one or more but not all exemplary embodiments of the present invention as contemplated by the inventor(s), and thus, are not intended to limit the present invention and the appended claims in any way.
The invention has been described above with the aid of functional building blocks illustrating the implementation of specified functions and relationships thereof. The boundaries of these functional building blocks have been arbitrarily defined herein for the convenience of the description. Alternate boundaries can be defined so long as the specified functions and relationships thereof are appropriately performed.
The foregoing description of the specific embodiments will so fully reveal the general nature of the invention that others can, by applying knowledge within the skill of the art, readily modify and/or adapt for various applications such specific embodiments, without undue experimentation, without departing from the general concept of the present invention. Therefore, such adaptations and modifications are intended to be within the meaning and range of equivalents of the disclosed embodiments, based on the teaching and guidance presented herein. It is to be understood that the phraseology or terminology herein is for the purpose of description and not of limitation, such that the terminology or phraseology of the present specification is to be interpreted by the skilled artisan in light of the teachings and guidance.
The breadth and scope of the present invention should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents.
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In a lithographic apparatus, slippage of a patterning device is substantially eliminated during movement of a patterning device stage by providing a magnetostrictive actuator to apply an accelerating force to the patterning device to compensate for forces that would otherwise tend to cause slippage when the patterning device stage moves.
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BACKGROUND OF THE INVENTION
Several previous studies have shown that γ-aminobutyric acid is a major inhibitory transmitter of the central nervous system as reported, for example, by Y. Godin et al., Journal Neurochemistry, 16, 869 (1969) and that disturbance of the excitation and inhibition interplay can lead to diseased states such as Huntington's chorea (The Lancet, Nov. 9, 1974, pp. 1122-1123) Parkinsonism, schizophrenia, epilepsy, depression, hyperkinesis and manic depression disorders, Biochem. Pharmacol. 23, 2637-2649 (1974). Certain compounds are known to elevate brain levels of γ-aminobutyric acid, for example, n-dipropylacetate [Simler et al., Biochem. Pharm., 22, 1701 (1973)] by competitively inhibiting γ-aminobutyric acid transaminase resulting in a reversible effect which lasts for only about 2 hours. Also, 4-aminotetrolic acid [P. M. Beart et al., J. Neurochem. 19, 1849 (1972)] is known to be a competitive reversible inhibitor of γ-aminobutyric acid transaminase. We have now made the unexpected finding that compounds of our invention are able to irreversibly inhibit γ-aminobutyric acid transaminase and increase significantly the brain level of γ-aminobutyric acid in animals, rendering them useful in the treatment of the aforementioned diseased states. Furthermore, this increase is long lasting (over 24 hours) and, therefore, compounds of the present invention are not only structurally novel but are quite different in their properties from known compounds which elevate brain levels of γ-aminobutyric acid only for a short period of time.
SUMMARY OF THE INVENTION
The compounds of the present invention may be represented by the following general Formula I: ##EQU6## R is selected from hydrogen, alkylcarbonyl wherein the alkyl moiety contains from 1 to 4 carbon atoms, alkoxycarbonyl wherein the alkoxy moiety contains from 1 to 4 carbon atoms and may be straight or branched, and ##EQU7## wherein R 10 is selected from hydrogen, a straight or branched lower alkyl group of from 1 to 4 carbon atoms, benzyl and p-hydroxybenzyl; R 2 is selected from hydroxy, a straight or branched alkoxy group of from 1 to 8 carbon atoms, a lower alkylamino group wherein the alkyl moiety contains from 1 to 4 carbon atoms and ##EQU8## wherein R 4 is selected from hydrogen, a straight or branched lower alkyl group of from 1 to 4 carbon atoms, benzyl, and p-hydroxybenzyl; [A] is selected from ##EQU9## and --CH=CH-- wherein R 1 is selected from hydrogen, lower alkyl of from 1 to 4 carbon atoms, phenyl and substituted phenyl wherein the substituents on the substituted phenyl may be attached at the ortho, meta and para positions of the phenyl ring and are selected from halogen, lower alkoxy of from 1 to 4 carbon atoms, and lower alkyl of from 1 to 4 carbon atoms; n is an integer of from 1 to 5; and the lactams of said compounds wherein [A] represents ##EQU10## R and R 1 represent hydrogen and n is the integer 2 or 3; and pharmaceutically acceptable salts and individual optical isomers thereof.
The compounds of general Formula I are useful as sedatives. The compounds of general Formula I wherein [A] represents --CH=CH-- and ##EQU11## wherein R 1 is hydrogen, and n is an integer of from 1 to 5, that is, compounds of the following general Formula II and the lactams of the compounds of Formula II wherein [A'] represents (--CH 2 --) n and n is the integer 2 or 3, as represented by Formula III, are useful as inhibitors of γ-aminobutyric acid transaminase resulting in an increase in brain levels of γ-aminobutyric acid rendering the compounds useful in the treatment of disorders of the central nervous system function consisting of involuntary movement associated with Huntington's chorea, Parkinsonism, extrapyramidal effects of drugs, for example, neuroleptics, seizure disorders associated with epilepsy, alcohol withdrawal, barbiturate withdrawal, psychoses associated with schizophrenia, depression, manic depression, and hyperkinesis. Compounds of this invention are also useful as hypothermic agents, myorelaxants, cholinergic agents, antibacterial agents, anticonvulsant agents, analgesics, anorexigenic agents, antiobesity agents, tranquilizers, sedatives and central nervous system stimulants. ##EQU12## In the above Formula II the substituent groups R and R 2 have the meanings defined in general Formula I, and [A'] is selected from --CH=CH-- and (--CH 2 --) n wherein n is an integer of from 1 to 5; and pharmaceutically acceptable salts and individual optical isomers; ##EQU13## In the above Formula III n' is the integer 2 or 3; and pharmaceutically acceptable salts and individual optical isomers thereof.
DETAILED DESCRIPTION OF THE INVENTION
As used herein, the term lower alkylcarbonyl means the substituent group ##EQU14##
As used herein the term alkoxycarbonyl means the substituent group ##EQU15## wherein the lower alkyl moiety may be straight or branched.
Illustrative examples of straight chain lower alkyl groups of from 1 to 4 carbon atoms referred to herein are methyl, ethyl, n-propyl and n-butyl, and of branched chain lower alkyl groups of from 1 to 4 carbon atoms are isopropyl, isobutyl, and tert-butyl.
Illustrative examples of straight chain lower alkoxy groups of from 1 to 4 carbon atoms as used herein are methoxy, ethoxy, n-propoxy and n-butoxy, and of branched chain lower alkoxy groups of from 1 to 4 carbon atoms are isopropoxy, isobutoxy, and tert-butoxy.
Illustrative examples of straight or branched alkoxy groups of from 1 to 8 carbon stoms as used herein are methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, tert-butoxy, neopentoxy, pentoxy, octyloxy, heptyloxy and hexyloxy.
Illustrative examples of lower alkylamino groups which R 2 may represent are methylamino, ethylamino, n-propylamino and n-butylamino.
Illustrative examples of pharmaceutically acceptable salts of the compounds of this invention include non-toxic acid addition salts formed with inorganic acids, such as, hydrochloric, hydrobromic, sulfuric and phosphoric acid, and organic acids such as methane sulfonic, salicylic, maleic, malonic, tartaric, citric and ascorbic acids; and non-toxic salts formed with inorganic or organic bases such as those of alkali metals, for example, sodium, potassium and lithium, alkaline earth metals, for example, calcium and magnesium, light metals of Group III A, for example, aluminum; organic amines such as primary, secondary or tertiary amines, for example, cyclohexylamine, ethylamine, pyridine, methylaminoethanol, ethanolamine, and piperazine. The salts can be prepared by conventional means.
The compounds of this invention wherein [A] represents the group ##EQU16## can be represented by the following Formula IV: ##EQU17## wherein the substituents R, R 1 , R 2 and n have the meanings defined in general Formula I.
The compounds of this invention wherein [A] represents --CH=CH-- can be represented by the following Formula V: ##EQU18## wherein the substituents R and R 2 have the meanings defined in general Formula I.
The lactams which are included within the scope of this invention are represented by the compounds of general Formula III, described hereinabove.
Illustrative examples of compounds of this invention are the following:
3-amino-4-yne-pentanoic acid,
4-amino-5-yne-hexanoic acid,
7-amino-8-yne-nonanoic acid,
6-amino-3-ethyl-7-yne-octanoic acid,
4-amino-2-(p-anisyl)-5-yne-hexanoic acid,
5-amino-3-(p-anisyl)-6-yne-heptanoic acid,
N-methyl-(2-amino-3-yne-butan-1-yl)carboxamide,
4-amino-3-phenyl-5-yne-hexanoic acid,
4-amino-5-yne-1-oxo-hexan-1-ylaminoacetic acid,
5-methoxycarbonylamino-6-yne-heptanoic acid,
3-amino-4-yne-pentanoic acid methyl ester,
4-amino-2-ene-5-yne-hexanoic acid,
4-acetylamino-5-yne-hexanoic acid
Preferred compounds of this invention are those of general Formula II. More preferred compounds of this invention are those of general Formula II wherein the substituent group R 2 is hydroxy or alkoxy of from 1 to 8 carbon atoms. Still more preferred compounds of this invention are those of general Formula II wherein the substituent group R 2 is hydroxy, and n is the integer 1 or 2. An even more preferred group of compounds of this invention are those of general Formula II wherein the substituent group R 2 is hydroxy, n is an integer of 1 or 2 and R is hydrogen. Of the preferred compounds of this invention, the (+) isomers are the most preferred compounds.
The compounds of this invention have a variety of pharmacological utilities. The compounds of this invention are useful as sedatives. The compounds of general Formula II are useful as inhibitors of γ-aminobutyric acid transaminase resulting in an increase in brain levels of γ-aminobutyric acid rendering the compounds useful in the treatment of disorders of the central nervous system function consisting of involuntary movement associated with Huntington's chorea, Parkinsonism, extrapyramidal effects of drugs, for example, neuroleptics, seizure disorders associated with epilepsy, alcohol withdrawal, and barbiturate withdrawal, psychoses associated with schizophrenia, depression and manic depression and hyperkinesis. Compounds of this invention are also useful as hypothermic agents, myorelaxants, cholinergic agents, antibacterial agents, anticonvulsant agents, analgesics, anorexigenic agents, antiobesity agents, tranquilizers, sedatives, and central nervous system stimulants.
The sedative properties of the compounds of this invention were determined by measuring spontaneous motor activity in rodents by the procedure described by P. Dews, Brit. J. Pharmacol. 8, 46 (1953). For example, administration of between 100-200 mg/kg (milligrams per kilogram) of the compound 4-amino-5-yne-hexanoic acid by either the intravenous, intraperitoneal or oral route to mice or rats produces a substantially decreased motor activity which appears 1 hour after administration of the compound and is still observable 48 hours after administration.
The ability of the compounds of general Formulas II and III to inhibit γ-aminobutyric acid transaminase is determined by in vitro and in vivo measure of γ-aminobutyric acid transaminase activity. γ-Aminobutyric acid levels are markedly increased in mice and rat brains after treatment with compounds of general Formula II at doses between 25-200 mg/kg by parenteral and oral routes. This ability is further shown by the protective effect of this treatment on audiogenic seizures in mice of the DBA strain measured by the general method described by Simler et al., Biochem. Pharmacol. 22, 1701 (1973), which is currently used to evidence antiepileptic activity. For example, administration of between 50-200 mg/kg of 4-amino-5-yne-hexanoic acid to mice of the DBA strain which are susceptible to audiogenic seizures resulted in complete protection one hour after treatment, such protection lasting for over 16 hours.
The ability of the compounds of this invention at doses ranging from 50 to 200 mg/kg, to alleviate reserpine ptosis has been shown by the classical test of B. Rubin et al., J. Pharmacol. 120, 125 (1957), which is currently used to determine anti-depressant activity. For instance, in intraperitoneal injection 50 mg/kg of 4-amino-5-yne-hexanoic acid in mice, one hour after an intravenous injection of 2 mg/kg reserpine dissolved in 2% ascorbic acid/water results in a palpebral aperture of 5.5, 3 hours after drug administration as compared to 6.5 for control reserpinized animals.
The ability of the compounds to this invention to promote loss of body weight in rats has been demonstrated by weighing animals which were given daily doses ranging from 10-50 mg/kg of these compounds. For instance, rats weighing 190 g, when given for four days, oral doses of 25 mg/kg 4-amino-5-yne-hexanoic acid (which is not a sedative dose) weigh only 170 gms as compared to 250 g for animals of the same group which were given saline for the same period.
The compounds of this invention can be administered orally or parenterally to animals, particularly warm blooded animals and mammals and humans either alone or in the form of pharmaceutical preparations containing as the active ingredient compounds of this invention to achieve the desired effect. Pharmaceutical preparations containing compounds of this invention and conventional pharmaceutical carriers can be employed in unit dosage forms such as solids, for example, tablets, pills and capsules or liquid solutions, suspensions or elixirs for oral administration or liquid solutions, suspensions and emulsions for parenteral use. The quantity of compounds administered can vary over a wide range to provide from about 0.1 mg/kg to about 300 mg/kg of body weight of the patient per day. Unit doses of these compounds can contain, for example, from about 50 mg to 2000 mg of the compounds and may be administered, for example, from 1 to 4 times daily. Following are illustrative examples of pharmaceutical preparations containing the compounds of this invention:
Per Tablet(a) 3-amino-4-yne-pentanoic acid 100.0 mg(b) wheat starch 15.0 mg(c) lactose 33.5 mg(d) magnesium stearate 1.5 mg
A portion of the wheat starch is used to make a granulated starch paste which together with the remainder of the wheat starch and the lactose is granulated, screened and mixed with the active ingredient (a) and the magnesium stearate. The mixture is compressed into tablets weighing 150 mg each.
An illustrative composition for a parenteral injection is the following, wherein the quantities are on a weight to volume basis:
Amount(a) (+)4-amino-5-yne-hexanoic acid 100.0 mg(b) sodium chloride q.s.(c) water for injection to make 20 ml
The composition is prepared by dissolving the active ingredient (a) and sufficient sodium chloride in water for injection to render the solution isotonic. The composition may be dispensed in a single ampule containing 100 mg of the active ingredient for multiple dosage or in 20 ampules for single dosage.
An illustrative composition for hard gelatin capsules is as follows:
Amount(a) 3-amino-4-yne-pentanoic acid 200.0 mg(b) talc 35.0 mg
The composition is prepared by passing the dry powders of (a) and (b) through a fine mesh screen and mixing them well. The powder is then filled into No. 0 hard gelatin capsules at a net fill of 235 mg per capsule.
The compounds of general Formula I wherein R is hydrogen, and R 2 is other than ##EQU19## are prepared by reacting a suitably protected propargylamine derivative, as represented by compound 1 below, with an alkylating reagent in the presence of a base and subsequently unmasking the protected groups by treatment with acid or base as represented by the following reaction: ##EQU20##
In the above reaction sequence, [A] has the meaning defined in general Formula I; R 8 is selected from hydroxy, a straight or branched lower alkoxy of from 1 to 8 carbon atoms and a lower alkylamino group wherein the alkyl moiety contains from 1 to 4 carbon atoms; R 5 is selected from a lower alkyl group having from 1 to 4 carbon atoms, such as methyl, ethyl and n-propyl; R 6 is selected from hydrogen and phenyl; and R 7 is selected from phenyl, tert-butyl and triethylmethyl.
In the above reaction, the protected propargylamine derivative compound 1, is treated with a strong base to form the carbanion intermediate. Suitable strong bases are those which will abstract a proton from the carbon adjacent to the acetylene moiety, such as, alkyl lithium, for example, butyl lithium, or phenyl lithium, lithium di-alkylamide, for example, lithium diisopropylamide, lithium amide, tertiary potassium butylate sodium amide and sodium hydroxide.
Following addition of the base, the alkylating reagent is added. The alkylating reagents employed in the above reaction are selected from derivatives having the structures:
(A) when [A] is ##EQU21## and n is equal to 2, ##EQU22##
(B) when [A] is ##EQU23## and n is equal to 1 or 3 to 5, ##EQU24## or ##EQU25## and
(C) when [A] is --CH=CH--,
haloCH=CHCOR.sub.9,
or
HC.tbd.C--COR.sub.9
wherein R 1 has the meaning defined in general Formula I; Z is selected from cyano or ##EQU26## R 9 is selected from a straight or branched alkoxy group of from 1 to 8 carbon atoms; m is the integer 1 or 3 to 5; and halo is iodine or bromine.
When the alkylating reagent employed is the di-haloalkyl derivative as set forth in (B), subsequent to the alkylation reaction the ω-halogen is displaced with cyanide, and as when Z is cyano the reaction mixture is treated with an acid or base to hydrolyze the nitrile to the corresponding acid or amide derivative as represented by Formula VI by procedures well known in the art. Similarly, the protecting groups, that is, the acetylene and the amino protecting groups and the ester or amide functions, if desired, can be removed with aqueous acid, for example, hydrochloric or toluene sulfonic acid or aqueous base, for example, sodium hydroxide or potassium hydroxide. The protecting groups can also be removed by using hydrazine or phenylhydrazine.
The alkylation reaction is carried out in an aprotic solvent, for example, benzene, toluene, ethers, tetrahydrofuran, dimethylsulfoxide, dimethyl formamide, dimethyl acetamide, hexamethyl phosphoramide and hexamethyl phosphortriamide. The reaction temperature varies from -120° to about 25°C, and a preferred reaction temperature is about -70°C. The reaction time varies from 1/2 hour to 24 hours. The protected propargylamine derivatives, compound 1, are prepared by the addition of protecting groups on the acetylene function and the nitrogen function of propargylamine. Protection of the nitrogen function of propargylamine is accomplished by forming in a known manner a Schiff's base with a non-enolizable carbonyl bearing compound, such as benzaldehyde, benzophenone, or trialkylacetaldehyde. Protection of the acetylenic function is accomplished by reacting the above described Schiff's base with trimethylsilylchloride, triethylsilylchloride or higher trialkylsilylchloride forming in a known manner (E. J. Corey and H. A. Kirst, Tetrahedron Letters, 1968, 5041) the corresponding trialkylsilyl derivatives.
The alkylating reagents employed in the above reaction are known in the art or can be prepared by procedures well known in the art.
Compounds of this invention wherein R represents alkylcarbonyl are prepared from the corresponding acid wherein R represents hydrogen using the appropriate acid anhydride or halide of acetic acid, propionic acid, butyric acid or valeric acid. The amide derivatives can be isolated as the acid or a derivative thereof, for example, the ester by converting the acid to the acid halide, for example, by treating with thionyl chloride followed by alcoholysis, to give the appropriate ester by procedures generally known in the art.
Compounds of this invention wherein R represents alkoxycarbonyl are prepared from the corresponding acid wherein R represents hydrogen using an appropriate alkyl chloroformate, for example, methyl chloroformate, ethyl chloroformate, n-propyl chloroformate, n-butylchloroformate, isobutyl chloroformate or tert-butyl chloroformate, in the presence of a base by procedures well known in the art.
Compounds of general Formula I wherein R is ##EQU27## are prepared by treating an ester of a compound of Formula I, wherein R is hydrogen with a protected acid of the formula ##EQU28## wherein the amino function is protected with a suitable blocking group, such as, benzyloxycarbonyl or tert-butoxycarbonyl. Either the free acid or a reactive derivative thereof, for example, an acid anhydride may be employed. When the free acid is used, a dehydrating agent such as N, N'-dicyclohexylcarbodiimide is used. The substituent R 10 has the meaning defined in general Formula I.
Compounds of this invention wherein R 2 represents ##EQU29## are prepared from the corresponding acid derivative wherein the amino function is protected with a suitable blocking group, such as, benzyloxycarbonyl or tert-butoxycarbonyl. The amino protected derivatives either as the free acid, in which case a dehydrating agent such as N, N'-dicyclohexylcarbodiimide is used, or a reactive derivative of acid, such as, an acid anhydride, is reacted with a compound of the structure ##EQU30## wherein R 4 has the meaning defined in general Formula I, and R 11 is a lower alkyl group, for example, methyl, or ethyl, followed by base hydrolysis to remove the protecting group by procedures well known in the art.
The lactams of this invention, as described by general Formula III, are prepared from the corresponding amino acid, that is, a compound of the formula ##EQU31## or ester thereof wherein n' is the integer 2 or 3, by procedures generally known in the art, for example, by treating the amino acid with a dehydrating agent such as dicyclohexylcarbodiimide or by heating the appropriate ester derivative.
The optical isomers of the compounds of this invention may be separated by using a (+) or (-) binaphthylphosphoric acid derivative or a salt of said derivative and an optically active base by the method described by R. Viterbo et al., in Tetrahedron Letters 48, 4617-4620 (1971) and in U.S. Pat. No. 3,848,030.
The following specific examples are illustrative of the compounds of this invention.
EXAMPLE 1
Propan-1-yne-3-iminobenzyl
A solution of propargylamine (26.1 g, 0.47 M) and benzaldehyde (52 g, 49 M) in benzene (150 ml) is treated with MgSO 4 (20 g). The reaction mixture is stirred at room temperature for 30 minutes, then filtered. Excess water is removed by way of azeotropic distillation, the solution concentrated, and the residue distilled to give propan-1-yne-3-iminobenzyl (55.5 g, 82%) b.p. 107°-110°C (10 mm Hg).
EXAMPLE 2
1-Trimethylsilyl-1-propynyl-3-iminobenzyl
To a mechanically-stirred solution of propan-1-yne-3-iminobenzyl (43.5 g, 0.30 M) in tetrahydrofuran (400 ml) at 0°C is added, during 30 minutes, ethyl magnesium bromide (285 ml of a 1.12 M solution, 0.316 M). After 30 minutes at 0°C, the resulting solution is treated with a solution of trimethylsilylchloride (32.4 g, 0.30 M) in tetrahydrofuran (100 ml), the addition taking 45 minutes. After stirring at 0°C for an additional 11/2 hours, the solution is treated with brine (8 × 100 ml), then dried and concentrated on a rotorvapor. The residue is distilled to afford a liquid (52.2 g, 80%) b.p. 92°-110°C, 0.6 mm Hg. An aliquot was redistilled to give 1-trimethylsilyl-1-propynyl-3-iminobenzyl.
EXAMPLE 3
4-Amino-5-yne-hexanoic acid
To 11.25 g (50 mM) of 1-trimethylsilyl-1-propynyl-3-iminobenzyl in 500 ml of tetrahydrofuran is added n-butyllithium (25 ml of a 2 M solution, 50 mM) at -70°C. After 20 minutes at -70°C, freshly distilled methyl acrylate (4.3 g, 50 mM) is added. After 30 minutes at -70°C, 10 ml of water is added and the reaction mixture is allowed to come to room temperature. The tetrahydrofuran is then evaporated and concentrated HCl (20 ml) in water (150 ml) is added and the mixture heated at reflux overnight. On cooling, the aqueous solution is washed with methylene chloride, adjusted to a pH of 8 and reextracted with methylene chloride. The aqueous base is adjusted to a pH of 6. The product is isolated by ion exchange chromatography on an acid resin followed by recrystallization from ethanol-water.
EXAMPLE 4
3-Amino-4-yne-pentanoic acid
In 250 ml of tetrahydrofuran is dissolved 3.8 g (17.75 mM) of 1-trimethylsilylpropan-1-yne-3-iminobenzyl and the solution is cooled at -78°C. To the solution, 9 ml of tetramethylethylenediamine and 9 ml of 2-molar n-butyllithium are added successively. After a few minutes, stirring 2.98 g (17.75 mM) of ethylbromoacetate dissolved in 20 ml tetrahydrofuran is added. The reaction mixture is stirred for 5 minutes, cooling is stopped and 100 ml NaCl saturated water is added. The reaction mixture is extracted with ether and the organic phase is dried and concentrated and 6.5 g of an oily residue is obtained.
One-half of the above residue is dissolved in 30 ml tetrahydrofuran and 30 ml 6N HCl is added. The reaction mixture is refluxed overnight and the neutral components of the reaction mixture are extracted with methylenechloride in basic and acid conditions. The organic phase is evaporated to dryness and applied on a column of Amberlite I.R. 120 H. Fractions eluted with 1 N NH 4 OH are collected, evaporated to dryness and recrystallized from EtOH/H 2 O 1:1 to give 50 mg of 3-amino-4-yne-pentanoic acid.
C 5 H 7 NO 2 --Calculated: C: 53.08, H: 6.25, N: 12.38. Found: C: 53.23, H: 6.40, N: 12.19.
______________________________________I.R. (film) 32 cm.sup.-.sup.1 (C CH) 2150 cm.sup.-.sup.1 (C C, N.sup.+H.sub.2) 1570 cm.sup.-.sup.1 (COO.sup.-)______________________________________
EXAMPLE 5
(-) 4-Amino-5-yne-hexanoic acid and (+) 4-amino-5-yne-hexanoic acid
300 mg of the racemic compound 4-amino-5-yne-hexanoic acid is dissolved in 5 ml of absolute methanol, and 900 mg of (+) binaphthylphosphoric acid (BNPA) is added. After the solution is almost clear and an eventual solid residue has been filtered off, the solvent is evaporated and the dry residue dissolved at about 80°C in EtOH/H 2 O 1:1. On cooling, 440 mg of the crystallized enantiomer A is collected. The mother liquor is treated with HCl 1/ N to pH 1 and filtered. The pH of the filtrate is adjusted to 6 and filtered through a column of Amberlite I.R. 120. The amino acid is eluted with 1M NH 4 OH. After evaporation to dryness, the residue is recrystallized in EtOH/H 2 O 9:1 and 40 mg of (-) 4-amino-5-yne hexanoic acid is obtained: (α) D 20 = -29 (H 2 O C: 1.33 ).
The 440 mg of enantiomer A are processed in the same way as the corresponding mother liquor. After recrystallization in ethanol water (9:1), 30 mg of (+) 4-amino-4-ynehexanoic acid are obtained. [α] D 20 = +30 (H 2 O C = 1.05).
EXAMPLE 6
4-Acetamido-5-Yne-Hexanoic Acid Methyl Ester
A suspension of 1.27 g (10 mM) of 4-amino-5-yne-hexanoic acid in 25 ml of acetic anhydride in 10 ml of water is heated in an oil bath for 1 hour. The acetic anhydride is evaporated under vacuum, the residual syrup taken up in chloroform, and the solution is evaporated to dryness. This process is repeated several times to remove the acetic acid. The syrup is dissolved in 10 ml of chloroform, the solution cooled in ice water and under moisture exclusion 0.9 ml of thionyl chloride is added. The solution is stirred in the cold for 30 minutes and 2 ml of methanol is added while the cooling bath is removed. Stirring is continued for 1 hour. The evaporation of the solvent yields the product as an oil.
EXAMPLE 7
5-Amino-6-yne-heptanoic acid
To 1-trimethylsilyl-1-propynyl-3-iminobenzyl (10 mM) in 200 ml of tetrahydrofuran at -70°C was added n-butyllithium (10 mM) followed by 4-iodobutanoic acid methyl ester (10 mM) in 200 ml of tetrahydrofuran. The temperature was allowed to rise to -20°C and maintained at this temperature for 10 hours. The reaction product was extracted into ether to afford an oil. This oil was hydrolyzed in acid in the same manner as described in Example 3. The product is isolated by ion exchange chromotography and purified by recrystallization from ethanol-water.
Alternatively, 5-amino-6-yne-heptanoic acid may be prepared by the following procedure.
1-Trimethylsilyl-1-propynyl-3-iminobenzyl (10 mM) in 200 ml of tetrahydrofuran at -70°C was treated with n-butyllithium (10 mM), then with 1-iodo-3-chloropropane (10 mM) in 10 ml of tetrahydrofuran. After 10 hours at -70°C, the tetrahydrofuran was removed by evaporation at room temperature, and replaced by 20 ml of dimethylformamide. To the reaction mixture were added sodium iodide (10 mM) and sodium cyanide (20 mM), and the solution was maintained at 50°C overnight. On cooling, the mixture was poured into 300 ml of water and extracted with ether. The ether solution was washed with water, dried over magnesium sulfate and concentrated. The resulting oil was treated with HCl (6 N, 200 ml) and refluxed for 24 hours. On cooling, the mixture was extracted with methylene chloride, the aqueous base was adjusted to pH 9 using sodium carbonate and washed again with methylene chloride. The aqueous base was concentrated to about 50 ml, adjusted to a pH of 5, and the product isolated by ion exchange chromotography and purified by recrystallization from ethanol-water.
EXAMPLE 8
4-Amino-3-phenyl-5-yne-hexanoic acid hydrochloride
To a solution of 2:15 g of 1-trimethylsilyl-1-propynyl-3-iminobenzyl (10 mM) in 250 ml of tetrahydrofuran cooled to -78°C is added 10 m moles of n-butyllithium. After 10 to 15 minutes, a solution of 1.65 g of trans-cinnamic acid methyl ester (10 mM) is added. The solution is stirred at -78°C for 45 minutes and treated with brine. The product of the reaction is extracted by ether. The solution is dried over magnesium sulfate and evaporated to dryness leaving an oil which is treated with 6 NHCl for 24 hours. Upon evaporation to dryness, the remaining syrup is dissolved in water. The product is isolated by ion exchange chromotography on an acid resin and purified by recrystallization from ethanolether.
EXAMPLE 9
4-Amino-5-yne-2-ene-hexanoic acid
1Trimethylsilyl-1-propynyl-3-iminobenzyl (10 mM) in 100 ml of tetrahydrofuran at -70°C was treated with n-butyllithium (10 mM). To the reaction mixture was added 2-yne-propionic acid methyl ester (10 mM) in 10 ml of tetrahydrofuran. After 20 minutes at -70°C, 10 ml of water was added. On warming to room temperature, 6 NHCl (100 ml) was added and the mixture was refluxed overnight. On cooling, the aqueous solution was washed with methylene chloride, adjusted to a pH of 8 and reextracted with methylene chloride. The aqueous base was adjusted to a pH of 6. The product was isolated by ion exchange chromotography on an acid resin and purified by recrystallization from methanol-water.
Alternatively, 4-amino-5-yne-2-ene-hexanoic acid may be prepared by the following process.
1-Trimethylsilyl-1-propynyl-3-iminobenzyl (10 mM) in 100 ml of tetrahydrofuran to -70°C was treated with n-butyllithium (10 mM). To the reaction mixture was added methyl trans-3-chloroacrylate (10 mM) in 10 ml of tetrahydrofuran. After 1 hour at -70°C, 10 ml of water was added. On warming to room temperature, 6 NHCl (100 ml) was added and the mixture was refluxed overnight. The product was isolated in the same manner as described above.
EXAMPLE 10
4-(2-Aminoproprionamido)-5-yne-hexanoic acid
4-Amino-5-yne-hexanoic acid methyl ester is prepared by refluxing a suspension of 1.27 g of 4-amino-5-yne-hexanoic acid in 20 ml of methanol with continuous anhydrous HCl bubbling through the reaction mixture for 3 hours followed by evaporation of the solvent, dissolution in water, neutralization with aqueous NaOH in the cold and ether extraction. The ether solution is dried over magnesium sulfate, filtered, and cooled to 0°C. Under moisture exclusion a solution of 10 mMoles of α-alanine wherein the amino function is protected with benzyloxycarbonyl and the acid function is activated with ethoxycarbonyl, prepared by the methods known in the art, in ether is added slowly with stirring. When addition is complete, the cooling bath is removed and stirring continued overnight. The solution is evaporated, leaving a syrupy residue which is taken up in 2 ml of methanol and 10 ml of 2 N aqueous ammonia added. The suspension is stirred at 50°C for 1 day, then extracted with ether. The product is isolated by ion exchange chromotography on an acid resin.
EXAMPLE 11
N-(2-propionic acid)--3-amino-4-yne-pentan-1yl carboxamide
To a solution of 1.27 g of 4-amino-5-yne-hexanoic acid (10 mM) in 10 ml of water was added 10.0 ml of 2 N NaOH. This solution was cooled in ice water and 1.87 g (11 mM) of benzylchloroformate was added slowly with stirring. When the addition was complete, stirring was continued for 1 hour. The solution is acidified to a pH of 4 by addition of aqueous HCl and the oily precipitate is extracted into ether. The ether solution is dried over magnesium sulfate, filtered and cooled. After addition of 700 mg of triethylamine, an ethereal solution of 11 g of freshly distilled ethylchloroformate is added slowly over 1 hour with stirring. The precipitate is filtered off and to the ether solution a solution of alanine methyl ester in ether is added at once. The solution is kept overnight and then evaporated to dryness. The residue is taken up in 2 ml of methanol and 20 ml of 2 N aqueous NaOH is added. The suspension is stirred for 1 day at 50°C, then the solution is extracted with ether and adjusted to a pH of 7. The product is isolated by ion exchange chromotography on an acid resin.
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Novel compounds of the following general formula are useful pharmacologic agents: ##EQU1## R is selected from hydrogen, alkylcarbonyl wherein the alkyl moiety contains from 1 to 4 carbon atoms, alkoxy-carbonyl wherein the alkoxy moiety contains from 1 to 4 carbon atoms and may be straight or branched, and ##EQU2## wherein R 10 is selected from hydrogen, a straight or branched lower alkyl group of from 1 to 4 carbon atoms, benzyl and p-hydroxybenzyl; R 2 is selected from hydroxy, a straight or branched alkoxy group of from 1 to 8 carbon atoms, a lower alkylamino group wherein the alkyl moiety contains from 1 to 4 carbon atoms, and ##EQU3## wherein R 4 is selected from hydrogen, a straight or branched lower alkyl group of from 1 to 4 carbon atoms, benzyl, and p-hydroxybenzyl; [A] is selected from ##EQU4## AND --CH=CH-- wherein R 1 is selected from hydrogen, lower alkyl of from 1 to 4 carbon atoms, phenyl and substituted phenyl wherein the substituents on the substituted phenyl may be attached at the ortho, meta or para positions of the phenyl ring and are selected from halogen, lower alkoxy of from 1 to 4 carbon atoms, and lower alkyl of from 1 to 4 carbon atoms; n is an integer of from 1 to 5; and the lactams of said compounds wherein [A] represents ##EQU5## R and R 1 represent hydrogen and n is the integer 2 or 3; and pharmaceutically acceptable salts and individual optical isomers thereof.
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FIELD OF THE INVENTION
The invention relates to devices for reducing the apparent recoil of a conventional projectile firing weapon, such as a rifle, pistol or shotgun, and more particularly, to an improvement in muzzle brakes.
BACKGROUND OF THE INVENTION
It is well known that projectile firing weapons, such as rifles, pistols, and shotguns generate a substantial recoil. The force exerted by the weapon against the body of a shooter, or against the structure supporting the weapon is proportional to the mass and velocity of the projectile. It is also proportional to the mass and type of propellant and inversely proportional to the mass of the weapon. For an individual firing a small caliber weapon, the recoil forces are manageable. A .22 caliber firearm, utilizing a relatively small charge of powder, generates forces which even a small child can anticipate and accommodate if properly trained. However, for larger caliber weapons, which utilize large powder charges, the recoil forces are substantially larger. They can result in great discomfort to the person firing the weapon and, in extreme cases, can cause personal injury.
A desirable object is to control or limit the recoil generated by such weapons. It has long been known that the undesirable recoil characteristics of firearms can be diminished by the use of a muzzle gas dispersing device, commonly known as a muzzle brake. By diverting a portion of the hot muzzle gases to a direction different than that of the bore of the gun barrel, the recoil forces are reduced. However, substantial room for improvement in the reduction of recoil utilizing this method may yet be realized by improved technologies.
Muzzle brakes currently in use have substantial undesirable side effects. Such muzzle brakes cause a significant increase in the amount of perceived noise generated by the discharge of the weapon. This is due, in large measure, to the use of relatively few openings or diverters having relatively large areas. Commonly, two to four identical large backward leaning slots are cut into the top of a barrel's muzzle or an attached muzzle brake in an irregular pattern. Such diverters remove hot gasses rapidly and thereby shift the sonic energy to frequencies that are undesirable, cause muzzle blast, and concentrate sonic energy near specific frequencies. A need exists in the art for a muzzle brake that meters the escaping gasses so they are removed more slowly.
SUMMARY OF THE INVENTION
It is the object of this invention to provide a novel and improved gun muzzle brake that significantly reduces recoil of the gun without appreciatively increasing relative noise levels.
In accordance with the present invention, the improved gun muzzle brake is formed in the barrel or in a removable steel cylindrical body having properties similar to those of the steel used to make gun barrels. This muzzle brake has a longitudinal chamber including various sections, and the whole muzzle brake is pierced by a large number of small openings. These openings are preferably angled forward. The various sections of the chamber are coaxial with each other and with the bore of the gun. Further, they do not interfere with the passage of the bullet. Two special types of sections are:
(a) The "gas slip" formed as a truncated cone allowing expansion of the propellant gases. The gas slip could alternatively be a cylindrical section of increased diameter. The gas slip is pierced by a number of openings.
(b) The thrusting shoulder having an abrupt narrowing of the chamber in a direction away from the muzzle of the gun thus forming an annular shoulder. The thrusting shoulder also has a number of openings.
The expectation is that a thrusting shoulder and a gas slip are particularly effective in facilitating the dispersing of the propelling gases. The preferred embodiment has a section closest to the muzzle of the gun that is significantly larger in cross section than the bore of the gun and contains at least one gas slip. This wide section is followed by a thrusting shoulder or a tapered narrowing section and then a relatively long narrow section slightly larger in diameter than the bore of the gun. The narrow section ends at the front of the muzzle brake. An additional gas slip is included a short distance inside of the front of the narrow section.
This muzzle brake is an improvement over prior muzzle brakes in that the numerous small openings modify the acoustical intensity versus pitch distribution of the noise. Thus, the perceived noise is very small and no greater than that of a gun without a muzzle brake.
The sonic energy is then neither shifted to undesirable pitches nor concentrated near specific undesirable frequencies.
Comparing the discharge of the same gun with and without the use of the present invention reveals a significant reduction in the amount of recoil, without appreciably increasing the measured and perceived noise.
The present invention is also advantageous as compared to other muzzle brakes on the same gun, because the measured discharge noise and perceived noise are lower when using the present invention.
The present invention is further advantageous in that the small openings of the present invention resist collection of the debris typically encountered in the field.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective side view of the invention, showing the body and selected openings.
FIG. 2 is a cross section of the preferred embodiment of the invention, affixed to the muzzle of a gun.
FIG. 3 is a cross section of a simplified embodiment of the invention, affixed to the muzzle of a gun.
FIG. 4 is a cross section of a further simplified embodiment of the invention, affixed to the muzzle of a gun.
FIG. 5 is a cylindrical cross section of the invention.
FIG. 6 is a detailed and close-up view of a section of FIG. 2.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The invention operates to divert propelling gas in a direction other than the direction of the bore. The diameter of the first interior chamber of the muzzle brake immediately following the bore is greater than the bore. This increased dimension allows for expansion of the propelling gas. Thereafter, the chamber decreases in diameter, which tends to compress the gas. However, a plurality of relatively small openings located adjacent to the diameter decrease in this narrowed section allows the gas to escape in a direction other than the bore. Thus, with a series of decreasing diameters and small openings portions of the gases are progressively metered and diverted in a series of steps without increasing the sonic energy. This rapid, step-wise diameter decreases serve to channel portions of the gas through specific openings to a direction other than along the bore axis.
On FIG. 1 is shown the external appearance of the preferred embodiment of the invention as a removable body. The external appearance is that of a cylindrical body 10 pierced by numerous small circular openings 20. The body 10 is composed of a steel having properties of hardness, ability to be polished, and ability to be blued, Parkerized, nickel plated, or finished similar to the steel used in making the barrel to which the muzzle brake is attached. The outside diameter of the body 10 is somewhat larger than the outside diameter of the associated barrel.
The pattern of openings 20 has one blank or missing band corresponding roughly to the widest part of the diverter cone 14 (FIG. 4). Typically, there are three bands of fifteen openings 20 into first section 12, followed by the blank or missing band, and continuing with thirteen bands of fifteen openings 20.
The number of openings varies somewhat with the outside diameter of the body, with no fewer than one hundred eighty (180) openings 20 used and roughly two hundred (100) openings 20 being typical. The openings 20 have a diameter of no more than 0.125 inches. These small openings 20 do not allow foreign matter to readily lodge therein.
The openings 20 are spaced along the surface of a body 10 in a series of regular spiral patterns inclined essentially 45 degrees from the bore axis of the body 10 (such as along dotted line A). For each particular opening 20, each of its nearest openings 20 lie along line segments extending essentially 45°, 135°, 225°, or 315° (relative to the longitudinal bore axis of the body 10) from the center of the particular opening 20. The pattern of openings 20 immediately surrounding and including a particular opening 20 looks very much like the five dots on the value five side of a common game die. The pattern of openings 20 may also be described as being one of equally spaced openings 20 lying on a series of regularly spaced bands circumscribing the body 10 where the openings 20 on adjacent bands are all rotated with respect to each other essentially one half of the spacing between openings 20. (Such as along dotted line B.) Alternatively, one may describe the pattern of openings 20 as being one of openings 20 lying along straight rows essentially parallel to the axis of the body 10 (such as along dotted line C).
FIG. 4 illustrates a cross section of a first embodiment of the invention affixed to the muzzle end of the barrel 2. The muzzle brake is affixed to barrel 2 by mating barrel threads 6 cut into the outside of the barrel 2 and into the inside of the body 10. The threads 6 are thus cut into body 10. Alternatively, mating threads may be cut into the bore 8 and the outside of the body 10.
Interior chamber 22 freely communicates with openings 20 and is composed of several coaxial sections of differing diameters and tapers. Immediately forward of the barrel 2, first gas slip section 12 allows for expansion of the propelling gas. The diameter of gas slip section 12 tapers to a diameter significantly greater than that of the bore 8 as it proceeds away from barrel 2. First thrusting shoulder 17 abruptly narrows the interior chamber 22 between gas slip 12 and diverter cone 14. Thrusting shoulder 17 forces a significant portion of the propelling gas away from the axis of the bore 8 through a plurality of openings 20. More specifically, a radial series of openings 20 (such as along line B in FIG. 1) intersects the thrusting shoulder 17 to maximize the available outlet area for the thrusting shoulder 17.
Diverter cone 14 appears as a truncated cone with its widest diameter most distant from the muzzle end of the muzzle brake and decreases the diameter of interior chamber 22 and further force propelling gases into openings 20. Although it does not possess an abrupt narrowing, the diverter cone 14 constricts and forces the gas to further be diverted through openings 20. Cylindrical section 18 roughly corresponds to the bore 8 diameter. Cylindrical section 18 roughly corresponds to the bore 8 diameter. Cylindrical section 18 communicates with a number of openings 20 and does allow for the diversion of the gas.
Toward the muzzle end 19 of the muzzle brake, an additional gas slip 24 and thrusting shoulder 25 allow for final diversion of the gas. Again, the preferred embodiment provides for a radial series of openings 20 to intersect the thrusting shoulder 25. However, since the diagrams show a reduced number of openings 20 for clarity, the intersection of the openings 20 by a thrusting shoulder is not always depicted. Forward gas slip 24 and thrusting shoulder 25 function similarily to the previously described arrangement. They are typically machined into the muzzle brake from the muzzle end using conventional means.
With reference now to a second embodiment disclosed in FIG. 3, the first gas slip 12 is followed by more than one thrusting shoulder. FIG. 3 illustrates first thrusting shoulder 17 as previously described. A first cylindrical section 13 follows thrusting shoulder 17. Thereafter, an additional thrusting shoulder 17A and second cylindrical section 15 follow. Diverter cone 14 follows. This forms a series of thrusting shoulders which meter and deflect the propelling gas.
The diverter cone 14 tapers from the diameter of the second cylindrical section 15 to the diameter of the cylindrical section 18. The diameter of cylindrical section 18 remains slightly greater than that of the bore 8.
FIG. 2 illustrates a third embodiment designed to maximize deflection of propelling gas which contains at least one additional gas slip 21. Gas slip 21 is cut into the second cylindrical section 15 and is followed by an additional thrusting shoulder 23 to form yet another annular deflecting surface.
It is anticipated that the present invention would be machined into the muzzle end of barrel 2 using conventional techniques.
The ultimate goal of the invention is deflection of propelling gases by the progression of shoulder sections. The initial gas slip is used to reach a maximum diameter for the first shoulder section. Multiple shoulders can then progress in a stepwise fashion through smaller diameters. Should additional shoulders be necessary, the working diameter of chamber 22 is increased by an additional truncated cone, such as gas slip 21, and the progression continues to the muzzle 19. Thus, an infinite variety of slip/shoulder combinations are possible.
An alternative embodiment may be effected by the use of sections that are essentially in the shape of a cylinders of the largest diameter of each gas slip, in place of the gas slip 12. A cylinder would similarily allow for the expansion of propelling gases.
FIG. 5 is a cross section of the invention normal to the chamber 22 along the lines 5--5 of FIG. 4. FIG. 5 illustrates the openings 20 communicating radially from the chamber 22 to the outside of the body 10. The bore 8 is seen central to the drawing.
FIG. 6 illustrates a further feature of the invention. The openings 20 are angled forward from the perpendicular to the bore axis. Preferably this angle 30 is in the range of three to fifteen degrees forward from a position perpendicular to the bore axis. This increases the ability of the thrusting shoulder 17 and gas slip 12 to deflect the propelling gas.
As the propelling gas leaves the barrel 2 it tends to expand into any available space. This factor alone tends to force the gas out of openings 20. To amplify this tendency, an area of increased diameter is followed by an abruptly narrowing annular shoulder, such as thrusting shoulder 17. This provides a wall which deflects a portion of the gas out of the intersected openings 20. Each of these shoulders divert a significant portion of the gas. Further, converging diameters, such as of the diverter cone 14, function to further divert the gas. The gas will oppose compression and be diverted out the related openings 20.
Overall, the propelling gas is metered through all the openings 20 of the muzzle brake, instead of being diverted by a relatively few such openings. This effectively diffuses the recoil energy, but does not increase or concentrate the sonic energy.
The invention is manufactured using conventional machining techniques. These techniques include matching, drilling, heat treating to impart hardness, steel shot blasting, centerless grinding, polishing, and bluing, Parkerizing, or the use of other coatings or platings.
Although a preferred embodiment of the invention has been disclosed in detail, it will be recognized that variations or modifications lie within the scope of the present invention.
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The invention is an improved muzzle brake with the outer appearance of a perforated metal cylinder and an inner chamber composed of cylindrical sections, tapering sections, conical sections, and abrupt and gradual changes between the various sections. The brake is intended to be attached to the muzzle of a gun such as a rifle, pistol or shotgun. Holes running radially from the surface of the brake into the inner chamber divert a portion of the propelling gases away from the normal direction of such gases, resulting in a reduction in recoil. The holes are spaced about the surface of the brake along spirals. The use of many small regularly patterned holes results in a decrease in the perceived discharge noise.
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This is a continuation of U.S. application Ser. No. 463,913, filed on Jan. 10, 1990, which is a continuation of U.S. application Ser. No. 309,447, filed on Feb. 10, 1989.
TECHNICAL FIELD
The present invention relates to the field of washing and cleaning of fabrics in a machine.
BACKGROUND INFORMATION
European Patent Application No. 85/400,652.5, published under No. 0,151,549, in the name of The Procter & Gamble Company, describes an original process for washing fabrics in a machine with a liquid detergent. According to this process, a device containing a liquid detergent and comprising unoccluded vents, is employed. This device is placed with the clothing to be washed in the drum of the machine and the machine is started up allowing the washing cycle to proceed, with the detergent thus flowing progressively into the fabrics and the washing bath as soon as the machine is started up. According to an embodiment, a predetermined quantity of liquid detergent is poured into the device, which comprises a filling orifice for this purpose and, at the end of the washing, the device is recovered and may be reused. A process of this kind improves the efficiency of the washing of fabrics in a machine very appreciably and it is widely developed, with great commercial success in Europe.
Devices permitting the use of the process indicated above are described, for example, in U.S. Pat. No. 4,703,872, issued Nov. 3, 1987 to Cornette et al. A device of this kind comprises at least one filling orifice and vents for the progressive release of the liquid within the fabrics in the course of washing. By way of example, the device comprises a body and an added assembly which is intended for filling and/or for distributing the liquid. An assembly of this kind can be mounted permanently onto the body or, on the other hand, may be removable. An assembly of this kind may comprise a central filling orifice and vents distributed at its periphery. According to an advantageous embodiment, the filling orifice is in the shape of an open shaft descending inside the body. It will also be noted that an arrangement which is advantageous in practice consists in imparting an essentially spherical shape to the device. Nevertheless, this shape is not limiting in any way, and for example, other shapes of revolution may be used.
For the purpose of washing, the device is filled with liquid detergent and, thus filled, it is placed in the drum of the machine, where the fabrics are already present, the liquid detergent contained in the device being progressively distributed in the course of washing within the washing medium and within the fabrics.
It is desirable to have available a simple process capable of being implemented with inexpensive devices, in order to solve simultaneously a number of technical problems which arise with the detergent compositions currently available commercially. The first problem to be solved is to place at the user's disposal a process and a device for adapting the washing conditions to the degree of soiling of the fabrics, in order thus to provide "wash with options". This problem is general and it exists both in the case of liquid detergent compositions and in the case of compositions which are in particulate form. An additional problem results from the fact that it is desirable to perform the washing of fabrics with a detergent composition whose constituents exert their activity at their optimum time, both by being involved in the washing process, for example in order to play a role in protecting the components of the washing machine, and in order to fulfill their specific function during the washing, which is the case, for example, with enzymes, softeners, grease stain removers, peroxygen compound, bleaching catalysts, bleaching activators, bactericides, foam regulators, optical brighteners and other similar constituents with a specific function. Such constituents must be available at determined times during the washing cycle and the technical problem to be solved is to find a simple and practical process for presenting these constituents so as to make them available for the washing to proceed according to a predetermined and optimum sequence.
Another problem to be solved, which arises more particularly in the case of liquid detergents, is that of the mutual incompatibility of certain constituents of the composition with regard to others. This incompatibility may be more or less pronounced, but people who specialize in this subject are well aware of this problem. It is also desirable to deliver certain constituents of the composition in a separate form so as to enable them to have a delayed effect by virtue, for example, of their being dissolved more slowly during the washing.
The invention provides a solution to the problems just mentioned, whatever the type of detergent employed, and does so while exploiting the currently existing devices which are described, for example, in the above mentioned U.S. Pat. No. 4,703,872 and which have in practice been found highly appropriate for the use of the general washing technique described particularly in the above mentioned European Patent Application 0,151,549.
SUMMARY OF THE INVENTION
In order to solve the technical problems set out above, and others, the subject matter of the invention is an improved process for washing fabrics in a machine, in which a device comprising unoccluded vents and containing a detergent is employed, this device is placed with the fabrics to be washed in the drum of the machine and the machine is started up allowing the washing cycle to proceed, the said process being characterized in that a detergent composition is employed some of whose constituents are separate, in that at least one of the said constituents is introduced into the device and in that at least one other of the said constituents is associated separately with the said device with the result that, during the washing, all of the constituents diffuse into the fabrics and the washing bath.
According to the invention, the process can be applied to detergent compositions some of whose constituents have a specific mode of action on the soiling. It may also be employed in the case where some constituents are insufficiently compatible with others within the detergent composition.
Nonlimiting examples of constituents which may be separated in the process according to the invention from the detergent composition as such are: bleaching agents such as agents releasing chlorine or active oxygen (peroxygen compound), brightening agents, agents preventing redeposition of the soiling, enzymes, softeners and grease stain removers. Such constituents have a specific action on the soiling, which takes place either at the beginning of the washing cycle or during the latter. The process of the invention may also be employed for using agents which, strictly speaking, do not act directly on the soiling, but which can nevertheless be involved in a process of washing linen in a machine. This is the case particularly with agents which provide protection of the internal parts and components of the washing machine, for example agents based on sodium silicates.
According to the invention, the fact of combining with the device at least one constituent which has a specific mode of action on the soiling means both that a constituent of this kind is made integral with the device as soon as the latter is placed in the machine and as soon as the washing cycle begins or else that a constituent of kind is presented in a separate form in order to produce its effects during the washing cycle, in combination with the other constituents contained in the device.
It can be seen, therefore, that there are many possibilities of associating these separate constituents with the device containing the detergent, depending on the nature of these constituents and their mode of action. Illustrative examples, which do not imply any limitation, will be given in the description which follows.
Thus, the constituents presented in a separate form may be contained in pouches or sachets, for example as an individual measured quantity, made of a nonwoven substance or, on the other hand, of a substance which is soluble in the washing bath (for example of PVA polyvinyl alcohol). These constituents may also be gelatin capsules or tablets or pastilles which are soluble in the washing bath, as well as granules, sheets, for example nonwoven, impregnated or coated with active ingredients, or substances having the consistency of a paste.
In an embodiment of the process, the detergent composition as such is presented in liquid or granular form and is supplied individually to the user. The latter also has available products or constituents with a specific action which are offered to him separately and, for example, have tints or colors which are characteristics for each of them, so that the user may adapt the formulation of the detergent composition to the precise need of the washing, as a function of the state of soiling of the fabrics, according to indications he is given. In the same way, the problem of an insufficient incompatibility of some constituents of the detergent composition can be solved. A separate and delayed action of certain constituents, such as bleaching agents can also be produced, by virtue of their separate presentation which enables them to dissolve more slowly during the washing cycle.
As mentioned before, the process of the invention may be implemented with a device or receptacle which is very simple, for example of the general type described in U.S. Pat. No. 4,703,872.
The constituents presented separately, according to the invention, are advantageously integral with the device or receptacle placed in the drum of the washing machine.
For this purpose, the device or receptacle may comprise housings, for example in its outer periphery, which are capable of receiving the separate constituents in any of the above-mentioned forms.
However, it is also possible to exploit the structure of the currently known devices or to modify it slightly so as to arrange the separate constituents in question in the device.
By way of example, if a receptacle comprising a body of revolution and an assembly, removable or not, with a central filling orifice in the shape of an open shaft, and vents distributed on its periphery, is available, then, once the detergent composition has been placed in the body of the receptacle, it is possible to house in the open shaft the constituents of the said composition which are intended to be associated with the receptacle and which are, for example, presented in the form of a sachet made of a nonwoven substance or soluble in the washing bath. However, it is also possible to provide a receptacle comprising a double open shaft, one permitting filling with the detergent composition as such and the other being used for placing the sachets, which then have a specific housing. If these sachets are made of a nonwoven substance they are simply recovered at the end of the washing operation. The open shaft(s) in question may be left free in their upper part or may, on the other hand, comprise a snap-on lid or a movable lid, for example with a hinge, so as to enclose the constituents in their housings and to let them diffuse through the vents of the receptacle at the same time as the remainder of the detergent composition.
Forms of presentation of the separate constituents in units which correspond to a solid structure or one that can be handled like a solid have been primarily indicated above and are preferable. However, these constituents may also be presented in a different form, for example as a liquid or gel. In such cases, theses separate constituents of the detergent composition as such may be placed in the receptacle in an individual housing. The receptacle may be supplied to the user with a housing which is thus filled in advance, in which case it suffices to fill the receptacle with detergent and to unblock the opening of this housing, in order to permit the diffusion of the detergent as well as of the constituent which has already been placed in position.
However, it is not a departure from the scope of the invention to employ a receptacle or device of a general design such as described in U.S. Pat. No. 4,703,872 for example, and to present a particular constituent separately, because of its specific action, so long as this constituent is associated, at the time of use, with the receptacle in question, that is to say that it is placed in the machine with this receptacle.
The person skilled in the art will therefore understand that the process of the invention may be implemented with a very wide variety of devices or of receptacles, the examples given above being merely for guidance and not limiting in any manner.
The invention contributes a simple and efficient solution to the technical problems mentioned at the beginning of the present specification. In the prior art, certain processes for washing fabrics in a machine involved the use of a machine capable of picking up from separate vats the corresponding ingredients of a detergent formulation. This technical solution is extremely complicated, because not only does the structure of the machines have to be modified, but also costly programming equipment which comes into operation as the washing cycle progresses must be provided.
On the other hand, the process of the invention exploits all the advantages of simplicity and efficiency of the general technique of washing forming the subject matter of European Patent Application 0,151,549. To the advantages of this technique, namely a better washing efficiency and getting rid of the losses of detergent in the machine draining circuit, the invention adds a great flexibility of washing conditions, the user being in a position to perform a "wash with options" depending on the nature and the state of the fabrics to be washed and on the soiling to be removed.
The description which follows gives still further concrete examples of embodiment of the invention.
The invention will now be illustrated without being limited in any manner, with reference to the attached drawings, which illustrate devices permitting the use of the process of the invention, namely:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an axial section of a device incorporating constituents presented in the form of tablets or pastilles.
FIG. 2 is a view of the indicated detail of FIG. 1.
FIG. 3 is a view similar to FIG. 1, illustrating a device wherein some constituents are presented in a sachet or pouch.
FIG. 4 is a perspective view of an alternative form of the device employing tablets.
FIG. 5 is an axial section of the device of FIG. 4.
FIG. 6 is a perspective view of a component of the device in FIGS. 4 and 5.
FIG. 7 is a perspective view of a tablet which can be employed in the process of the invention.
FIG. 8 is an axial section of a device showing another embodiment with constituents presented in the form of tablets.
FIG. 9 is a top view of the part of the embodiment of FIG. 8 containing the tablets.
FIG. 10 is a view similar to FIG. 9 and illustrating an alternative embodiment.
FIG. 11 is an axial section of another device which can be used with tablets.
FIG. 12 is an axial section of a device incorporating tablets in its upper part.
FIG. 13 is an axial section of a device having a housing on its outer wall.
FIG. 14 is an axial section of a device having a housing for tablets in its lower part.
FIG. 15 is an axial section illustrating an alternative construction of a component of the device.
FIG. 16 is an axial section illustrating another alternative construction.
DETAILED DESCRIPTION OF THE INVENTION
For the sake of simplicity of the description and uniformity of the text, most of the devices which will be described are of the general type forming the subject matter of U.S. Pat. No. 4,703,872. As illustrated in Figure in particular, they comprise a body 1 of generally spherical shape and an added assembly 2, to which the body 1 is attached by a planar surface 4 positioned radially and extended by a cylindrical surface 5 in an upward direction. The added assembly 2 comprises a bowl-shaped upper part 6 providing a central opening 7. The wall of the bowl 6 has peripheral perforations 8. The bowl 6 is extended downwards by a cylindrical part 9 in the form of an open shaft descending into the device 1, which is intended to be used as a receptacle for the detergent composition. Furthermore, the added assembly 2 also has parts 10, projecting outwards and at the periphery, which come to bear on the surface 4 of the body 1 and serve essentially as means of grasping.
The process of the invention may be advantageously used with a device of this type, which makes it possible to associate some separate constituents of the basic detergent composition which is introduced into the body 1.
In the embodiment illustrated in FIG. 1, a number of tablets containing ingredients or constituents having a specific function for the washing are placed inside the open shaft 9. As illustrated in detail in FIG. 2, the inner surface of the open shaft 9 may have annular projections 13 which make it possible to provide between them housings where the tablets 12 are housed respectively. In FIG. 1 it can also be seen that the open shaft is limited by a wall 14 situated at an intermediate level of its height, and this makes it possible to avoid having to push a tablet into the open shaft as far as its lowest level.
In the drawing of Figure the open shaft 9 has been illustrated as comprising lengthwise side openings, which are conventional in devices of this type that are already employed. However, for the requirements of the invention, it may be advantageous to provide an open shaft with continuous walls, so that the detergent, for example liquid, composition introduced into the body 1 does not immediately come into contact with the tablets housed in the open shaft. These embodiments depend on the type of constituents present in the tablets, as will be seen later. Also, FIGS. 1 and 2 illustrate tablets housed in the open shaft, but the same arrangements could be applied with constituents presented in the form of gelatin capsules or of any other structure having sufficient rigidity to be inserted and maintained in the open shaft.
To simplify matters, the description with reference to FIG. 3 of the device whose constituent parts are the same as those of the device in FIGS. 1 and 2 will not be repeated. In the alternative form shown in FIG. 3, the separate constituent(s) of the detergent composition is (are) presented in the form of a sachet or pouch 15 which is arranged inside the open shaft 9. FIG. 3 shows a lid 16 which can move around a hinge 18 and can be manipulated by a ring 17. This lid can be useful if the substance of which the sachet 15 is made is a nonwoven textile which does not dissolve in the washing bath, in which case it is better, when the washing is finished, to prevent the sachet from escaping from the device and possibly causing damage to the mechanical components of the washing machine. In this case, the lid 16 is brought down onto the upper part of the open shaft, so that the latter is closed. As usual, the open shaft 9 has lengthwise openings 19 which also make it possible to bring the sachet into contact with the washing liquid, to ensure the diffusion of the constituent which it contains. If the sachet 15 is made of a water-soluble material such as polyvinyl alcohol, it suffices to place it in the open shaft, which then does not need to be provided with a lid in its upper part.
FIGS. 4 to 6 illustrate an alternative embodiment, according to which tablets of constituents which have a specific function for the washing are placed not in the open shaft as shown in FIGS. 1 to 3, but in the bowl 6 of the assembly 2 added onto the body 1. To maintain the tablet(s) 12 in this bowl 6, a component 20 ha$ been provided, and this is pushed into the bowl, clamping the tablets. This component 20 is shown in perspective in FIG. 6. It can be seen that it has skirts 21, 22 in the form of cylindrical walls which extend vertically so as to match the vertical walls of the bowl 6, but only of a limited region of the latter, while passages or orifices 23, 24, 25 are also provided to permit subsequent diffusion of the active products into the washing bath. In its upper part, the component 20 also comprises two recesses 26, opposite each other, which makes it easier to grasp this component. FIG. 4 clearly shows the location of the device when the component 20 is placed in position and pushed into the bowl 6. This same arrangement appears in cross-section in FIG. 5, where two tablets 12 housed in the bowl 6 can also be seen.
FIG. 7 illustrates a tablet which may be employed in any one of the above-mentioned devices, and also in those which will be illustrated later. A tablet of this kind may be obtained directly by compacting a substance which has an activity in the washing process, for example an inorganic compound such as a peroxygen compound, especially sodium perborate. However, it is also possible to use constituents with a specific function which are themselves not capable of forming a tablet and which must therefore be incorporated in a matrix or carrier which can dissolve under the washing conditions. This matrix may, for example, consist of calcium bicarbonate. Alternatively, the faces of the tablets may also be coated with a substance which is impervious to the aqueous medium, so that the progressive dissolution of the tablet takes place not via its main faces, but via its narrow section, and this can ensure a slower dissolution, which may be desirable in certain cases in order to ensure a predetermined sequence in the washing cycle.
FIG. 8 illustrates an alternative form of a device according to which tablets or gelatin capsules are simply housed in the compartments arranged in the bowl 6. FIG. 9 which is a top view of the bowl 6 and of the central opening 7, shows that a crescent-shaped partition 27 extends across the bowl to form, together with radial partitions 28 and 29, housings into which tablets or gelatin capsules 12 can be inserted.
FIG. 10 illustrates an alternative form according to which the partitions 27, 28, and 29 are replaced by cylindrical walls 31, 32, 33 which from corresponding cells in which stick-shaped tablets or gelatin capsules 30 can be housed.
FIG. 11 shows a device comprising a tablet 12 which is housed in the bottom of the bowl 6. To hold the tablet 12 in place, an annular rib 34 has simply been provided inside the bowl 6. To place the tablet 12 in position it suffices to push the latter into the bowl and the tablet is then held by its upper part. The rib 34 does not need to be continuous. It is sufficient for the wall 6 to comprise projections which act as stops when the tablet has been pushed in. Since all the components in question are made of plastic, the flexibility of the walls and ribs allows the tablets or gelatin capsules to be placed in position without any difficulty.
The devices illustrated in FIGS. 1 to 11 are of the type comprising an open shaft 9 descending inside of body 1, but this is not obligatory in any manner, as will be described with reference to FIGS. 12 and 13, if this open shaft is not employed for placing the solid product 12.
FIG. 12 shows a device of the type comprising a lid 35 screwed onto the body 1 by means of additional threading 36. In this alternative form, it is the lid 35 which comprises a cylindrical wall 37 which makes it possible to form a housing inside which a tablet 12 can be housed.
FIG. 13 illustrates a device without an open shaft, but comprising, for the purpose of the present invention, on at least a part of its peripheral surface, a wall 38 provided with openings 40 and capable of being closed with a removable lid 39. Active constituents for the washing, presented in the form of tablets, gelatin capsules, sachets and any other similar forms can be housed in the housing 41 formed between the wall 38 and the outer surface of the body 1.
FIG. 14 illustrates a device which is distinguished in that the open shaft 9 is limited by a wall 14 and that the lower part of the body 1 is arranged to form a housing 42 capable of receiving tablets 12, which may be held in place therein by annular ribs such as 43.
Shown diagrammatically in FIG. 15 is an arrangement of an open shaft 9 according to which a diametral partition 44 extends inside the open shaft, to form two cylindrical compartments 45, 46, semicircular in section. Compartment 45 is the only one to communicate with the part of the device corresponding to the bowl 6, where the liquid detergent enters the device and diffuses during the washing. The other compartment 46, is not in communication with the liquid and may house at least one tablet 12 and/or one sachet 15, as shown.
The cylindrical wall 47 of the open shaft 9 delimiting the compartment 46 is generally continuous, while the compartment 45 has openings 9, as indicated earlier.
FIG. 16 illustrates another alternative form of an open shaft 9 comprising an outer cylindrical part 49 provided with orifices 19, which is made to communicate with the bowl 6 for filing and diffusion of the liquid detergent composition, and an internal part 50, delimited by a cylindrical wall 48 with a circular base. The part 50 can receive at least one tablet 12 and/or one sachet 15, as shown. This part 50 is thus separated from the part of the device which is intended to contain the liquid detergent composition.
It can be seen, therefore, that the process of the invention can be implemented with a very wide variety of devices, of which solely illustrative examples have been given above.
The description which follows gives concrete examples of the use of the process for the invention with a device of the kind illustrated in FIGS. 1 to 16.
In these examples, the same single basic liquid detergent composition is employed, and is introduced into the device at a rate of a dose of approximately 180 g. This composition is the following:
______________________________________Ingredients % by weight______________________________________Dodecenylsuccinic acid 12Dodecylbenzenesulphonic acid 12Alkylsulphonic acid 4C.sub.12 --C.sub.16 fatty alcohols - 7 moles of ethylene 16oxide per mole of alcoholCitric acid 1Protease (Maxatease R) - (1.5 AU/g) 0.9Amylase (Maxamyl R) - (300,000 KNU/g) 0.2Phosphonic acid 0.8Ethanol 8Minor constituents such as optical brightening agent, foamregulator based on a silicone emulsion, colorant, perfume,opacifier.Water Remainder to 100______________________________________
In accordance with the invention, at least one additive performing a specific function is associated with this basic liquid detergent composition. In what follows, concrete examples of the said additives are given, their percentage being shown as equivalent by weight relative to the basic liquid detergent composition. The actual weights of the solid product will vary according to the active concentrations of the additives or of the active constituents which they contain. It is clear that the physical form: gelatin capsules, tablets, sachets, and the like, must be taken into consideration in order to provide the appropriate quantity of additives which will be shown.
The description which follows lists certain additives, together with their specific function.
A. For better protection of the internal parts of the washing machine (new or worn machine):
1% of sodium silicates - immediate suspension.
B. For "renovating" worn or "pearled" cotton textiles. Improvement in the general appearance and softness of fabrics:
5% of cellulose-based enzymes - immediate dissolution.
C. For a softening action on fabrics:
5% of cellulose-based enzymes +0.2% of clay.
D. For better grease stain removal:
0.2% of enzymes (amylase) +1.2% of polyoxyethylene/polyoxypropyleneterephtlalate +3% of sodium laurylsulphate +3% of concentrated nonionic surfactant (Zoharex N.25 from Zoher, for example) +2% of soiling suspending agent (zeolites or polyacrylates) - immediate dissolution.
E. For better "oxidizable" soiling stain removal and superior whiteness on cottons:
14% of sodium perborate +4% TAED +0.5% diethylenetriaminepentamethylenephosphonic acid.
F. For a superior "brightness" of fabrics (improved bleaching):
2% of citric acid +0.2% of optical brightening agent (Stilbene type).
It will be noted that, in accordance with the process of the invention, a fabric wash with options can be carried out by employing one or more of the above-mentioned additives, in combination with the basic liquid detergent composition. It is obviously possible to combine the benefits of the constituents having specific function which are used separately from the said composition. For example in the case where the fabrics to be washed are worn and very dirty, a combination of additives A+C+D+E+F may be employed. It is also known that the process of the invention makes it possible to make the said additives available at predetermined times during the washing cycle, for example in some cases by exploiting their immediate action as soon as washing has commenced and, on the other hand, in the case of others, their delayed action (peroxygen compounds, softeners).
Practical machine washing trials carried out in accordance with the process of the invention have shown that this washing with options was being performed in an optimum manner, using very simple means.
In the above illustrative examples, the use of the process of the invention has been referred to essentially with a basic liquid detergent composition and separate components, but it will be understood that the process of the invention can be applied in the same manner to a basic detergent composition presented in a granular form. Although the detailed description given above illustrated a certain number of embodiments of devices to carry out the process of the invention, modifications or alternative forms can be employed by persons skilled in the art without departing from the scope of the present invention.
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A device comprising unoccluded vents and containing a detergent is employed. This device is placed with fabrics to be washed in the drum of a washing machine and the machine is started up, allowing the washing cycle to proceed. A detergent composition some of whose constituents are separate is employed and at least one of the constituents is introduced into the device and at least one other of the constituents is associated separately with the said device, so that during the washing all the constituents diffuse into the fabrics and the washing bath.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This technology relates to oil and gas wells, and in particular to pipe connectors within the wells.
2. Brief Description of Related Art
Typical oil and gas wells include strings of pipe that extend into the well in conjunction with drilling, casing, and production operations. These strings of pipe generally consist of discrete pipe segments that are joined together by pipe connectors as the pipe is run into the well. The pipe connectors may be threaded, with adjacent connectors having male and female threads configured to engage and join the pipe. Generally, the pipe end having the male thread is known as the pin, and the pipe end having the female thread is known as the box. When joining the pipe segments, it is desirable to limit circumferential movement between the connectors so that the connectors remain firmly attached. To limit such circumferential movement, a lock key may be employed.
Some known lock keys require corresponding grooves in the pin and the box that align when the pin and the box are threaded together. The key is then inserted into the aligned grooves to prevent relative circumferential movement between the pin and the box. However, many pipe connectors that are threaded together cannot be repeatedly assembled to the same relative angle to each other due to manufacturing variations in the thread, as well as changes to the thread of connectors previously used under load. This is because the pipe connectors must be fully torqued to ensure that the joint properly seals, regardless of the relative positions of the locking grooves on the pin and box.
Additionally, some threaded connectors have small overall wall thickness (e.g., subsea drill pipe and casing), thereby requiring a key that is low profile. Furthermore, under some circumstances there is not enough space surrounding the pipe connectors to incorporate large external mechanisms to drive locking pins or keys into place, as required for many types of locking keys.
SUMMARY OF THE INVENTION
Disclosed herein is a system for locking adjacent pipe connectors. In an example, the system includes a first pipe connector, or box, a second pipe connector, or pin, and a locking key. The first and second pipe connectors have male and female connecting ends, and are configured to thread together. Either the first pipe connector or the second pipe connector has a recess in its connecting end, and the locking key is inserted into the recess to prevent further relative circumferential movement between the first and second pipe connectors.
In this example, the key includes inner and outer surfaces. When the key is inserted into the recess, the inner surface is positioned radially inward, and the outer surface is positioned radially outward relative to the pipe connectors. The key also includes upper and lower surfaces. The upper surface and the lower surface extend from the inner surface to the outer surface. The key also includes locking protrusions positioned on at least the lower surface. In some embodiments, these locking protrusions are ridges that are pressed into, and become embedded in the first or second pipe connectors when the key is inserted into the recess. In other embodiments, some of the locking protrusions may be splines that correspond to notches or grooves in the first or second pipe connectors and are received by the notches when the key is inserted. In either instance, the locking protrusions prevent relative circumferential movement of the pipe connectors.
Also disclosed herein is a method of locking adjacent threaded pipe connectors to prevent relative rotational movement between the pipe connectors. The pipe connectors have threaded male and female connecting ends. In addition, the end of one of the pipe connectors has a recess. According to the method, the pipe connectors are first threaded together. Then, a key is radially inserted into the recess. The key has locking protrusions, as described above, to prevent relative circumferential movement of the pipe connectors.
BRIEF DESCRIPTION OF THE DRAWINGS
The present technology will be better understood on reading the following detailed description of nonlimiting embodiments thereof, and on examining the accompanying drawings, in which:
FIG. 1 is a perspective view of a pipe connector locking system having a key according to an example embodiment of the present technology;
FIG. 2A is an enlarged sectional view of a portion of the connector locking system of FIG. 1 , with a key disengaged from pipe connectors;
FIG. 2B is an enlarged sectional view of a portion of the connector locking system of FIG. 1 , with a key inserted between pipe connectors;
FIG. 2C is an enlarged sectional side view of a portion of the connector locking system of FIG. 1 , with a key disengaged from pipe connectors;
FIG. 2D is a perspective view of the key according to one embodiment of the present technology;
FIG. 3A is an enlarged sectional view of a portion of the connector locking system according to another embodiment of the present technology, with the key disengaged from the pipe connectors;
FIG. 3B is an enlarged sectional view of a portion of the connector locking system of FIG. 3A , with the key inserted between the pipe connectors;
FIG. 3C is a perspective view of a key according to an alternate embodiment of the present technology.
FIG. 4A is an enlarged exploded sectional view of a portion of an alternate embodiment of the connector locking system according to an embodiment of the present technology;
FIG. 4B is an enlarged side view of a portion of the connector locking system of FIG. 4A , with the key inserted between the pipe connectors;
FIG. 4C is an outer perspective view of a key according to an embodiment of the present technology; and
FIG. 4D is an inner perspective view of the key of FIG. 4C .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The foregoing aspects, features, and advantages of the present technology will be further appreciated when considered with reference to the following description of preferred embodiments and accompanying drawings, wherein like reference numerals represent like elements. In describing the preferred embodiments of the technology illustrated in the appended drawings, specific terminology will be used for the sake of clarity. However, the technology is not intended to be limited to the specific terms used, and it is to be understood that each specific term includes equivalents that operate in a similar manner to accomplish a similar purpose.
FIG. 1 is a perspective view of one example of a pipe connector locking system 10 according to the present technology, including a first pipe connector 12 , a second pipe connector 14 , and a key 16 . The first and second pipe connectors 12 , 14 are configured to engage one another and become attached. For example, the first pipe connector 12 may be a male pipe connector, or pin, having external threads (not shown), and the second pipe connector 14 may be a female pipe connector, or box, having internal threads (not shown). In such an embodiment, the first pipe connector 12 may engage the second pipe connector 14 by connecting the threaded end of the first pipe connector 12 with the threaded end of the second pipe connector 14 , and rotating the pipe connectors 12 , 14 relative to one another until the threads are engaged. When the threads are fully engaged, an external annular shoulder 13 of first pipe connector 12 abuts an external annular shoulder 15 of second pipe connector. With the threads engaged, and the pipe connectors 12 , 14 attached, the key 16 may be inserted between shoulders 13 , 15 of the first and second pipe connectors 12 , 14 to limit or substantially prevent relative circumferential movement between the pipe connectors 12 , 14 . In this embodiment, the key 16 may include a material that is harder than the material of first and second pipe connectors 12 , 14 .
The structure and function of the key 16 is shown in detail in FIGS. 2A-2D . For example, the key 16 has an inner surface 18 (best shown in FIGS. 2C and 2D ), and an outer surface 20 . The inner surface 18 may be configured so that, upon insertion between the first and second pipe connectors 12 , 14 , it is positioned radially inward from the outer surface 20 . The key 16 also has an upper surface 22 and a lower surface 24 (best shown in FIGS. 2C and 2D ). In some embodiments, the upper surface 22 may be tapered axially upward relative to the pipe connectors 12 , 14 from the inner surface 18 to the outer surface 20 . Similarly, the lower surface 24 may be tapered axially downward relative to the pipe connectors 12 , 14 . Thus, the thickness the distance between upper and lower surfaces 22 , 24 ) increases with distance from the inner surface 18 . In the embodiment of FIGS. 2A-2D , the key 16 include locking ridges 26 protruding therefrom and extending radially from the inner surface 18 to the outer surface 20 of the key 16 . Locking ridges 26 each have a generally triangular cross-section with opposing lateral sides that depend towards one another and join a distance from the main body to form a peak. In an example, the key 16 is an elongate member and is set lengthwise along a portion of a circumference of an interface between the first and second connectors 12 , 14 .
FIGS. 2A and 2C further show a recess 28 in shoulder 13 of the first pipe connector 12 . The recess 28 has outer edges 46 . Although the recess 28 is shown in the first pipe connector 12 , it may alternately be located in the second pipe connector 14 . As best shown in FIG. 2C , the height of the recess 28 is greater than or equal to the height of the inner surface 18 of the key 16 , but smaller than the height of the outer surface 20 of the key 16 . Thus, when the key 16 is inserted into the recess, the inner surface 18 of the key 16 initially enters the recess, but the locking ridges 26 on the tapered upper and lower surfaces 22 , 24 of the key 16 contact the edge 46 of the recess 28 and the outer surface of the adjacent pipe connector, and resist further entry of the key 16 into the recess 28 . The position of the recess 28 entirely in one pipe connector is advantageous because it allows use of the key 16 regardless of the relative circumferential positions of the pipe connectors when they are fully joined, thereby allowing for clocking independence.
To complete insertion of the key 16 into the recess 28 , an external force may be applied to the outer surface 20 of the key 16 . For example, the key 16 may be pressed into the recess 28 using a press tool, or hammered in with hand tools. Because the material of the key 16 is harder than the material of the first and second pipe connectors 12 , 14 , the locking ridges 26 become embedded in shoulders 13 , 15 of the first and second pipe connectors 12 , 14 as the key 16 is driven into the recess 28 . Thus, when fully inserted, the ridges 26 of the key are engaged with, and may be embedded in, the first and second pipe connectors 12 , 14 , as shown in FIG. 2B . Thus embedded, the locking ridges 26 prevent relative rotational movement between the first and second pipe connectors 12 , 14 . Furthermore, the key 16 will act bi-directionally, preventing both over-tightening and un-tightening of the pipe connectors 12 , 14 .
In an alternate embodiment, a portion of the outer edge 46 of the recess 28 may have pre-cut grooves (not shown) configured to accept some of the locking ridges 26 . In such an embodiment, the number of locking ridges 26 that become embedded in the first or second pipe connectors 12 , 14 would be reduced, thereby reducing the amount of force required to press the key 16 into the recess 28 . The key 16 may be removed using a specialty tool or hand tools, for example, by inserting a screw driver or pry bar into a notched area 42 at either end of the key 16 . The ability to insert and remove the key 16 using hand tools or other small tools is advantageous because it allows use of the key 16 in circumstances where there is little space surrounding the pipe connectors 12 , 14 , a circumstance that tends to limit or prevent the use of large external pressing mechanisms or removal tools.
Referring to FIG. 2B , there are shown optional fasteners 30 that may be inserted into the surface of the first pipe connector 12 . The fasteners may be, for example, screws or bolts, each with threaded elongate shafts and a larger diameter head attached to an end of the shaft. The fasteners 30 are positioned so that a portion of the head of each fastener 30 overlaps a portion of the key 16 . Thus, the fasteners 30 may help to secure the key 16 radially relative to the pipe connectors 12 , 14 , thereby preventing the key 16 from backing out due to, for example, vibrations, or torsional loads. In the embodiments shown, the fasteners are inserted into holes 32 (shown in FIG. 2A ) in the first pipe connector 12 . Use of screws or other fasteners may be beneficial to prevent debris from entering removal notch areas 42 . In addition, the fasteners may double as anchors for attaching a press tool (for pressing the key 16 into the recess) using external bolts or screws.
Optionally, the fasteners 30 may be countersunk, so that the heads of the fasteners 30 do not protrude beyond the surface of the first pipe connector 12 when the fasteners 30 are fully inserted into the holes 32 . Thus, a countersink 40 may be drilled or otherwise bored into the surface of the first pipe connector 12 and a portion of the key 16 , In certain embodiments, the heads of the fasteners 30 may be configured to accept a fastener insertion tool, such as, for example, a screwdriver, or a hexagonal alien wrench. For example, the fasteners 30 of the present technology are shown to have hexagonal sockets 34 for accepting such an alien wrench. In an embodiment where the recess 28 is in the second pipe connector 14 , the fasteners 30 may correspondingly be inserted into the second pipe connector 14 , rather than the first pipe connector 12 . In such an embodiment, the holes 32 and countersinks 40 would also be drilled into the second pipe connector 14 . Although the fasteners shown in FIG. 2B are bolts, any appropriate mechanism may be used to retain the key 16 radially in place relative to the first and second pipe connectors 12 , 14 . For example, the key 16 could be retained using flexible tabs, clips, spring mechanisms, or any other appropriate mechanism. In addition, any number of fasteners or retaining mechanisms could be used, including a single fastener or retaining mechanism.
Referring now to FIGS. 3A-3C , there is shown an alternate embodiment of the present technology, including a first pipe connector 112 , a second pipe connector 114 , and a key 116 . The key 116 has an inner surface 118 , an outer surface 120 , an upper surface 122 , and a tapered lower surface 124 . The inner surface 118 may be configured so that, upon insertion between the first and second pipe connectors 112 , 114 , it is positioned radially inward relative to outer surface 120 . Conversely, the outer surface 120 may be configured so that, upon insertion between the first and second pipe connectors 112 , 114 , it is positioned radially outward from inner surface 110 . The lower surface 124 may be tapered axially downward relative to the pipe connectors 112 , 114 . In addition, the key 116 includes locking ridges 126 protruding from the lower surface 124 and extending radially from the inner surface 118 to the outer surface 120 . Furthermore, in the embodiment of FIGS. 3A-3C , the first pipe connector 112 has a recess 128 configured to at least partially accept the key 116 , and holes 132 for accepting fasteners 130 . The recess 128 has notches 136 in the upper surface thereof which may be pre-machined into the pipe connector. Notches 136 extend radially into connector 112 and have generally rectangular outer peripheries.
In the embodiment of FIGS. 3A-3C , the upper surface 122 of the key 116 has rectangular splines 138 with rectangular outer peripheries that extend transverse to the elongate side of the key 116 , so that when the key 116 is inserted into the recess 128 , the rectangular splines 138 are received by the notches 136 . The locking ridges 126 of the bottom surface 124 contact, and become embedded into, the second pipe connector 114 when the key 116 is pressed into the recess 128 , as described above. A fully inserted key 116 , according to this embodiment, is shown in FIG. 3B . Thus configured, with the key 116 fully inserted, the first and second pipe connectors 112 , 114 are restrained from rotating relative to one another. One advantage of the key 116 , is that it will act bi-directionally, preventing both over-tightening and un-tightening of the pipe connectors 112 , 114 , The key 116 may be removed using a specialty tool or hand tools, for example, by inserting a screw driver or pry bar into a notched area 142 at either end of the key 116 .
It is to be understood that variations of the embodiment shown in FIGS. 3A-3C are also contemplated. For example, the recess 128 could be in the second pipe connector 114 instead of the first pipe connector 112 , as shown. Alternately, the rectangular splines 138 could be positioned on the bottom surface 124 of the key, and the locking ridges 126 on the top surface 122 . In such an embodiment, the notches 136 of the recess 128 would be cut into the portion of the second pipe connector 114 adjacent to the recess 128 .
Referring to FIG. 3B , there are shown optional fasteners 130 that may be inserted into the surface of the first pipe connector 112 . The fasteners may be, for example, screws or bolts. The fasteners 130 are positioned so that a portion of the head of each fastener 130 overlaps a portion of the key 116 . Thus, the fasteners 130 may help to secure the key 116 radially relative to the pipe connectors 112 , 114 , thereby preventing the key 116 from backing out due to, for example, vibrations, or torsional loads. In the embodiments shown, the fasteners 130 are inserted into holes 132 (shown in FIG. 3A ) in the first pipe connector 112 . Use of screws of other fasteners may be beneficial to prevent debris from entering removal notch areas 142 . In addition, the fasteners may double as anchors for attaching a press tool (for pressing the key 116 into the recess) using external bolts or screws.
Optionally, the fasteners 130 may be countersunk, so that the heads of the fasteners 130 do not protrude beyond the surface of the first pipe connector 112 when the fasteners 130 are fully inserted into the holes 132 . Thus, a countersink 140 may be drilled or otherwise bored into the surface of the first pipe connector 112 and a portion of the key 116 . In certain embodiments, the heads of the fasteners 130 may be configured to accept a fastener insertion tool, such as, for example, a screwdriver, or a hexagonal alien wrench. For example, the fasteners 130 of the present technology are shown to have hexagonal sockets 134 for accepting such an alien wrench. In an embodiment where the recess 128 is in the second pipe connector 114 , the fasteners 130 would correspondingly be inserted into the second pipe connector 114 , rather than the first pipe connector 112 . In such an embodiment, the holes 132 and countersinks 140 would also be drilled into the second pipe connector 114 . Although the fasteners shown in FIG. 3B are bolts, any appropriate mechanism may be used to retain the key 116 radially in place relative to the first and second pipe connectors 112 , 114 . For example, the key 116 could be retained using flexible tabs, clips, spring mechanisms, or any other appropriate mechanism. In addition, any number of fasteners or retaining mechanisms could be used, including a single fastener or retaining mechanism.
Referring now to FIGS. 4A-4D , there is shown another embodiment of the present technology, including a first pipe connector 212 , a second pipe connector 214 , and a key 216 . The key 216 has an inner surface 218 , an outer surface 220 , an upper surface 222 , and a tapered lower surface 224 . The inner surface 218 may be configured so that, upon insertion between the first and second pipe connectors 212 , 214 , it is positioned radially inward relative to the pipe connectors 212 , 214 . Conversely, the outer surface 220 may be configured so that, upon insertion between the first and second pipe connectors 212 , 214 , it is positioned radially outward relative to the pipe connectors 212 , 214 . The tower surface 224 may be tapered axially downward relative to the pipe connectors 212 , 214 . In addition, the key 216 includes locking ridges 226 protruding from the lower surface 224 and extending radially from the inner surface 218 to the outer surface 220 , Furthermore, in the embodiment of FIGS. 4A-4D , the first pipe connector 212 has a recess 228 configured to at least partially accept the key 216 , and holes 232 for accepting fasteners 230 . The recess has grooves 236 in the upper surface thereof which may be pre-machined into the pipe connector.
In the embodiment of FIGS. 4A-4D , the upper surface 222 of the key 216 has radially extending splines 238 , each with an upper surface that is curved about an axis of each spline 238 . Splines 238 are positioned so that when the key 216 is inserted into the recess 228 , the curved splines 238 are received by the grooves 236 . Splines 238 have ridges shown extending radially from the front surface 220 to the rear surface 218 . The locking ridges 226 of the bottom surface 224 contact, and become embedded into, the second pipe connector 214 when the key 216 is pressed into the recess 228 , as described above. A fully inserted key 216 , according to this embodiment, is shown in FIG. 4B . Thus configured, with the key 216 fully inserted, the first and second pipe connectors 212 , 214 are restrained from rotating relative to one another.
One advantage to the key 216 , is that it will act hi-directionally, preventing both over-tightening and un-tightening of the pipe connectors 212 , 214 . Moreover, the curved splines 238 can be either symmetric, as shown in FIGS. 4A, 4C, and 4D , or asymmetric, as shown in FIG. 4B . If symmetric, the curved splines 238 will have a substantially equal capacity to prevent relative circumferential rotation of the pipe connectors 212 , 214 in both directions. If asymmetric, the curved splines 238 will have additional load bearing capacity in one direction, depending on the orientation of the curved splines 238 . Another advantage to the key 216 having curved splines 238 , is that as the surfaces of the curved splines absorb the forces F (shown in FIG. 4B ) exerted on the key 216 by the first pipe connector 212 , the locking ridges 226 are driven deeper into the second pipe connector 214 . Accordingly, the ability of the key 216 to prevent relative circumferential rotation between the pipe connectors 21 214 is increased. The key 216 may be removed using a specialty tool or hand tools, for example, by inserting a screw driver or pry bar into a notched area 242 at either end of the key 216 .
It is to be understood that variations of the embodiment shown in FIGS. 4A-4D are also contemplated. For example, the recess 128 could be in the second pipe connector 214 instead of the first pipe connector 212 , as shown. Alternately, the curved splines 238 could be positioned on the bottom surface 224 of the key, and the locking ridges 226 on the top surface 222 . In such an embodiment, the grooves 236 of the recess 228 would be cut into the portion of the second pipe connector 214 adjacent to the recess 228 .
Referring to FIG. 4A , there are shown optional fasteners 230 that may be inserted into the surface of the first pipe connector 212 . The fasteners may be, for example, screws or bolts. The fasteners 230 are positioned so that a portion of the head of each fastener 230 overlaps a portion of the key 216 when installed in recess 228 . Thus, the fasteners 230 may help to secure the key 216 radially relative to the pipe connectors 212 , 214 , thereby preventing the key 216 from hacking out due to, for example, vibrations, or torsional loads. In the embodiments shown, the fasteners 230 are inserted into holes 232 (shown in FIG. 4A ) in the first pipe connector 212 . In certain embodiments, the heads of the fasteners 230 may be configured to accept a fastener insertion tool, such as, for example, a screwdriver, or a hexagonal allen wrench. For example, the fasteners 230 of the present technology are shown to have hexagonal sockets 234 for accepting such an alien wrench. Use of screws or other fasteners may be beneficial to prevent debris from entering removal notch areas 242 . In addition, the fasteners may double as anchors for attaching a press tool (for pressing the key 216 into the recess) using external bolts or screws.
Optionally, the fasteners 230 may be countersunk, so that the heads of the fasteners 230 do not protrude beyond the surface of the first pipe connector 212 when the fasteners 230 are fully inserted into the holes 232 . Thus, a countersink 240 may be drilled or otherwise bored into the surface of the first pipe connector 212 and a portion of the key 216 . Alternatively, the key 216 may include a flat retaining surface 244 instead of a curved countersink. Such a flat retaining surface 244 allows the fastener 230 to be recessed relative to the surface of the pipe connector, while at the same time allowing the key 216 to move slightly relative to the second pipe connector 214 , thereby increasing drive pressure and capacity of the locking ridges 226 .
In an embodiment where the recess 228 is in the second pipe connector 214 , the fasteners 230 would correspondingly be inserted into the second pipe connector 214 , rather than the first pipe connector 212 . In such an embodiment, the holes 232 and countersinks 240 would also be drilled into the second pipe connector 214 . Although the fasteners shown in FIG. 4B are bolts, any appropriate mechanism may be used to retain the key 216 radially in place relative to the first and second pipe connectors 212 , 214 . For example, the key 216 could be retained using flexible tabs, clips, spring mechanisms, or any other appropriate mechanism, In addition, any number of fasteners or retaining mechanisms could be used, including a single fastener or retaining mechanism.
Providing multiple locking ridges 26 , 126 , 226 or splines 138 , 238 on both the upper 22 , 122 , 222 and lower 24 , 124 , 224 surfaces of the key 16 , 116 , 216 is advantageous because such a structure helps to prevent unintentional decoupling of the first 12 , 112 , 212 and second 14 , 114 , 214 pipe connectors. Furthermore, such a structure allows the key 16 , 116 , 216 to be low profile because the bearing and shear areas that transfer the load across the key 16 , 116 , 216 are distributed across all the locking ridges 26 , 126 , 226 and/or splines 138 , 238 . Thus, the key 16 , 116 , 216 of the present technology is compatible with very low profile connectors.
While the technology has been shown or described in only some of its forms, it should be apparent to those skilled in the art that it is not so limited, but is susceptible to various changes without departing from the scope of the invention. Furthermore, it is to be understood that the above disclosed embodiments are merely illustrative of the principles and applications of the present invention. Accordingly, numerous modifications may be made to the illustrative embodiments and other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims.
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A system for joining pipe segments, the system including a first pipe connector connected to a first pipe segment, and a second pipe connector threadingly connectable to the first pipe connector, and connected to a second pipe segment. The system further includes a recess in the outer surface of the first pipe connector, and an elongated key having first and second lengthwise surfaces. One of the lengthwise surfaces has protrusions that embed into a transverse surface of the second pipe connector when the key is mounted into the recess. The thickness of the key decreases with distance radially inward from the outer surface.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The invention described herein is related to commonly assigned U.S. Patent application Ser. No. 888,701 filed Mar. 21, 1978 on Apparatus For Remotely Repairing Tubes In A Steam Generator by L. R. Golick; commonly assigned copending patent application Ser. No. 952,431 on A Method And Apparatus For Servicing A Steam Generator by Cooper and Castner, filed concurrently herewith; and commonly assigned copending U.S. Patent application Ser. No. 952,430 on Heat Exchanger Tube And Tubesheet Location Sensing Device And Method by Gerkey, Castner and Stiller, also filed concurrently herewith.
BACKGROUND OF THE INVENTION
This invention relates to nuclear steam generators and more particularly to a method and apparatus for set-up of a particular piece of equipment as disclosed in copending commonly assigned U.S. Patent application Ser. No. 888,701 filed Mar. 21, 1978 of L. R. Gollick directed to apparatus for remotely repairing tubes and/or the tube sheet in such a nuclear steam generator.
In pressurized water nuclear reactors primary fluid or coolant is pumped through a reactor and a steam generator, radioactive contaminants in the primary fluid are deposited on the tubes and in the channel head of the steam generator so that repair crews are subjected to significant radioactivity when working within the channel head. Therefore, in behalf of minimizing the exposure of personnel to radiation, apparatus and equipment of the type disclosed in the aforementioned copending patent application has been devised for inspection and repair of the tubes and the tube sheet within the steam generator under remote control, and in a manner as set forth in a copending patent application Ser. No. 952,431. It becomes important, in view of such minimal radiation exposure desirability, to provide for set-up of such equipment in minimal time, and to this the method and apparatus of the present invention is directed.
SUMMARY OF THE INVENTION
The method and apparatus of the present invention provides for rapid installation of a rotary support block member in the bottom spherical wall adjacent to the divider plate at the interior of the channel head of a nuclear steam generator undergoing tube repair. Which rotary bottom support member is intended for the lower-most end of a vertical column embodied in the tube repair apparatus of the aforementioned patent application Ser. No. 888,701. The present invention also involves installation of an anchor or pillow block member on the divider plate within the channel head adapted to accommodate attachment of a rotary column guide bracket at a selected vertical sight above the bottom support member for the column of the tube repair apparatus. On behalf of assuring trouble-free performance of the tube repair apparatus it becomes important that the bottom support bearing block member on the bottom wall of the channel head and the anchor block member on the divider plate be accurately positioned to provide for alignment of the column of the tube repair apparatus in an attitude of perpendicularity with respect to the tube-sheet in which the tubes undergoing repair are affiliated. To accomplish this in minimal time the apparatus in the method of the present invention determines and indicates the extent that the undersurface of the tube sheet is tilted from the horizontal by use of a special instrument introduced to the underside of the tube sheet and which includes a pair of commercially available inclinometers that give degree of tilt information in two mutually perpendicular directions readable via pick-off wires and a display at the exterior of the channel head.
Using a plumb-bob fixture that is adapted to be accurately positioned with respect to a specific hole in the tube sheet, a center punch mark is made on the bottom spherical wall of the channel head directly beneath the chosen hole sight.
By use of a center layouts template placed over the plumb-bob point on the bottom wall of the channel head locating marks for a positioning jig can be made on such bottom wall.
A positioning jig for the location of the bottom column bearing block is then placed on the bottom wall of the channel head in accord with such markings and tack-welded in place; the bottom column-bearing rotary-support block is then placed in the center of the positioning jig and centered by use of adjusting screws affiliated with such jig.
The bottom end of a vertical aligning post is then introduced into the bottom bearing block and locating pins at the top of the post are introduced into preselected holes in the bottom tube sheet by use of a hydraulic hand pump affiliated with such post to locate the upper end of the post in a selected site in the bottom of the tube sheet.
By use of a pair of inclinometers affiliated with the locating post and the adjusting screws on the positioning jig the bottom of the post can be moved in selected directions until accord is reached between the output of the aligning post inclinometers and the previous inclinometer output of the tilt determining instrument.
By application of additional pressure through use of the previously mentioned hydraulic hand pump, the bottom of the post can be made to introduce sufficient force to hold the bottom bearing block in place while it is then being welded to the bottom wall of the channel head.
Monitoring of the readings of the inclinometers on the post while performing such welding, together with utilizing a sequence welding technique, assures that the desired alignment of the post will not be disturbed during the welding of the bottom bearing block.
By use of a spring bias fixture mounted at a selected vertical location on the aligning post, the anchor block is positioned on the divider plate and held by spring pressure in position while being welded to such plate.
By use of a shim of selected size and proximity sensing heads disposed in a simulated rotary column guide bracket on the post, the gap between such simulated rotary column giode bracket and the anchor block welded to the divider plate can be determined with a high degree of accuracy.
By use of the hydraulic cylinder at the top of the column the aligning pins can be withdrawn from the locating holes in the tube sheet, the simulated rotary guide bracket on the post can be disconnected from the anchor block on the channel head by the simple withdrawal of a pair of coupling pins, and the aligning post assembly removed from the channel head by way of the usual manhole affiliated with such head.
The vertical column of the tube repairing apparatus can then be introduced through the manhole, its bottom end inserted into the bottom bearing block on the bottom of the channel head and the real rotary guide bracket for the column secured to the anchor block by reinsertion of the coupling pins and adjustment made for affecting precise alignment of such column perpendicularly with respect to the bottom of the tube sheet and along a selected rotary axis by introduction of a proper size shim between the anchor block and the guide bracket chosen in accord with information derived by the previous measurement of the clearance between the simulated bracket member and such anchor block.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a vertical sectional view of a portion of a channel head of a steam generator with the tube and tube sheet reparing apparatus of copending patent application Ser. No. 888,701 disposed in working attitude therein;
FIGS. 2 and 3 are top and side views, respectively of the tilt measuring instrument utilized in the present invention;
FIG. 4 is a elevation view of a plumb-bob device utilized in the invention of the present application;
FIG. 5 is a plan view of a template used in the present invention;
FIG. 6 is a plan view of a positioning jig utilized in the present invention;
FIG. 7 is a vertical view of an aligning post assembly disposed in the steam generator channel head adjacent to the divider plate for location of the bottom column-bearing rotary support block and anchor block for the tube repairing apparatus of the aforementioned copending patent application Ser. No. 888,701, used in the present invention;
FIG. 8 is a plan view showing details of the simulated rotary column guide bracket affiliated with the alignment post and the rectangular anchor block affiliated with divider plate of the steam generator in which the present invention is utilized; and
FIG. 9 is a vertical section view showing details of a shim assembly involved in the gap measuring step of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, the present invention is concerned with installation of a bottom rotary support block 1 to the spherical bottom wall 2 of a channel head 3 of a nuclear steam generator and the location and attachment of an anchor block 4 to the divider plate 5 in such channel head beneath the bottom of the tube sheet 6 in which the terminal open ends of the vertical tubes 7 of the steam generator terminate. The bottom support block 1 and the side anchor block are utilized for alignment and support of a tube and tube sheet repairing apparatus 9 as shown in FIG. 1 and described in detail in aforementioned copending patent application Ser. No. 888,701 which apparatus utilizes a vertical column 10 supported at its lower end in the bottom bearing block 1 for rotation positioning by a motor 11 about a vertical axis 12 aligned with a particular tube hole in the tube sheet and extending perpendicularly from the bottom of such tube sheet by a rotary guide supbracket 13 removably attached to the anchor block 4. A horizontal boom 14 is pivotally carried at the top of the vertical column and supports a tool assembly 15 movable horizontally along the boom by way of a screw actuated carriage means 16. The boom is held in such horizontal position by a hydraulic cylinder assembly 17 operable to lower the boom to a retracted position adjacent to the column 10 and thereby realize a compacted state of the apparatus that affords its insertion and removal by way of the usual manway 18 affiliated with the channel head 3 of the steam generator. Removal of a pin 19 means affiliated with rotary guide bracket on the column provides for disconnection of the apparatus from the tube head.
The present invention is concerned with installation of the bottom bearing block 1 for the vertical column 10 of the tube repairing apparatus 9 and the anchor or pillow block 4 at one side of such column at a selected heighth thereon. It will be appreciated that, at such initial preparatory stage, the tube repair apparatus 9 depicted in FIG. 1 will be absent from the interior of the channel head as also will be the bottom support block 1 and the pillow block 4.
In accord with the present invention a worker or workers will enter the interior of the channel head 3 through the manway 18 and will use the tilt sensing instrument of FIGS. 2 and 3 to determine the degree of tilt of the bottom of the tube sheet 6 relative to the horizontal. Referring to FIGS. 2 and 3, the instrument is specifically adapted to this purpose and includes an inclinometer sensor means 20 adapted to feed signals to a digital readout located externally of the channel head by way of lead wires (not shown). The inclinometer sensor means 20 is capable of detecting the degree of tilt in mutually perpendicular directions in the horizontal plane and the instrument includes two pairs of horizontally spaced apart aligning pins 21 adapted for insertion in four tube holes opening downwardly from the bottom of the tube sheet. By proper selections of particular holes, the orientation of the instrument will be such that the tilt information derived from the inclinometer sensor means will be made with reference to a line extending centrally from and perpendicular to the divider plate 5. The instrument includes a horizontal arm 22 that carries such locating pins at its opposite ends as well as such inclinometer means at its midlength. The instrument also includes a pair of handles 23 to facilitate its manipulation during use and two pairs of pin-actuated interlock switch assemblies 24 at its opposite ends that operate to indicate when the arm of the instrument is parallel to the bottom surface of the tube sheet in the selected direction of extension of such arm. Each of the interlock switch assemblies includes an actuating pin 25 that has an end projecting upwardly from the top surface of the horizontal arm of the instrument and which is displaceable inwardly against the bias of a helical compression spring 26 by engagement with the undersurface of the tube sheet to actuate a microswitch 27 at the time a limit position defined by an annular shoulder 23 on the pin reaches its travel limit position. When the instrument is free of the tube sheet the extent of projection of the actuating pin is determined by a second annular stop surface 29 affiliated with the opposite end of such pin. The second annular stop surface may be formed in a removable part of the pin to accommodate assembly and disassembly.
The readings from the inclinometer tilt measuring instrument with respect to tilt of the tube sheet 6 in the x and y direction relative to the perpendicular line (not shown) extending from the divider plate 5 is noted and recorded for subsequent use.
By use of a plumb-bob 30, FIG. 4, aligned with a particular tube hole or location on the tube sheet, a punch mark is made on the bottom wall 2, FIG. 7, of the channel head. Plumb-bob 30 forms part of an assembly including a horizontal arm 31 and a locating pin assembly 32 extending above the upper surface of the arm and adapted for insertion in a particular tube hole in the tube sheet. Such assembly includes a rubber portion 33 squeezed between rigid members 34 and 35 in an axialwise direction by operation of a rocking level 36 via a tension member 37 to cause such rubber portion to expand radially into friction locking squeezed engagement with the inner wall of the respective opening. The lever has a camlike portion 38 affiliated with it to enable such squeezing action on the rubber member to be established or disestablished according to direction of turning of the leaver.
Following such punch marking of the vertical alignment from the tube sheet on the spherical bottom wall 2 of the channel head a template 40 such is depicted in FIG. 5 having a center hold 41 is brought into registry with the punch mark and location markings are made on the wall by use of suitable location-marking openings 42 in the template.
A rectangular, open frame positioning jig 44, FIGS. 6 and 7, is centered and located on the markings on the channel head wall 2 and tackwelded in place. The jig has two pairs of spaced apart screw-threaded lugs 45 extending from its upper surface which are aligned along two mutually perpendicular directions, x and y. One of which is perpendicular to the divider plate surface and the other of which is parallel to such surface; it being appreciated that the desirable alignment is arrived initially by proper orientation of the template that was used to obtain the markings from which such positioning jig was located.
A bottom bearing block 1 is then inserted into the jig 44 and centered therein on the wall 2 by adjusting screws 46.
The lower end of a vertically extending aligning post 50, FIG. 7, is then inserted into the bottom 1 bearing block and a locating pin means 51 affiliated with a locating assembly 52 at the top end of the aligning post is introduced into a selected tube hole in the tube sheet by operation of a hydraulic cylinder 53 affiliated with such locating assembly. A guide pin means 54 is affiliated with such locating assembly that operates to assure that the selected rotary aligned position of the locating pin means with respect to the tube sheet 6 and to the divider plate 5 will apply also to the aligning post assembly generally, so that an inclinometer means 55 mounted near the top of such aligning post will be properly aligned with respect to the divider plate 5 to give x and y tilting information relative to a line extending perpendicular to such divider plate. While monitoring the output readings of the inclinometers on the aligning post, the bottom thereof is moved in unison with the bearing block 1 by selective turning manipulation of the adjusting screws 46 affiliated with the positioning jig until the inclinometer readings coincide with the previous readings obtained from the inclinometer means of the tilt measuring instrument; it being appreciated that the inclinometer means affiliated with the aligning post is so arranged as to be responsive to tilting of the column in a generally-horizontal plane perpendicular to the central vertical axis of such post.
While applying additional pressure to the hydraulic cylinder 53 at the top of the column such as by the use of the hand pump (not shown) the bottom of the aligning post is made to hold the bottom bearing block 1 tightly in place on the bottom wall of the channel head. The adjusting screws 46 are then backed off and the positioning jig freed from its tackwelding attachment to the channel head. The positioning jig is then raised free of the bottom block by upward movement along the aligning post and storage attachment thereto by such as taping.
While being so held against the bottom wall of the channel head the bearing block 1 is secured to the bottom wall by welding at the edges of the block in a manner which prevents shifting in the position of such block relative to the channel head. During such welding the output from the inclinometer means 55 at the top of the post can be monitored to detect any tendency for such shifting.
Having thus installed the bottom bearing block 1 onto the bottom wall of the channel head chamber the rectangular anchor or pillow block 4, FIGS. 7 and 8 is placed into position on the divider plate 5 and held in selected desired position by action of helical compression springs 58 affiliated with a simulated rotary guide bracket assembly 59 clamped to the aligning post by a pair of quarter-turn screws 60 and located at the desired vertical height on such aligning post by a pair of alignment tabs 61 removably secured to such guide bracket in a selected rotary position on the post by screws 62. The tabs are slideable on the upper surface of a locating collar 63 on the rotary guide bracket which has a sliding fit with the outer periphery of the aligning post to provide frdeedom for sidewise position-adjusting movement of the anchor or pillow block 4 while abutting the divider plate. The extent of such adjusting movement is limited and once the proper position is obtained the rotary guide bracket can be clamped in place by tightening the mounting screws 62. A master dowell pin 65 cooperating between the anchor block and the guide bracket maintains centering relationship between these two members. While thus being held in place by the action of the helical compression springs 58 of the guide bracket, the anchor or pillow block 4 is welded to the wall of the divider plate 5.
Referring to FIGS. 7, 8, and 9, the horizontal gap 68 between the anchor or pillow block 4 attached to the divider plate and the adjacent end of the simulated rotary guide bracket 59 is measured by a pair of proximity sensors 69 in the end face of such bracket, a suitable sensor being such as the Kaman sensor number 2UB bonded in place in a cavity in the end face of such guide bracket. To suit the operating ramge of the sensors, a shim means 70 of known thickness may be introduced into the gap in a region of the sensors and held in place against the gap-defining face of the pillow block 4 by a leaf spring clip 71 attached to the shim and abutting the corresponding face of the forward end of the guide bracket. The gap width is then arrived at by adding the thickness of the shim 70 to the reading from the sensors 69. This information is subsequently utilized to determine the thickness of a shim means (not shown) to be introduced between such pillow block and the rotary guide bracket 13 affiliated with the vertical column 10 of the tube repair apparatus with which such pillow block is intended to be affiliated. It being appreciated that the simulated rotary guide bracket 59 attached to the aligning post 50 is similar in critical dimensions to the corresponding rotary guide bracket 13 affiliated with the vertical post 10 of the tube repair apparatus so that the gap measuring can be translated directly into thickness of the mounting shim for such apparatus.
Finally, the aligning post 50 together with bracket 59 can be freed from the tube sheet by retraction of the locating pins by operation of the hydraulic cylinder 53 in the locating assembly atop such post and from the anchor or pillow block now welded to the divider plate by removal of coupling pins 72 that connect such block at opposite end to the guide bracket 59 through the medium of adjustable stop pin assemblies 73 disposed in end slots 74 of such guide bracket. Such arrangement enabling initial installation of an anchor block 4 to the bracket 59 by connecting the adjustable stop pin assemblies 73 to the block by the coupling pins 72 and then swinging the adjustable stop pin asemblies sideways into the end slots 74 of the bracket 59, with springs 58 in place. The installation of the anchor, or pillow block 4 together with the bottom bearing block 1 within the channel head chamber is now complete, in accord with the objectives of the present invention, and the aligning post assembly can then be removed from such interior chamber by way of the manway 18.
While the invention has been shown and disclosed herein in what is conceived to be a practical and preferred embodiment, it is recognized that departures may be made therefrom within the scope of the following claims.
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Method and apparatus for expeditious installation of bottom-supporting and side-anchoring blocks for a tube and tube sheet bottom repair apparatus in the interior of the channel head of a steam generator at one side of the divider plate in a nuclear power plant, involving use of special tools and fixtures for location and welding of such blocks in position by use of information derived from measurement of the extent and direction of tilt of the tube sheet bottom from a purely horizontal attitude.
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FIELD
[0001] Provided herein are aqueous suspension concentrate compositions comprising biologically active 3,5-disubstituted-1,2,4-oxadiazoles or salts thereof that are useful, for example, in the control of nematodes.
BACKGROUND
[0002] Nematodes are active, flexible, elongate organisms that live on moist surfaces or in liquid environments, including films of water within soil and moist tissues within other organisms. Many species of nematodes have evolved to be very successful parasites of plants and animals and, as a result, are responsible for significant economic losses in agriculture and livestock.
[0003] Plant parasitic nematodes can infest all parts of the plant, including the roots, developing flower buds, leaves, and stems. Plant parasites can be classified on the basis of their feeding habits into a few broad categories: migratory ectoparasites, migratory endoparasites, and sedentary endoparasites. Sedentary endoparasites, which include root knot nematodes ( Meloidogyne ) and cyst nematodes ( Globodera and Heterodera ), can establish long-term infections within roots that may be very damaging to crops.
[0004] There is an urgent need in the industry for effective, economical, and environmentally safe methods of controlling nematodes. Continuing population growth, famines, and environmental degradation have heightened concern for the sustainability of agriculture.
[0005] Recently, a class of 3,5-disubstituted-1,2,4-oxadiazoles has been shown to exhibit potent, broad spectrum nematicidal activity. See generally U.S. Pat. No. 8,435,999 and U.S. Pat. No. 8,017,555, the contents of which are expressly incorporated herein by reference. The 3,5-disubstituted-1,2,4-oxadiazoles disclosed in U.S. Pat. No. 8,435,999 and U.S. Pat. No. 8,017,555 are generally characterized by low water solubility.
[0006] Two-phase suspension concentrates, which comprise solid particles of a compound suspended in an aqueous medium, are generally known in the art. In the context of seed treatment applications, suspension concentrates are known to offer several potential advantages, including high active loading, ease of handling, and reduced toxicity and flammability associated with solvents. The suspension concentrate compositions known in the art, however, are also prone to instability and settling upon storage, and may not provide a uniform distribution of the active nematicide compound in a manner that enhances bioavailability.
[0007] To be effective for use as a seed treatment composition, a nematicidal suspension concentrate desirably satisfies several key requirements. The nematicidal active ingredient must be effectively incorporated into a suspension having commercially acceptable storage stability. The suspension should exhibit acceptable storage stability over a wide temperature range and even where the nematicidal active ingredient is present in a high loading, which reduces the required volume of the composition and, therefore, reduces the expense of storage and shipping. The nematicidal active ingredient must also be amenable to transfer from the suspension concentrate to the surface of the seed, such that the desired loading can be efficiently achieved. Moreover, following application to the seed, it may be desirable for the nematicidal active ingredient to effectively migrate from the seed surface to the root zone of the surrounding soil.
[0008] Accordingly, there remains a need in the art to develop compositions that enable the efficient use of the above-mentioned potent and effective 3,5-disubstituted-1,2,4-oxadiazole nematicidal compounds in large-scale, commercial agricultural applications, particularly in seed treatment applications, to protect against nematode infestations.
SUMMARY OF THE INVENTION
[0009] In one aspect, the present invention is therefore directed to a nematicidal aqueous suspension concentrate composition, wherein the composition comprises a continuous aqueous phase comprising a dispersant component, and a dispersed solid particulate phase comprising a nematicidal component, the nematicidal component comprising a 3,5-disubstituted-1,2,4-oxadiazole compound or a salt thereof, wherein the median size of solid particulates in the dispersed solid particulate phase is less than about 10 μm.
[0010] In one embodiment, the present invention is directed to a nematicidal aqueous suspension concentrate composition as described above, wherein the nematicidal component comprises a compound of Formula (I) or a salt thereof,
[0000]
[0011] wherein A is selected from the group consisting of phenyl, pyridyl, pyrazyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of halogen, CF 3 , CH 3 , OCF 3 , OCH 3 , CN, and C(H)O; and C is selected from the group consisting of thienyl, furanyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of F, Cl, CH 3 , and OCF 3 .
[0012] In another embodiment, the present invention is directed to a nematicidal aqueous suspension concentrate composition as described above, wherein the nematicidal component comprises a compound of Formula (II) or a salt thereof,
[0000]
[0013] wherein A is selected from the group consisting of phenyl, pyridyl, pyrazyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of halogen, CF 3 , CH 3 , OCF 3 , OCH 3 , CN, and C(H)O; and C is selected from the group consisting of thienyl, furanyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more with substituents selected from the group consisting of F, Cl, CH 3 , and OCF 3 .
[0014] Another aspect of the present invention is directed to methods of preparing the nematicidal aqueous suspension concentrate compositions described above. In one embodiment, the method comprises mixing the nematicidal compound, the dispersant, and water to form an aqueous suspension; and wet milling the aqueous suspension to produce a milled suspension having a reduced particle size.
[0015] Another aspect of the present invention is directed to methods of protecting the roots of a plant against damage by a nematode, the method comprising applying a nematicidal aqueous suspension concentrate composition as described above the soil surrounding the root zone of a plant.
[0016] Another aspect of the present invention is directed to methods of protecting a seed and/or the roots of a plant grown from the seed against damage by a nematode, the method comprising treating a seed with a seed treatment composition, the seed treatment composition comprising a nematicidal aqueous suspension concentrate composition as described above.
[0017] Another aspect of the present invention is directed to a seed that has been treated with a seed treatment composition, the seed treatment composition comprising a nematicidal aqueous suspension concentrate composition as described above.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 depicts a representative photomicrograph of polymorphic Form I of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0019] FIG. 2 depicts a representative photomicrograph of polymorphic Form II of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0020] FIG. 3 depicts a sample cyclic differential scanning calorimetry (DSC) thermogram from a cyclic DSC analysis conducted on 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole at a cooling rate of 30° C. per minute.
[0021] FIG. 4 depicts an X-ray diffraction (XRD) overlay of polymorphic Forms I and II of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0022] FIGS. 5A and 5B depict XRD overlay results for polymorphic Forms I and II of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole, respectively.
[0023] FIG. 6 depicts the results of a powder XRD analysis of the Form I polymorph of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0024] FIG. 7 depicts the results of a powder XRD analysis of the Form II polymorph of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0025] FIG. 8 depicts a graphical XRD overlay of the competitive slurry experiment between polymorphic Forms I and II of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0026] FIGS. 9A through 9C depict the relevant DSC thermograms for polymorphic Form I, polymorphic Form II, and a mixture of polymorphic Forms I and II, respectively, of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole.
[0027] FIG. 10 depicts the results of an XRD analysis on samples of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole material after 4 weeks of storage.
[0028] FIG. 11 depicts the XRD overlays of Forms I, II and the sample of Form II which showed signs of transformation to Form I.
DETAILED DESCRIPTION OF THE INVENTION
[0029] Provided herein are aqueous suspension concentrate nematicidal compositions comprising 3,5-disubstituted-1,2,4-oxadiazoles and having improved effectiveness for seed treatment applications.
[0030] It has been discovered that the dispersibility of solid particulates of these generally hydrophobic, nematicidal compounds in an aqueous medium can be significantly increased through the application of milling techniques that substantially reduce the mean and median particle size characteristics of the dispersed solid phase, and by employing selected dispersants. The reduced size of the solid particulates enables the preparation of storage-stable, high-load suspension concentrate compositions. Increasing the aqueous dispersibility of these active nematicidal agents is highly beneficial, particularly in agricultural applications. For example, the compositions of the present invention may be advantageously applied to seeds as a prophylactic treatment against nematode infestation. Improved aqueous dispersibility provides for a more effective dispersion and more consistent loading of the nematicidal compound during initial application of the composition to the seed. In addition, the improved aqueous dispersibility provided by the present compositions is beneficial during the post-planting stage, as it allows the nematicide to more effectively disperse throughout the hydrophilic environment in the soil surrounding the seed and, subsequently, the root zone of the plant. Furthermore, it has been discovered that by controlling the particle size distribution of the nematicide particles as described herein, the adhesion characteristics of the active compound on the surface of the seeds allows for the efficient production of treated seeds having the desired active loading, and later enhances the bioavailability of the active compound in the soil.
[0031] The aqueous suspension concentrate nematicidal compositions described herein are sometimes referred to herein as “suspension concentrate compositions,” or more briefly as “suspension concentrates” or “the composition.” The suspension concentrate composition may also be referred to herein as a “seed treatment composition,” particularly in the context of seed treatment applications.
[0032] Nematicide
[0033] The aqueous compositions described herein generally comprise a nematicide component comprising one or more 3,5-disubstituted-1,2,4-oxadiazole compounds.
[0034] For example, in one embodiment, the nematicide component comprises a compound of Formula I or a salt thereof,
[0000]
[0035] wherein A is selected from the group consisting of phenyl, pyridyl, pyrazyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of halogen, CF 3 , CH 3 , OCF 3 , OCH 3 , CN, and C(H)O; and C is selected from the group consisting of thienyl, furanyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of F, Cl, CH 3 , and OCF 3 .
[0036] In a more specific embodiment, the nematicide component comprises a 3,5-disubstituted-1,2,4-oxadiazole of Formula Ia or a salt thereof,
[0000]
[0037] wherein R 1 and R 5 are independently selected from the group consisting of hydrogen, CH 3 , F, Cl, Br, CF 3 and OCF 3 ; R 2 and R 4 are independently selected from the group consisting of hydrogen, F, Cl, Br, and CF 3 ; R 3 is selected from the group consisting of hydrogen, CH 3 , CF 3 , F, Cl, Br, OCF 3 , OCH 3 , CN, and C(H)O; R 7 and R 8 are independently selected from hydrogen and F; R 9 is selected from the group consisting of hydrogen, F, Cl, CH 3 , and OCF 3 ; and E is O, N or S. Typically, E is selected from the group consisting of O and S.
[0038] In another embodiment, the nematicide component comprises a compound of Formula Ib or a salt thereof,
[0000]
[0039] wherein R 1 and R 5 are independently selected from the group consisting of hydrogen, CH 3 , F, Cl, Br, CF 3 and OCF 3 ; R 2 and R 4 are independently selected from the group consisting of hydrogen, F, Cl, Br, and CF 3 ; R 3 is selected from the group consisting of hydrogen, CH 3 , CF 3 , F, Cl, Br, OCF 3 , OCH 3 , CN, and C(H)O; R 8 is selected from hydrogen and F; R 6 and R 9 are independently selected from the group consisting of hydrogen, F, Cl, CH 3 , and OCF 3 ; and E is N, O or S. Typically, E is selected from the group consisting of O and S.
[0040] In another embodiment, the nematicide component comprises a 3,5-disubstituted-1,2,4-oxadiazole of Formula II or a salt thereof,
[0000]
[0041] wherein A is selected from the group consisting of phenyl, pyridyl, pyrazyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more substituents selected from the group consisting of halogen, CF 3 , CH 3 , OCF 3 , OCH 3 , CN, and C(H)O; and C is selected from the group consisting of thienyl, furanyl, oxazolyl and isoxazolyl, each of which can be optionally independently substituted with one or more with substituents selected from the group consisting of F, Cl, CH 3 , and OCF 3 .
[0042] In a more specific embodiment, the nematicide component comprises a compound of Formula IIa or a salt thereof,
[0000]
[0043] wherein R 1 and R 5 are independently selected from the group consisting of hydrogen, CH 3 , F, Cl, Br, CF 3 and OCF 3 ; R 2 and R 4 are independently selected from the group consisting of hydrogen, F, Cl, Br, and CF 3 ; R 3 is selected from the group consisting of hydrogen, CH 3 , CF 3 , F, Cl, Br, OCF 3 , OCH 3 , CN, and C(H)O; R 7 and R 8 are independently selected from hydrogen and F; R 9 is selected from the group consisting of hydrogen, F, Cl, CH 3 , and OCF 3 ; and E is N, O or S. Typically, E is selected from the group consisting of O and S.
[0044] In another embodiment, the nematicide component comprises a compound of Formula IIb or a salt thereof,
[0000]
[0045] wherein R 1 and R 5 are independently selected from the group consisting of hydrogen, CH 3 , F, Cl, Br, CF 3 and OCF 3 ; R 2 and R 4 are independently selected from the group consisting of hydrogen, F, Cl, Br, and CF 3 ; R 3 is selected from the group consisting of hydrogen, CH 3 , CF 3 , F, Cl, Br, OCF 3 , OCH 3 , CN, and C(H)O; R 8 is selected from hydrogen and F; R 6 and R 9 are independently selected from the group consisting of hydrogen, F, Cl, CH 3 , and OCF 3 ; and E is N, O or S. Typically, E is selected from the group consisting of O and S.
[0046] In a preferred embodiment, the nematicidal component comprises a 3,5-disubstituted-1,2,4-oxadiazole of Formula (Ia) or a salt thereof. Non-limiting examples of species include 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole of Formula (Ia-i),
[0000]
[0000] 3-(4-chlorophenyl)-5-(furan-2-yl)-1,2,4-oxadiazole of Formula (Ia-ii),
[0000]
[0000] 3-(4-chloro-2-methylphenyl)-5-(furan-2-yl)-1,2,4-oxadiazole of Formula (Ia-iii),
[0000]
[0000] and 5-(furan-2-yl)-3-phenyl-1,2,4-oxadiazole of Formula (Ia-iv).
[0000]
[0047] In another embodiment, the nematicidal component comprises a 3,5-disubstituted-1,2,4-oxadiazole of Formula (Ib) or a salt thereof Non-limiting examples of species include 3-(4-bromophenyl)-5-(furan-3-yl)-1,2,4-oxadiazole of Formula (Ib-i),
[0000]
[0000] and 3-(2,4-difluorophenyl)-5-(thiophen-3-yl)-1,2,4-oxadiazole of Formula (Ib-ii).
[0000]
[0048] In another embodiment, the nematicidal component comprises a 3,5-disubstituted-1,2,4-oxadiazole of Formula (IIa) or a salt thereof. Non-limiting examples of species include 3-(thiophen-2-yl)-5-(p-tolyl)-1,2,4-oxadiazole of Formula (IIa-i),
[0000]
[0000] 5-(3-chlorophenyl)-3-(thiophen-2-yl)-1,2,4-oxadiazole of Formula (IIa-ii),
[0000]
[0000] and 5-(4-chloro-2-methylphenyl)-3-(furan-2-yl)-1,2,4-oxadiazole of Formula (IIa-iii).
[0000]
[0049] Polymorphs of the Nematicidal Compounds
[0050] The aqueous suspension concentrate composition can comprise any of the polymorphic forms of the nematicidal compounds described herein.
[0051] Generally, polymorphism refers to the potential of a chemical entity to exist in different three-dimensional arrangements in the solid state. Different polymorphic forms of a compound can have different physical properties, including: solubility and dissolution rate; crystal shape; solid state stability; batch-to-batch manufacturing reproducibility; stability; ease of formulation; and bioavailability, among others. In deciding which polymorph of a given compound is preferable for a specific application, the relevant properties of each polymorph should be determined and compared, so that the polymorph with the most desirable combination of attributes can be selected for use.
[0052] For example, it has been discovered that the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole, referred to herein as the compound of Formula (Ia-i), exists in two distinct polymorphic forms, referred to herein as Form I and Form II. Form I is believed to be the thermodynamically stable form under ambient conditions, while Form II is metastable at room temperature and pressure. The polymorphs are enantiotropically related. The transition temperature between the two forms is believed to be approximately 102° C., wherein Form I is the stable form below the transition temperature, and Form II is the more thermodynamically stable form above that temperature.
[0053] Form I is believed to correspond to a dry crystalline polymorphic form of the compound. Generally, Form I does not appear to be prone to hydrate formation. Microscopic evaluation of Form I showed birefringent acicular to columnar shaped particles ranging from approximately 50 to 100 microns in length. FIG. 1 shows the representative photomicrograph at room temperature.
[0054] Form II is also believed to correspond to a dry crystalline polymorphic form of the compound. Microscopic evaluation of Form II showed birefringent acicular, columnar, and flake shaped particles ranging from approximately 25 to 150 microns in length. FIG. 2 shows the representative photomicrograph at room temperature.
[0055] Generally, the aqueous suspension concentrate composition can comprise any of the polymorphic forms of the nematicidal compounds described herein. For example, in one embodiment, the suspension concentrate composition comprises polymorphic Form I of the compound of Formula (Ia-i). In another embodiment, the suspension concentrate composition comprises polymorphic Form II of the compound of Formula (Ia-i). Mixtures of more than one polymorph are also considered to be within the scope of the invention. For example, in one embodiment, the suspension concentrate composition comprises a mixture of polymorphic forms I and II of the compound of Formula (Ia-i).
[0056] Concentration
[0057] The suspension concentrate composition in some embodiments comprises at least about 10%, at least about 15%, at least about 20%, at least about 25%, at least about 30%, at least about 35%, at least about 40%, at least about 45%, or at least about 50% by weight of the nematicide component comprising one or more active nematicidal compounds as described above. In one embodiment, the suspension concentrate composition comprises at least about 40% by weight of the nematicide component. In some embodiments, the suspension concentrate composition comprises at least about 45% by weight of the nematicide component, or even higher (e.g., at least about 50% by weight).
[0058] The suspension concentrate composition comprises the nematicide component in a concentration of at least about 100 g/L, at least about 200 g/L, at least about 250 g/L, at least about 300 g/L, at least about 350 g/L, at least about 400 g/L, at least about 450 g/L, at least about 500 g/L, at least about 550 g/L, at least about 600 g/L, at least about 650 g/L, or at least about 700 g/L. The nematicide concentration ranges from about 400 g/L to about 700 g/L, from about 450 g/L to about 750 g/L, or from about 450 g/L to about 700 g/L.
[0059] Particle Size
[0060] The suspension concentrate compositions of the present invention comprise a continuous aqueous phase and a dispersed solid phase comprising solid particulates of the nematicide component as described herein. The solid nematicidal particulates have a particle size distribution selected to enhance dispersibility of the particles suspended in the composition and improve the stability of the suspension concentrate composition.
[0061] It has been discovered, however, that further reductions in particle size provide a number of benefits, including improved adhesion characteristics of the 3,5-disubstituted-1,2,4-oxadiazole compounds when the composition is applied as a seed treatment. The particle size reduction described herein provides enhanced adhesion of the nematicidal active ingredient to the seed surface when the composition is applied as a seed treatment and thereby allows for efficient production of treated seeds having a uniform active loading. Furthermore, and without being bound to a particular theory, it is believed that further reducing the particulate size of the 3,5-disubstituted-1,2,4-oxadiazole compounds facilitates improved dispersibility of the solid nematicidal active within the aqueous environment of the root zone after planting the treated seed in the soil. Dispersion of the nematicide throughout the surrounding root zone helps prevent soil nematodes from coming into contact with the seed and, later, the newly formed roots of the plant emerging from the seed, and ultimately manifests as an improvement in nematicidal efficacy (i.e., a reduction in plant damage attributable to nematodes).
[0062] In the preparation of suspension concentrates, there are considerable energy costs and time requirements associated with reducing the particle size of the solid phase. These costs tend to increase significantly as the particle size decreases. Accordingly, efficient production of suspension concentrates must take into account the additional costs and benefits associated with the particle size reduction step.
[0063] Accordingly, the particle size characteristics of the dispersed solid phase of the suspension concentrate composition comprising the 3,5-disubstituted-1,2,4-oxadiazole compounds described above are selected so as to not only provide a stable suspension, but also to allow for efficient production of treated seeds having a uniform active loading and enhanced nematicidal efficacy. More particularly, the dispersed solid phase of the suspension concentrate has a median particle size less than about 50 μm, less than 30 μm, less than 20 μm, less than 10 μm, less than about 5 μm, less than about 4 μm, less than about 3 μm, less than about 2 μm, or less than about 1 μm. The suspension concentrate composition typically has a median particle size falling within the range of from about 0.5 μm to about 10 μm, from about 1 μm to about 5 μm, from about 1 μm to about 4 μm, from about 1 μm to about 3 μm, or from about 1 μm to about 2 μm. In some embodiments, the median particle size falls within the range of from about 0.5 μm to about 5 μm, from about 0.5 μm to about 4 μm, from about 0.5 μm to about 3 μm, from about 0.5 μm to about 2 μm, or from about 0.5 μm to about 1 μm. In one embodiment, the median particle size falls within the range of from about 1 μm to about 2 μm.
[0064] The dispersed solid phase of the suspension concentrate composition typically has a mean particle size less than about 20 μm, less than about 10 μm, less than about 5 μm, less than about 4 μm, less than about 3 μm, less than about 2 μm, or less than about 1 μm. The mean particle size typically falls within the range of from about 0.5 μm to about 20 μm, from about 0.5 μm to about 10 μm, from about 1 μm to about 5 μm, from about 1 μm to about 4 μm, from about 1 μm to about 3 μm, or from about 1 μm to about 2 μm. In some embodiments, the mean particle size falls within the range of from about 0.5 μm to about 5 μm, from about 0.5 μm to about 4 μm, from about 0.5 μm to about 3 μm, from about 0.5 μm to about 2 μm, or from about 0.5 μm to about 1 μm.
[0065] The mean and/or median particle size of the solid particulates in the dispersed phase can be determined by means known in the art, including laser diffraction particle size analysis. A non-limiting example of a suitable apparatus for determining the particle size characteristics of the solid particulates is a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320).
[0066] The dispersed solid phase of the suspension concentrate typically has a polydispersity index, defined as the arithmetic mean particle size divided by the median particle size, of less than about 10. In some embodiments, the polydispersity index is less than about 5, less than about 2, or less than about 1.5. The polydispersity index typically falls within the range of from about 1 to about 2.
[0067] Dispersant
[0068] The suspension concentrate composition additionally comprises a dispersant component comprising one or more dispersants selected to enhance dispersibility of the solid particles suspended in the composition and improve the stability of the suspension concentrate composition. The dispersant may be selected from non-ionic dispersants, anionic dispersants, or cationic dispersants.
[0069] In a preferred embodiment, the dispersant is anionic. Examples of anionic dispersants include alkyl sulfates, alcohol sulfates, alcohol ether sulfates, alpha olefin sulfonates, alkylaryl ether sulfates, arylsulfonates, alkylsulfonates, alkylaryl sulfonates, sulfosuccinates, mono- or diphosphate esters of polyalkoxylated alkyl alcohols or alkyl phenols, mono- or disulfosuccinate esters of alcohols or polyalkoxylated alkanols, alcohol ether carboxylates, phenol ether carboxylates.
[0070] In one embodiment, the dispersant is an alkylaryl sulfonate. Alkylaryl sulfonates have been found to be effective at forming a stable aqueous suspension comprising the 3,5-disubstituted-1,2,4-oxadiazole compounds used in the practice of the present invention, particularly at high concentrations of the nematicidal active ingredient.
[0071] Non-limiting examples of commercially available anionic dispersants include sodium dodecylsulfate (Na-DS, SDS), MORWET D-425 (a sodium salt of alkyl naphthalene sulfonate condensate, available from Akzo Nobel), MORWET D-500 (a sodium salt of alkyl naphthalene sulfonate condensate with a block copolymer, available from Akzo Nobel), sodium dodecylbenzene sulfonic acid (Na-DBSA) (available from Aldrich), diphenyloxide disulfonate, naphthalene formaldehyde condensate, DOWFAX (available from Dow), dihexylsulfosuccinate, and dioctylsulfosuccinate. For example, the anionic dispersant may comprise an alkyl naphthalene sulfonate condensate or a salt thereof.
[0072] Examples of non-ionic dispersants include sorbitan esters, ethoxylated sorbitan esters, alkoxylated alkylphenols, alkoxylated alcohols, block copolymer ethers, and lanolin derivatives. In accordance with one embodiment, the dispersant comprises an alkylether block copolymer
[0073] Non-limiting examples of commercially available non-ionic dispersants include SPAN 20, SPAN 40, SPAN 80, SPAN 65, and SPAN 85 (available from Aldrich); TWEEN 20, TWEEN 40, TWEEN 60, TWEEN 80, and TWEEN 85 (available from Aldrich); IGEPAL CA-210, IGEPAL CA-520, IGEPAL CA-720, IGEPAL CO-210, IGEPAL CO-520, IGEPAL CO-630, IGEPAL CO-720, IGEPAL CO-890, and IGEPAL DM-970 (available from Aldrich); Triton X-100 (available from Aldrich); BRIJ S10, BRIJ S20, BRIJ 30, BRIJ 52, BRIJ 56, BRIJ 58, BRIJ 72, BRIJ 76, BRIJ 78, BRIJ 92V, BRIJ 97, and BRIJ 98 (available from Aldrich); PLURONIC L-31, PLURONIC L-35, PLURONIC L-61, PLURONIC L-81, PLURONIC L-64, PLURONIC L-121, PLURONIC 10R5, PLURONIC 17R4, and PLURONIC 31R1 (available from Aldrich); Atlas G-5000 and Atlas G-5002 L (available from Croda); ATLOX 4912 and ATLOX 4912-SF (available from Croda); and SOLUPLUS (available from BASF), LANEXOL AWS (available from Croda).
[0074] Non-limiting examples of cationic dispersants include mono alkyl quaternary amine, fatty acid amide surfactants, amidoamine, imidazoline, and polymeric cationic surfactants.
[0075] The suspension concentrate composition comprises from about 0.5% about 20%, from about 0.5% to about 10%, from about 0.5% to about 5%, or from about 0.5% to about 8% of the dispersant component by weight. In one embodiment, the composition comprises the dispersant in an amount of from about 0.5% to about 5% by weight.
[0076] The suspension concentrate composition may comprise the dispersant in a concentration of at least about 5 g/L, at least about 10 g/L, at least about 15 g/L, at least about 20 g/L, at least about 25 g/L, at least about 30 g/L, at least about 35 g/L, at least about 40 g/L, at least about 45 g/L, or at least about 50 g/L. In some embodiments, the dispersant is present in a concentration of from about 1 to about 100 g/L, from about 5 to about 75 g/L, or more typically from about 20 to about 50 g/L.
[0077] In some embodiments, the suspension concentrate composition comprises a dispersant component comprising a primary dispersant in combination with one or more secondary dispersants. The secondary dispersant may also be referred to herein as a wetting agent. In one embodiment, the secondary dispersant comprises an alkylether block copolymer.
[0078] In one embodiment, the secondary dispersant is non-ionic when used in conjunction with an ionic primary dispersant. For example, in some embodiments, the dispersant component comprises a mixture of an anionic primary dispersant (described above) and a non-ionic (described above) secondary dispersant. In other embodiments, the dispersant component comprises a mixture of a cationic primary dispersant and a non-ionic secondary dispersant. In accordance with another embodiment, it has been found that the pairing of an anionic primary dispersant with a non-ionic secondary dispersant, in particular, imparts improved stability to the aqueous suspension concentrates described herein.
[0079] The secondary dispersant typically comprises from about 0.05% to about 10%, from about 0.5% to about 5%, from about 1% to about 5%, from about 1% to about 4%, or from about 1% to about 2.5% by weight of the composition.
[0080] The composition typically comprises a ratio of primary dispersant to secondary dispersant, on a weight basis, of from about 1:1 to about 10:1, from about 1:1 to about 5:1, and from about 2:1 to about 3:1.
[0081] Dendrimers
[0082] In some embodiments, the composition may further comprise one or more functionalized dendrimers to enhance the efficacy and/or stability of the composition. Non-limiting examples of classes of functionalized dendrimers include poly(amidoamine) (PAMAM, Generations 0-7), poly(amidoamine-organosilicone) (PAMAMOS), poly(propylene imidine) (PPI, Generations 0-5), poly(benzylethers) (Frechet-type), Arobols (Newkome type), poly(phenylacetylenes) and surface engineered dendrimers (e.g. PEGylated dendrimers, glycodendrimers, peptide funtionalized dendrimers, and galabiose-functionalized dendrimers). In some embodiments, the dendrimers comprise at least about 0.1% and up to 10% or more, or from about 1% to about 10% by weight of the composition.
[0083] Antifreeze Agents
[0084] In some embodiments, the composition may further comprise one or more antifreeze agents. In one embodiment, the antifreeze agent is an alcohol. Non-limiting examples of antifreeze agents include ethylene glycol, propylene glycol, butanediol, pentanediol, mannitol, sorbitol, and glycerol (glycerin).
[0085] The suspension concentrate composition may comprise the antifreeze agent in a concentration of at least about 5 g/L, at least about 10 g/L, at least about 15 g/L, at least about 20 g/L, at least about 30 g/L, at least about 40 g/L, at least about 50 g/L, at least about 60 g/L, at least about 70 g/L, or at least about 80 g/L. The antifreeze agent is typically present in a concentration of from about 1 to about 150 g/L, from about 10 to about 100 g/L, or more typically from about 20 to about 80 g/L.
[0086] Antifoam Agents
[0087] In some embodiments, the composition may further comprise one or more antifoam agents. Examples of antifoam agents include organosilicone or silicone-free compounds. Non-limiting examples of commercially available antifoam products include Break-Thru OE441 (available from Evonik), Break-Thru AF9905 (available from Evonik), AGNIQUE DF 6889 (available from Cognis), AGNIQUE DFM 111S (available from Cognis), BYK-016 (available from BYK), FG-10 antifoam emulsion (available from Dow Corning), 1520-US (available from Dow Corning), 1510-US (available from Dow Corning), SAG 1538 (available from Momentive), and SAG 1572 (available from Momentive).
[0088] Buffer
[0089] In some embodiments, the composition may comprise a buffer solution that helps maintain the pH within a desired range. It has been discovered that, at a pH greater than about 10, wet milling and/or ball milling the nematicidal component described herein results in excessive clumping and/or agglomeration making the particle size reduction difficult, instability or degradation of the nematicidal component, and/or instability or degradation of the other suspension concentrate components described herein. As a result, a pH buffer may be selected to provide an aqueous suspension concentrate composition having a pH of less than 10, from about 5 to about 9, from about 6 to about 8, or about 7. Buffer solutions suitable for a variety of pH ranges are generally known in the art.
[0090] Thickener
[0091] In some embodiments, the composition may comprise a thickener (referred to hereinafter as “stabilizer”) component. Examples of stabilizers include anionic polysaccharides and cellulose derivatives. In some embodiments, the stabilizer comprises a clay or a silica, or a colloidal hydrophilic silica. Non-limiting examples of commercially available stabilizers include KELZAN CC (available from Kelco), methyl cellulose, carboxymethylcellulose and 2-hydroxyethylcellulose, hydroxymethylcellulose, kaolin, and microcrystalline cellulose. A non-limiting example of a commercially available colloidal hydrophilic silica is AEROSIL (available from Evonik).
[0092] The stabilizer component typically comprises from about 0.05% to about 10% by weight of the composition. For example, in some embodiments, the stabilizer component comprises from about 0.1% to about 5%, from about 0.1% to about 2%, or from about 0.1% to about 1% by weight of the composition.
[0093] Crystal Growth Inhibitor
[0094] In some embodiments, the composition may comprise a crystal growth inhibitor. Examples of crystal growth inhibitors include acrylic copolymers, polyethylene glycol, polyethylene glycol hydrogenated castor oil and combinations. Non-limiting examples of commercially available crystal growth inhibitor include ATLOX 4913 (available from Croda).
[0095] The crystal growth inhibitor component may comprise from about 1% to about 10% by weight of the composition.
[0096] Co-Solvent
[0097] In some embodiments, the composition may further comprise a co-solvent in addition to water. Non-limiting examples of co-solvents that can be used include, ethyl lactate, methyl soyate/ethyl lactate co-solvent blends (e.g., STEPOSOL, available from Stepan), isopropanol, acetone, 1,2-propanediol, n-alkylpyrrolidones (e.g., the AGSOLEX series, available from ISP), a petroleum based-oil (e.g., AROMATIC series and SOLVESSO series available from Exxon Mobil), isoparaffinic fluids (e.g. ISOPAR series, available from Exxon Mobil), cycloparaffinic fluids (e.g. NAPPAR 6, available from Exxon Mobil), mineral spirits (e.g. VARSOL series available from Exxon Mobil), and mineral oils (e.g., paraffin oil).
[0098] Non-limiting examples of preferred commercially available organic solvents include pentadecane, ISOPAR M, and ISOPAR V and ISOPAR L (available from Exxon Mobil).
[0099] Rheology Modifying Agent
[0100] In some embodiments, the composition may further comprise one or more rheology modifying agents.
[0101] Examples of rheology modifying agents include humic acid salts, fulvic acid salts, humin, and lignin salts.
[0102] In one embodiment, the rheology modifying agent is the sodium or potassium salt of humic acid. Generally, a humic substance is one produced by biodegradation of dead organic matter, particularly dead plant matter (e.g., lignin). With respect to the compositions of the present invention, it has been discovered that compositions comprising a humic acid exhibit a lower viscosity than similarly-loaded compositions in the absence of a humic acid. Fulvic acids, which are humic acids of lower molecular weight and higher oxygen content than other humic acids, are used in some embodiments.
[0103] Additional Excipients
[0104] In some embodiments, composition comprises one or more additional excipients that improve the adhesion of the composition to the seed, provide a visual indication of successful coating (e.g., coloring agents), or otherwise impart improved characteristics to the coating.
[0105] Biocidal Agents
[0106] In some embodiments, the composition may further comprise one or more biocidal agents. Typically, a biocidal component is included to prevent fungal and/or bacterial growth within the suspension concentrate composition, particularly when the composition is placed into storage. Examples of biocidal agents include dichlorophen or benzyl alcohol hemiformal based compounds, benzoisothiazolinones and rhamnolipids. Non-limiting examples of commercially available biocidal agents include ACTICIDE (available from THOR), PROXEL (available from Arch Chemical), and ZONIX (available from Jeneil).
[0107] Additional Active Ingredients
[0108] In some embodiments, the composition may be formulated, mixed in a seed treater tank or combined on the seed by overcoating with one or more additional active ingredients in combination with the nematicidal 3,5-disubstituted-1,2,4-oxadiazoles described herein.
[0109] The additional active ingredient may be, for example, an additional pesticide. The pesticide may be, for example, an insecticide, a fungicide, an herbicide, or an additional nematicide.
[0110] Non-limiting examples of insecticides and nematicides include carbamates, diamides, macrocyclic lactones, neonicotinoids, organophosphates, phenylpyrazoles, pyrethrins, spinosyns, synthetic pyrethroids, tetronic and tetramic acids. In particular embodiments insecticides and nematicides include abamectin, aldicarb, aldoxycarb, bifenthrin, carbofuran, chlorantraniliprole, clothianidin, clothianidin and a Bacillus firmus, cyantraniliprole, cyfluthrin, cyhalothrin, cypermethrin, deltamethrin, dinotefuran, emamectin, ethiprole, fenamiphos, fipronil, flubendiamide, fluopyram, fosthiazate, imidacloprid, ivermectin, lambda-cyhalothrin, milbemectin, nitenpyram, oxamyl, permethrin, spinetoram, spinosad, spirodichlofen, spirotetramat, tefluthrin, thiacloprid, thiamethoxam, and thiodicarb,
[0111] Non-limiting examples of useful fungicides include aromatic hydrocarbons, benzimidazoles, benzthiadiazole, carboxamides, carboxylic acid amides, morpholines, phenylamides, phosphonates, quinone outside inhibitors (e.g. strobilurins), thiazolidines, thiophanates, thiophene carboxamides, and triazoles. Particular examples of fungicides include acibenzolar-S-methyl, azoxystrobin, benalaxyl, bixafen, boscalid, carbendazim, cyproconazole, dimethomorph, epoxiconazole, fluopyram, fluoxastrobin, flutianil, flutolanil, fluxapyroxad, fosetyl-Al, ipconazole, isopyrazam, kresoxim-methyl, mefenoxam, metalaxyl, metconazole, myclobutanil, orysastrobin, penflufen, penthiopyrad, picoxystrobin, propiconazole, prothioconazole, pyraclostrobin, sedaxane, silthiofam, tebuconazole, thifluzamide, thiophanate, tolclofos-methyl, trifloxystrobin, and triticonazole.
[0112] Non-limiting examples of herbicides include ACCase inhibitors, acetanilides, AHAS inhibitors, carotenoid biosynthesis inhibitors, EPSPS inhibitors, glutamine synthetase inhibitors, PPO inhibitors, PS II inhibitors, and synthetic auxins, Particular examples of herbicides include acetochlor, clethodim, dicamba, flumioxazin, fomesafen, glyphosate, glufosinate, mesotrione, quizalofop, saflufenacil, sulcotrione, and 2,4-D.
[0113] Additional actives may also comprise substances such as, biological control agents, microbial extracts, natural products, plant growth activators or plant defense agents. Non-limiting examples of biological control agents include bacteria, fungi, beneficial nematodes, and viruses.
[0114] In certain embodiments, the biological control agent can be a bacterium of the genus Actinomycetes, Agrobacterium, Arthrobacter, Alcaligenes, Aureobacterium, Azobacter, Beijerinckia, Brevibacillus, Burkholderia, Chromobacterium, Clostridium, Clavibacter, Comomonas, Corynebacterium, Curtobacterium, Enterobacter, Flavobacterium, Gluconobacter, Hydrogenophage, Klebsiella, Methylobacterium, Paenibacillus, Pasteuria, Phingobacterium, Photorhabdus, Phyllobacterium, Pseudomonas, Rhizobium, Serratia, Stenotrophomonas, Variovorax, and Xenorhadbus. In particular embodiments the bacteria is selected from the group consisting of Bacillus amyloliquefaciens, Bacillus cereus, Bacillus firmus, Bacillus, lichenformis, Bacillus pumilus, Bacillus sphaericus, Bacillus subtilis, Bacillus thuringiensis, Chromobacterium suttsuga, Pasteuria penetrans, Pasteuria usage, and Pseudomona fluorescens.
[0115] In certain embodiments the biological control agent can be a fungus of the genus Alternaria, Ampelomyces, Aspergillus, Aureobasidium, Beauveria, Colletotrichum, Coniothyrium, Gliocladium, Metarhisium, Muscodor, Paecilonyces, Trichoderma, Typhula, Ulocladium, and Verticilium. In particular embodiments the fungus is Beauveria bassiana, Coniothyrium minitans, Gliocladium virens, Muscodor albus, Paecilomyces lilacinus, or Trichoderma polysporum.
[0116] In further embodiments the biological control agents can be plant growth activators or plant defense agents including, but not limited to harpin, Reynoutria sachalinensis, jasmonate, lipochitooligosaccharides, gibberellic acid, and isoflavones.
[0117] Methods of Preparation
[0118] Another aspect of the present invention is directed to methods of preparing the nematicidal suspension concentrate compositions described herein.
[0119] As described above, it has been discovered that significant benefits in the aqueous dispersibility of 3,5-disubstituted-1,2,4-oxadiazoles can be obtained and other advantages realized by reducing the particulate size of the solid phase in the suspension concentrate composition. Generally, the particulate size of the nematicide component may be reduced by any method known in the art. In accordance with one preferred embodiment, the particle size of the nematicide component is reduced by wet milling. Additionally, air milling, high pressure homogenization, spinning disc, grinding and solvent evaporation techniques can be used to reduce the particle size of the nematicide component.
[0120] Typically, the first step in the process comprises a pre-milling step wherein the nematicidal component comprising one or more active nematicidal compounds is combined with water and agitated to form an aqueous suspension. Typically, the dispersant is also added to the aqueous suspension prior to the particle size reduction step and acts as a wet-milling aid. Other optional components which may be added to the aqueous suspension before the particle size reduction step include a secondary dispersant and/or an antifreeze agent, each of which may be selected as described above. Additionally, in one embodiment, a buffer solution is added to the suspension prior to the particle size reduction step; as discussed above, the pH of the suspension during the particle size reduction step is preferably less than 10 in order to minimize excessive clumping and/or agglomeration making the particle size reduction difficult, instability or degradation of the nematicidal component, and/or instability or degradation of the other suspension concentrate components described herein.
[0121] The aqueous suspension is then wet-milled to obtain a suspension concentrate having the desired particle size distribution as described above. The wet-milling process may be carried out using techniques and apparatus known in the art. Ball milling is a particularly preferred technique, wherein the aqueous suspension is placed inside a rotating cylinder containing grinding media. The grinding media are preferably selected from the group consisting of stainless steel beads, zirconium oxide beads, glass beads and ceramic beads. Non-limiting examples of suitable ball milling apparatus include a SIZEGVARI ATTRITOR milling system made by UNION PROCESS, and a MINI ZETA II milling machine made by Netzsch.
[0122] The wet-milling step typically produces a fine suspension comprising a dispersed solid phase having a particle size distribution characterized by the median and mean particle sizes and polydispersity index described above. Using laser diffraction particle size analysis or other suitable means, the duration and intensity of the wet-milling operation is controlled to provide a suspension concentrate composition having the desired particle size characteristics.
[0123] Following the particle size reduction, the milled aqueous suspension may be combined with an optional stabilizer component and/or one or more additional biocidal agents, each of which may be selected as described above.
[0124] Storage Stability
[0125] In one embodiment, the aqueous suspension concentrate composition described herein exhibits commercially acceptable storage stability across a wide range of temperatures and environmental conditions. In this context, storage stability is generally defined as the absence of sedimentation and the lack of any significant change in the rheological properties of the composition (e.g., viscosity). Commercially acceptable storage stability can be reliably achieved by selecting the various components of the aqueous suspension concentrate, particularly the primary dispersant, optional secondary dispersant, and/or optional stabilizer component, in accordance with the respective embodiments described in detail above. The suspension concentrate composition may be storage-stable at 25° C. for at least about 1 week, at least about 2 weeks, at least about 1 month, at least about 2 months, at least about 3 months, at least about 6 months, at least about 12 months or at least about 18 months.
[0126] Methods of Application
[0127] Another aspect of the present invention is directed to methods for protecting the roots of a plant against damage by nematodes.
[0128] Application to Seeds
[0129] In one embodiment, the method comprises protecting a seed, and/or the roots of a plant grown from the seed, against damage by a nematode by treating the seed with a seed treatment composition described herein and diluted as necessary to attain the desired nematicide compound loading on the treated seeds.
[0130] The methods described herein can be used in connection with any species of plant and/or the seeds thereof. In preferred embodiments, however, the methods are used in connection with seeds of plant species that are agronomically important. In particular, the seeds can be of corn, peanut, canola/rapeseed, soybean, cucurbits, crucifers, cotton, beets, rice, sorghum, sugar beet, wheat, barley, rye, sunflower, tomato, sugarcane, tobacco, oats, as well as other vegetable and leaf crops. In some embodiments, the seed is corn, soybean, or cotton seed. The seed may be a transgenic seed from which a transgenic plant can grow and incorporate a transgenic event that confers, for example, tolerance to a particular herbicide or combination of herbicides, increased disease resistance, enhanced tolerance to stress and/or enhanced yield. Transgenic seeds include, but are not limited to, seeds of corn, soybean and cotton.
[0131] In one embodiment, the treatment composition is applied to the seed prior to sowing the seed so that the sowing operation is simplified. In this manner, seeds can be treated, for example, at a central location and then dispersed for planting. This permits the person who plants the seeds to avoid the complexity and effort associated with handling and applying the seed treatment compositions, and to merely handle and plant the treated seeds in a manner that is conventional for regular untreated seeds.
[0132] The seed treatment composition can be applied to seeds by any standard seed treatment methodology, including but not limited to mixing in a container (e.g., a bottle or bag), mechanical application, tumbling, spraying, immersion, and solid matrix priming Seed coating methods and apparatus for their application are disclosed in, for example, U.S. Pat. Nos. 5,918,413, 5,891,246, 5,554,445, 5,389,399, 5,107,787, 5,080,925, 4,759,945 and 4,465,017, among others. Any conventional active or inert material can be used for contacting seeds with the seed treatment composition, such as conventional film-coating materials including but not limited to water-based film coating materials.
[0133] For example, in one embodiment, a seed treatment composition can be introduced onto or into a seed by use of solid matrix priming. For example, a quantity of the seed treatment composition can be mixed with a solid matrix material and then the seed can be placed into contact with the solid matrix material for a period to allow the seed treatment composition to be introduced to the seed. The seed can then optionally be separated from the solid matrix material and stored or used, or the mixture of solid matrix material plus seed can be stored or planted directly. Solid matrix materials which are useful in the present invention include polyacrylamide, starch, clay, silica, alumina, talc, mica, soil, sand, polyurea, polyacrylate, or any other material capable of absorbing or adsorbing the seed treatment composition for a time and releasing the nematicide of the seed treatment composition into or onto the seed. It is useful to make sure that the nematicide and the solid matrix material are compatible with each other. For example, the solid matrix material should be chosen so that it can release the nematicide at a reasonable rate, for example over a period of minutes, hours, days, or weeks.
[0134] Imbibition is another method of treating seed with the seed treatment composition. For example, a plant seed can be directly immersed for a period of time in the seed treatment composition. During the period that the seed is immersed, the seed takes up, or imbibes, a portion of the seed treatment composition. Optionally, the mixture of plant seed and the seed treatment composition can be agitated, for example by shaking, rolling, tumbling, or other means. After imbibition, the seed can be separated from the seed treatment composition and optionally dried, for example by patting or air drying.
[0135] The seed treatment composition may be applied to the seeds using conventional coating techniques and machines, such as fluidized bed techniques, the roller mill method, rotostatic seed treaters, and drum coaters. Other methods, such as spouted beds may also be useful. The seeds may be pre-sized before coating. After coating, the seeds are typically dried and then transferred to a sizing machine for sizing. Such procedures are generally known in the art.
[0136] If the seed treatment composition is applied to the seed in the form of a coating, the seeds can be coated using a variety of methods known in the art. For example, the coating process can comprise spraying the seed treatment composition onto the seed while agitating the seed in an appropriate piece of equipment such as a tumbler or a pan granulator.
[0137] In one embodiment, when coating seed on a large scale (for example a commercial scale), the seed coating may be applied using a continuous process. Typically, seed is introduced into the treatment equipment (such as a tumbler, a mixer, or a pan granulator) either by weight or by flow rate. The amount of treatment composition that is introduced into the treatment equipment can vary depending on the seed weight to be coated, surface area of the seed, the concentration of the nematicide and/or other active ingredients in the treatment composition, the desired concentration on the finished seed, and the like. The treatment composition can be applied to the seed by a variety of means, for example by a spray nozzle or revolving disc. The amount of liquid is typically determined by the assay of the formulation and the required rate of active ingredient necessary for efficacy. As the seed falls into the treatment equipment the seed can be treated (for example by misting or spraying with the seed treatment composition) and passed through the treater under continual movement/tumbling where it can be coated evenly and dried before storage or use.
[0138] In another embodiment, the seed coating may be applied using a batch process. For example, a known weight of seeds can be introduced into the treatment equipment (such as a tumbler, a mixer, or a pan granulator). A known volume of seed treatment composition can be introduced into the treatment equipment at a rate that allows the seed treatment composition to be applied evenly over the seeds. During the application, the seed can be mixed, for example by spinning or tumbling. The seed can optionally be dried or partially dried during the tumbling operation. After complete coating, the treated sample can be removed to an area for further drying or additional processing, use, or storage.
[0139] In an alternative embodiment, the seed coating may be applied using a semi-batch process that incorporates features from each of the batch process and continuous process embodiments set forth above.
[0140] In still another embodiment, seeds can be coated in laboratory size commercial treatment equipment such as a tumbler, a mixer, or a pan granulator by introducing a known weight of seeds in the treater, adding the desired amount of seed treatment composition, tumbling or spinning the seed and placing it on a tray to thoroughly dry.
[0141] In another embodiment, seeds can also be coated by placing the known amount of seed into a narrow neck bottle or receptacle with a lid. While tumbling, the desired amount of seed treatment composition can be added to the receptacle. The seed is tumbled until it is coated with the treatment composition. After coating, the seed can optionally be dried, for example on a tray.
[0142] In some embodiments, the treated seeds may also be enveloped with a film overcoating to protect the nematicidal coating. Such overcoatings are known in the art and may be applied using conventional fluidized bed and drum film coating techniques. The overcoatings may be applied to seeds that have been treated with any of the seed treatment techniques described above, including but not limited to solid matrix priming, imbibition, coating, and spraying, or by any other seed treatment technique known in the art.
[0143] Application to Soil
[0144] In another aspect of the present invention, the nematicidal treatment composition, diluted as necessary to attain the desired nematicide compound loading, is directly applied to the soil surrounding the root zone of a plant. The application may be performed using any method or apparatus known in the art, including pressurized spray application to the soil surface or injected in the planting furrow, as well as chemigation via overhead sprinkler or drip systems, transplant water treatments, and plant or root dips prior to planting. The rates used for the suspension concentrate formulations for soil application may require 0.5 to 2 kgs per hectare on a broadcast basis (rate per treated area if broadcast or banded).
[0145] Treated Seeds
[0146] Another aspect of the present invention is directed to a seed that has been treated with a nematicidal seed treatment composition as described herein. Typically, the seed has been treated with the seed treatment composition using one of the seed treatment methods set forth above, including but not limited to solid matrix priming, imbibition, coating, and spraying. The seed may be of any plant species, as described above.
[0147] Typically, the treated seeds comprise the nematicidal compound in an amount of at least about 0.05 mg/seed, more typically from about 0.05 to about 1 mg/seed, and even more typically from about 0.05 to about 0.5 mg/seed.
[0148] In some embodiments, wherein the composition comprises a paraffinic hydrocarbon solvent, the loading of active ingredient per treated seed can be significantly reduced without compromising nematicidal efficacy. For example, when the seed treatment composition comprises a paraffinic hydrocarbon solvent, the treated seeds may comprise the nematicidal compound in an amount of less than about 0.2 mg/seed, in an amount of about 0.1 mg/seed, from about 0.01 to about 0.2 mg/seed, or from about 0.02 to about 0.08 mg/seed.
[0149] The following examples are to be considered as merely illustrative, and are not intended to limit the scope of this invention.
EXAMPLES
[0150] Several active nematicidal compounds were combined with selected dispersants and other excipients and used in preparation of suspension concentrate compositions in the following examples. The nematicidal compounds are identified in Table 1.
[0000]
TABLE 1
Ia-i
3-phenyl-5- (thiophen-2- yl)-1,2,4- oxadiazole
Ia-ii
3-(4- chlorophenyl)- 5-(furan-2-yl)- 1,2,4-oxadiazole
Ia-iii
3-(4-chloro-2- methylphenyl)- 5-(furan-2-yl)- 1,2,4-oxadiazole
Example 1
Preparation of a suspension concentrate comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i)
[0151] A quantity of the nematicidal compound Ia-i (25.00 g) was added to an aqueous solution of water (25.00 g), glycerin (2.15 g), MORWET D-500 dispersant (0.32 g), and AGNIQUE DF 6889 antifoam agent (0.05 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 100 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0152] After milling the mixture for 1 hour 40 minutes at a speed of 50 v/140 v, a white aqueous suspension (45.25 g) was collected. The particle size characteristics of the suspension were analyzed with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The results indicated a mean particle size of 4.896 μm, with a median particle size of 2.937 μm. The suspension was determined to contain 47.6% (w/w) of the Ia-i nematicide.
Example 2
Preparation of a Suspension Concentrate Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i)
[0153] A quantity of the nematicidal compound Ia-i (30.00 g) was added to an aqueous solution of water (25.00 g), glycerin (3.00 g), MORWET D-500 dispersant (0.60 g), and AGNIQUE DF 6889 antifoam agent (0.05 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 100 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0154] After milling the mixture for 1 hour 30 minutes at a speed of 50 v/140 v, and an additional 2 hours 15 minutes at 40 v/140 v, a white aqueous suspension (45.20 g) was collected. The suspension was determined to contain 51.2% (w/w) of the Ia-i nematicide.
Example 3
Preparation of a suspension concentrate comprising 3-(4-chlorophenyl)-5-(furan-2-yl)-1,2,4-oxadiazole (Ia-ii)
[0155] A quantity of the nematicidal compound Ia-ii (34.00 g) was added to an aqueous solution of water (25.00 g), glycerin (3.00 g), MORWET D-500 dispersant (0.60 g), and AGNIQUE DF 6889 antifoam agent (0.10 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 100 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0156] After milling the mixture for 4 hours at a speed of 50 v/140 v, a white aqueous suspension (45.40 g) was collected. The particle size characteristics of the suspension were analyzed with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The results indicated a mean particle size of 4.58 μm, with a median particle size of 3.14 μm. The suspension was determined to contain 54.2% (w/w) of the Ia-ii nematicide.
Example 4
Preparation of a Suspension Concentrate Comprising 3-(4-chloro-2-methylphenyl)-5-(furan-2-yl)-1,2,4-oxadiazole (Ia-iii)
[0157] A quantity of the nematicidal compound Ia-iii (34.00 g) was added to an aqueous solution of water (25.00 g), glycerin (3.00 g), MORWET D-500 dispersant (0.60 g), and AGNIQUE DF 6889 antifoam agent (0.05 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 100 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0158] After milling the mixture for 4 hours at a speed of 50 v/140 v, a white aqueous suspension (49.10 g) was collected. The particle size characteristics of the suspension were analyzed with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The results indicated a mean particle size of 3.217 μm, with a median particle size of 2.192 μm. The suspension was determined to contain 54.2% (w/w) of the Ia-iii nematicide.
Example 5
Preparation of a Suspension Concentrate Comprising 3-(4-chlorophenyl)-5-(furan-2-yl)-1,2,4-oxadiazole (Ia-ii)
[0159] A quantity of the nematicidal compound Ia-ii (34.00 g) was added to an aqueous solution of water (141.67 g), glycerin (17.00 g), and MORWET D-500 dispersant (3.40 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 500 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0160] After milling the mixture for 1 hour at a speed of 75 v/140 v, a small amount of AGNIQUE DF 6889 antifoam agent (0.10 g) was added. The mixture was then further stirred at 75 v/140 v for 45 minutes, and at 60 v/140 v for an additional 1 hour 45 minutes.
[0161] Following the milling process, a white aqueous suspension (330.5 g) was collected from the container. The particle size characteristics of the suspension were analyzed with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The results indicated a mean particle size of 2.90 μm, with a median particle size of 1.74 μm. The suspension was determined to contain 52.8% (w/w) of the Ia-ii nematicide.
Example 6
Preparation of a Suspension Concentrate Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i)
[0162] A quantity of the nematicidal compound Ia-i (34.00 g) was added to an aqueous solution of water (141.67 g), glycerin (17.00 g), and MORWET D-500 dispersant (3.40 g). The resulting mixture was milled with a SIZEGVARI ATTRITOR milling system made by UNION PROCESS containing stainless steel beads having a diameter of ⅛ inch in a 500 mL jacketed metal container. The stirring speed was controlled by a VARIAC variable autotransformer.
[0163] After milling the mixture for 1 hour at a speed of 75 v/140 v, a small amount of AGNIQUE DF 6889 antifoam agent (0.10 g) was added. The mixture was then further milled at 75 v/140 v for 45 minutes and at 60 v/140 v for an additional 1 hour 45 minutes.
[0164] Following the milling process, a white aqueous suspension (305.3 g) was collected from the container. The particle size characteristics of the suspension were analyzed with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The results indicated a mean particle size of 3.334 μm, with a median particle size of 2.071 μm. The suspension was determined to contain 52.8% (w/w) of the Ia-i nematicide.
Example 7
Effect of Milling Time on the Mean/Median Particle Size Diameter of a Suspension Concentrate Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i)
[0165] A quantity of the nematicidal compound Ia-i (362.4 g) was added to an aqueous solution of water (283.34 g), glycerin (34.00 g), and MORWET D-500 dispersant (6.80 g). The resulting mixture was pre-milled with a dissolver apparatus at 1900 rpm for 20 minutes. A portion of the resulting pre-milled slurry (60% of the total volume) was added to a NETZSCH MINI ZETA II milling machine filled with zirconium beads having a diameter of 1.6-2 mm. The slurry was milled for 1 hour, after which a sample of the resulting white slurry (250 g) was collected.
[0166] During the milling process, samples were periodically extracted for analysis using a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320). The resulting mean and median particle diameters for each sample are summarized in Table 2 below:
[0000]
TABLE 2
Milling Time (mins)
Mean (μm)
Median (μm)
Mean/Median
15
4.073
2.834
1.437
30
3.041
2.062
1.475
45
2.872
1.851
1.551
60
2.781
1.760
1.580
[0167] The final suspension was determined to contain 44.2% (w/w) of the Ia-i nematicide. This example demonstrates that the mean and/or median particle size of the formulation can be controlled as a function of the total milling time.
Example 8
Preparation of seed treatment compositions
[0168] Seed treatment compositions were prepared using the suspension concentrate compositions prepared in Examples 2-4 above.
[0169] Composition 1: A seed treatment composition comprising the nematicidal compound Ia-i was prepared by mixing a portion of the composition prepared in Example 2 (8.00g) with CF CLEAR seed coat polymer (0.30 g), BECKER-UNDERWOOD seed gloss (1.00 g), and BECKER-UNDERWOOD red color coating (2.00 g).
[0170] Composition 2: A seed treatment composition comprising the nematicidal compound Ia-iii was prepared by mixing a portion of the composition prepared in Example 3 (18.40g) with CF CLEAR seed coat polymer (0.69 g), BECKER-UNDERWOOD seed gloss (2.30 g), and BECKER-UNDERWOOD red color coating (4.60 g).
[0171] Composition 3: A seed treatment composition comprising the nematicidal compound Ia-ii was prepared by mixing a portion of the composition prepared in Example 4 (18.40 g) with CF CLEAR seed coat polymer (0.69 g), BECKER-UNDERWOOD seed gloss (2.30 g), and BECKER-UNDERWOOD red color coating (4.60 g).
Example 9
Treatment of Seeds with Nematicidal Compositions
[0172] Soybean seeds (2.2 kg) were added to a WILLY NIKLAUS GMBH seed treating apparatus. The seeds were tumbled inside the treater while a quantity of seed treatment formulation was added. To ensure full dispersion of the treatment composition, seeds were allowed to tumble for an additional 30 seconds before being collected.
[0173] The amount of seed treatment composition used in each prepared sample was varied in accordance with the targeted amount of active ingredient per seed. As shown in the table below, the targeted amount ranged from 0.1 to 0.5 mg/seed for Ia-i, and from 0.1 to 1 mg/seed for Ia-iii and Ia-ii. The actual amount of active ingredient per seed was analyzed upon removal from the seed treatment apparatus. The results are summarized in the table below, where the “Composition No.” refers to the compositions 1-3 prepared in Example 8.
[0000]
TABLE 3
Targeted
Actual
Amount of
Composition
Active
Active Loading
Active Loading
Composition
No.
Ingredient
(mg/seed)
(mg/seed)
(g)
1
Ia-i
0.1
0.07
0.98
1
Ia-i
0.3
0.22
2.94
1
Ia-i
0.5
0.37
4.90
3
Ia-ii
0.1
0.07
0.92
3
Ia-ii
0.3
0.25
2.77
3
Ia-ii
0.5
0.46
4.62
3
Ia-ii
0.0
0.83
9.24
2
Ia-iii
0.1
0.04
0.92
2
Ia-iii
0.3
0.21
2.77
2
Ia-iii
0.5
0.40
4.62
2
Ia-iii
0.0
0.65
9.24
[0174] The results indicate that, for each sample, a significant portion of the active nematicidal ingredient added to the seed treatment apparatus was successfully transferred to the seed.
Example 10
Preparation of Suspension Concentrate Compositions
[0175] An additional series of suspension concentrate compositions were prepared using the procedures set forth below.
[0176] A stock buffer solution was prepared by adding anhydrous monobasic potassium phosphate (9.361 g) and dibasic sodium phosphate heptahydrate (32.732 g) to a 1 liter volumetric flask, the balance of which was filled with deionized water. The flask was shaken until the salts were fully dissolved, providing a clear buffer solution with a pH of 7.
[0177] For each sample, a blank solution was then prepared by combining MORWET D-425 dispersant, PLURONIC L-35 secondary dispersant, propylene glycol, and a quantity of the stock buffer solution as prepared above. The relative proportions of these components in each sample, respectively, are provided in Table 4 below.
[0178] In the next step of the process, the blank solution was mixed with a quantity of Ia-i nematicide and a small amount of BYK-016 antifoam agent in a 1 liter beaker. The formulation was then agitated with a Tekmar homogenizer at 9,000 rpm for 10 to 12 minutes, resulting in a slurry. The particle size of the pre-milled slurry was measured with a BECKMAN COULTER LS Particle Size Analyzer (model LS 13 320).
[0179] For formulation Sample A and Sample C the pre-milled slurry was then added to a NETZSCH MINI ZETA II apparatus filled with either glass or zirconium oxide beads (200 mL) equipped with cooling water. After milling for 35 minutes, the resulting white slurry was collected, and the particle size was measured as described above. Formulation Sample B was pre-milled only to give a median particle size of 5.8 μm. The particle size can be reduced further through optimization of the pre-milling process.
[0180] A stabilizer composition was prepared by adding KELZAN CC stabilizing agent (4.00 g) and PROXEL GXL biocide (8.00 g) to deionized water (388.00 g). After agitation with a mechanical stirrer at room temperature for 30 minutes, a homogeneous viscous liquid was obtained.
[0181] The milled slurry was then mixed with a stabilizer composition in a 9:1 weight ratio to provide a flowable suspension concentrate composition. A summary of three representative composition samples prepared according to this process is provided below:
[0000]
TABLE 4
Sample A
Sample B
Sample C
Ingredient
(wt. %)
(wt. %)
(wt. %)
Ia-i
45.91
45.91
45.91
MORWET D-425
1.13
1.13
4.52
Propylene glycol
5.65
5.65
5.65
Water
35.99
35.99
32.60
BYK-016
0.31
0.31
0.31
PLURONIC ® L-35
0.06
0.06
0.06
Buffer solution
0.94
0.94
0.94
Stabilizer (1% solution)
10.00
10.00
10.00
[0182] As indicated above, the compositions prepared according to this process were all able to achieve an active ingredient loading of at least about 45% by weight. Each of the compositions was measured to have an average median particle size of from 1.0 to 1.2 microns, with a polydispersity index (median/mean) of from 1.4 to 1.5. Each of the compositions was observed to be storage stable at room temperature for more than three months.
[0183] The formulations can also be prepared with Netzch Mini Zeta II milling machine via a pass mode. In a typical example, the formulation was first pre-milled with a homogenizer and then added to the milling machine. After the formulation was passed through the milling machine, it was collected and then added to the milling machine again. After passing through the milling machine at 3504 rpm three times, the formulation was collected and mixed with the KELZAN stabilizer composition to give the final formulation. The particle size of the formulation was measured before the stabilizer was added. The formulations prepared by the multiple pass mode are shown in Table 5. The particle sizes for these formulations are shown in Table 6.
[0000]
TABLE 5
Sample D
Sample E
Sample F
Ingredient
(wt. %)
(wt. %)
(wt. %)
Ia-i
47.79
47.79
47.79
MORWET D-425
2.26
2.26
2.26
ISOPAR M
2.26
2.26
—
humic acid, sodium salt
2.26
—
2.26
Propylene glycol
5.65
5.65
5.65
Water
39.06
41.32
41.32
BYK-016
0.31
0.31
0.31
PLURONIC ® L-35
0.06
0.06
0.06
Buffer solution
0.039
0.039
0.039
Stabilizer composition
0.10
0.10
0.10
1,2-benzisothiazolin-3-one
0.20
0.20
0.20
[0000]
TABLE 6
Formulation
Mean (μm)
Median (μm)
Mean/Median
Sample D
2.63
1.87
1.41
Sample E
2.80
1.93
1.45
Sample F
2.37
1.62
1.46
Example 11
Differential Scanning Calorimetry Analysis
[0184] Eleven batches of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) were characterized for polymorphic form using differential scanning calorimetry (DSC) analysis. DSC data were collected using a TA INSTRUMENTS Q2000 DSC apparatus.
[0185] For each batch, samples in the mass range of 1 to 10 mg were crimped in aluminum sample pans and scanned over a range of 25° C. to about 120° C., increasing at a rate of 2° C. to 10° C. per minute, and using a nitrogen purge at 50 mL/min.
[0186] The melting point onset ranged from approximately 106° C. to 108° C., with enthalpy of fusion ranging from approximately 108 to 122 J/g. The results are shown below in Table 7. Enthalpy of fusion measurements were obtained on single sample analysis using a relatively small sample size of approximately 2 mg.
[0000]
TABLE 7
DSC Analysis Summary
Batch
Melting Point Onset
Enthalpy of Fusion (J/g)
A
107.0 C.
116.6
B
107.7 C.
117.1
C
107.3 C.
118.9
D
107.0 C.
119.4
E
107.4 C.
110.1
F
107.7 C.
121.7
G
107.0 C.
118.9
H
106.1 C.
107.5
I
106.7 C.
110.0
J
107.3 C.
108.7
K
107.9 C.
111.0
[0187] The thermal behavior of batch G was determined using differential scanning calorimetry and thermogravimetric analysis. The DSC thermogram exhibited a sharp melting endotherm with an onset of 106.9° C. and an enthalpy of fusion of 118.9 J/g.
[0188] Microscopic evaluation of lot G showed birefringent acicular to columnar shaped particles, ranging in size from approximately 5 to 100 microns. FIG. 1 shows the representative photomicrograph.
Example 12
Solvent Recrystallization
[0189] To perform the solvent-based portion of the polymorph screen, the 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole test material was recrystallized using various solvents under approximately 240 different crystal growth conditions. The scale of the recrystallization experiments was from approximately 0.5 mL to 15 ml. The crystal growth conditions were changed by using binary gradient arrays of solvent mixtures and by changing the saturation temperature, growth temperature and evaporation rate (rate of supersaturation generation).
[0190] Saturated solutions were prepared by agitating excess (as possible) test material in contact with the various solvent systems at the saturation temperature. If solids did not completely dissolve in the solvent, the mother liquor was separated from the residual solids by filtration. The mother liquor was then heated above the saturation temperature (overheated) to dissolve any remaining solids. The temperature of each solution was then adjusted to the growth temperature and a controlled nitrogen shear flow was introduced to begin solvent evaporation.
[0191] The recrystallization conditions for the seven solvent based panels used during the study are summarized in Table 8A. Each recrystallization panel contained from 27 to 96 wells. The wells within each panel contained different solvent compositions. Because of the different solvent composition in each well, each well acted as a different crystal growth experiment. The compositional solvent matrices for the five recrystallization panels used during the solvent-based portion of the polymorph screen are shown below in Tables 8B through 8F, respectively. Based on the XRD analysis carried out on the screening samples (see Example 18, below) a new polymorph of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole was discovered in these experiments. The starting material was designated as Form I, while the new polymorph was designated as Form II.
[0000]
TABLE 8A
Summary of Recrystallization Panels
N 2
Saturation
Overheat
Growth
Flow
No. of
Scale
Temp.
Temp.
Temp.
Rate
Panel
Wells
(mL)
Solvent
(° C.)
(° C.)
(° C.)
(psi)
1
34
15
Single/
25
55
25
1.5
Binary
2
34
15
Single/
25
NA
80
1.5
Binary
4
27
15
Binary
25
55
50
1.5
6
27
15
Binary
25
NA
65
1.5
7
96
0.5
Binary
25
50
40
2
[0000]
TABLE 8B
Recrystallization Panel 1 (Evaporated at Room Temp)
Well
Solvent
Sample ID
XRD Form
1
methanol
RC1-1
Form I
2
ethanol
RC1-2
Form I
3
trifluoroethanol
RC1-3
Form I
4
1-propanol
RC1-4
Form I
5
2-propanol
RC1-5
Form I
6
1-butanol
RC1-6
Form I
7
2-butanol
RC1-7
Form I
8
water
RC1-8
NA
9
dimethyl formamide
RC1-9
Form I
10
dimethylacetamide
RC1-10
Form I
11
butyl amine
RC1-11
Form I
12
diisopropyl amine
RC1-12
Form I
13
pyridine
RC1-13
Form I
14
nitromethane
RC1-14
Form I
15
acetone
RC1-15
Form I
16
methyl ethyl ketone
RC1-16
Form I
17
isopropyl ether
RC1-17
Form I
18
Ethyl acetate
RC1-18
Form I
19
methyl tert butyl ether
RC1-19
Form I
20
isopropyl acetate
RC1-20
Form I
21
tetrahydrofuran
RC1-21
Form I
22
acetonitrile
RC1-22
Form I
23
methylene chloride
RC1-23
Form I
24
chloroform
RC1-24
Form I
25
toluene
RC1-25
Form I
26
heptane
RC1-26
Form I
27
1,4 dioxane
RC1-27
Form I
28
NMP
RC1-28
NA/T
29
DMSO
RC1-29
NA/T
30
xylene
RC1-30
Form I
31
butyl acetate
RC1-31
Form I
32
2-methyl tetrahydrofuran
RC1-32
Form I
33
propylene glycol
RC1-33
NA/T
34
glycerol/pyridine (2:13)
RC1-34
NA/T
[0000]
TABLE 8C
Recrystallization Panel 2 (Evaporated at 80° C.)
Well
Solvent
Sample ID
XRD Form
1
methanol
RC2-1
Form I + II
2
ethanol
RC2-2
Form I
3
trifluoroethanol
RC2-3
Form I
4
1-propanol
RC2-4
Form I II
5
2-propanol
RC2-5
Form I
6
1-butanol
RC2-6
Form I
7
2-butanol
RC2-7
Form I + II
8
water/acetone (7.5/7.5)
RC2-8
Form I
9
DMF/1-butanol (7.5/7.5)
RC2-9
Form II
10
DMA/IPE (7.5/7.5)
RC2-10
Form II
11
butyl amine
RC2-11
Form I
12
diisopropyl amine
RC2-12
Form I + II
13
pyridine
RC2-13
Form I
14
nitromethane
RC2-14
Form I + II
15
acetone
RC2-15
Form I
16
methyl ethyl ketone
RC2-16
Form II
17
isopropyl ether
RC2-17
Form I
18
Ethyl acetate
RC2-18
Form I + II
19
methyl tert butyl ether
RC2-19
Form I
20
isopropyl acetate
RC2-20
Form I + II
21
tetrahydrofuran
RC2-21
Form I
22
acetonitrile
RC2-22
Form I + II
23
methylene chloride
RC2-23
Form I + II
24
chloroform
RC2-24
Form I
25
toluene
RC2-25
Form I + II
26
heptane
RC2-26
Form I + II
27
1,4 dioxane
RC2-27
Form I + II
28
NMP/MeOH (7.5/7.5)
RC2-28
Form II
29
DMSO/EtOH (7.5/7.5)
RC2-29
Form I
30
xylene
RC2-30
Form I
31
butyl acetate
RC2-31
Form I + II
32
2-methyl tetrahydrofuran
RC2-32
Form I
33
PropGly/CHCl3 (7.5/7.5)
RC2-33
Form I
34
glycerol/pyridine (1:14)
RC2-34
Form I
[0000]
TABLE 8D
Recrystallization Panel 4 (Evaporated at 50° C.)
Solvent Matrix and XRD Result for Recrystallization Panel 4
Sample
Ratio of Solvents
Co/Anti-
Solvent
ID
1
2
3
Solvent
DMF
A
12:3
7.5:7.5
3:12
1-butanol
DMA
B
12:3
7.5:7.5
3:12
IPE
MEK
C
12:3
7.5:7.5
3:12
EtOH
NMP
D
12:3
7.5:7.5
3:12
MeOH
TFE
E
12:3
7.5:7.5
3:12
Water
Xylene
F
12:3
7.5:7.5
3:12
IPA
EtOAc
G
12:3
7.5:7.5
3:12
2-butanol
1,4 dioxane
H
12:3
7.5:7.5
3:12
Heptane
DCM
I
12:3
7.5:7.5
3:12
Acetonitrile
Sample
XRD Form
Co/Anti-
Solvent
ID
1
2
3
Solvent
5
A
Form I
Form
Form
1-butanol
I + II
I + II
DMA
B
Form I
Form II
Form
IPE
I + II
MEK
C
Form
Form I
Form I
EtOH
I + II
NMP
D
Form II
Form I
Form I
MeOH
TFE
E
Form II
Form I
No sample
Water
Xylene
F
Form I
Form I
Form I
IPA
EtOAc
G
Form I
Form I
Form I
2-butanol
1,4 dioxane
H
Form I
Form I
Form I
Heptane
DCM
I
Form I
Form I
Form I
Acetonitrile
[0000]
TABLE 8E
Recrystallization Panel 6 (Evaporated at 65° C.)
Solvent Matrix and XRD Result for Recrystallization Panel 6
Sample
Ratio of Solvents
Co/Anti-
Solvent
ID
1
2
3
Solvent
TFE
A
12:3
7.5:7.5
3:12
Isopropyl
Acetate
1-propanol
B
12:3
7.5:7.5
3:12
MEK
THF
C
12:3
7.5:7.5
3:12
Chloroform
Butylamine
D
12:3
7.5:7.5
3:12
Toluene
Diisopropyl-
E
12:3
7.5:7.5
3:12
butyl
amine
acetate
Pyridine
F
12:3
7.5:7.5
3:12
2-meth THF
Nitromethane
G
12:3
7.5:7.5
3:12
DMA
Acetone
H
12:3
7.5:7.5
3:12
NMP
MTBE
I
12:3
7.5:7.5
3:12
DMF
Sample
XRD Form
Co/Anti-
Solvent
ID
1
2
3
Solvent
TFE
A
Form
Form II
Form
Isopropyl
I + II
I + II
Acetate
1-propanol
B
Form
Form
Form I
MEK
I + II
I + II
THF
C
Form
Form I
Form I
Chloroform
I + II
Butylamine
D
Form I
Form I
Form I
Toluene
Diisopropyl-
E
Form I
Form
Form I
butyl
amine
I + II
acetate
Pyridine
F
Form
Form I
Form I
2-meth THF
I + II
Nitromethane
G
Form
Form I
Form I
DMA
I + II
Acetone
H
Form
Form I
Amorphous/
NMP
I + II
LC
MTBE
I
Form I
Form I
Form I
DMF
[0000]
TABLE 8F
Recrystallization Panel 7 (96 Well Plate, Evaporated at 40° C.)
Nitro-
Isopropyl
1,4
Pyridine
methane
Acetone
MEK
EtOAc
MTBE
acetate
THF
DCM
CHCl3
Toluene
dioxane
1
2
3
4
5
6
7
8
9
10
11
12
A
TFE
Form I
Form I
Form
Form
Form I
LC
NA
NA
Form I
NA
Form
Form I
II
II
II
B
1-
NA
Form I +
Form
NA
Form I
Form I
Form I
NA
NA
LC
Form
Form I
propanol
II
II
II
C
IPA
NA
Form
Form
NA
Form
NA
Form I
NA
NA
NA
NA
NA
II
II
II
D
2-
LC
Form
Form
NA
Form I
NA
Form I
NA
NA
NA
NA
NA
butanol
II
II
E
DMF
NA
NA
NA
Form
NA
NA
NA
Form I
Form
NA
NA
NA
II
II
F
DMA
NA
NA
NA
NA
Form I
NA
NA
NA
NA
NA
Form I
NA
G
butyl-
NA
Form
NA
NA
NA
Form I
NA
NA
Form I
NA
NA
NA
amine
II
H
Di-
Form
Form I
Form I
NA
NA
NA
NA
NA
NA
NA
NA
NA
isopropyl
II
amine
Example 13
Recrystallization from the Melt
[0192] Cyclic DSC analysis was performed on lot G (Form I) to determine if 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole would recrystallize from the melt as a different form (solvent-less recrystallization). Experiments were performed by heating the material above the melting temperature, then cooling the material at a rate of 5° C., 10° C., 20° C., 30° C., 40° C. or 50° C. per minute, followed by reheating above the melting temperature. At the 5° C. to 30° C. per minute cooling rates, the first enthalpy of fusion values (for the starting material) were approximately 120 J/g while the second values (for the melting of the solids obtained after cooling the original melt) were approximately 100 J/g. There was also a slight change in the melting point onset (approximately 0.5° C.). It is believed that melting Form I, followed by recrystallization, may result in the formation of Form II.
[0193] The results of the experiments performed at cooling rates of 40° C. and 50° C. per minute were unclear, and may indicate that the experiment was uncontrolled under these conditions.
[0194] FIG. 3 shows a sample cyclic DSC thermogram from the run conducted at a cooling rate of 30° C. per minute.
[0195] In a further experiment, approximately 300-400 mg of Form I starting material was heated to melting in a forced air oven at approximately 120° C. for approximately 40 minutes. The sample was slow cooled to room temperature, and XRD, DSC and proton NMR analyses were performed on this sample. The XRD pattern was different from the starting material (Form I) and was similar to the Form II pattern. DSC exhibited a melting onset temperature of 107.8° C. and enthalpy of fusion of 103.2 J/g.
Example 14
Grinding Analysis
[0196] Batches of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole polymorphic Forms I and II were ground using a CRESCENT WIG-L-BUG ball mill for 2 minutes at 4800 oscillations per minute (3.2 m/s) in two separate experiments. Under these conditions, no transformation was observed in Form I, while the Form II sample transformed to Form I. FIG. 4 shows the XRD overlay of the milled Form I and Form II samples and the reference patterns of Forms I and II. The Form II used in this experiment was obtained by recrystallization from the melt of Form I, as described in Example 14, above,
Example 15
Mechanical Pressure Analysis
[0197] Batches of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole polymorphic Forms I and II were placed in a CARVER press and compressed at approximately 15,000 psi for approximately 20 seconds in two separate experiments. XRD analysis was performed on the samples. The resulting XRD pattern matched the starting material in both experiments, as shown in FIGS. 5A and 5B for Forms I and II, respectively. The pressurized treatment did not reveal any changes in the polymorphic form of the starting material in both experiments. The Form II used in this experiment was obtained by recrystallization from the melt of Form I, as described in Example 14, above.
Example 16
Non-Competitive Slurry Experiments
[0198] In addition to the solvent recrystallization experiments, non-competitive slurry experiments were performed to search for new solid-state forms of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole. These experiments rely on solubility differences of different polymorphic forms (if the compound exists in different polymorphic forms). As such, only polymorphs having a lower solubility (that is, are more stable) than the original crystalline form can result from a noncompetitive slurry experiment.
[0199] Essentially, when a solid is mixed with solvent to create slurry, a saturated solution eventually results. The solution is saturated with respect to the polymorphic form dissolved. However, the solution is supersaturated with respect to any polymorphic form that is more stable (more stable forms have lower solubility) than the polymorphic form initially dissolved. Therefore, any of the more stable polymorphic forms can nucleate and precipitate from solution. In addition, noncompetitive slurry experiments are often useful in identifying solvents that form solvates with the compound.
[0200] The slurry experiments were performed by exposing excess supplied material to solvents and agitating the resulting suspensions for several days at ambient temperature. The solids were filtered using a WHATMAN Grade 1 apparatus (11 μm pore size) and analyzed by XRD to determine the resulting form(s). To avoid possible desolvation or physical change after isolation, the samples were not dried before X-ray analysis. A summary of non-competitive slurry experiments is shown in Table 9.
[0000]
TABLE 9
Vehicle
Initial Form
Duration
Final Form
Methanol
I
12 days
I
Ethanol
I
12 days
I
Trifluoroethanol
I
12 days
I
1-propanol
I
12 days
I
Isopropyl alcohol
I
12 days
I
1-butanol
I
12 days
I
2-butanol
I
12 days
I
water
I
12 days
I
heptane
I
12 days
I
glycerol/water (1:10)
I
12 days
I
propylene glycol/water (1:10)
I
12 days
I
Isopropyl alcohol/water (1:1)
I
12 days
I
ethanol
II
7 days
I
trifruoroethanol
II
7 days
I
1-propanol
II
7 days
I
Isopropyl alcohol
II
7 days
I
1-butanol
II
7 days
I
2-butanol
II
7 days
I
heptane
II
7 days
I
glycerol/water (1:10)
II
7 days
I
propylene glycol/water (1:10)
II
7 days
I
Isopropyl alcohol/water(1:1)
II
7 days
I
[0201] Based on their X-ray scattering behavior, the slurry experiments with Form I as the starting material resulted in Form I after approximately 12 days of slurring (indicating no transformation). The slurry experiments with Form II as the starting material (obtained by recrystallization from the melt, as set forth in Example 14, above) resulted in Form I after approximately 7 days of slurring. These data indicate that Form I is more stable than Form II at ambient temperature and pressure. No new polymorphs, solvates, or hydrates were isolated in these experiments.
Example 17
X-Ray Analysis of Screening Samples
[0202] Batches of solid 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole polymorphs generated from the solvent based recrystallization panels and from other means (slurry, recrystallization from melt in an oven, etc.) were analyzed by powder XRD. To mitigate preferred grain effects, a two dimensional detection system was used to collect all the XRD screening data. The two dimensional detector integrates along the concentric Debye cones which helps reduce pattern variation. An example of the Debye cone integration using a two dimensional detector is shown below. If bright spots appear in the conical rings, it indicates strong preferred grain effects that can lead to considerable variability in the observed diffraction patterns including changes in peak intensities. Some samples of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole exhibited preferred grain effects based on the appearance of the scattering behavior.
[0203] The results of this analysis revealed the material exists as two different polymorphs. The polymorphs were designated as Forms I and II. A powder XRD analysis of the Form I polymorphs, corresponding to the initial test samples, is set forth in FIG. 6 . A powder XRD analysis of the Form II polymorphs is set forth in FIG. 7 .
[0204] The initial test material was designated as Form I. The resulting form designation for each individual (solvent-based) recrystallization experiment is shown in Tables 7B through 7F, above.
Example 18
Summary of Formation of Forms I and II
[0205] A number of different crystallization conditions were used to produce the samples utilized in Examples 12 through 18, above. Polymorphic Form I of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole was obtained in approximately 50% of the experiments under various crystallization conditions. Polymorphic Form II was obtained in approximately 10% of the experiments also under various crystallization conditions. Mixtures of Forms I and II were obtained in approximately 11% of the experiments indicating that the two polymorphs have a tendency to nucleate and grow concomitantly. Form I appears to be the thermodynamically stable form under ambient conditions based on the results of the non competitive slurry experiment. The exact crystallization conditions are shown in Tables 7A through 7F, above.
[0206] Table 10 shows a summary of the results obtained in all the experiment panels in this study. Note that Panels 1, 2, 4, 6, and 7 are described in Example 13, above. Panel 3 corresponds to the recrystallization from the melt as set forth in Example 14, above. Panels 5 and 8 correspond to the noncompetitive slurry experiments conducted with respect to Form I and Form II, respectively, in Example 17, above.
[0000]
TABLE 10
Mix of
No. of
Forms I
No
Panel No.
Experiments
Form I
Form II
and II
Result
Panel 1
34
29
0
0
5
Panel 2
34
17
4
13
0
Panel 3 (Melt)
5
0
3
0
2
Panel 4
27
19
3
4
1
Panel 5 Form 1
12
12
0
0
0
NC Slurry
Panel 6
27
16
1
9
1
Panel 7 96 well
96
19
14
1
62
Panel 8 Form 2
10
10
0
0
0
NC Slurry
Total
245
122
25
27
71
% of total
100%
50%
10%
11%
29%
Example 19
Competitive Slurry Experiments
[0207] In addition to the solvent recrystallization experiments, a competitive slurry experiment was also performed to determine the most stable polymorphic form of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole. These experiments rely on the solubility differences of different polymorphic forms. As such, only polymorphic forms (and solvates) having a lower solubility (more stable) than the form initially dissolved can result from a competitive slurry experiment.
[0208] Essentially, when a solid is dissolved in a (slurry) solvent, a saturated solution eventually results. The solution is saturated with respect to the polymorphic form dissolved. However, the solution is supersaturated with respect to any polymorphic form that is more stable (more stable forms have lower solubility) than the polymorphic form initially dissolved. Therefore, any of the more stable polymorphic forms can nucleate and precipitate from solution. In addition, competitive slurry experiments are often useful in identifying solvents that form solvates with the API.
[0209] The slurry experiment was performed by exposing excess material of Forms I and II to a small volume of neat solvent and agitating the resulting suspensions for several days at ambient temperature. The solids were filtered and analyzed by XRD to determine the resulting form. To avoid possible desolvation or physical change after isolation, the sample was not dried before x-ray analysis. Table 11 shows the results of the competitive slurry experiment.
[0000]
TABLE 11
Initial Forms
Slurry
Final Form
(XRD)
Solvent
Duration
(XRD)
I & II
Isopropyl alcohol
1 week
I
[0210] The thermal data obtained above was used to calculate an approximate value for the transition temperature of conversion of Forms I and II using methods known in the art. The value obtained using this method was approximately 102° C. Based on these calculations, Form I is expected to be the stable form below this temperature and Form II above it. This is another characteristic of an enantiotropic polymorphic relationship.
[0211] A graphical XRD overlay of the competitive slurry experiment is depicted in FIG. 8 .
Example 20
Estimation of Transition Temperature
[0212] Polymorphic Forms I and II of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole, as well as a 50/50 mixture thereof, were analyzed by DSC at a slow heating rate of 2° C. per minute, with similar sample sizes. The melting temperatures and enthalpy of fusion data are shown in Table 12, below. These data indicate that Form I has a lower melting temperature and a higher enthalpy of fusion. Form II has a higher melting temperature and a lower enthalpy of fusion. In accordance with the Heat of Fusion Rule, this indicates that Form I and II have an enantiotropic relationship. FIGS. 9A through 9C show the relevant DSC thermograms for Form I, Form II, and a mixture of Forms I and II, respectively.
[0213] The thermal data using the procedure set forth above was used to calculate an approximate value for the transition temperature of conversion of Forms I and II, resulting in an estimated transition temperature value of 102° C. Based on these calculations, Form I is expected to be the stable form below this temperature, while Form II is expected to possess greater thermodynamic stability above that temperature. This further indicates that Forms I and II exhibit an enantiotropic polymorphic relationship.
[0000]
TABLE 12
Onset
Maximum
Enthalpy of Fusion
Sample ID
(° C.)
(° C.)
(J/g)
Batch G Form I
106.9
107.9
117.9
54478-21-4 Form II
108.0
108.8
98.3
50/50, Form I/II
108.0
108.0, 108.8
114.6
Example 21
Storage Stability of Polymorphs
[0214] To determine the storage stability and/or hydrate formation of 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole Form I material during storage at ambient conditions, samples were monitored in two static humidity chambers. In these studies, samples were stored in open Petri dishes in chambers containing saturated salt solutions to maintain the relative vapor pressure. Solutions of saturated potassium chloride (84% RH) and sodium chloride (75% RH) salts at ambient temperature were used.
[0215] FIG. 10 shows the XRD pattern of the samples stored at 75 and 84% RH after 4 weeks of storage. As indicated in the figure, Form I does not form a hydrate and appears to be thermodynamically stable over time at ambient conditions.
[0216] In contrast, samples of Form II stored in a scintillation vial in a hood under ambient conditions showed signs of transformation to Form I when analyzed by XRD after approximately 6 days of storage. FIG. 11 shows the XRD overlays of Forms I, II and the sample of Form II which showed signs of transformation to Form I.
Example 22
Soybean Cyst Nematode Assay
[0217] Formulations were tested for nematicidal activity against soybean cyst nematode (SCN) in an SCN cup assay.
[0218] The formulations were prepared as follows:
[0219] Preparation of the phosphate buffer solution: To a 1 L volumetric flask were added potassium phosphate monobasic anhydrous (9.329 g) and sodium phosphate dibasic heptahydrate (32.756 g). DI water was added to the flask to the mark and it was inverted 15 times to give a clear solution.
[0220] Preparation of Formulation Blank A: To a 2 L beaker were added MORWET D-425 (43.6 g), DI water (1,386.9 g), the phosphate buffer solution (36.3 g), propylene glycol (217.7 g), and PLURONIC L-35 (2.2 g). The mixture was stirred with a spatula to give a brown solution.
[0221] Preparation of Formulation Blank B: To a 2 L beaker were added MORWET D-425 (174.3 g), DI water (1.256.0 g), the phosphate buffer solution (36.3 g), propylene glycol (217.8 g), and PLURONIC L-35 (2.1 g). The mixture was stirred with a spatula to give a dark brown solution.
[0222] Preparation of the KELZAN stabilizer solution: To a 1 L beaker were added KELZAN CC (4.060 g), PROXEL GXL (7.978 g), and DI water (388.273 g). The mixture was then agitated with a Melton mechanical stirrer (model CM -100) at 2,000 rpm for 30 minutes to give a viscous liquid.
[0223] Preparation of Suspension Concentrate Formulation 3: To a 2 L beaker were added Formulation Blank A (497.3 g), Compound Ia-i (521.4 g), and BYK-016 (3.6 g). The mixture was stirred with a spatula to give a slurry. The mixture was placed in an ice bath and a Tekmar T554 homogenizer (model TR-10) was used for the pre-milling. During the pre-milling, the slurry (1022.3 g) was agitated with the homogenizer at 9,000 rpm for 12 mins. An Eiger mill (model M250) was filled with zirconium oxide beads with an average diameter of 0.3-0.4 mm. Nearly half of the pre-milled slurry (501.4 g) was then added to the Eiger mill and was milled with a speed of 5000 rpm in recycle mode at room temperature. After 30 minutes, the resulting white liquid formulation (412.4 g) was collected and mixed with the KELZAN stabilizer solution (45.8 g) to give the final formulation (458.2 g). The particle size of the formulation was analyzed with a Beckman Coulter particle size analyzer (Model LS 13 320) before the stabilizer was added.
[0224] Preparation of Suspension Concentrate Formulation 4: The pre-milled slurry (501.4 g) from the suspension concentrate formulation above was also milled with the same Eiger mill filled with zirconium oxide beads with an average diameter of 0.3-0.4 mm. After milling for 120 minutes, the resulting white liquid formulation (408.5 g) was collected and mixed with the KELZAN stabilizer solution (45.4g) to give the final formulation (453.9 g). The particle size of the formulation was also analyzed with a Beckman Coulter particle size analyzer (Model LS 13 320) before the stabilizer was added.
[0225] Preparation of Suspension Concentrate Formulation 5: To a 1 L beaker were added Formulation Blank B (383.3 g), Compound Ia-i (261.1 g), and BYK-016 (2.5 g). The mixture was stirred with a spatula to give a slurry. The mixture was placed in an ice bath and a Tekmar T554 homogenizer (model TR-10) was used for the pre-milling. During the pre-milling, the slurry was agitated with the homogenizer at 9,000 rpm for 10 mins. The milling was divided into two stages. Both Netzsch Mini Zeta II filled with glass beads with an average diameter of 0.8-1 mm and Eiger mill (model M250) filled with zirconium oxide beads with an average diameter of 0.1-0.2 mm were used in the milling. In the first stage, the slurry was passed through the Netzsch miller three times and the miller was operated at 3,504 rpm for each pass. In the second stage, the slurry was passed through the Eiger miller ten times and the milling was operated at 5,000 rpm. A white liquid (452.1 g) was collected and part of the white liquid (349.0 g) mixed with the KELZAN stabilizer solution (38.8 g) to give the final formulation (387.8 g). The particle size of the formulation was also analyzed with a Beckman Coulter particle size analyzer (Model LS 13 320) before the stabilizer was added.
[0226] Preparation of Suspension Concentrate Formulation 6: To an 8 dram vial were added MORWET D-425 (0.714 g), DI water (3.75 g), the phosphate buffer solution (0.147 g), ISOPAR M (1.45 g), propylene glycol (0.898 g), PLURONIC L-35 (0.009 g), Compound Ia-i (7.315 g), and BYK-016 (0.067 g). The mixture was stirred followed by addition of 3 mm diameter stainless steel beads (14 mL). The vial was capped and placed on a US Stoneware roller (Ser. No. CK-11009) and rotated at a speed setting of 50. After 2 days the slurry (5.903 g) was collected and mixed with the KELZAN stabilizer solution (0.660 g) to give the final formulation (6.563 g). The particle size of the formulation was analyzed with a Beckman Coulter particle size analyzer (Model LS 13 320) before the stabilizer was added.
[0227] Table 13 below depicts the compositions of each formulation used for seed treatment in the SCN efficacy assay.
[0000]
TABLE 13
Composition of Formulation for
Seed Treatment
Ia-i
Commercial
Formula-
Formula-
Seed
Compound
Treat-
tion
tion
Treatment
Water
Ia-i Rate
ment
Ia-i
(g)
(g)
(g)
(mg/seed)
1
NA
N/A
N/A
N/A
N/A
2
NA
0
1.557
0.64
N/A
3A
3
0.36
0
0.64
0.05
3B
3
2.16
0
1.01
0.3
4A
3
0.36
1.557
0.64
0.05
4B
3
2.16
1.557
1.01
0.3
5A
4
0.36
0
0.64
0.05
5B
4
2.16
0
1.01
0.3
6A
4
0.36
1.557
0.64
0.05
6B
4
2.16
1.557
1.01
0.3
7A
5
0.45
0
1.21
0.05
7B
5
2.73
0
1.16
0.3
8A
5
0.45
1.557
1.21
0.05
8B
5
2.73
1.557
1.16
0.3
9A
6
0.36
0
0.64
0.05
9B
6
2.16
0
1.01
0.3
10A
6
0.36
1.557
0.64
0.05
10B
6
2.16
1.557
1.01
0.3
[0228] SCN Efficacy Assay
[0229] A4630 soybean plants were grown in cups filled with full strength Murashige & Skoog basal salts fertilizer (Phytotech Cat. No. 201080-52) followed by 180 ml of 20:80 soil/sand mixture (sterile St. Charles sand and US 10 soil premixed by Hummert). A Gustafson Batch Modular Coater (BMC) Treater was used to the treat the soybean seeds with the formulations as described in Table 13.
[0230] The untreated seed and treated seed were placed on top of 20:80 soil and pushed ½ inch deep into the soil. The cups were placed in the growth chamber and the soil was misted with water to saturation. Propagation domes were placed over the cups until the seeds had germinated (about 3 to 5 days). Conditions in the growth chamber were as follows: 28° C., 60% relative humidity, and 16 h/14 h day/night periods, with 347 μ Einsteins of light.
[0231] Ten days after planting, soybean cyst inoculum (2×500 μL, 5000 eggs/cup) was delivered into the soil on two sides of the soybean plant. The plants were grown for an additional 5 weeks after inoculation and watered as needed with overhead watering.
[0232] The efficacy of the formulations was determined by harvesting plants (45 days) and counting cysts. Table 14 summarizes the bioefficacy against SCN at 50 μg/seed and 300 μg/seed.
[0000]
TABLE 14
Treat-
Particle
Rate
Cyst Counts
ment
Size (μm)
(mg/seed)
Mean
Std Dev
Std Err Mean
1
N/A
227
159
65
2
N/A
337
205
84
3A
0.8
0.05
149
80
33
3B
0.3
67
47
19
4A
0.8
0.05
247
244
100
4B
0.3
92
106
43
5A
0.48
0.05
146
55
22
5B
0.3
90
58
24
6A
0.48
0.05
203
193
79
6B
0.3
57
71
29
7A
0.065
0.05
137
86
35
7B
0.3
150
55
25
8A
0.065
0.05
176
101
41
8B
0.3
86
70
29
9A
1.7
0.05
147
97
40
9B
0.3
80
89
36
10A
1.7
0.05
92
63
28
10B
0.3
76
64
26
Example 23
Preparation of Suspension Concentrates Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) and imidacloprid
[0233] Several suspension concentrate co-formulation compositions comprising the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) and imidacloprid were prepared. A summary of five representative co-formulation compositions prepared in this Example is provided below in Tables 15-19.
[0234] The phosphate buffer was prepared by adding potassium phosphate monobasic anhydrous (9.361 g) and sodium phosphate dibasic heptahydrate (32.732 g) to a 1 L volumetric flask. Then DI water was added to the flask to the mark. After it was shaken for a while, all the salts were dissolved to give a clear phosphate buffer with pH at 7.
[0235] The KELZAN thickener/stabilizer was prepared by adding KELZAN CC (4.00 g) and PROXEL GXL (8.00 g) to DI water (388.00 g) and agitating with a mechanical disperser at 2,900 rpm at room temperature for 30 minutes to obtain a viscous liquid (400 g).
[0236] The suspension concentrate co-formulation compositions were prepared by mixing all the ingredients in Part A at 300 rpm for 30 minutes or until the MORWET D-425 dissolved; adding all the ingredients in Part B to Part A and mixing at 300 rpm for 5 minutes; adding all the ingredients in Part C to the mixture of Parts A and B and homogenizing the solution at 9,000 rpm for 10 minutes; preparing a combination of ground (grinding was done using the roller with grinding media (Very High Density Zirconium Oxide Grinding Media, Yttria stabilized ½×½ cylinders)) Ia-i and imidacloprid (Part D) in a jar and pouring the solution above (Parts A, B, and C) in a controlled path; homogenizing the solution at 9000 rpm for 30 minutes with an ice bath; milling the solution 4 times to achieve the desired particle size; adding Part E to the collected sample and mixing at 500 rpm for 10 minutes; and adding Parts F, G and H (if present) to the collected sample and mixing at 900 rpm for 30 minutes.
[0237] ATLOX 4913 (available from Croda) is used as a crystal growth inhibitor. The weight percentage values reported in Tables 15-19 are theoretical, and were calculated based upon the weight of the actives added. Particle sizes reported in Tables 15-19 were measured by Beckman Coulter particle size analyzer (Beckman Coulter LS 13 320 laser diffraction particle size analyzer).
[0000]
TABLE 15
Co-Formulation of Ia-i and Imidacloprid (particle size 2.196 μm)
Amount
Theoretical
Actual
Part
Ingredient
(g)
Wt %
Wt %
A
MORWET D-425
0.36
2.17
DI water
2.45
14.78
B
Buffer
0.15
0.90
DI water
2.44
14.72
C
Propylene glycol
0.90
5.43
ISOPAR M
0.36
2.17
Antifoam
0.05
0.30
PLURONIC L-35
0.009
0.05
D
Ia-i
5.93
35.77
34.1
Imidacloprid
1.68
10.13
8.7
E
Stabilizer
1.59
9.60
Humic acid sodium salt
0.66
3.98
[0000]
TABLE 16
Co-Formulation of Ia-i and Imidacloprid (particle size 1.91 μm)
Amount
Theoretical
Actual
Part
Ingredient
(g)
Wt %
Wt %
A
MORWET D-425
0.36
2.17
DI water
2.45
14.74
B
Buffer
0.15
0.90
DI water
2.44
14.68
C
Propylene glycol
0.90
5.42
ISOPAR M
0.36
2.17
Antifoam
0.05
0.30
PLURONIC L-35
0.009
0.05
D
Ia-i
5.17
31.11
28.97
Imidacloprid
2.44
14.68
13.17
E
ATLOX 4913
0.34
2.05
F
Stabilizer
1.59
9.58
G
Humic acid sodium salt
0.36
2.17
[0000]
TABLE 17
Co-Formulation of Ia-i and Imidacloprid (particle size 1.95 μm)
Amount
Theoretical
Actual
Part
Ingredient
(g)
Wt %
Wt %
A
MORWET D-425
0.36
2.17
DI water
2.45
14.74
B
Buffer
0.15
0.90
DI water
2.44
14.68
C
Propylene glycol
0.90
5.42
ISOPAR M
0.36
2.17
Antifoam
0.05
0.30
PLURONIC L-35
0.009
0.05
D
Ia-i
5.17
31.11
28.82
Imidacloprid
2.44
14.68
12.97
E
ATLOX 4913
0
0
F
Stabilizer
1.59
9.58
G
Humic acid sodium salt
0
0.00
H
Water
0.7
4.21
[0000]
TABLE 18
Co-Formulation of Ia-i and Imidacloprid (particle size 1.94 μm)
Amount
Theoretical
Actual
Part
Ingredient
(g)
Wt %
Wt %
A
MORWET D-425
0.36
2.17
DI water
2.45
14.74
B
Buffer
0.15
0.90
DI water
2.44
14.68
C
Propylene glycol
0.90
5.42
ISOPAR M
0.36
2.17
Antifoam
0.05
0.30
PLURONIC L-35
0.009
0.05
D
Ia-i
5.17
31.11
29.11
Imidacloprid
2.44
14.68
13.19
E
ATLOX 4913
0
0
F
Stabilizer
1.59
9.58
G
Humic acid sodium salt
0.36
2.17
H
Water
0.34
2.05
[0000]
TABLE 19
Co-Formulation of Ia-i and Imidacloprid (particle size 1.92 μm)
Amount
Theoretical
Actual
Part
Ingredient
(g)
Wt %
Wt %
A
MORWET D-425
0.36
2.17
DI water
2.45
14.74
B
Buffer
0.15
0.90
DI water
2.44
14.68
C
Propylene glycol
0.90
5.42
ISOPAR M
0.36
2.17
Antifoam
0.05
0.30
PLURONIC L-35
0.009
0.05
D
Ia-i
5.17
31.11
28.95
Imidacloprid
2.44
14.68
13.36
E
ATLOX 4913
0.34
2.05
F
Stabilizer
1.59
9.58
G
Humic acid sodium salt
0
0.00
H
Water
0.36
2.17
Example 24
Aged Stability Studies of Suspension Concentrates Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) and imidacloprid
[0238] The five suspension concentrate co-formulation compositions comprising the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) and imidacloprid prepared in Example 23 were subjected to an aged stability study.
[0239] In this study, particle size was measured by Beckman Coulter particle size analyzer (Beckman Coulter LS 13 320 laser diffraction particle size analyzer), viscosity was measured by Brookfield R/S plus Rheometer, and the wt % values of Ia-i and imidacloprid were determined using HPLC.
[0240] Each concentrate co-formulation composition was sampled into individual jars and labeled for room temperature (RT) time 0, RT 4 weeks, RT 8 weeks, 50° C. 4 weeks and 50° C. 8 weeks. Both 50° C. 4 weeks and 50° C. 8 weeks samples were stored in a lab oven with temperature set at 50° C.
[0241] At time 0, RT time 0 samples were tested. At 4 weeks, the 50° C. 4 weeks samples were taken out of oven and set on the bench for 24 hours to let the temperature reach RT. Then the RT 4 weeks samples and 50° C. 4 weeks samples were tested. At 8 weeks, the 50° C. 8 weeks samples were taken out of oven and set on the bench for 24 hours to let the temperature reach RT. Then the RT 8 weeks samples and 50° C. 8 weeks samples were tested.
[0242] The testing results of the aged stability study for the five suspension concentrate co-formulation compositions summarized in Tables 15-19 are reported below in Tables 20-24, respectively. Note that there is a slight discrepancy in the measured concentrations of Ia-i and imidacloprid as compared to the theoretical values reported above in Tables 15-19 for reasons known in the art; for example, the actives may not have been 100% pure, or there may have been loss of active during the milling and/or processing of the sample.
[0000]
TABLE 20
Aged Stability Studies for Composition in Table 15
Time
4 weeks
4 weeks
8 weeks
8 weeks
0
(RT)
(50° C.)
(RT)
(50° C.)
Concentration Ia-i (wt %)
34.1
34.3
34.2
33.8
33.7
Concentration
8.7
8.88
9.08
8.8
8.6
imidacloprid (wt %)
Particle size (μm)
2.196
1.949
2.061
2.094
1.927
Viscosity (cP)
134.68
185.35
212.85
164.97
202.32
pH
9.28
9.25
9.09
9.32
8.91
[0000]
TABLE 21
Aged Stability Studies for Composition in Table 16
Time
4 weeks
4 weeks
8 weeks
8 weeks
0
(RT)
(50° C.)
(RT)
(50° C.)
Concentration Ia-i (wt %)
28.97
29.43
29.43
30.13
30.12
Concentration
13.17
14.45
14.42
13.9
13.86
imidacloprid (wt %)
Particle size (μm)
1.913
1.97
1.972
1.86
1.904
Viscosity (cP)
92.46
101.54
123.32
99.82
119.71
pH
9.09
8.91
8.44
8.83
8.55
[0000]
TABLE 22
Aged Stability Studies for Composition in Table 17
Time
4 weeks
4 weeks
8 weeks
8 weeks
0
(RT)
(50° C.)
(RT)
(50° C.)
Concentration Ia-i (wt %)
28.82
29.49
28.95
30.1
30.09
Concentration
12.97
14.52
14.21
13.98
13.95
imidacloprid (wt %)
Particle size (μm)
1.95
1.917
1.961
1.813
1.832
Viscosity (cP)
49.68
61.6
68.1
52.19
61.92
pH
8.55
8.36
8.39
8.22
8.28
[0000]
TABLE 23
Aged Stability Studies for Composition in Table 18
Time
4 weeks
4 weeks
8 weeks
8 weeks
0
(RT)
(50° C.)
(RT)
(50° C.)
Concentration Ia-i (wt %)
29.11
29.38
29.4
29.97
30.21
Concentration
13.19
14.37
14.13
13.91
13.76
imidacloprid (wt %)
Particle size (μm)
1.939
1.867
1.924
1.817
1.883
Viscosity (cP)
77.03
86.7
104.39
82.64
101.28
pH
9.5
9.29
8.86
9.18
8.78
[0000]
TABLE 24
Aged Stability Studies for Composition in Table 19
Time
4 weeks
4 weeks
8 weeks
8 weeks
0
(RT)
(50° C.)
(RT)
(50° C.)
Concentration Ia-i (wt %)
28.95
29.34
29.22
29.73
30.12
Concentration
13.36
14.4
14.4
13.89
13.99
imidacloprid (wt %)
Particle size (μm)
1.916
1.902
1.885
1.859
1.864
Viscosity (cP)
61.23
63.54
70.48
56.8
64.73
pH
7.36
7.29
7.3
7.16
7.21
Example 25
Preparation of Suspension Concentrates Comprising 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i)
[0243] Several suspension concentrate formulation compositions comprising the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) were prepared. A summary of three representative suspension concentrate formulation compositions prepared in this Example is provided below in Tables 25-27.
[0244] The phosphate buffer was prepared by adding potassium phosphate monobasic anhydrous (9.361 g) and sodium phosphate dibasic heptahydrate (32.732 g) to a 1 L volumetric flask. Then DI water was added to the flask to the mark. After it was shaken for a while, all the salts were dissolved to give a clear phosphate buffer with pH at 7.
[0245] The KELZAN thickener/stabilizer was prepared by adding KELZAN CC (4.00 g) and PROXEL GXL (8.00 g) to DI water (388.00 g) and agitating with a mechanical disperser at 2,900 rpm at room temperature for 30 minutes to obtain a viscous liquid (400 g). The same composition and preparation procedure were used to prepare KELZAN thickener/stabilizer with a scale up to 1 kg.
[0246] Ground Ia-i was prepared by adding it to a plastic bottle half filled with cylindrical ceramic beads (½″ O.D.×½″ long) and rotated for 30 minutes on a roller. Ground Ia-i was then collected after sieving through a screen and used in preparation of the suspension concentrate formulation.
[0247] The suspension concentrate formulation compositions were prepared by first preparing a formulation blank by adding MORWET D-425 (81.6 g) to DI water (1027.4 g) in a 1 gallon jar. After MORWET D-425 was dissolved, propylene glycol (204.1 g) phosphate buffer (34.0 g), PLURONIC L-35 (2.04 g), antifoam (11.34 g), and ISOPAR M (81.6 g) were added to the jar and it was then agitated in an ice bath with a homogenizer at 9,000 rpm for 6 minutes to give a brown emulsion (1442.1 g).
[0248] To a 1 gallon jar were added the formulation blank and ground Ia-i, and the resulting mixture was well stirred with a spatula. Then the jar was placed in an ice bath and a Tekmar homogenizer (model T 45 S4) was inserted into the slurry and the head of the homogenizer in the center of the jar was about 5 mm above the bottom of the jar. Initially it was operated at 10,000 rpm for 3 minutes and then at 9,000 rpm for 27 minutes. The particle size of the resulting slurry was measured after it was milled for 30 minutes. If large particles still existed in the formulation slurry, it was milled for additional 5 to 10 minutes. Particle size was measured by Beckman Coulter particle size analyzer (Beckman Coulter LS 13 320 laser diffraction particle size analyzer).
[0249] A NETZCH MINI ZETA II mill apparatus filled with glass beads with a diameter of 0.7-1 mm (200 ml) was used in the milling. The mill was connected to the water line and cold water was used to control the temperature increase during the milling. Before it was used, small amount of the formulation blank (15.0 g) was added to the machine first and the machine was then run at 3504 rpm for 30 s. Compressed nitrogen was used to push the residual formulation blank out of the machine.
[0250] For the preparation of the suspension concentrate formulations in this example, the pass method was used to reduce the particle size of the formulation. During the milling, the formulation slurry obtained from pre-milling as described above was added to the mill when operated at 3504 rpm. After milled through the mill, the formulation was collected. Then the same milling was repeated twice to give the formulation with an average median particle of about 2 μm with a particle size range of from about 1.6 to about 2.5 μm. If the particle size is still large, the fourth or additional milling is required.
[0251] In post treatment, the KELZAN thickener/stabilizer, humic acid sodium salt, and ATLOX 4913 were added to the collected formulation slurry and it was then stirred with a mechanical stirrer at room temperature for 30 minutes to obtain the suspension concentrate formulation in the form of a brown slurry. The wt % values reported in Tables 25-27 for the ATLOX 4913, stabilizer, humic acid sodium salt, and water are based on sample amounts recovered after milling (for example, if a total of 1000 g of formulation blank and nematicidal component are milled and 800 g are recovered after milling, the amount of post milling components added are based on 800 g).
[0000]
TABLE 25
Formulation 7
Ingredient
Wt %
MORWET D-425
2.17
Buffer
0.91
Propylene glycol
5.43
ISOPAR M
0.36
Antifoam (1520-US)
0.30
PLURONIC L-35
0.05
Ia-i
45.88
ATLOX 4913
4.00
Stabilizer
9.60
Humic acid sodium salt
2.17
Water
4.53
[0000]
TABLE 26
Formulation 8
Ingredient
Wt %
MORWET D-425
2.17
Buffer
0.91
Propylene glycol
5.43
ISOPAR M
2.17
Antifoam (1520-US)
0.30
PLURONIC L-35
0.05
Ia-i
45.88
ATLOX 4913
4.00
Stabilizer
9.60
Humic acid sodium salt
2.17
Water
27.32
[0000]
TABLE 27
Formulation 9
Ingredient
Wt %
MORWET D-425
2.17
Buffer
0.91
Propylene glycol
5.43
ISOPAR M
2.17
Antifoam (BYK-016)
0.30
PLURONIC L-35
0.05
Ia-i
45.88
ATLOX 4913
4.00
Stabilizer
9.60
Humic acid sodium salt
2.17
Water
27.32
Example 26
Preparation of Suspension Concentrates Comprising Nematicidal Compound and a Second Active
[0252] Several suspension concentrate co-formulation compositions comprising the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i) or 3-(4-chloro-2-methylphenyl)-5-(furan-2-yl)-1,2,4-oxadiazole (Ia-iii) and various fungicides or insecticides as a second active were prepared. A summary of sixteen representative co-formulation compositions (A-P) prepared in this Example is provided below in Tables 28-33.
[0253] The co-formulation compositions were prepared by adding DI water, MORWET D-425, phosphate buffer (as described above in Example 23) and propylene glycol to a 30 ml vial equipped with cap. After MORWET D-425 was dissolved, humic acid sodium salt, ISOPARM, antifoam (AGNIQUE DFM 111S), and PLURONIC L-35 were added to the vial and it formed a brown liquid after stirring. Then the actives were added to the vial according to the composition in each formulation. Stainless steel beads (14 ml) with a diameter of 2 mm were added to the vial and the vial was capped tightly. The vial was placed in a large jar (16 oz.) and the large jar was caped. The large jar with four vials was placed on a roller (model 764 AVM from U.S. Stoneware), and it was rolled at half of the maximum speed for 2 days at ambient temperature. KELZAN thickener/stabilizer (as described above in Example 23) was then added to the vial and rolled at 10-20% of the maximum speed for 4 hrs. The formulation, which was flowable in the vial, was collected and a small amount of the sample was taken for particle size analysis. The wt % values reported in Tables 28-33 are theoretical based on the weight of the active added. The purities of the metalaxyl, tebuconozole and kresoxim methyl actives used in this Example were 90%, 96.8% and 97.5%, respectively.
[0000]
TABLE 28
Co-Formulation of Ia-i and Imidacloprid
A
B
C
Amount
Amount
Amount
Ingredient
(g)
Wt %
(g)
Wt %
(g)
Wt %
MORWET D-425
0.36
2.26
0.36
2.26
0.36
2.26
Buffer
0.15
0.94
0.15
0.94
0.15
0.94
Propylene glycol
0.90
5.66
0.90
5.66
0.90
5.66
ISOPAR M
0.36
2.26
0.36
2.26
0.36
2.26
Antifoam
0.05
0.31
0.05
0.31
0.05
0.31
PLURONIC L-35
0.009
0.06
0.009
0.06
0.009
0.06
Ia-i
3.80
23.88
0.76
4.77
6.85
43.03
Imidacloprid
3.80
23.88
6.85
43.03
0.76
4.77
Humic acid sodium
0.36
2.26
0.36
2.26
0.36
2.26
salt
Stabilizer
1.59
10.00
1.59
10.00
1.59
10.00
Water
4.53
28.47
4.53
28.47
4.53
28.47
[0000]
TABLE 29
Co-Formulation of Ia-i and Tebuconazole
D
E
F
Amount
Amount
Amount
Ingredient
(g)
Wt %
(g)
Wt %
(g)
Wt %
MORWET D-425
0.36
2.26
0.36
2.26
0.36
2.26
Buffer
0.15
0.94
0.15
0.94
0.15
0.94
Propylene glycol
0.90
5.66
0.90
5.66
0.90
5.66
ISOPAR M
0.36
2.26
0.36
2.26
0.36
2.26
Antifoam
0.05
0.31
0.05
0.31
0.05
0.31
PLURONIC L-35
0.009
0.06
0.009
0.06
0.009
0.06
Ia-i
3.80
23.88
0.76
4.77
6.85
43.03
Tebuconazole
3.80
23.88
6.85
43.03
0.76
4.77
Humic acid
0.36
2.26
0.36
2.26
0.36
2.26
sodium salt
Stabilizer
1.59
10.00
1.59
10.00
1.59
10.00
Water
4.53
28.47
4.53
28.47
4.53
28.47
[0000]
TABLE 30
Co-Formulation of Ia-i and kresoxim-methyl
G
H
I
Amount
Amount
Amount
Ingredient
(g)
Wt %
(g)
Wt %
(g)
Wt %
MORWET D-425
0.36
2.26
0.36
2.26
0.36
2.26
Buffer
0.15
0.94
0.15
0.94
0.15
0.94
Propylene glycol
0.90
5.66
0.90
5.66
0.90
5.66
ISOPAR M
0.36
2.26
0.36
2.26
0.36
2.26
Antifoam
0.05
0.31
0.05
0.31
0.05
0.31
PLURONIC L-35
0.009
0.06
0.009
0.06
0.009
0.06
Ia-i
3.80
23.88
0.76
4.77
6.85
43.03
kresoxim-methyl
3.80
23.88
6.85
43.03
0.76
4.77
Humic acid
0.36
2.26
0.36
2.26
0.36
2.26
sodium salt
Stabilizer
1.59
10.00
1.59
10.00
1.59
10.00
Water
4.53
28.47
4.53
28.47
4.53
28.47
[0000]
TABLE 31
Co-Formulation of Ia-i and metalaxyl
J
K
L
Amount
Amount
Amount
Ingredient
(g)
Wt %
(g)
Wt %
(g)
Wt %
MORWET D-425
0.36
2.26
0.36
2.26
0.36
2.26
Buffer
0.15
0.94
0.15
0.94
0.15
0.94
Propylene glycol
0.90
5.66
0.90
5.66
0.90
5.66
ISOPAR M
0.36
2.26
0.36
2.26
0.36
2.26
Antifoam
0.05
0.31
0.05
0.31
0.05
0.31
PLURONIC L-35
0.009
0.06
0.009
0.06
0.009
0.06
Ia-i
3.80
23.88
0.76
4.77
6.85
43.03
metalaxyl
3.80
23.88
6.85
43.03
0.76
4.77
Humic acid
0.36
2.26
0.36
2.26
0.36
2.26
sodium salt
Stabilizer
1.59
10.00
1.59
10.00
1.59
10.00
Water
4.53
28.47
4.53
28.47
4.53
28.47
[0000]
TABLE 32
Co-Formulation of Ia-iii and imidacloprid
M
N
O
Amount
Amount
Amount
Ingredient
(g)
Wt %
(g)
Wt %
(g)
Wt %
MORWET D-425
0.36
2.26
0.36
2.26
0.36
2.26
Buffer
0.15
0.94
0.15
0.94
0.15
0.94
Propylene glycol
0.90
5.66
0.90
5.66
0.90
5.66
ISOPAR M
0.36
2.26
0.36
2.26
0.36
2.26
Antifoam
0.05
0.31
0.05
0.31
0.05
0.31
PLURONIC L-35
0.009
0.06
0.009
0.06
0.009
0.06
Ia-iii
3.80
23.88
0.76
4.77
6.85
43.03
imidacloprid
3.80
23.88
6.85
43.03
0.76
4.77
Humic acid
0.36
2.26
0.36
2.26
0.36
2.26
sodium salt
Stabilizer
1.59
10.00
1.59
10.00
1.59
10.00
Water
4.53
28.47
4.53
28.47
4.53
28.47
[0000]
TABLE 33
Co-Formulation of Ia-i, imidacloprid, and metalaxyl
P
Ingredient
Amount (g)
Wt %
MORWET D-425
0.36
2.26%
Propylene glycol
0.90
5.65%
water
4.53
28.46%
ISOPAR M
0.36
2.26%
Humic Acid sodium salt
0.36
2.26%
Ia-i
2.54
15.93%
Imidacloprid
2.54
15.93%
Metalaxyl
2.54
15.93%
Antifoam
0.05
0.31%
PLURONIC L-35
0.009
0.06%
Buffer Solution
0.15
0.94%
Stabilizer
1.59
9.99%
[0254] A small amount of each sample of co-formulation compositions A-P was taken for particle size analysis. Particle size was measured by Beckman Coulter particle size analyzer (Beckman Coulter LS 13 320 laser diffraction particle size analyzer). The results are set forth below in Table 34.
[0000]
TABLE 34
Particle Size for Co-Formulations
Co-
Mean
Median
Mean/Median
Formulation
(μm)
(μm)
(μm)
A
3.387
2.263
1.496
B
3.561
2.083
1.709
C
3.146
2.213
1.422
D
3.757
2.525
1.488
E
5.697
3.442
1.655
F
2.993
2.052
1.459
G
3.139
2.415
1.300
H
2.794
1.824
1.532
I
3.487
2.424
1.438
J
3.514
2.142
1.640
K
5.046
2.473
2.040
L
3.569
2.380
1.499
M
5.491
4.025
1.364
N
4.004
2.893
1.384
O
5.102
4.157
1.227
P
3.356
2.272
1.477
Example 27
Field Trial
[0255] In this Example, various nematicidal formulations were tested for nematicidal activity against soybean cyst nematode (SCN) in a soy microplot field trial. The tested formulations included ACCELERON F/I, a fungicide/insecticide seed treatment package available from Monsanto Company and containing pyraclostrobin, metalaxyl, fluxapyroxad and imidacloprid, both alone and in combination with a composition in accordance with the present invention containing the nematicidal compound 3-phenyl-5-(thiophen-2-yl)-1,2,4-oxadiazole (Ia-i), in particular Formulation 9 as described above in Table 27. Also tested was the combination of ACCLERON F/N, a fungicide+nematicide seed treatment package available from Monsanto Company and containing pyraclostrobin, metalaxyl, fluxapyroxad, clothianidin and Bacillus firmus with Formulation 9.
[0256] Microplots containing a Stough fine sandy loam soil were fumigated with methyl bromide. These plots were covered with a 114-p.m (4.5-mil) thick polyethylene tarp for 72 hours. The tarp was removed and plots were planted 45 days later. Four seeds were planted in each microplot. Treatments were arranged in a randomized complete block design with five replications. Microplots were watered with drip irrigation as needed. Maximum and minimum weekly temperatures and amount of rainfall were recorded for duration of the test.
[0257] A race 3 population of Heterodera glycines was increased on soybean (Coker 156) in a greenhouse. Light brown to tan colored cysts were dislodged from the roots with a strong water spray and collected on nested sieves with pore sizes of 850 and 250 I˜m. Cysts were placed into 20-ml glass test tubes and crushed with a modified Seinhorst cyst crusher (21). The resultant suspension was passed through a 75-t×m-pore sieve nested on a 28-˜m-pore sieve to remove broken cysts and debris. The inoculum was incorporated in the appropriate treatments by pipetting the nematode suspension into 10 depressions 5 cm deep and 2 cm wide within each microplot. Soil was then mixed with a garden hoe to a depth of 15 cm, obtaining an inoculum level of 2,000 eggs and J2/250 cm 3 soil.
[0258] Plant stand, height and plant vigor evaluations were made at 20 to 40 days after planting. The number of Heterodera glycines in each microplot was determined at soybean maturity. Six soil cores 2.25-cm-d×15-cm deep were collected from the soybean root zone in each microplot. Heterodera glycines cysts were extracted from 250 cm a soil by sieving as described for inoculum production. J2 passing through the sieves used to collect cysts were extracted from the suspension using gravity-screening. Final separation of J2 in the fraction collected on the 28-um pore sieve was by sucrose centrifugal flotation (sucrose specific gravity=1.13). Data was reported as the number of J2s, cysts, eggs, J2+eggs. Additionally, the treatment reproductive factor (Rf) was provided; Rf=final population (Pf)/the initial population (Pi).
[0259] Table 35 summarizes the SCN Reproductive Factor for the tested formulations.
[0000]
TABLE 35
SCN
Repro-
Treat-
ductive
ment
Factor
Trt 1
ACCELERON F/I
pyraclostrobin, metalaxyl,
138
fluxapyroxad, imidacloprid
Trt 2
ACCELERON F/I +
pyraclostrobin, metalaxyl,
73
Formulation 9 in
fluxapyroxad, imidacloprid +
Table 27 (0.25
Formulation 9 (0.25 mg/seed)
mg/seed)
Trt 3
ACCELERON F/I +
pyraclostrobin, metalaxyl,
34
Formulation 9 in
fluxapyroxad, imidacloprid +
Table 27 (0.50
Formulation 9 (0.50 mg/seed)
mg/seed)
Trt 4
ACCELERON F/N +
pyraclostrobin, metalaxyl,
28
Formulation 9 in
fluxapyroxad, clothianidin,
Table 27 (0.50
Bacillus firmus +
mg/seed)
Formulation 9 (0.50 mg/seed)
[0260] When introducing elements of the present invention or the preferred embodiments(s) thereof, the articles “a”, “an”, “the” and “said” are intended to mean that there are one or more of the elements. The terms “comprising”, “including” and “having” are intended to be inclusive and mean that there may be additional elements other than the listed elements.
[0261] In view of the above, it will be seen that the several objects of the invention are achieved and other advantageous results attained.
[0262] As various changes could be made in the above products and methods without departing from the scope of the invention, it is intended that all matter contained in the above description and the associated drawings shall be interpreted as illustrative and not in a limiting sense.
|
Provided herein are aqueous suspension concentrate compositions comprising biologically active 3,5-disubstituted-1,2,4-oxadiazoles or salts thereof that are useful, for example, in the control of nematodes. Nematodes are active, flexible, elongate organisms that live on moist surfaces or in liquid environments, including films of water within soil and moist tissues within other organisms. Many species of nematodes have evolved to be very successful parasites of plants and animals and, as a result, are responsible for significant economic losses in agriculture and livestock.
| 0
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates in general to a fluid pressure regulator assembly and, more particularly, to a fluid pressure generator assembly, which produces energy from fluid pressure regulation.
2. Description of the Prior Art
Fluid pressure regulators are well known in the art. Regulators are used to regulate the pressure of liquid propane in an outdoor gas grill, airflow in self-contained underwater breathing apparatuses, and oxygen flow in medical applications. Regulators may be designed for regulating the pressure of virtually any type of fluid. One drawback associated with prior art fluid pressure regulators is the loss of energy between the high-pressure fluid entering the regulator and the low-pressure fluid exiting the regulator. It would be desirable to convert this potential energy into work. Another drawback with prior art systems is that a large reduction in pressure typically requires a more costly regulator. It would, therefore, be desirable to provide an assembly which reduces pressure before reaching a prior art regulator, to allow a more inexpensive regulator to be used. Additionally, single stage regulators often do an inadequate job of modulating large variances in pressure. Accordingly, it would be desirable to find a fluid pressure regulator which reduced the effects of large pressure variances on a fluid output pressure. The difficulties encountered in the prior art discussed herein are substantially eliminated by the present invention.
SUMMARY OF THE INVENTION
In an advantage provided by this invention, a fluid pressure regulator assembly is provided for generating power while regulating a fluid pressure.
Advantageously, this invention provides a fluid pressure regulator assembly for reducing variances in an output pressure as the result of large differences in input pressure.
Advantageously, this invention provides a fluid pressure regulator assembly which is inexpensive to manufacture and maintain.
Advantageously, this invention provides a fluid pressure regulator assembly which is lightweight and portable.
Advantageously, this invention provides a fluid pressure regulator assembly which reduces the size and cost of a regulator needed to regulate the pressure of a fluid.
Advantageously, in a preferred example of this invention, a fluid pressure regulator assembly is provided, comprising means for providing a pressurized fluid, as well as first means and second means for transporting a pressurized fluid. A fluid regulator is coupled to both the first means and second means, and means are coupled between the first means and the fluid regulator for converting a pressurized fluid into mechanical power.
In a preferred embodiment of the present invention, the converting means is a vane pump, coupled into fluid communication with the first means for converting pressurized fluid into movement of the vanes. The movement of the vanes may, thereafter, be converted into rotational and/or electrical energy.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings in which:
FIG. 1 illustrates a front elevation of a gas grill, utilizing the fluid pressure regulator of the present invention;
FIG. 2 illustrates a top elevation in cross-section of the pressure regulator of FIG. 1;
FIG. 3 illustrates a perspective view of the vane motor of the pressure regulator of FIG. 1;
FIG. 4 illustrates a side elevation in cross-section of the vane motor of FIG. 3;
FIG. 5 illustrates a side elevation of an alternative embodiment of the present invention, utilizing dual vane motors; and
FIG. 6 illustrates a side elevation of a diver and diving gear, utilizing the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A fluid pressure regulator assembly is shown generally as ( 10 ) in FIG. 1 . The assembly ( 10 ) comprises a pressurized fluid source, such as a liquid propane tank ( 12 ), such as those well known in the art. Coupled to the compressor is a high-pressure line ( 14 ) which, in turn, is coupled to a vane motor ( 16 ). The vane motor ( 16 ) is coupled by a transfer line ( 18 ) to a fluid regulator ( 20 ). The fluid regulator ( 20 ) is coupled to an output line ( 22 ) which, in turn, is coupled to the burner ( 24 ) of a gas grill ( 26 ). The grill ( 26 ) may be provided with an electrically actuated rotisserie ( 28 ), or any other desired components. As shown in FIG. 1, coupled to the vane motor ( 16 ) is a generator ( 30 ), which is electrically coupled to a battery ( 32 ) which, in turn, is coupled to the rotisserie ( 28 ). The liquid propane tank ( 12 ), high-pressure line ( 14 ), fluid regulator ( 20 ), output line ( 22 ), burner ( 24 ), gas grill ( 26 ), and rotisserie ( 28 ) may be of any type, such as those well known in the art.
As shown in FIG. 2, the fluid regulator ( 20 ) is preferably of the type known in the art, constructed of steel, defining a high-pressure cavity ( 34 ) in fluid communication with a low-pressure cavity ( 36 ). The high-pressure cavity ( 34 ) is coupled to the transfer line ( 18 ), while the low-pressure cavity ( 36 ) is coupled to the output line ( 22 ). The cavities ( 34 ) and ( 36 ) are provided in fluid communication with one another via an opening ( 38 ). Provided through the opening ( 38 ) is a valve stem ( 40 ), designed to completely seal off fluid communication between the high-pressure cavity ( 34 ) and low-pressure cavity ( 36 ), when seated in the opening ( 38 ). Coupled to the valve stem ( 40 ) is a threaded shaft ( 42 ), around which is provided a compressed spring ( 44 ), coupled to a resilient diaphragm ( 46 ). At ambient pressure, the spring ( 44 ) presses the valve stem ( 40 ) downward, opening communication between the high-pressure cavity ( 34 ) and low-pressure cavity ( 36 ). When a fluid ( 48 ), such as liquid propane, enters the high-pressure cavity ( 34 ), the fluid ( 48 ) moves into the low-pressure cavity ( 36 ) through the opening ( 38 ). As the fluid ( 48 ) fills the low-pressure cavity ( 36 ), pressure increases, thereby moving the diaphragm ( 46 ) to lift the valve stem ( 40 ) to begin to close the opening ( 38 ). The valve stem ( 40 ) continues to move until the flow of fluid ( 48 ) across the opening ( 38 ) is reduced when the compressed spring ( 44 ) overcomes the upward pressure on the diaphragm ( 46 ), the valve stem ( 40 ) lowers and increases the flow of fluid ( 48 ) from the high-pressure cavity ( 34 ) to the low-pressure cavity ( 36 ). In this manner, the spring ( 44 ) and diaphragm ( 46 ) continually act to regulate the pressure within the low pressure cavity ( 36 ) and exiting through the output line ( 22 ), as long as the pressure in the high pressure cavity ( 34 ) remains as least as high as the pre-determined pressure for which the spring ( 44 ) and diaphragm ( 46 ) are set. Although the foregoing describes the regulator utilized in the preferred embodiment of the present invention, any regulator, such as the air regulator on a scuba system, or fluid regulator on a welding assembly, may be utilize.
As shown in FIG. 3, the motor ( 16 ) is preferably a vane motor, although it may be any suitable device for translating fluid pressure into mechanical motion. Preferably, as shown in FIGS. 3 and 4, the motor ( 16 ) is provided with a drive shaft ( 52 ), coupled to a casing ( 54 ) by a bushing ( 54 ). The casing ( 54 ) defines a fluid inlet ( 58 ) and a fluid outlet ( 60 ). In the preferred embodiment, the fluid inlet ( 58 ) is coupled into fluid communication with the high-pressure line ( 14 ). (FIGS. 1 - 3 ). The casing ( 54 ) is provided with a hollow interior ( 62 ) in fluid communication with the inlet ( 58 ) and outlet ( 60 ). The hollow interior ( 62 ) is defined by an outer race ( 64 ). Provided within the hollow interior ( 62 ) is an inner drum ( 66 ), which comprises a front plate ( 68 ), a back plate ( 70 ), and a cylindrical inner race ( 72 ). (FIGS. 2 and 3 ). As shown in FIG. 3, the inner race ( 72 ) is provided with a first aperture ( 74 ), a second aperture ( 76 ), a third aperture ( 78 ), and a fourth aperture ( 80 ).
Provided within the inner drum ( 66 ) is a first vane assembly ( 82 ), which includes a first vane ( 84 ) and a third vane ( 86 ), each secured to a lost motion linkage ( 88 ). The first vane ( 84 ) and third vane ( 86 ) are wider than the first lost motion linkage ( 88 ), leaving a first C-shaped cutout ( 90 ) in the first vane assembly ( 82 ). A second vane assembly ( 92 ) is also provided, comprising a second vane ( 94 ), a fourth vane ( 96 ) and a second lost motion linkage ( 98 ). The second vane ( 94 ) and fourth vane ( 96 ) are secured to the second lost motion linkage ( 98 ) in a manner similar to that described above to provide a second C-shaped cutout ( 100 ).
The first vane assembly ( 82 ) and second vane assembly ( 92 ) are constructed in a manner which positions the first vane ( 84 ) and third vane ( 86 ) perpendicular to the second vane ( 94 ) and fourth vane ( 96 ). The first lost motion linkage ( 88 ) is provided within the second C-shaped cutout ( 100 ) of the second vane assembly ( 92 ), and the second lost motion linkage ( 98 ) is provided within the first C-shaped cutout ( 90 ) of the first vane assembly ( 82 ). Preferably, the vane assemblies ( 82 ) and ( 92 ) are constructed of stainless steel and are provided near their ends ( 102 ) with wear resistant tips ( 104 ), constructed of an aluminum nickel bronze alloy, such as those alloys well known in the art to be of superior wear resistance. The tips ( 104 ) are rounded with a tighter radius of curvature than the outer race ( 64 ). The tips ( 104 ) are secured to the vane assemblies ( 82 ) and ( 92 ) by weldments or similar securement means. The first lost motion linkage ( 88 ) defines an interior space ( 106 ) with a width approximately one-half of its length. Provided within this interior space ( 106 ) is a stainless steel drum shaft ( 108 ). Secured around the drum shaft ( 108 ) is a guide block ( 110 ). The guide block ( 110 ) has a square cross-section with a width only slightly smaller than the width of the interior space ( 106 ), defined by the first lost motion linkage ( 88 ). The guide block ( 110 ) is preferably the same depth as the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ), and extends from the interior space ( 106 ) of the first lost motion linkage ( 88 ) into an interior space (not shown) defined by the second lost motion linkage ( 98 ). This construction allows longitudinal movement of the vane assemblies ( 82 ) and ( 92 ) relative to the guide block ( 110 ) and drum shaft ( 108 ), but prevents lateral movement in relationship thereto.
The drum shaft ( 108 ) is coupled to a back plate ( 112 ) bolted to the casing ( 54 ). FIGS. 2 and 3 ). As shown in FIG. 4, the drum shaft ( 108 ) is centered within the hollow interior ( 62 ) defined by the outer race ( 64 ). The drive shaft ( 52 ) is positioned slightly higher than the drum shaft ( 108 ), and is coupled to a front plate ( 114 ) bolted to the casing ( 54 ). The drive shaft ( 52 ) is parallel to, but on a different axis than the drum shaft ( 108 ). Since the shafts ( 52 ) and ( 108 ) each rotate on a different axis, the back plate ( 112 ) must be provided with a large, circular aperture ( 116 ), into which is secured a bearing ( 118 ). The bearing ( 118 ) supports the inner drum ( 66 ) against the casing ( 54 ) and allows the drum shaft ( 108 ) to extend out of the casing ( 54 ) and rotate on its own axis. The bearing ( 118 ) also maintains a substantially fluid tight seal to prevent the escape of pressurized fluid out of the casing ( 54 ).
As fluid ( 48 ) enters the fluid inlet ( 58 ) under pressure, the water presses against a face ( 122 ) of the second vane ( 94 ), forcing the inner drum ( 66 ) into a counterclockwise rotation. (FIG. 3 ). When the fourth vane ( 96 ) is closest to a ceiling ( 124 ) of the casing ( 54 ), the majority of the fourth vane ( 96 ) is located within the inner drum ( 66 ). Accordingly, the amount of the fourth vane ( 96 ) exposed to the fluid ( 48 ) is reduced, as is its drag coefficient. A larger drag coefficient would allow the fluid ( 48 ) to force the inner drum ( 66 ) toward a clockwise rotation, thereby reducing the efficiency of the motor ( 16 ).
As the fluid ( 48 ) presses against the face ( 114 ) of the second vane ( 94 ), the second vane ( 94 ) moves along an abrasion plate ( 125 ), preferably constructed of titanium or similar abrasion resistant material, preferably being less than five millimeters and, more preferably, less than one millimeter, while being preferably greater than {fraction (1/100)}th of a millimeter and, more preferably, more than {fraction (1/50)}th of a millimeter from the tips ( 104 ) of the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ) as they rotate past. As the second vane ( 94 ) rotates toward the end of the abrasion plate ( 125 ), the first vane ( 84 ) moves toward the abrasion plate ( 125 ) and the fluid ( 48 ) presses against a face ( 126 ) of the first vane ( 84 ), thereby continuing the counterclockwise rotation of the drum shaft ( 108 ) and the inner drum ( 66 ). As the inner drum ( 66 ) continues to rotate, the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ) extend and retract relative to the inner drum ( 66 ). The retraction reduces the drag coefficient of the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ) when the vanes are near the ceiling ( 124 ) to reduce reverse torque on the inner drum ( 66 ). Conversely, the extension increases the drag coefficient of the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ) as the vanes approach the abrasion plate ( 125 ) to allow the fluid ( 48 ) to provide maximum forward torque to the inner drum ( 66 ) through the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ). As the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ) move past the abrasion plate ( 125 ), the fluid ( 48 ) exhausts through the fluid outlet ( 60 ). Obviously, the motor ( 16 ) can be constructed of any desired material of any suitable dimensions.
As shown in FIG. 1, coupled to the drive shaft ( 52 ) of the motor ( 16 ) is an electrical generator ( 30 ). While the generator ( 30 ) is preferably electric, it may, of course, be of any suitable type of power storage or transmission device known in the art, actuated by heat, mechanical, pneumatic or hydraulic power. As shown in FIG. 1, an electrical cord is coupled to the generator ( 30 ), and is coupled to a battery ( 134 ). The battery, in turn, is coupled to the rotisserie ( 28 ) to provide power when needed. Accordingly, when a valve ( 136 ) on the gas grill ( 26 ) is actuated to draw fluid from the liquid propane tank ( 12 ), the fluid ( 48 ) flows from the liquid propane tank ( 12 ) through the high-pressure line ( 14 ) into the vane motor ( 16 ). The pressure of the fluid ( 48 ) turns the vanes ( 84 ), ( 86 ), ( 94 ) and ( 96 ), thereby driving the drive shaft ( 52 ) and the generator ( 30 ). The generator ( 30 ) thereby sends an electric current to the battery ( 32 ) for use in driving the rotisserie ( 28 ) when desired. From the vane motor ( 16 ), the fluid ( 48 ) having been reduced in pressure, flows through the transfer line ( 18 ) to the fluid regulator ( 20 ), whereby after a further step-down in pressure, the fluid ( 48 ) flows through the output line ( 28 ) to the burner ( 24 ) for use in the grill ( 26 ). Although in the preferred embodiment the vane motor ( 16 ) is used to generate electricity to drive the rotisserie ( 28 ), the vane motor ( 16 ) may, of course, be used to generate electricity for any desired function, or used directly for mechanical power to drive the rotisserie ( 28 ) wheels ( 138 ) provided on the gas grill ( 26 ), or for any other desired utility.
In an alternative embodiment of the present invention, as shown in FIG. 5, a high pressure fluid source such as a compressor ( 140 ) is coupled to a first vane motor ( 142 ) which, in turn, is coupled to a second vane motor ( 144 ). The second vane motor ( 144 ) is coupled to a regulator ( 146 ), such as that described above, and an output line ( 148 ) is also coupled to the regulator ( 146 ). As shown in FIG. 5, the first vane motor ( 142 ) is coupled to a generator ( 150 ) which, in turn,is coupled to a battery ( 152 ). The second vane motor ( 144 ) is coupled to a pulley ( 154 ) which, in turn, is coupled to a belt ( 156 ), used to drive an axle ( 158 ). Although one vane motor ( 142 ) is used in this embodiment to produce electricity, and the other vane motor ( 144 ) is used to produce mechanical work, any number of vane motors may be utilized to produce electricity, and any other number of vane motors may be used to produce mechanical work, if desired. Such an assembly would be particularly well suited to a vehicle driven by a pressurized flammable fluid, such as liquid propane.
In yet another alternative embodiment of the present invention, FIG. 6 illustrates a self-contained underwater breathing apparatus (scuba diver) ( 160 ), coupled to a compressed air tank ( 162 ), such as those well known in the art. Coupled directly to the compressed air tank ( 162 ) is a vane motor ( 164 ), such as that described above. Coupled to the vane motor ( 164 ) is a first stage regulator ( 166 ), such as those well known in the art to reduce pressures from the compressed air tank ( 162 ) on the order of two hundred plus atmospheres to preferably less than ten atmospheres. By running air ( 168 ) through the vane motor ( 164 ), a percentage of the potential energy of this compressed air ( 168 ) can be recovered before being stepped down through the first stage regulator ( 166 ). From the first stage regulator ( 166 ), the air passes through a line ( 170 ) to the second stage regulator ( 172 ), which reduces the pressure to approximately one to five atmospheres. As the scuba diver ( 160 ) breaths, drawing air ( 168 ) from the compressed air tank ( 162 ), the air ( 168 ) drives the vane motor ( 164 ) and the generator ( 174 ), which is coupled to the vane motor ( 164 ).
The generator ( 174 ) may be of any desired construction, but is preferably of the type described above. Coupled to the generator ( 174 ) is a wire ( 176 ) coupled to a headlight ( 178 ), strapped around the head ( 180 ) of the scuba diver ( 160 ). Although in the preferred embodiment the generator ( 174 ) is used to power a headlight ( 178 ), the generator ( 174 ) may, of course, be used to drive any electrical appliance or may be eliminated if it is desired to utilize the vane motor ( 164 ) to generate mechanical work. It should also be noted that the vane motor ( 164 ) may be positioned between the first stage regulator ( 166 ) and second stage regulator ( 172 ), or a plurality of vane motors may be coupled at any desired location to retrieve additional work from the air ( 168 ).
An advantage provided by all of the foregoing embodiments, is that the vane motor extracts work from the pressurized fluid ( 48 ), while reducing the pressure of the pressurized fluid ( 48 ). By performing a portion of the work typically done by a pressure regulator, the assembly ( 10 ) of the present invention allows the use of a smaller or more inexpensive pressure regulator to accommodate the lower pressures.
Although the invention has been described with respect to a preferred embodiment thereof, it is also to be understood that it is not to be so limited, since changes and modifications can be made therein which are within the full intended scope of this invention as defined by the appended claims. For example, it should be noted that any desired motor may be used, including a standard turbine or piston motor, and that any type of generator, including both direct current and alternating current generators, may be utilized in accordance with the present invention. It is additionally anticipated that any number of motors and generators may be used in conjunction with any number of regulators to recover work from a pressurized fluid. It is additionally anticipated that the motor and generator may be of any desired dimensions and design, to accommodate any desired pressures.
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A fluid pressure regulator assembly is provided for generating power from a pressurized fluid. A vane motor is coupled between a high-pressure fluid source and a regulator, to extract power from the pressurized fluid and reduce the burden on the fluid regulator. The assembly may be used in association with many devices, including gas grills and self-contained underwater breathing apparatuses. A plurality of vane motors may be provided and generators may be coupled thereto for producing electricity from the pressurized fluid.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Divisional of application Ser. No. 12/461,242 filed Aug. 5, 2009, which is a Continuation of application Ser. No. 11/241,957 filed Oct. 4, 2005, which is a Divisional of application Ser. No. 10/765,972 filed Jan. 29, 2004, which is a Continuation of application Ser. No. 09/601,313 filed Sep. 11, 2000, which is a U.S. National Stage application from PCT/CH99/00586 filed Dec. 7, 1999, which claims priority from Swiss Patent Application No. 2448/98 filed Dec. 10, 1998. The disclosures of the prior applications are hereby incorporated by reference herein in their entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of Invention
[0003] The invention relates to a plastic object for use in personal hygiene and to a method of producing the plastic object.
[0004] 2. Description of Related Art
[0005] A plastic object of this type takes the form, for example, of a toothbrush. Toothbrushes are mass-produced articles and must therefore allow cost-effective production. Toothbrushes made of a single plastic material and toothbrushes made of two plastic components, which are produced for example by the two-component injection-molding process, are known. In the latter case, the toothbrush comprises two plastic parts: a first plastic part made of a first plastic material, for example polypropylene, extends from the handle of the toothbrush up to the brush head and has interconnected recesses. A second plastic part made of a second plastic material, for example thermoplastic elastomer, fills the recesses of the first plastic part. These two plastic materials bond with one another at the surface where the two plastic parts touch. In comparison with a toothbrush made of only one plastic material, this provides greater scope for design. Since, however, the two plastic materials have to bond with one another during the injection-molding operation, there are restrictions in the selection of the plastic materials and consequently in the design of the toothbrush.
[0006] This problem also affects other plastic objects for use in personal hygiene comprising at least two parts made of different plastic materials, such as for example containers or closure caps for containers intended for personal-hygiene preparations and substances, or for medical and dental preparations. There are restrictions in the selection of materials for the two parts in the case of such plastic objects as well.
SUMMARY OF THE INVENTION
[0007] The present invention is based on the object of providing a plastic object of the type mentioned at the beginning with which varied design is possible along with cost-effective production.
[0008] This object is achieved according to aspects of the invention. The method of producing such a plastic object is distinguished according to aspects of the invention. Preferred developments of the plastic object according to the invention and of the method according to the invention form additional aspects of the invention.
[0009] The fact that the two parts of the plastic object are formed by at least two molded parts consisting of different plastic materials which do not bond with one another during the injection-molding operation and are joined to one another in particular by a non-positive and/or positive fit means that there are many possibilities for an expedient design of the plastic object. Plastic materials of different chemical character can be used. They may differ to a greater or lesser extent in their structural formula and their chemical components. At the surfaces where they touch, there do not have to be any chemical or physical bonds, for example in the form of bridge formations or van der Waals forces, between the plastic materials. The frictional forces alone between the molded parts in the joint, preferably constructed in the manner of a shrink fit, are adequate to join the two molded parts firmly to one another. The positive fit realized by means of parts engaging in one another at the surfaces where the two molded parts touch prevents gaps into which water and contaminants can penetrate, or which can even lead to rupture, from forming between the two molded parts during the shrinking operation.
[0010] Therefore, in the case of a toothbrush for example, plastic materials with advantageous properties can be used at the right place. The one molded part may consist, for example, of polypropylene (polypropylene is available inexpensively, is flexible, chemically resistant but not completely transparent), while styrene acrylonitrile (SAN) (likewise inexpensive, transparent, esthetic) may be chosen for example for the other molded part. The molded part bearing the brush head is advantageously produced from polypropylene, since polypropylene is resistant to the often aggressive substances of the tooth-cleaning agents.
[0011] The two plastic materials advantageously have a different shrinkage behavior, since a firm shrink fit can be achieved more easily in this way. In this case, that molded part which is produced from plastic material with the lower degree of shrinkage is advantageously produced in a first step. The second molded part is produced from plastic material with the greater degree of shrinkage in a second step, thereby achieving a natural pressure of the second plastic material pressing against the first plastic material.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The invention is explained in more detail below with reference to the drawing, in which:
[0013] FIG. 1 shows a first exemplary embodiment of a toothbrush comprising two molded parts in side view and partially in longitudinal section;
[0014] FIG. 2 shows the toothbrush according to FIG. 1 in plan view;
[0015] FIG. 3 shows the toothbrush according to FIG. 1 in a view from below;
[0016] FIG. 4 shows a first molded part of the toothbrush according to FIG. 1 in elevation and partially in longitudinal section;
[0017] FIG. 5 shows the molded part according to FIG. 4 in plan view;
[0018] FIG. 6 shows a second molded part of the toothbrush according to FIG. 1 in plan view;
[0019] FIG. 7 shows a section along line VII-VII in FIG. 6 ;
[0020] FIG. 8 shows a joint of the two molded parts according to FIG. 1 on an enlarged scale;
[0021] FIG. 9 shows a section along line IX-IX in FIG. 2 on an enlarged scale;
[0022] FIG. 10 shows a second exemplary embodiment of a toothbrush comprising two molded parts in side view;
[0023] FIG. 11 shows the toothbrush according to FIG. 10 in plan view; and
[0024] FIG. 12 shows the toothbrush according to FIG. 10 on an enlarged scale, in side view and partially in section, a closure part for closing a handle cavity from the remaining part of the toothbrush being represented separately.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0025] According to FIGS. 1 to 3 , a toothbrush 1 has a first molded part 2 , which bears a brush head 3 in its front region 2 a. The first molded part 2 , consisting of a plastic material A, is enclosed over a portion of its length, to be specific its rear handle region 2 b, by a second molded part 4 , consisting of a plastic material B, and is non-positively joined to the latter in the manner of a shrink fit. The plastic materials A and B are plastic materials of a kind which do not bond with one another during the injection-molding operation at the surfaces where they touch.
[0026] For better illustration, the two molded parts 2 , 4 are represented separately from one another in FIGS. 4 to 7 . The two molded parts 2 , 4 have—as described further below—in the region where they touch diametrically opposite projections and recesses engaging in one another, by means of which a positive fit of the two molded parts 2 , 4 is realized in addition to the non-positive fit of the same. It goes without saying that this joint is only produced during the injection-molding operation, in which one of the molded parts is injection-molded in a first step and then the other molded part is injection-molded around or into the first part in a second step. With the different degree of shrinkage of the two molded parts 2 , 4 , that molded part which is to be produced from plastic material with a lower degree of shrinkage is advantageously injection-molded first. In the second step, injection-molding of the other molded part takes place from plastic material with a greater degree of shrinkage, whereby a natural pressure of the second plastic material pressing against the first plastic material is produced.
[0027] The second molded part 4 , represented individually in FIGS. 6 and 7 and essentially forming the toothbrush handle, is designed in the form of a sleeve, i.e. is provided with an internal longitudinal bore 7 , which corresponds in its shape and diameter to the rear handle region 2 b of the first molded part 2 , represented individually in FIGS. 4 and 5 . The sleeve-shaped molded part 4 has an outer surface 6 .
[0028] A front end face 8 of the sleeve-shaped second molded part 4 is assigned to an offset surface 9 of the first molded part 2 ( FIG. 4 ), seen in the longitudinal direction of the toothbrush. In this case, an annular, front projection 10 of the second molded part 4 protrudes into a diametrically opposite recess 11 of the first molded part 2 , which can be seen particularly well from FIG. 8 . A rear end face 14 of the sleeve-shaped second molded part 4 is assigned to an offset surface 16 of an end piece 15 of the first molded part 2 . Here, too, an annular, rear projection 17 of the second molded part 4 protrudes into a diametrically opposite recess 18 of the end piece 15 .
[0029] The second molded part 4 is provided with a cross-sectionally oval, elongate cross-bore 20 , which is arranged transversely to the longitudinal bore 7 and is intended for a diametrically opposite part 21 of the first molded part 2 , penetrating through the cross-bore 20 . The oval part 21 has an upper edge surface 22 and a lower edge surface 22 ′. The second molded part 4 is provided with offset surfaces 23 , 23 ′, which run around the cross-bore 20 and are diametrically opposite the edge surfaces 22 , 22 ′. The edge surfaces 22 , 22 ′ and the offset surfaces 23 , 23 ′ in turn form a type of projection/recess positive-fitting joint between the two molded parts 2 , 4 .
[0030] Together with outer surfaces 19 , 19 ′ ( FIG. 4 ) of the oval part 21 , the outer surface 6 of the sleeve-shaped molded part 4 forms a handle surface.
[0031] As far as the material for the two molded parts 2 , 4 is concerned, polypropylene (PP) may be advantageously chosen, for example, as the plastic material A for the first molded part 2 , while the second molded part 4 may consist, for example, of the following plastic materials B:
[0032] styrene acrylonitrile (SAN) and subgroups,
[0033] acrylonitrile-butadiene styrene (ABS) and subgroups,
[0034] polyamide (PA) and subgroups,
[0035] polycarbonate (PC) and subgroups,
[0036] polyester (PBT) and subgroups, or other transparent plastic materials not bonding with polypropylene (PP).
[0037] The respective subgroups comprise the plastic materials belonging to the corresponding family.
[0038] This combination of materials provides a special advantage. Since modern tooth-cleaning agents often contain aggressive substances, such as peppermint-oil for example, cheap plastics, such as SAN for example, are often attacked. If the first molded part 2 , bearing the brush head 3 , is made of PP, which is resistant to the aggressive substances but not completely transparent, and the second molded part 4 , comprising the handle, is made of transparent, but less resistant SAN, this special embodiment of the invention constitutes a toothbrush which can be produced cost-effectively, is resistant to the aggressive substances of the tooth-cleaning agents and is also able to be esthetically pleasing. Of course, any other resistant plastic material may be used instead of PP and one of the cheaper, and therefore generally less resistant, plastic materials mentioned above may be used, for example, instead of SAN.
[0039] With these combinations of materials, preferably the second, sleeve-shaped molded part 4 is produced first, by means of injection molding, in a first step. Subsequently, the first molded part 2 is injection-molded in a second step, the positive fit already described being produced in the region where the two molded parts 2 , 4 touch. The greater degree of shrinkage of the last-molded material A (PP) of the first part 2 has the effect of producing a natural pressure, pressing against the second part 4 consisting of material B (for example SAN), and a non-positive and positive fit of the two molded parts 2 , 4 is brought about by the projections 10 , 17 , 22 , 22 ′ engaging in recesses 11 , 18 , 23 , 23 ′, without gaps into which water and contaminants can penetrate, or which can even lead to a rupture, forming between the plastic materials A, B, which actually do not bond with one another.
[0040] As an example, a toothbrush 1 comprising two molded parts 2 , 4 has been presented and described. A different configuration of the two molded parts would be quite possible. The sleeve-shaped configuration of one of the molded parts is not absolutely necessary.
[0041] It goes without saying that a toothbrush could also have a plurality of molded parts made of plastic materials not bonding with one another during the injection-molding operation, which are joined to one another by a non-positive and/or positive fit.
[0042] Instead of the shrink fit and positive fit described, the individual molded parts, which do not enter into an adhesive or cohesive bond during the injection-molding operation, could be non-positively and/or positively joined to one another in any other way.
[0043] However, molded parts comprising two or more plastic components of which, for example, one (or more) component(s) of the one molded part cannot be bonded with one (or more) component(s) of the other molded part, could also be non-positively and/or positively joined to one another.
[0044] Represented in FIGS. 10 and 11 is a second exemplary embodiment of a toothbrush 1 ′, which likewise has two molded parts 32 , 34 consisting of different plastic materials A and B which do not bond with one another during the injection-molding operation. Here, too, the first molded part 32 forms a toothbrush part bearing the brush head 3 ′ (the bristles of the brush head 3 ′ are not represented in FIGS. 10 and 11 ; only the depressions 35 intended for anchoring tufts of bristles can be seen). The second molded part 34 forms a toothbrush handle. This is provided over part of its length with a cylindrical hollow 36 , by which a cavity 37 which is open toward the rear and can be closed by means of a closure part 38 is formed in the toothbrush handle. The second molded part 34 preferably consists of an at least partially transparent or translucent material component, for example SAN, so that various esthetically acting means (loose objects, liquid, powder, printed rollers etc.) can be visibly accommodated in the cavity 37 . The closure part 38 may be joined undetachably or detachably to the second molded part 34 . In the latter case, useful objects, such as toothpicks or ampoules with mouth wash or toothpaste, may also be accommodated, for example, in the cavity 37 .
[0045] In the case of this embodiment of a toothbrush as well, the surfaces where the two molded parts 32 , 34 touch are provided with parts 40 , 41 engaging in one another, so that the two plastic parts are brought into a non-positive and positive fit during injection molding. The parts 40 , 41 engaging in one another are formed, for example, by a projection 40 on the end face of the molded part 34 forming the handle and a diametrically opposite recess 41 on the end face of the other molded part 32 .
[0046] If the handle is produced from the transparent SAN, it is also the case with this embodiment that this handle-forming molded part 34 is preferably produced first in the injection-molding process and the molded part 32 , bearing the brush head, is subsequently injection-molded, for example from more resistant polypropylene.
[0047] Both the bristle-bearing part of the toothbrush and the handle may have parts consisting of further material components. For example, a depression for a thumb rest 42 , of a further material component, for example a thermoplastic elastomer (TPE), may be provided, for example, in the molded part 34 .
[0048] The toothbrush shown in FIG. 12 corresponds to the toothbrush 1 ′ according to FIGS. 10 and 11 , but is represented on an enlarged scale in comparison with FIG. 10 and partially in section (the same parts are denoted by the same reference numerals). This toothbrush 1 ′ is intended for the insertion of variously filled ampoules 45 , for which a holder 46 of an elastically compliant plastic is present in the front region of the hollow 36 . The closure part 38 is provided on the inside with an elastically compliant counterholder 38 ′. The ampoule 45 is held both radially and axially in its position by the two holders 46 , 38 ′. The holder 46 may, for example, be injection-molded from the same plastic (preferably from PP) and in the same step with the molded part 32 bearing the brush head 3 ′ (the joining channel present for this is denoted by 47 in FIG. 12 ). From the same plastic material and in the same step, a cross-bore 48 may also be filled in the molded part 34 injection-molded first (for example from SAN), whereby the thumb rest 42 is formed on the outer side of the handle.
[0049] The ampoules 45 may contain various esthetically acting objects (loose or suspended in a liquid), liquid, powder etc.
[0050] As already mentioned, other plastic objects similar to toothbrushes for use in personal hygiene could be formed from at least two molded parts which consist of different plastic materials which do not bond with one another during the injection-molding operation, and which are joined to one another by a non-positive and/or positive fit. For example, in the case of containers or closure caps for containers which are intended for personal-hygiene preparations and substances, or for medical and dental preparations, plastics with advantageous properties could likewise be used at the right place in cost-effective production.
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A unitary two component article for personal hygiene, such as a toothbrush, wherein the same is formed by injection molding of two differing plastic materials. The plastics do not adhesively or chemically bond to each other. The two differing plastic parts of the toothbrush are mechanically connected, such as by interfitting portions of the two plastic components or by shrinking one plastic component about the other.
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FIELD OF THE INVENTION
The present invention relates to an apparatus and method for either temporarily or permanently sealing water or other similar wells.
BACKGROUND OF THE INVENTION
In recent years the problem of abandoned wells in many areas of this country, particularly in the Midwest, has increased dramatically. Many years ago, the vast majority of the farms in operation in the Midwest were comparatively small, with each farm having its own well to provide for the individual farmer's water needs. However, due to the increased cost of farm machinery and other materials which are needed to adequately farm the land, many of these farms have been consolidated into larger and more efficient units. Since in many cases only one water system is needed to operate these larger farms, a large number of wells have become abandoned and in some cases polluted due to neglect.
If these abandoned wells are not adequately sealed, not only does the water contained therein become polluted, but also these wells pollute the water in adjoining operational wells. The abandoned wells can pollute these operational wells because the wells are usually connected by underground rivers or streams. Pollutants can enter these subterranean waterways by flowing down the unattended wells thereby polluting the water source used by functional wells in the immediate area.
Moreover, in more recent years many wells have become unsafe because of ground water contamination due to overuse of various types of pesticides including insecticides and herbicides, and in some sites mine acid run off, mine tailings contamination and/or even radioactive waste pollution. The underground waters, which can become polluted by spillage into abandoned wells or vice versa, service countless numbers of irrigation systems. If the water in those systems becomes polluted, crops cannot be safely produced and the soil can be permanently ruined. Furthermore, these underground rivers or streams can empty into above-ground rivers and streams thus polluting these water sources, also.
In addition, there is a continuing problem, particularly in the Midwest, of the ravages of flood damage which can pollute wells which are still in working order. Another problem in regard to abandoned wells is the danger of someone accidently falling into such a well thereby creating great risk of bodily injury or death.
Due to the great depth of some of these wells, and the fact that the bottom of the well shaft opens directly into the water source, it is quite impractical and nearly impossible to merely pour concrete or other hardenable substances into the well shaft to seal the well without first implanting a base structure in the shaft of the well. This base structure serves as a support for the hardenable material, and since the base is situated at a reasonably close distance to the top of the well, only a manageable amount of concrete need be used for filling the cavity formed between the base and ground level.
A device for solving these problems is shown in the Freiburger U.S. Pat. No. 3,995,694 which discloses an inflatable well seal using a releasable coupling. Such patent (also see attached FIG. 4) shows such a coupler 24 threaded internally at one end to fit a standard pipe thread which is on the outer surface of a valve stem 22 while the other end of the coupler 24 is threaded on the outside surface to engage an air hose 34 through the use of a standard inwardly threading coupling element 23 connected to the air hose 34. A gasket 59 is provided to ensure a tight fit between the stem 22 and the coupler 24. This coupler is fashioned of a plastic material well known in the art which can be constructed so that it breaks along a shear zone 26 of reduced thickness at predetermined internal pressure of the inflatable bag 20 such as 100 psi. At this pressure, the inflatable bag 20 will completely seal the well shaft. The coupler 24 contains a plurality of air holes 46 which allow the air to pass from the air hose 34 to the inflatable bag 20, through an orifice 54 located in the inflation valve stem 22.
A movable valve pin 42, which may be made of metal, is provided in the valve stem 22 which opens and closes orifice 54 thereby enabling the bag 20 to be filled with air and, when coupler 24 breaks, ensuring that air contained in the bag does not escape to the atmosphere but would remain in the bag 20. The valve pin 42 contains a substantially conical valve head 48 with the base portion 49 facing the interior of inflatable bag 20. The exterior surface 47 of the valve head 48 is adapted to be operatively engages with a valve seat 50 disposed on an annular flange which encircles the interior of valve stem 22. When the valve head 48 abuts against the valve seat 50, no air can enter or exit from the bag 20, but when the head 48 is not in contact with the seat 50, air may enter the bag 20 through orifice 54.
Coupler 24 also contains a valve pin 28 having a substantially cylindrical head 29. Valve pin 42 also contains a substantially cylindrical valve head 43 which cooperates with the valve head 29 of valve pin 28. When the coupler 24 is connected to the inflatable bag 20, the valve head 29 of the coupler 24 depresses valve head 43, thereby forcing the valve head 48 away from the valve seat 50. A compression spring 52 encircles the upper portion 56 of valve pin 42 between the head 13 of the valve pin 42 contained in valve stem 22 and the top portion 58' of flange 51. Therefore, before valve head 48 can be dislodged from valve seat 50, the force of this spring 52 must be overcome.
FIG. 5 attached depicts an automatically releasable coupler according to the an alternative embodiment of the Freiburger U.S. Pat. No. '694. This coupler 62, screw joined to the coupling element 23, is constructed without the shear zone 26 of coupler 24, but instead utilizing a pair of shear pins 60. A number of holes, corresponding to the number of shear pins used, are drilled or otherwise fashioned in the valve stem 22 and coupler 62 so that they align with one another. Therefore, the shear pins 60 provide for the attachment between the valve stem 22 and the coupler 62 and therefore no threading is between the valve stem 22 and the coupler 62 is needed for this connection. The shear pins 60 are then inserted into these holes thereby joining the stem 22 to the coupler 62. Thereafter, when the entire device is lowered into the well, these pins 60 will rupture when the internal pressure of the inflatable bag 20 reaches a predetermined level thereby releasing the coupler 62 from the stem 22.
The use of these constructions enables both the air hose 34 and the coupler 62 to be recovered and reused, but not without some difficultly for installation, and some possible damage upon removal thereof. Moreover, these constructions are more expensive than desirable because of the need to provide a threaded connection between the coupling element 23 and the coupler 24 or 62 so that the remnant of the coupler 24, 62 can be unscrewed and discarded after use, so the coupling element 23 can be reused.
SUMMARY OF THE INVENTION
It is accordingly an object of the present invention to overcome the deficiencies of the prior art, such as noted above.
Another object of the present invention is to provide an improved and simplified device for temporarily or permanently sealing a water well or similar well, or an abandoned well.
Another object of the present invention is to produce a device which adequately seals abandoned wells in a simple and economic manner.
A further object of the present invention is to produce a well-sealing device which utilizes a releasable coupler so that an air hose and the coupler can be recovered.
A still further object of the present invention is to produce a device that seals wells utilizing a releasable coupler which detaches from a seal when a predetermined pressure has been obtained.
Yet another object of the present invention is to provide a method for permanently or temporarily sealing an abandoned well.
These and other objects of the present invention are fulfilled by a simple and easy-to-use well seal tool utilizing an inflatable bag and an automatically releasable coupler. An air hose is connected to the bag by way of the coupler using a resiliently deformable connecting element, and this air hose is in communication with an air supply means such as an air compressor so that air can be introduced into the bag for purposes of inflation. When used in abandoned wells, the inflatable bag, coupling and air hose are lowered into the shaft of the well, and when inflated the bag frictionally grips the sides of the well shaft in order to remain in a fixed position in the shaft just as in the aforementioned Freiburger U.S. patent. When a predetermined pressure is reached in the interior of the bag, the bag acts against a loose washer and the coupler automatically releases by deformation of the deformable connecting element, thereby disconnecting the air hose from the inflatable bag. This enables the air hose and the coupler to be recovered so that they can be reused in a simplified manner to seal additional well shafts.
The present invention has a coupler which is constructed in a unitary piece. This unitary coupler reduces construction costs and allows for recovery of the entire coupler so that it can be reused without replacement.
This device may also be used to temporarily seal a well in a situation in which flood waters could possibly cause pollution in existing wells. The inflatable bag is lowered to just below the ground level and may be directly connected to the air hose. In this situation, the compressor inflates the bag and when the opening is completely sealed off, it is disconnected from the air hose either automatically or manually. Thus, when the danger of pollution has passed, the tube can be deflated and withdrawn from the well shaft.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects and benefits of the invention will be described in greater detail below in conjunction with the drawings in which:
FIG. 1 is a diagrammatical view of the well seal lowered in an abandoned well.
FIG. 2 is a diagrammatical view of the well seal after the air hose has been recovered and cement deposited into the bore.
FIG. 3 is a diagrammatical view of the well seal lowered for temporary sealing.
FIG. 4 is a cross-sectional view of the releasable coupler and the valve stem according to the prior art.
FIG. 5 is a cross-sectional view of another embodiment of the releasable coupler according to the prior art.
FIG. 6 is a cross-sectional view of a releasable coupler and the valve stem according to the present invention.
FIG. 7 is a sectional view of the releasable coupler taken through 9--9 of FIG. 6.
FIG. 8 is a cross-sectional view of a releasable coupler being separated from the valve stem according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a well seal apparatus 10 after it has been lowered into an abandoned well shaft 12, inflated to seal the shaft, but before the releasing of a coupler 63. The apparatus includes an inflatable bag 20 of rubber or other similar elastomeric material which is generally cylindrical in configuration and has a closed lower end 40 and a valve stem 22' similar to a common inner tube valve. Although the exact dimensions of the inflatable bag 20 may be varied, a bag having dimensions of 2 feet in length and 8 inches in diameter performs quite satisfactorily. One end of an air hose 39 is connected to the valve stem 22' by means of the separable coupler 63, and the other end is connected to an air supply means 36 such as a compressor which is positioned at ground level 16 near the well shaft 12. The coupler is desirably constructed of a plastic material so that it can withstand substantial pressure, e.g. at least 100 and preferably at least 125 pounds of air pressure, or it can be made of metal.
FIG. 3 shows a slightly different embodiment used to temporarily seal an operating well in order to prevent contaminated water from flowing therein, e.g. in case of a flood. As shown in FIG. 3, the inflatable bag 20 may be connected to the air hose 39 with a coupler. The bag is lowered until it is only slightly below the ground level and then inflated by use of the air compressor 36 so as to seal the shaft opening, after which the air hose 39 is disconnected leaving a well with a temporary seal therein. When the flood waters have subsided, the bag 20 is deflated and then removed entirely from the well shaft 12.
FIG. 6 shows an automatically releasable coupler according to the present invention which ensures an air tight fit between the stem 22' and the coupler 63, with the aid of a gasket 59. The coupler is fashioned of a plastic or metal material and is constructed as described below so that it separates from the valve stem 22' at an elevated internal pressure of the inflatable bag 20, such as 80-100 psi. At this pressure, the inflatable bag 20 will completely seal the well shaft. The coupler 63 contains a plurality of air holes 46, which allow the air to pass from the air hose 39 to the inflatable bag 20, through an orifice 54' located in the inflatable valve stem 22'. Coupler 63 also contains a valve pin 42 having a substantially cylindrical head 43, the function of which will be described in detail hereinbelow.
A movable valve pin 42, which may be made of metal, is provided in the valve stem 22' which opens and closes orifice 54' thereby enabling the bag 20 to be filled with air and, when coupler 63 separates from the valve stem 22', ensuring that air contained in the bag does not escape to the atmosphere but remains in the bag 20. The valve pin 42 contains a substantially conical valve head 48 with the base portion 49 facing the interior of inflatable bag 20. The exterior surface 47 of the valve head 48 is adapted to be operatively engaged with a valve seat 50' disposed on an annular flange which encircles the interior of valve stem 22'. When the valve head 48 abuts against the valve seat 50', no air can enter or exit from the bag 20, but when the head 48 is not in contact with the seat 50', air may enter the bag 20 through the orifice 54'.
The substantially cylindrical valve head 43 of the valve pin 42 which cooperates with the valve head 29' of valve pin 28'. When the coupler 63 is connected to the inflatable bag 20, the valve head 29' of the coupler 63 depresses valve head 43, thereby forcing the valve head 48 away from the valve seat 50'. A compression spring 52 encircles the upper portion 56 of the valve pin 42 in the valve stem 22' between the valve head 43 and the top surface or shoulder 58' of an inwardly directed annular flange 51'. Therefore, before valve head 48 can be dislodged from valve seat 50', the force of this spring 52, which normally biases the valve closed, must be overcome.
The coupler 63 of FIG. 6, unlike those of the prior art, is constructed without the shear zone 26 of coupling 24 and without the upper thread sections of couplers 24 and 62 which connect them to the coupling element 23. Coupler 63 uses a pair of elastomeric O-rings 64 to achieve the function of separating the coupler 63 from the stem 22'. A number of holes, corresponding to the number of O-rings used, are drilled or otherwise fashioned in valve stem 22' and the coupler 63 so that they align with one another, such as shown in FIG. 7. A loose washer 65 is located between the coupler 63 and the valve stem 22'. The interior diameter of the washer 65 is large enough so as to easily slide upwardly on and along the exterior surface of the valve stem 22'. When the entire device is lowered into the well and the bag 20 inflated as described below, the O-rings 64 will collapse and no longer hold the coupler 63 and the valve stem 22' together; i.e., when the internal pressure of the inflatable bag 20 reaches a predetermined level, it expands against the loose washer 65 thus driving the coupler 63 upwardly and releasing the coupler 63 from the stem 22'. The use of this type of arrangement enables both the air hose 39 and the coupler 63 to be recovered and reused without any damage thereto.
The operation of the inflatable well seal according to the present invention will now be explained in more detail with reference to FIGS. 6 and 8.
Before the inflatable bag 20 is lowered into the well shaft 12, it is connected to the air hose 39 by means of the separable coupler 63 which is permanently connected to the air hose 34. A gauge 44 can be used in conjunction with the air hose 39 to indicate the pressure therein. The air hose is then connected to the compressor 36 and the entire assembly (except for the compressor 36) is then lowered into the metal casing 14 or other liner which is contained in most well shafts, to a point near the bottom thereof.
Next, the air compressor 36 is activated and the bag 20 begins to inflate. The inflatable bag 20 is used as the well plug, since it can inflate to seal wells having many different diameters. When the air pressure inside the bag 20 reaches approximately 100 psi, the bag 20, restrained from further radial expansion by the well casing 14, expands upwardly driving the loose washer 65 before it, the loose washer in turn driving the bottom edge of the coupler 63 upwardly. Because the elastomeric O-rings 64 collapse thereby permitting separation of the coupler 63 from the valve stem 22'. As this movement occurs, the valve heads 29' and 43 separate allowing the force of spring 52 to drive the valve head 48 to abut valve seat 50', thereby sealing the valve stem 22' and ensuring that the air contained in the inflatable bag 20 does not escape.
After the coupler 63 has separated from the stem 22', the air hose 39 and the coupler 63 are then removed from the well casing 14, leaving the inflatable bag 20 in situ wedged against the casing 14 or natural wall of the well shaft 12. A hardening substance such as concrete 38 or the like is then poured into the well shaft 12 until the ground level 16 has been reached, as shown in FIG. 2. This concrete permanently closes the well and also alleviates the danger of a person or an animal inadvertently stumbling into an uncovered, unattended abandoned sealed well. The concrete may also cover the area immediately surrounding the well opening thus ensuring a more permanent closure. Additionally, information such as the date that the well has been sealed can be applied into the concrete forming a permanent record of this data.
Coupler 63 can also be used to temporarily seal an opening of a operating well in order to prevent contaminated water from flowing therein, e.g. in case of a flood. As shown in FIG. 3, the inflatable bag 20 is connected to the air hose 39 by coupler 63. The inflatable bag 20 is lowered until it is only slightly below the ground level and then is inflated by use of an air compressor 36. When the bag has been inflated as to seal the well opening, the air hose 39 and the coupler 63 are disconnected from the valve stem leaving a well having a temporary seal therein. When the floodwaters have subsided, the bag is deflated by the reattachment of the air hose 39 and the coupler 63, which causes the valve head 48 to be disengaged from the valve seat 50' thereby allowing the air in the inflatable bag 20 to escape. Once the air from the bag 20 has been removed, the inflatable bag can be lifted out of the well opening to allow the normal use of the well.
The foregoing description of the specification will reveal the general nature of the invention so that others can, by applying current knowledge, rarely modify and/or adapt various applications specific embodiments without departing from the generic concept, and therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalent of the disclosed embodiment. It is to be understood that the phraseology or terminology employ herein is for the purpose of the description and not of limitations. For example, for the sake of clarity, it has been stated that the inflatable bag 20 is filled with air produced by an air compressor 36. However, it should be appreciated that any suitable fluid such as water could be used for this purpose along with any suitable supply means. Additionally, the present invention is not to be construed to be limited to sealing only water wells. Rather, this device may be utilized in sealing other types of wells or conduits having a generally circular cross-section.
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A method and apparatus for sealing wells utilizing an inflatable bag and an automatically separable coupler. An air compressor or other fluid source supplies a fluid to the inflatable bag via a hose connected to the bag by this coupler and a valve. The bag is lowered into the well and it is then inflated until the coupler separates thereby disconnecting the hose from the bag, thus allowing the hose and the coupler to be recovered and used again. The well is thus sealed by the inflated bag. Concrete or any other similar substance can then be deposited into the well to fill the cavity formed between the bag and the level of the ground. Once the bag has been inflated to cover the well opening, it is then disconnected from the hose and coupler. Disconnection is effected automatically by collapse of flexible gaskets which join the coupler and the valve.
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TECHNICAL FIELD
Rig skidding apparatus and method.
BACKGROUND
It is often desirable to move drilling rigs short distances between wells within a drill site. Disassembling the rig and reassembling it at the new location is time and labor intensive, and increases the rate of wear of some rig components. To avoid disassembly and reassembly, one solution has been to skid the rig structure across steel framed rig matting. However, the force required to overcome the metal-to-metal sliding friction between rig and track was problematic. Other solutions have included sliding the rig on rollers and using rig walkers.
SUMMARY
It is desired to achieve a means of moving a rig structure to a well site without requiring extensive disassembly of the rig structure that is labor and time efficient.
In one embodiment, there is disclosed a method of skidding a rig structure, comprising raising the rig structure; after raising the rig structure, placing a skid track under the rig structure, wherein the skid track comprises a low friction plastic sheet; lowering the rig structure onto the skid track; and sliding the rig structure along the skid track. The low friction plastic sheet may be supported by a base and the skid track may comprise a cooperating sheet, for example a continuous flexible metal sheet, placed between the plastic sheet and the rig structure. In one embodiment, there is disclosed a method of skidding a rig structure comprising placing beams in a position to support the rig structure; using jacks to raise the beams; raising the rig structure with the jacks; placing a skid track under the rig structure; lowering the rig structure onto the skid track; removing the jacks and the beams; and sliding the rig structure along the skid track, wherein the skid track comprises a low friction plastic sheet.
In various embodiments, there may be included any of the following features: upon sliding the rig structure to a desired location, placing beams in a position to support the rig structure; using jacks to raise the one or more beams, raising the rig structure with the jacks, removing the skid track from under the rig structure, lowering the rig structure and removing the jacks; sliding the rig structure along the skid tracks may occur by towing; the low friction plastic sheet may be a lubricant filled plastic sheet; the low friction plastic sheet may be self-lubricating; and the low friction plastic sheet may be ultra-high-molecular-weight polyethylene.
These and other aspects of the device and method are set out in the claims, which are incorporated here by reference.
BRIEF DESCRIPTION OF THE FIGURES
Embodiments will now be described with reference to the figures, in which like reference characters denote like elements, by way of example, and in which:
FIG. 1 is a perspective view of a portion of a rig structure resting on skid tracks.
FIG. 2 is a front view of a portion of a rig structure raised on beams by jacks with skid tracks comprising a sliding layer and base placed underneath the structure.
FIG. 3 is a side view of a portion of a rig structure raised on beams by jacks with skid tracks placed underneath the structure.
FIG. 4 is a perspective view of a portion of a rig structure lowered onto skid tracks with a cooperating layer in this instance comprising a metal sheet.
FIG. 5 is a side view of a portion of a rig structure lowered onto skid tracks.
FIG. 6 is a perspective of a representative portion of a rig structure being towed on skid tracks, with beams and jacks removed.
FIG. 7 is a side view of a representative portion of a rig structure being towed on skid tracks, with beams and jacks removed.
FIGS. 8A, 8B and 8C are respectively a perspective exploded view, a top view and an exploded section of an exemplary skid track.
FIG. 9 shows a rig structure resting on a ground surface.
DETAILED DESCRIPTION
Immaterial modifications may be made to the embodiments described here without departing from what is covered by the claims.
At the beginning and end of moving a rig, the rig rests on the ground as shown in FIG. 9 . Removal and later replacement of catwalks and related peripheral equipment will also be carried out. The rig is represented by rig structure 10 , which comprises conventional elements of a rig. The rig structure 10 comprises a ground contacting portion on which the mast, power sources, pumps, drill pipe, etc., are carried. The ground contacting portion may comprise I-beams. When preparing to move the rig structure 10 , a set of jacks 12 are arranged to support the rig structure 10 while the skid tracks 14 are positioned underneath it, for example, under the I-beams if the rig structure 10 is supported on I-beams. The jacks 12 may, for example, be hydraulic jacks. In an embodiment beams 16 are placed through portions of the rig structure 10 , resting upon the jacks 12 . The jacks 12 are activated, raising the beams 16 and with them the rig structure 10 (see FIGS. 2 and 3 ). The beams 16 may in some embodiments be fabricated aluminum beams. The rig structure 10 only needs to be raised sufficiently to place the skid tracks 14 underneath the rig structure 10 . Only a few inches of clearance may be required.
Once the rig structure 10 has been raised off the ground, skid tracks 14 are slid underneath those portions of the rig structure which would contact the ground surface 19 when lowered. The ground surface 19 may be any surface on which the rig rests including a manufactured or prepared surface such as conventional rig matting. The skid tracks 14 include a sliding layer 18 of continuous or sectioned low friction plastic sheet (see FIGS. 8A, 8B and 8C for construction of an exemplary skid track 14 ). In an embodiment, this plastic sheet is a sheet or sheets of ultra-high-molecular-weight polyethylene (UHMW-PE) such as TIVAR® DrySlide UHMW-PE produced by Quadrant Engineering Plastic Products. The sliding layer 18 may comprise a porous polymer having pores that include a lubricant. The particular plastic used for the sliding layer 18 should be selected for appropriate strength, corrosion resistance, and abrasion resistance. The lubricant may be a dry film lubricant or solid, such as PTFE, molybdenum disulfide, or graphite, selected for compatibility with the plastic.
As shown in FIGS. 8A, 8B and 8C , in some embodiments, the layer 18 is supported by a base 20 , for example a layer of plywood sheets. The base 20 may be formed of overlapping plywood sheets, for example two layers of overlapping 8 foot long ¾ inch×24 inch sheets screwed together at 6 inch intervals. A cooperating layer 22 of stainless steel sheet may be placed between the rig structure and the sliding layer 18 . The cooperating layer 22 may be a continuous flexible metal sheet. Continuous in this context means extending the full distance along the ground engaging part of the rig structure. Flexible in this context means sufficiently flexible that the continuous sheet can be placed under the rig structure when the rig structure is raised off the ground by jacks. In an embodiment, the layer 22 may be a continuous sheet of 16-gauge 304 annealed stainless steel, 12 inches wide. The layer 22 may run the length of the rig structure or more. The layer 22 may be secured to the front of the rig structure 10 by any suitable means, so that the layer 22 moves with the rig structure 10 when it is towed. For example, if the rig structure 10 has a tubular or other element connecting I-beams, the layer 22 may be bent around the tubular element to hold the layer 22 stationary in relation to the rig structure 10 . It may be sufficient in some cases that the friction between the layer 22 and the ground contacting portions of the rig structure 10 is sufficient to cause the layer 22 to move with the rig structure 10 when it is moved.
In an embodiment, the sliding layer 18 may be ½ inch thick. The sliding layer 18 may be the same width as or narrower than the base 20 . The cooperating layer 22 may be as wide as the ground contacting parts of the rig structure. The layer 22 may be narrower than the layer 18 . The layer 18 may be provided in sections 24 inches wide. The layer 18 may be screwed onto the base 20 . A dry film coefficient of friction of 0.08 between the layers 18 and 22 has been found adequate, for example, as occurs between TIVAR® DrySlide UHMW-PE used as the sliding layer 18 and stainless steel used as the cooperating layer 22 but other levels of friction may be adequate depending on the towing ability of a vehicle used to pull the rig structure and the integrity of the rig structure 10 at the tow points. With the skid tracks 14 in position, the rig structure 10 may then be lowered onto the skid tracks 14 with the rig structure 10 contacting the cooperating layer 22 when present or the sliding layer 18 (see FIGS. 4 and 5 ).
Once the weight of the rig structure 10 is off of the jacks 12 , the beams 16 and jacks 12 may be removed (as shown in FIGS. 4 and 5 ). The rig structure 10 is then connected to be pulled or pushed along the skid tracks 14 ( FIGS. 6 and 7 ). In a preferred embodiment the rig structure 10 is towed by one or more vehicles 24 . Additional vehicles (not shown), positioned alongside or behind the rig structure can also be used to stabilize the rig structure on the skid tracks.
When towed, the rig structure slides on the sliding layer 18 , usually with the sliding interface being between the plastic sheet forming the sliding layer 18 and the cooperating layer 22 formed of stainless steel. The plastic sheet such as sheets of UHMW-PE are self-lubricating, thereby significantly reducing the sliding friction despite the substantial weight of the rig structure. In an embodiment, the cooperating layer 22 moves in relation to the sliding layer 18 , while the rig structure remains stationary with respect to the cooperating layer 22 . In this instance, the important coefficient of friction for sliding purposes is the coefficient of friction between the sliding layer 18 and the cooperating layer 22 . Depending on the rig structure base, the cooperating layer 22 could be omitted in some circumstances, but it is recommended to use a cooperating layer 22 in most instances. Instead of a metal cooperating layer 22 , other smooth and strong cooperating layers may be used.
Once the rig structure 10 has arrived at the desired location, the rig structure 10 may be raised again upon the jacks 12 as shown in FIGS. 2 and 3 , and the skid tracks 14 removed. The rig structure 10 can then be lowered, the jacks 12 removed, leaving the rig structure on the ground surface 19 again as shown in FIG. 9 after which rig operations may resume at this new location.
In an experimental design, a base layer 20 was made of high density hardwood (oak) plywood painted to reduce moisture and oil absorption was too brittle and would fracture when a raise pad was encountered. Therefore, it was found that a fracture resistant base layer 20 was needed, for example, ¾ inch cabinet grade fir plywood was found to have the required flexibility and strength. Other materials could also be used in place of the fir plywood having substantially the same or better fracture resistance. In the experimental design, a sliding layer 18 made of Jaytrex Virgin Natural White UHMW did not work well in higher temperatures (+25 C). It seemed to get a little “sticky.” The Dry Slide UHMW by Quadrant Plastics was firmer at higher temperatures exhibiting less friction. Therefore, it is preferred to use a sliding layer 18 that is temperature resistant, namely that retains its sliding properties above 25 C, for example, up to 40 C. For the cooperating layer, it has been found that lighter stainless steel (18 gauge) did not disperse the weight at the edges of the load, reducing the effective surface area between the cooperating layer 22 and sliding layer 18 . 16 gauge stainless steel has alleviated this issue. Therefore, it is preferred to use a cooperating layer 22 that is sufficiently flexible to be slid under the lifted drilling structure when it is lifted a very short distance, yet being bending resistant under the load of the drilling structure to disperse the weight of the drilling structure at the edges of the load and maximize the effective surface are of contact between the cooperating layer 22 and sliding layer 18 .
In the claims, the word “comprising” is used in its inclusive sense and does not exclude other elements being present. The indefinite articles “a” and “an” before a claim feature do not exclude more than one of the feature being present. Each one of the individual features described here may be used in one or more embodiments and is not, by virtue only of being described here, to be construed as essential to all embodiments as defined by the claims.
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A rig skidding method involving raising a rig on jacks, positioning skid tracks comprising low friction plastic underneath the rig, lowering the rig, and skidding the rig along the skid tracks to a new site for rig operations. At the new site, the process is reversed to leave the rig on the ground at the new location.
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[0001] The present invention relates to a card reading device for a self-service terminal and in particular for an automated teller machine (ATM) according to the preamble of claim 1 . Furthermore the invention relates to a self-service terminal equipped with the same and to a method for monitoring the same according to the preambles of the independent claims.
BACKGROUND OF THE INVENTION
[0002] Very often, the card reading devices in self-service terminals are a primary target for manipulation-attempts and skimming-attacks. This is because a user, attempting to use the self-service terminal that in particular can be an ATM, requires a banking-card that usually comprises a chip and/or a magnet strip on which card data including the personal customer and account access data are stored. Unfortunately, self-service terminals are becoming subject of manipulation by third persons who try to obtain these data in a criminal manner. Amongst other techniques they try to insert a spy-device into the card-slot of the card reading device in an inconspicuous manner, wherein this spy-device is capable to directly read out the magnetic strip or to attach to an internal interface (such as an USB-interface) of the card reading-device. This shall finally realize a readout of the banking-card data in order to make an illegal copy of the card. Moreover, skimming-attempts are known in which an alien card reader is attached to the card reading device as an unobtrusive superstructure, capable to e.g. send the read out card data via a radio transmission. If the frausdster is also capable to obtain the personal identification number (so-called PIN) of the card he/she can easily withdraw money from accompanying account. Moreover, skimming-attacks are known in which an internal interface directly simulates/pretends a card reading process and thus manipulates the software control of the self-service terminal or ATM.
[0003] Moreover, direct trapping of a card is another known attack scenario. Within this trapping scenario a superstructure is mounted in front of the card reading device to steal the card. This superstructure comprises a “Lebanese loop” extending towards the card reading device and being mounted directly behind the card insert slot and having a flap which only allows one way insertion of the card. Once a customer inserts a card, said card is captured and trapped by the Lebanese loop; the flap blocks the card from being ejected. By this behaviour of the apparatus the user believes his/her card that a (rightfully) withheld or retract of the card occurs. Then he/she consequently leaves the self-service terminal. In the following the frauder or deceiver takes the card together with the superstructure.
[0004] In order to detect card trapping, the process of card-retract has been modified in the prior art. The card is first retracted, then driven out and then retracted again by the card reading device. If this procedure is not possible in a perfect manner, i.e. ejecting a card is not possible, it can be assumed that a card theft has been attempted. However, this security procedure/approach increases the transaction time at the device.
[0005] It is also known to counteract such manipulation attempts of self-service terminals be using sensors. The German patent application DE 196 05 102 A1 discloses to use one or more infrared sensors for safeguard the self-service terminal, wherein the signals of these sensors are processed by an evaluator device to detect superstructures.
[0006] In the German patent application DE 10 2008 012 231 A1 a protection device is proposed that comprises a protection-shield-generator and a connected induction coil to create an electromagnetic protection shield that covers the electromagnetic fields which are created during (illegally) reading-out the card and therefore influence/interfere the functionality of the alien card reading device (spy-device) such that it fails to deliver useful data. To avoid that the deceiver may detect this protection device, the electromagnetic protection-field is generated with a special protection signal simulating a standard card-reading signal that only contains unuseful psuedo-data. However, this protection device can not be used to avoid or impede such skimming-attempts that are directly targeted to the interior of the card reading device and e.g. receive signals from an inserted spy-device or even from an interior data interface.
[0007] In this context there is also to mention the German patent application DE 10 2009 019 708 A1 which discloses to create a stray or noise field via permanent magnets that are moved by piezo-elements, in order to generate an induced magnetic alternating field which effectively interferes the skimming card reading device while reading-out the data. Furthermore the European patent application EP 1 394 728 A1 is cited in which supersonic sensors are disclosed to detect an attached superstructure to the self-service terminal. But also these solutions are not capable to avoid or impede skimming-attempts that occur in the interior of the card reading device.
[0008] In the US patent application US 2006/0249574 A1 the misuse of a card is mentioned, but not a manipulation within the interior of the card reading device as such. Herein, it is proposed to equip the card with a microcontroller and an encryption function (cf. FIG. 2 ). For the power supply of the microcontroller there are photovoltaic or piezo-electric components proposed. However, monitoring of or defense against skimming-attempts via sensors is not described.
[0009] Furthermore, it is well known to protect devices that are commonly used to store money or valuables, in particular vaults or bank-vaults with sensors. For instance the German patent application DE 2 318 478 A1 discloses a monitoring system for a strongroom, in which supersonic-sensors are used to determine motions therein via the Doppler-effect. Another disclosure that is relying on an ultrasonic alarm mechanism is disclosed in the German patent application DE 2 617 467 A1.
[0010] Accordingly, conventional self-service terminals comprise a card reading device into which a card can be inserted that contains data to be read, wherein the self-service terminal comprises at least one sensor for defense against manipulation attempts and an evaluator device. However, these solutions are not capable for protection against manipulations attempts that aim on the interior of the card reading device.
[0011] Therefore, it the object of the present invention to further develop a card reading device as mentioned before in order to be capable to protect against manipulation attempts and skimming-attacks at the interior of the card reading device or at least make such attempts more difficult. Also a self-service terminal being equipped with such a card reading device and a method to monitor such a self-service terminal is provided.
SUMMARY OF THE INVENTION
[0012] The preceding object is achieved by a card reading device comprising the features of claim 1 as well as by a self-service terminal and a method having the features of the according juxtaposed claims.
[0013] Accordingly a card reading device is presented wherein at least one sensor system is attached in the card reading device and comprises at least one linearly extending sensor arrangement, wherein the evaluator device verifies at least one spatial dimension of the card via at least one sensor system. Hence, a card reading device is presented, in which a sensor system is directly arranged inside the card reading device but is particularly arranged in or at the intake compartment for the cards to be read, wherein the card reading device verifies at least one spatial dimension, in particular the length or width, via the sensor system. The sensor system can be e.g. an opto-electric sensor system.
[0014] The present invention also provides a self-service terminal that in particular can be an ATM, comprising said card reading device. Furthermore, a method for monitoring the self-service terminal or the ATM via the sensor system and the evaluator device is presented, wherein the sensor system is arranged inside the card reading device and comprises at least one linearly extending sensor arrangement that particularly is arranged in the intake compartment and wherein at least one spatial dimension of the card is verified/checked via the evaluator device.
[0015] Consequently, a sensor system is installed inside the card reading device to compare the spatial dimensions of an inserted object to that of a conventional card, such that it can be effectively determined, whether a conventional card is present in the card reading device or an alienated object, e.g. a spy-device with similar dimensions as compared to the card.
[0000] Preferred embodiments can be found in the dependent claims.
[0016] In a preferred embodiment the sensor system is arranged as a sensor arrangement comprising a plurality of linearly arranged sensor elements, wherein the sensor arrangement extends in a vertical or a horizontal direction relative to the inserted card. Herein, a first sensor arrangement can detect the length of the card as a first spatial dimension and/or a second sensor arrangement can detect the width of the card as a second spatial dimension.
[0017] In another preferred embodiment only one sensor arrangement is present to detect the width and length. The second sensor arrangement can for instance be arranged to not only detect the width of the card but also the length of the card by determining the beginning and the end of the card and by operating the evaluating device to measure the insertion time and thus to determine the length of the card according to a constant insertion velocity.
[0018] Therefore, the sensor system installed in the card reading device is particularly a sensor arrangement with a plurality of sensor elements that are linearly arranged and extend in a horizontal or a vertical direction of the card that has been inserted into the intake compartment. Herein, the first sensor arrangement detects the length of the card as the first spatial dimension and/or the second sensor arrangement detects the width of the card as the second spatial dimension. Moreover, an additional sensor or sensor system can be arranged within the card reading device that detects the height of the card as a third dimension. Preferably the sensor elements of the at least one sensor arrangement and/or the additional sensor system are embodied as opto-electric sensor elements. However, other sensor types can be employed as an alternative to detect the spatial dimensions of the card.
[0019] Moreover, a further additional sensor arrangement, in particular an opto-electric sensor system, can be arranged in the card reading device within the vicinity of the surface of the card to verify material properties of the card by discrete spectroscopy in particular.
[0020] Moreover, an additional sensor or sensor system can be arranged at the card-feeding-portion but particular at the retraction compartment for cards to be withheld, wherein that sensor can particularly be a light barrier that is connected with the at least one evaluator device and in particular comprises one or more opto-electric sensor elements to detect manipulations at the card-feeding-portion. In a preferred embodiment the card reading device can thus be arranged such that a further sensor system is arranged in the card-feeding-portion, wherein that sensor system is connected with the card reading device and comprises one or more sensor elements to detect manipulations at the card-feeding-portion. Also the sensor elements preferably are opto-electric elements of a light barrier but can be other components or sensor types to monitor the area.
[0021] The card reading device that usually comprises an intake compartment into which the card is inserted/fed can be configured to comprise at least one evaluator device with mechatronic transducers but in particular with piezo-electric transducers comprising sensors and/or actuators. The mechatronic transducers are arranged in the intake compartment to check/verify the integrity of the card reading device, but in particular of the housing and/or the intake compartment, wherein the evaluator device is arranged to receive a signal that has been excited from a portion of the mechatronic transducers and is detected by another portion of the mechatronic transducers to compare it with reference data, and to send out a warning signal at a defined deviation that stands for a lack of integrity of the card reading device. Therefore, mechatronic transducers can be arranged in or at the intake compartment, wherein said transducers can in particular be piezo-electric transducers, comprising sensors and/or actuators connected with the evaluator device. Said transducers are used to cause a vibration being applied to the card reading device, wherein the vibration is in the hearable sonic-range or eigenfrequency-range to check the integrity of the card reading device and in particular of the housing and/or the intake compartment. To this end the evaluator device manages reference data, e.g. reference data from a mechatronic transducer, that represents an acceptable condition of the intake compartment. The mechatronic transducers can also be arranged in a sensor patch or array. Herein, the sensor patch preferably comprises multiple sonic-electric and in particular piezo-electric sensor elements. Such a sensor patch can also be attached in the intake compartment of the card reading device but preferably parallel to a surface of the card to also check the material properties of the card. Herein, single components of the sensor patch can function as actuators but in particular piezo-electric actuators to excite a part of the card reading device or the card to vibrate, such that the other sensor elements of the sensor patch can generate the signals to be evaluated. Therefore, the evaluator device can be extended to not only evaluate signals coming from the opto-electric sensor patch but also signals coming from the other sensor elements in particular those from the mechatronic sensor arrangement.
DESCRIPTION OF THE FIGURES
[0022] In the following the present invention is described in accordance with embodiments and the attached figures which show the following representations:
[0023] FIG. 1 a shows a cross-sectional view of an installation of the card reading device;
[0024] FIG. 1 b shows a three dimensional view of the card reading device to be installed within a self-service terminal;
[0025] FIG. 2 shows a schematic view of an arrangement of sensor patches to verify the dimensions (length, width, height) of a card;
[0026] FIGS. 3,5 show diagrams of a signal pre-evaluation that are executed in the method;
[0027] FIGS. 4 a - c show logical connections between the steps of the method; a=inserting the card, b=retracting the card, c=checking/verifying the housing integrity;
[0028] FIGS. 6 a & b show a content extraction and classification obtained with the method;
[0029] FIG. 7 shows a schematic view demonstrating the function of a classificator able to learn;
[0030] FIG. 8 shows the function of a fuzzy-pattern classificatory;
[0031] FIG. 9 shows the process of an exemplatory method.
DETAILED DESCRIPTION
[0032] FIGS. 1 a and 1 b show a schematical view of the card reading device 20 comprising an intake compartment 13 for a card to be read. The intake compartment 13 also comprises the card reader or card reading elements as such, that for instance comprise a contact area/pad for reading card chips and a reading head/pick-up to read magnetic strips. The card 11 or 11 ′ to be read is supplied to the intake compartment 13 via the inserting slot by conventional means to be optimally positioned with respect to the card reading elements for reading. For this purpose conventional guiding and supply elements can be used.
[0033] In the present invention “card reading device” refers to the device as a whole (cf. FIG. 1 b ) thus comprising the housing 1 , a base plate 2 , a card reader 3 , in some cases a so-called IDKG-add-on 5 , additional sensors 6 , in particular light sensors or sensor arrangements, and optionally a camera 10 , and card-supply/transportation means. Depending on the actual version it is also possible that the device comprises less components. The term “card reader” refers to the device 3 that is used for the actual reading of the card. The housing 1 circumferences the card reader 3 in connection with the base plate 2 completely. Preferably, the transducer elements (mechatronic transducers) are mounted at/in the housing 1 ; but basically a mounting at all other single components is possible, too. For this purpose it is useful to consider a superposition of the modal stretchings (functions of strain) in the frequency ranges to be considered. By doing so significant and therefore suitable positions can be visualized and a positioning can be done.
[0034] The sole openings of the housing are represented by the opening area for insertion of the card (IDKG-slot unit/module 5 ) comprising the detection (unit) including the sensors 6 and by the opening for retraction of cards being monitored by the light barrier 7 .
[0035] As is shown in particular in FIG. 1 b, the card reading device 20 comprises a retraction compartment 8 in its rear area that is intended for storing/withholding cards 11 which the self-service terminal, due to have not met specific conditions, cannot give back to the user. The compartment 8 which is referred to as retraction compartment is located at the end of the supply/transport chain, meaning even behind the intake compartment 13 in which the specific card is read. After reading or attempting to read the card 11 , said card is transported further to the retraction compartment 8 .
[0036] The card reading device 20 is equipped with a sensor system (cf FIG. 2 ) that is mounted to a sensor carrier (cf FIG. 1A ) and can exactly detect and check the spatial dimensions (length, width and optionally height) of the inserted card 11 . Optionally a material determination via discrete spectroscopy in the IR-range can be performed by means of the sensor system.
[0037] The sensor system is arranged such that at least one dimension can be captured/detected that is preferably the width b or the length l or optionally the height h of the card. The sensor system 6 B measures the width b of the card but can also be used to measure the length l of the card, e.g. by a temporally triggered capturing by the sensor 6 B, wherein the length of the card is determined via the intake velocity/intake time. Moreover, single sensors can be used for each dimension. Said sensors can particularly be sensor arrangements such as opto-electric sensor arrays or strips of the type TSL208R that are fabricated by the company TAOS and comprise a number of 512 photodiodes linearly arranged in a distance of 125 μm. Herewith a very precise measurement can be achieved. Furthermore, an additional sensor 6 C can be arranged within the card reader or the intake compartment 13 to measure or check the height of the card (in z-direction). Depending on the specific case it can be sufficient to measure only one or two dimensions that are preferably the length and/or the width.
[0038] By means of the integrated sensor systems 6 A, 6 B and/or 6 C (optional) as well as by means of the light barrier 7 in combination with connection with the signal to retract coming from the card reader 3 the slots of the housing can be secured. Additionally an installed camera 10 (cf FIG. 1 b ) can be used. The functional connections are explained according to the FIGS. 4 a - c.
[0039] First of all it is referred to the FIG. 4 a that shows the verification of the inserted card 11 , wherein said verification/check is executed with the opto-electric sensor arrangement. In FIG. 4 a there are functional blocks A 1 -A 12 that represent the following:
A 1 : The opto-electric sensor elements provide/generate measurement signals for a width b, a length l and optionally for the height of the card 11 . A 2 : The evaluator device/electronics 4 checks/verifies the measured data/values comparing said values with standardized values of normalized banking cards. A 3 : If the measured values match/correlate to the standardized values the banking card is supposed to be a normal one. A 4 : Exciting via the piezo-electric sensor arrangement field 6 D is preferably not done during operation of the card reader. A 5 : However, monitoring of the card readers is executed, in particular of the card reader signals and/or energy consumption of the card reader. A 6 : If the measured data, as determined in A 2 , do not correlate to the standardized values, this indicates that an manipulation attempt has occurred. A 7 : Shutting down the card reader, and retracting the manipulated card if possible. A 8 : The software control of the delf-service terminal, which can be a PC, provides a warning signal. A 9 : An excitation can be executed at determined times of operation to verify the integrity of the housing. A 10 : An optional camera surveillance (cf 10 in FIG. 1 a ) can generate signals (images, video and/or audio). A 11 : The camera-signals are sent to the evaluator device 19 or to the computer in order to document the manipulation attempt and to store images of suspicious individuals for a subsequent identification. A 12 : Optional step wherein it is indicated/signaled that block/step A 9 is executed if this is allowed by the card reader data/signals.
[0052] FIG. 4 b is about monitoring the retract compartment via the sensor system or light barrier 7 (cf FIG. 1 a ) installed therein. In FIG. 4 b there are functional blocks A 1 -A 12 that display the following:
B 1 : The opto-electric sensor system or light barrier 7 at the retract slot creates signals, if a card 11 , a fake card or another object is transported through this slot or if an alien object is attempted to be inserted trought the compartment 8 from behind. B 2 : The evaluator device compares the result to the status of the card reader, meaning that the result is ‘okay’ if there is a retract situation. All other results are considered to be manipulation attempts. B 3 : Depending on the signals and measuring values it is determined that a normal card has been transported/supplied trough the retract slot 7 or that a normal retract process has happened. B 6 : If the transport of an abnormal card trough the retract slot 7 or the absence of a normal retract procedure has been determined in block/step B 2 , this indicates that there is a manipulation attempt. B 7 : The card reader is the shut down/switched off.
[0058] FIG. 4 c refers to a verification of the integrity of the card reading unit. The functional principle shown in blocks/steps CI-CVII however refers to a material-check of the self-service terminal housing to determine if it has been manipulated. FIG. 4 c refers to the verification of the housing (cf 1 in FIG. 1 b ):
CI: The evaluator device 4 triggers the verification/check of the housing by exciting piezo-electric actuators that are mounted at the housing to vibrate and by evaluating the measured values coming from same wise mounted sensor arrangements. The actuators can be integrated within the sensor arrangements (comparable to 6 D in FIG. 1 b ) or can be single piezo-electric elements of a certain field/area that are controlled to vibrate. CII: First of all the piezo-electric actuators are excited at known frequencies by a sweep. CIII: The sensors capture the signals. CIV: The evaluator device evaluates via the described method. CV: If the integrity of the housing is verified, the cycle starts from CI. CVI: If the integrity of the housing is not verified, the card reader will be switched off. CVII:The card reader will be switched off; where required even the whole self-service terminal.
[0066] The verification of the housing can also be a part of the disclosed method or can be an independent solution. If it is an independent solution, there are mechatronic transducers installed at or in the card reading device, in particular piezo-electric transducers, comprising sensors and/or actuators connected to the evaluator device. These transducers serve to generate a vibration that preferably lies in the audible range of eigenfrequency range on the card reading device but in particular on the housing. The mechatronic transducers are arranged in such a way in, on or at the card reading device that the integrity of the card reading device can be checked/verified. The evaluator device is arranged to receive a signal from the mechatronic transducers that has been excited by a part of the mechatronic transducers and is detected by another part of the mechatronic transducers to be compared with reference data and to output a warning signal, if a defined deviation is present implying a loss of integrity of the card reading device.
[0067] In the following the verification of the card material via the piezo-electric or optical sensor arrangement 6 D (cf FIG. 2 ) that is installed in the card reader is described in detail. This solution can also be embodied/executed as an independent solution, but is described as a part of the disclosed method in the present description according to FIG. 2 and FIGS. 5-9 :
[0068] To verify the integrity of the housing 1 of the card reading device, the card material and/or the intake compartment for the card 11 , the measurement signals coming from the sensor arrangements 6 D are pre-processed in the evaluator device 4 . This procedure is done in steps 121 - 128 and is explained according to the FIGS. 3 and 5 :
[0069] At first, in step 121 the local extrema for a specific incoming signal (starting point E) are determined, i.e. the absolute and relative maxima and minima of the amplitude from the signal waveform during the process. Then the upper and lower envelope is constructed in step 122 , wherein said envelopes being the an upper curve/function connecting the maxima and an lower curve/function connecting the minima. Then, in step 123 , an mean value of said envelope is formed, preferably as an arithmetic (or alternative) mean value. In a further step 124 a possible intrinsic modal-function (also known as IMF) is extracted. The steps 121 - 124 are executed in an iterative way, wherein in step 125 it is checked if and how severe the difference of two consecutive iteration-steps is. Therefore, the intensity of the deviation of two IMFs is checked.
[0070] If said difference/deviation is larger that a certain threshold, the next iteration step is performed (steps 121 - 124 ). Otherwise the latest determined IMF is used (step 126 ). Furthermore, the residuum is extracted in step 127 and is consecutively compared to a threshold in step 128 . If said residuum is larger than the threshold, a further iterative step is performed (steps 121 - 124 ). Otherwise the procedure is stopped (end point A=“stop”). In this case the IMF us used which was found suitable in step 126 .
[0071] The process displayed in FIGS. 3 and 5 displays an empirical mode decomposition (EMD) with which the piezo-electrical sensor signals can be processed to accordingly obtain one or more suitable IMFs being particularly characteristic for the material-properties of the investigated card. The executed EMD correlates to an iterative filtering process or smoothing process, wherein the highest frequency components can be extracted in each step. Thereby superpositions at high frequencies can be eliminated and amplitudes can be effectively smoothed. By using the EMD characteristic features can be yielded in a multidimensional feature space thus allowing an effective and reliable classification.
[0072] The data of the IMF as comprised in the process 120 can be subject to further steps including a classification that allows a solid decision of whether a manipulated card or even an alien body has been inserted into the card reader or not.
[0073] First of all it must be noted that the following has to be considered while using the features represented by the IMF:
Features are used to differentiate certain states. Features should be derived from possible object features. Features shall be different from one another (cf FIG. 6 b case (i) and (iii)). Objects of the same class should be found at similar locations in the feature space (cf cluster points such as shown in FIG. 6 s ). The lesser the number of features needed, the more effective the decision can be made. Generating good features shall be done specifically for each use case.
[0080] The yielded IMFs do basically represent a statistic pool of features (cf FIG. 9 ) that is particularly characterized by the following parameters of each of the specific IMF, namely by the standard deviation σ, the loop C, the excess E, the average deviation from the Median MD as well as the Median MAD of the total deviation. These data (amongst others) are particularly useful for a classification using a modified fuzzy-pattern classifier (MFPC) that is described according to FIGS. 7-9 :
[0081] It must be noted first, that IMF as yielded from the signal pre-processing (step 120 in FIG. 5 ) can optionally be subject to segmentation and to a subsequent feature extraction. However, these steps of the method are not explained in detail since the key aspect of the present application lies in the classification.
[0082] For classification a classification unit KFE (cf FIG. 7 ) is used that treats the data DAT (here the data of the specific IMF) as obtained according to a classificator KF as verification data PDAT and compares said data to a pattern mapping MZ. The classificator KF is not static therein but can be learned or optimized via a learning unit LE. This is done by treating the data DAT as training data TDAT and by comparing it to a pattern mapping MZ. The optimized classification KF is then employed to the real measured data (PDAT).
[0083] As shown in FIG. 8 the classificator is conditioned/defined as a fuzzy-pattern-classificator (FPK) to allow a fuzzy-pattern-classification. Such a classification describes a problem associated evaluation and assignment of data in the context of being gradually associated (association function μ(x)) and being coupled amongst each other according to measuring values (aggregation). By expertise and training (see FIG. 7 ) association functions can be generated according to measurements. The fuzzy-pattern-classification takes into account the uncertainty of the classes being generated from single observations and employs the concept of association functions. The association function μKL: X→[0,1] correlates every object x of the feature space X to a number from the real valued interval [0,1], wherein this number designates the degree of belonging μKL(x) of the object to the un-sharp class KL. Furthermore, an uncertainty of every sole observation or every object due to methodological problems, measurement errors and so on is assumed. This uncertainty is expressed by designating an basic uncertainty to every object. For further details it referred to the literature.
[0084] The input for the fuzzy-pattern-classification, as displayed in FIG. 7 , are statistical features as displayed in FIG. 9 .
[0085] The extracted features comprise for instance the standard deviation, skewness, kurtosis average deviation from the median and the median of the absolute deviation. The standard deviation is a measure for the shattering of the values of a random variable around its expectation value. The skewness is a statistical characteristic number describing the type and strength of the probability distribution. It designates how strong the distribution tends to the right (positive skewness) or to the left (negative skewness). The kurtosis is a measure for the peakedness vs. tailness of a (single maximum) probability distribution, statistical density distribution or frequency distribution. The kurtosis is the central moment of order four. Distributions with a small kurtosis are distributed relatively uniformly; distributions with a higher kurtosis correspond to events that are distributed more extreme but for less events.
[0086] The median or also called central value is a mean value of distributions in statistics. The median of a list of numbers is the value that stands in the middle of said list after sorting the numbers in said list according to their value. The mean absolute deviation from the median is the variation/spreading around the median. Spreading/scattering (also called dispersion or average absolute deviation) combines various characteristic numbers in descriptive statistics and stochastics that describe the scattering widths of values of a frequency distribution or probability distribution around a suitable location parameter. The described calculation methods differ in being affected or being sensitive against runaway values. The scattering of the frequency distribution is called the standard error.
[0087] For the determination of the class the method uses a special procedure of supervised learning from structured, fuzzy example objects, i.e. objects that are defined to belong to a class by a “teacher” or “expert”. Both the elementary fuzziness of objects and the fuzziness of the classes is expressed by the asymmetric potential-function according to Aizerman.
[0088] Summarizing and by considering all FIGS. 1-9 the following can be said to the implementation of the method in a self-service terminal:
[0089] Besides the installation of the opto-electric sensors for verifying the card dimension (sensor array 6 A and 6 B as well as 6 C in FIG. 1 a ) and the opto-electric and/or piezo-electric sensor arrangement 6 D for checking the card material and/or the condition of the intake compartment, the housing 1 of the self-service terminal (see FIG. 1 b ) can also comprise piezo-electric patches monitoring the manipulations at the housing itself. The housing can be made out of steel and/or plastic. It forms a base plate 2 and IDKG-module 5 enclosed in the housing. The only openings are the card slots for card intake and card retract (region 8 ). The piezo-electric are attached adherently in the preferred version, but can alternatively also be directly be formed in a plastic part. The sensors are operated by the evaluator electronic or evaluator device 4 . The sensors can be operated as actuators or sensors. To this end the evaluator device 4 excites one of the sensors in an actuator fashion in a pre-defined pattern and the other piezo-electric patches obtain the excited signal. The electronics then compares the signal to a theoretical signal.
[0090] Furthermore the Computer of the self-service terminal (e.g. an ATM) is physically connected to the electronics. The electronics powers the card reader and is also optionally connected to the electronics in a logical way. The first (meaning the physical connection) serves a defined switching on and off of the card reader, the latter (meaning the logical connection) is used for processing possible firmware-signals of the card-reader, such as a retract or intake of the card. If the signal output of the card reader does not yet have firmware implemented, the energy intake of the card reader can be measured thus giving a reasoning for the modus of operation (intake/retract/output(stand-by) of the card reader.
[0091] The retract area (see FIG. 1 b ) guides and centers the card 11 to the card reader 3 . It is equipped with said opto-electric sensor system being a sensor and light barriers that obtain the geometrical dimensions of the card completely. By means of at least one sensor arrangement, e.g. 6 B in FIG. 2 it can be distinguished between a regular valid card and a non valid object, e.g. being a device for installing a skimmer in the interior of the device. The signals of the sensor arrangements 6 A and/or 6 B as well as the additional sensor 6 C are evaluated in the evaluator device 4 . The same is valid for the light barrier at the retract acompartment. However, in this case the light barrier 7 is not qualitatively evaluated but a fusion of information with the event “retract” of the card reader. Furthermore, the evaluator device 4 can send signals to the computer that activates a the optional surveillance camera 10 by a software (e.g. OSG) and checks the integrity of the card reader slot.
LIST OF REFERENCE SIGNS
[0000]
20 card reading device
1 housing
2 base plate
3 card reader
4 evaluator device
5 IDKG slot module
6 sensors
7 light barrier
8 retraction compartment
10 camera(s) (optional)
11 card (EC/Master/Visa) inserted
11 ′ card (EC/Master/Visa) in an insert slot
13 intake compartment
6 A, 6 B 6 B linearly extending sensor arrangement;
6 C additional sensor system
6 D sensor array with piezo-electric sensor elements
121 - 128 steps for signal pre-processing
A 1 -A 12 ; B 1 -B 7 ; CI-CVII functional blocks
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A card reading device ( 20 ) for a self-service terminal has an intake compartment ( 13 ) for a card ( 11 ) containing data to be read. The intake compartment ( 13 ) has at least one linearly extending sensor arrangement ( 6 A, 6 B) and an evaluator device ( 4 ) connected thereto to protect the card reading device ( 20 ) against manipulation attempts. The evaluator device ( 4 ) checks at least one spatial dimension (l,b) of the card via the sensor arrangement ( 6 A, 6 B), namely a dimension in a first direction (X) or a second direction (Y) in relation to the card ( 11 ) retracted into the intake compartment ( 13 ). Thus, it can be determined effectively whether a retracted card is a genuine card or if a manipulation is present that targets the inside of the card reading device.
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TECHNICAL FIELD
This invention relates to a light-reflecting plate with micro prism, especially to circular light-reflecting plate with triangular prisms having the same cross section and the circular plate lamps and circular plate lighting fixtures made therefrom.
BACKGROUND ART
In prior art, the light-reflecting sheet or plate is mainly used for reflection and refraction of light rays. Later strip-type micro prisms are added for better reflection and refraction of the sun light and further, lighting fixtures are added at both ends to function as both luminous panel and lighting. In Chinese patent No. 200510029375.1, the applicant invented a micro prism-type sunlight reflecting plate and its regulating device, wherein the surface of the light-reflecting plate is equipped with several parallel micro prism bodies having the shape of isosceles right triangles, the vertex angle of which is 90° and the base angle is 45°. On each end face, there is blind hole to receive the LED lamp bodies. This kind of light-reflecting plate is used for rooms with glass ceiling, windows or skylights, which gives sufficient access to sunlight in winter and completely or partially reflects back the sunlight in summer. It shades from direct sunlight while ensuring adequate lamination indoors. The lamp bodies on both ends can provide additional lighting at dark weather or at night. Although the light-reflecting plate of this structure can make the overall plate to function as a luminous surface under the action of the lamp bodies, its luminance is very low due to limitation by design structure.
Inspired after the aforesaid patent, the applicant envisages how to employ the combination of light-reflecting plate and LED with lighting fixtures and starts to study on changing the point light source of the light-reflecting plate to surface light source via LED. That is to use LED for lighting other than for decoration. For this purpose, the applicant has disclosed two light-reflecting plates in PCT/CN2007/002052 and PCT/CN2008/000031. Among them, one is flat light-reflecting plate, wherein one surface is arranged with several parallel strip-type micro prism bodies, the cross sections of the left and right scalene right-angle triangles adjacent to the symmetrical central plane are the largest and the cross sections towards the left and right sides are successively decreasing. The other is a circular light-reflecting plate consisting of right-angle triangular micro prisms with the central axis as the symmetrical center, wherein several annular micro prism bodies are formed in its radial direction with its cross section and section area being the same with those of the flat one. After blind holes and lamp bodies are equipped on both ends and circumferential faces of the two light-reflecting plates, for example, circular light-reflecting plate has lamp bodies which are arranged thereon, and the emission centers of these lamp bodies are parallel to the plane of the light-reflecting plate, or pass through the apexes of the inclusion angles of the annular prism bodies on the plane of the light-reflecting plate. The light emitted from the lamp bodies will reflect from the micro prism bodies, resulting in good lighting effect.
In further studies, it has been found that the flat and circular light-reflecting plates with the above-mentioned structures show the shortcomings that the reflecting and emitting light rays on one plane from the light-reflecting plate via the prisms are non-uniform (influencing the lighting effect) and small scale of light sheets made of light-reflecting plate, that is, asymmetrical one-side micro prism layout. The above both patent applications have not addressed these problems.
LED light source must be used for lighting based on its structural characteristics, but in its development process, LED currently has its setbacks, especially in the application of high-power LED. The biggest problem is light decay. LED's use in indoor lighting is also difficult. In sum, we have little knowledge on the light characteristics of LED light source, how LED lamps can be combined with lighting fixtures and how the optical and mechanical design can be ensured for lamps and lighting fixtures. Those are the problems to be solved in the present invention.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a light technology matching with LED properties so that LED can reflect and emit evenly distributed light rays on one plane of the prism of the light-reflecting plate, and to provide an oriented circular light-reflecting plate having oriented triangular prisms which have the same (equivalent) cross section, and an circular plate lamp or circular plate lighting fixture made therefrom.
The other object of the invention is to use low power and low current LED chips, instead of high-power LED so as to prevent from complicated lighting fixtures due to complicate LED heat-dissipating structure, and avoid decreasing of luminous flux due to high LED temperature resulting from high power, so that each beam of light can accurately orient its emission, transmission and reflection and the heat generated by LED chips can be quickly dissipated, thereby achieving better lighting effect.
To achieve the above-mentioned objects, the invention adopts a light-reflecting technology, called light-reflecting plate with triangular prisms having the same cross section, which constitutes the principal part of the circular plate lamp. In this light-reflecting plate, a series of triangular prisms having the same cross section are arranged outward from the center, forming a series of concentric triangular prisms having the same cross section. In the invention, a plurality of concentric annular micro prism bodies are arranged on the prism surface of the light-reflecting plate in the radial direction starting from the central axial line, the cross sections of prism bodies are triangles and continuously arranged in zigzag form in the vertical section through the central axial line, wherein that the triangles have the same shape and the same cross sectional area, the apex of the triangle closest to the central axial line has the shortest distance away from the smooth surface of the light-reflecting plate, and the apices of the triangles towards the periphery of the light-reflecting plate have the successively increasing distances away from the smooth surface of the light-reflecting plate. The radial connection lines among the apices of the triangles of the circular prism bodies are two inclined straight lines, intersecting at a point with the central axial line of the circular light-reflecting plate and forming an inclusion angle α with the smooth surface of the plate. The inclusion angle α is 45° and the distance or interval of all triangles is equal in the diameter direction.
In one embodiment of the above circular plate or lamp, the apices of the continuously zigzag-formed triangles have successively decreasing distance from the smooth surface, and the extension line of the marginal side, which is either of the right side and the left side of the triangles, intersects with the smooth surface relative to the prism surface and forms an inclusion angle ranging from 40° to 90° with the normal line thereof.
In one embodiment, the inclusion angle α of the circular light-reflecting plate is less than 10°.
In one embodiment, the triangles of the circular plate lamp are right-angle or non-right-angle triangles.
In one embodiment, the transparent plastic for the circular plate lamp is PC (polycarbonate).
In the invention, the circular plate lamp made of the circular light-reflecting plate comprises of a light-reflecting plate, a heat-dissipating frame and a plurality of lamp bodies, wherein the heat-dissipating frame comprises a plate surface with a central throughhole and a circular plate edge around the plate surface and the frame is sleeved around the light-reflecting plate so that the plate edge (wherein the throughhole is located on the surface) overlaps with the edge of the smooth surface of the light-reflecting plate, the lower part of the internal wall of the plate edge abuts with the flange of the light-reflecting plate, and the remaining part of the internal wall constitutes a gap with the cylindrical surface of the light-reflecting plate, thereby form a circular lamp groove having the same axle with the central axle; the lamp bodies comprise LED, light bulbs, electrode tubes, or prefabricated assemblies having a plurality of LEDs and are assembled in the circular lamp groove, respectively, wherein the emission plane of the LED intersects with the connection lines of the apices of the triangles and forms an inclusion angle of 90-α.
In one embodiment, the circular plate lamp comprises heat-dissipating plate, wherein the heat-dissipating plate is a circular plate, the upper surface of which is arranged with a plurality of evenly-distributed and concentric circular heat-dissipating ribs perpendicular to the plate surface and overlaps over the light-reflecting plate through the marginal part of the circular ribs with the plate edge of the heat-dissipating frame.
In one embodiment, the circular heat-dissipating ribs of the heat-dissipating plate have evenly-distributed gaps aligned in radial direction and the heat-dissipating plate is made of aluminum alloy.
In one embodiment, the circular plate lamp comprises a reflecting back sheet, wherein the reflecting back sheet has almost the same dimensions with the light-reflecting plate, which can be made of plastic, paper or metal and is installed between the light-reflecting plate and the heat-dissipating plate.
In one embodiment, the lamp bodies of the circular plate lamp are prefabricated circular lamp assemblies having a plurality of LED BONDING DIEs, resistor and circuit board and the lamp assemblies are bended into annular shape and are installed or embedded in the annular lamp groove so that the LED emission plane installed inside the lamp groove is close to or closely attached with the cylindrical surface of the light-reflecting plate of the lamp groove and forms an inclusion angle of 90-α by intersecting with the connection lines of the apices of the triangles on the cross section of the light-reflecting plate.
In one embodiment of the circular plate lamp, the heat-dissipating frame edge and its peripheral wall are arranged with several evenly distributed annular heat-dissipating ribs in the radial direction.
In one embodiment of the circular plate lamp, the side of the triangles where the triangular prism body radiates towards or the side adjacent to the light is the light-receiving side and also the marginal side where the triangle faces towards the central axis, and the circular surface where the light-receiving marginal side is located is the light-receiving marginal surface, wherein the extension line of the marginal side intersects with the smooth surface of the prism surface and forms an inclusion angle with the normal line of the smooth surface, ranging from 40°-90°.
In one embodiment of the circular plate lamp, the LED and LED BONDING DIE are dioxides and chips with low power and current, and several chips can be installed inside a LED BONDING DIE.
In one embodiment, the heat-dissipating frame and heat-dissipating plate of the circular plate lamp are made of aluminum alloy.
In one embodiment of the circular plate lamp, each of heat-dissipating plate, the reflecting back sheet and the light-reflecting plate is arranged with a central installation hole in the center.
In one embodiment, the circular plate lamp further comprises a screw socket and a constant current power supply, wherein the heat-dissipating plate is of conical shape, the apex of which is arranged on a plane and on the conical face of which are arranged with radial heat-dissipating ribs; the screw socket is installed on the plane of the conical apex; the constant current power supply is installed between the heat-dissipating plate and the reflecting back sheet by a support, the input terminal of which is connected with the screw socket and the output terminal is connected with the terminal block of the LED strip light source.
Therefore, the circular plate lamp with triangular prisms having identical cross section is an area source light-emitting engine consisting of constant current source for power driver, LED light-emitting strip-type light source, aluminum heat-dissipating frame for circular plate lamp (heat-dissipating device) and secondary optical elements of circular plate with triangular prisms having identical cross sections. The circular plate lamp is basically of circular plate structure, and when it is lit up, the light rays emit out from the circular plane wherein the driving voltage is of 12V or 24V DC and constant current ranges from dozens to hundreds of milliampere (mA). It can be made into sheet-type circular lamps with diameters ranging from dozens of millimeters to hundreds of millimeters and can thus be used for indoor lighting, such as ceiling lamps in bedrooms, washing room, and kitchens, as well as cupboard circular plate lams, and ceiling lamps for public alleys and public open spaces. The circular plate lamps can also be used as desk lamps. Further, the 1 w circular plate lamps with diameters of dozens of millimeters can be used for the senior people at night.
The circular plate lamps are flat and compact and the light emitted from the circular plane is uniform without glare. The shell temperature is often 10 degree higher than the ambient temperature. It uses 12V safe low voltage and the overall current is lower than 1000 mA, featuring long service life up to 40000 hours. Therefore, it can be widely used for indoor lighting.
Taking 4.6 w LED circular plate lamp with diameter of 190 mm as an example, the luminance at 400-500 mm is 900 Lux and 195 Lux at 1 m distance.
Just like the incandescent lamps, LED circular plate lamps have ideal and uniform light color without glare and flash, ensuring long service life.
LED circular plate lamps are a kind of energy-saving lamp, which can have the same luminance with the incandescent lamps at just 1/10 power compared with the incandescent lamps.
LED circular lamps are simple in structure, easy for use, safe in transport and environment-friendly for its materials and they can be recycled. LED sheet-type circular lamps can facilitate our life, work and study while ensuring highly efficient energy conservation.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 a and 1 b are perspective views of the light-reflecting plate with triangular prisms having the same cross section and the circular plate lamp made therefrom.
FIG. 2 a and FIG. 2 b are the sectional view of the circular plate lamp with triangular prisms having the same cross section and the enlarged view of A.
FIG. 3 a is the front view of the circular plate lamp, showing the part after the removal of the heat-dissipating plate.
FIG. 3 b is the sectional view along A-A in FIG. 3 a , showing a prism body design structure of the prism surface of the circular plate lamp and optical path analysis under LED exposure.
FIG. 4 a is the front view of No. 2 circular plate lamp, showing the part after removal of the heat-dissipating plate.
FIG. 4 b is the sectional view along A-A in FIG. 4 a , showing another prism body design of the prism surface of the circular plate lamp and the optical path analysis under LED exposure.
FIG. 5 a is the front view of the No. 3 circular plate lamp, showing the part after removal of the heat-dissipating plate.
FIG. 5 b is the sectional view along A-A in FIG. 5 a , showing another prism body design of the prism surface of the circular plate lamp and the optical path analysis under LED exposure.
FIG. 6 is the view showing the gaps among the triangular prism bodies alongside the central axis in the diameter direction and the relationship of the inclusion angles formed between the connection line of the apex of the adjacent triangle and the horizontal line.
FIG. 7 is the enlarged A view of FIG. 6 , showing that the light-receiving marginal face of the prism body is the side of the right-angle triangle and intersects with the normal line of the prism to form an inclusion angle of 45°.
FIG. 8 is the view showing the gap among the triangular prism bodies in their diameter direction on one side of the central axis of the circular plate lamps in FIG. 4 b and the relationship between the connection lines of the apexes of the adjacent triangles and the horizontal lines.
FIG. 9 is the enlarged B view of FIG. 8 , showing that the light-receiving marginal face of the prism body is right-angle triangle and intersects with the normal line of the prism to form an inclusion angle of 45°.
FIG. 10 is the view showing the gap among the triangular prism bodies in their diameter direction on one side of the central axis of the circular plate lamps in FIG. 5 b and the relationship between the connection lines of the apexes of the adjacent triangles and the horizontal lines.
FIG. 11 is the enlarged C view of FIG. 10 , showing that the light-receiving marginal face of the prism body is right-angle triangle and intersects with the normal line of the prism to form an inclusion angle of 45°.
FIG. 12 is the curve graph comparing the luminance of the 4 w circular plate lamp of the present invention with 60 w incandescent lamps at 0-1.5 m distance.
FIG. 13 is the curve graph comparing the luminance of the 4 w circular plate lamp of the present invention with 60 w incandescent lamps at 1.5-3 m distance.
FIG. 14 is the curve graph comparing the luminance of the 4 w circular plate lamps with triangular prisms having identical cross section but having different shapes under present invention at 0-1.5 m distance.
FIG. 15 is the curve graph comparing the luminance of the 4 w circular plate lamps with triangular prisms having identical cross section but having different shapes under present invention at 1.5-3 m distance.
FIG. 16 is the circular plate lighting fixtures made of the circular plate lamps of the invention.
FIG. 17 a and FIG. 17 b are the sectional view and top view of the circular plate lighting fixtures with screw holder, respectively.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1 a to FIG. 2 b , FIG. 1 shows the first embodiment the circular light-reflecting plate with triangular micro prism having identical cross section of the invention. A plurality of concentric annular micro prism bodies 111 are arranged on one surface of the prism surfaces 11 of the light-reflecting plate 1 starting from the symmetrical center OO′, and the cross section of each micro prism body 111 is of triangle, including right-angle and non-right-angle triangles, wherein the triangles are arranged in continuous zigzag form and have the same cross sections and the apex of the left and right triangles adjacent to the symmetrical center has the shortest distance away from the another surface (or the smooth surface) 12 of the light-reflecting plate in its vertical direction and the vertical distance from the apexes towards the left and rights sides to the another surface of the light-reflecting plate are gradually increases (the tow sides of the central plane of central axis are symmetrical and therefore the vertical distance of the left side is taken as an example), and all triangles have the same distance δ in their length direction. Therefore, the overall width of the triangular prism body is 2n×δ, wherein n refers to the number of concentric annular triangular prism bodies on one side of the symmetrical central plane. Moreover, in this invention, the light-reflecting plate can also connect the apexes of the triangles close to the smooth surface 12 and the apexes of the triangles far away from the smooth surface 11 to form two straight lines or connect the two planes (with the left side of the central axis as an example), in addition to two preset planes, namely the smooth surface 12 and the prism surface 11 of the zigzag-arranged triangles. The two straight lines is inclined but parallel and intersect with the central axial line OO′ of the cross section of the light-reflecting plate at Points A and H to form AN and HM, which form an inclusion angle α (α<45°) with the smooth surface 12 . The circular light-reflecting plate of the invention can be made of transparent plastic, such as PC (Polycarbonate).
In addition, for the purpose of design, we have introduced the concept of marginal edge in this application. That is, either of the right and left sides of each triangle towards the direction where the distance from the apex of the zigzag-arranged triangles to the smooth surface is gradually decreasing is called marginal edge, the extension line of which intersects with the smooth surface relative to the prism surface and forms an inclusion angle ranging from 40° to 90° with the normal line.
In the invention, when the circular plate lamps are made from the aforesaid light-reflecting plates with different triangles having identical cross section, heat dissipating frame and lamp bodies, we will explain how the circular plate lamps made therefrom reflect and refract under LED irradiation as follows.
Refer to FIG. 1 a and FIG. 1 b . The circular plate lamps of the invention consist of circular light-reflecting plate 1 , several lamp bodies 2 and heat-dissipating frames 3 , wherein the light-reflecting plate 1 has outward-extending edge 113 outside the circular micro prism body farthest to the central axial line OO′. The edge 113 remains with partial cylindrical surface 114 on its peripheral surface and in addition, has circular flange 115 at place adjacent to the smooth surface 12 under the cylindrical surface 114 .
The heat-dissipating frame 3 consists of a plate surface 31 with a central throughhole and a circular plate edge 32 around the plate surface, as shown in FIG. 2 a . The frame is sleeved around the light-reflecting plate so that the edge of the throughhole of the plate surface overlaps with the edge 113 of the smooth surface of the light-reflecting plate and abuts with the flange 115 through the bottom of the internal wall of the plate edge 32 of the heat-dissipating frame and the remaining part of the internal wall forms a gap with the cylindrical surface 114 of the light-reflecting plate to create a circular groove having the same axle with the central axial line OO′, namely, the lamp groove 14 . Preferably, several evenly-distributed circular heat-dissipating ribs can be arranged on the external wall of the plate edge 32 of the heat-dissipating frame to form heat-dissipating groove 27 among the ribs. The heat-dissipating frame 3 can be made of aluminum alloy materials to ensure good heat-dissipating effect.
In a preferred embodiment, heat-dissipating frame 3 is an independent element made of aluminum alloy, with heat-dissipating ribs 33 ′ arranged on its external wall. When sleeved onto the light-reflecting plate, the bottom of the internal wall abuts with the flange 115 of the light-reflecting plate and the remaining part of the internal wall forms a gap with the cylindrical surface 114 of the light-reflecting plate to create a circular groove having the same axle with the central axial line OO′. Part of the heat-dissipating circle 32 ′ is also made of aluminum alloy.
The lamp body 2 is an LED, wherein the bulb, or electrode tube or prefabricated LED assemblies are installed in the circular lamp groove 14 . The emission plane of the LED intersects with the apex of the triangle on each cross section to form an inclusion angle of 90-α.
In this embodiment, the lamp body 2 uses prefabricated LED assembly, which is a circular lamp assembly consisting of several LED bonding dies 21 , resistor and circuit board 22 . The LED bonding dies 21 are evenly arranged on the circuit board 22 , wherein the lamp body is changed into circular shape by bending the circuit board and is installed or embedded in the lamp groove 14 so that the emission plane of LED bonding die 21 is close to the cylindrical surface 113 of the light-reflecting plate of the lamp groove 14 and intersects with the connection lines of the apexes of the triangles on the cross sections of the light-reflecting plate to form an inclusion angle of 90-α.
The main axle of the light rays emitted by the LED bonding dies 21 (LED in general) installed in the lamp groove 14 is a beam of light parallel to the smooth surface 12 of the light-reflecting plate. When there are n triangular prism bodies having identical cross section on one side of the central axis of the light-reflecting plate 1 and the area for each LED boding die 21 will be A, then the LED area A is divided into n equal parts equivalent to the number of the prism body 111 . If the total photon energy provided is E, then the sufficient photon energy distributed to each equal area division is E/A/n so that each prism body 111 on the prism surface 11 can be illuminated evenly. The LED bonding dies used for this invention are low-power tubes and several chips can be arranged with one LED boding die. The multi-chip LED bonding dies are lined up in matrix form and installed in the lamp groove 14 .
Mathematic expression is used herein to illustrate the optical features of the triangular prism bodies having identical cross section. The inclusion angle α formed by the two straight lines AN and HM with the smooth surface can be obtained by drawing parallel lines on the smooth surface through Points A and M (inclusion angle α). Usually, the inclusion angle α is less than 10°. The two straight lines are AK and ME, as indicated in FIG. 2 . Suppose to take parallel line AK as an example, the first triangle FCA on the cross section of the prism body alongside the central axle is a non-isosceles right angle triangle. The vertical line from Point F (apex of the adjacent triangles) to the parallel line is FB, which functions as the squared edge of the right angle triangle, indicated by h 1 . A series of squared edges h 2 , h 3 . . . h n-1 , and h n can be obtained by drawing vertical lines with the parallel line AK from the 2 nd to n apex of the adjacent triangles, and therefore, h 1 , h 2 , h 3 . . . h n-1 , and h n indicate the vertical distance from the asymmetrical central axle to the apexes of the 1-n triangles on one side. BA is a section of the sectional triangle on the parallel line AK and also functions as another squared edge, and is equal to the gap δ of the sectional triangle in the length direction. Therefore, from the formula
tg α = FB AB or tg α = a n × δ ,
the vertical distance h 1 from the apex of the triangle adjacent to the first right triangle on one side of the central axle to the parallel line AK can be obtained. For FB=h 1 , BA=δ, then h 1 =δ×tgα. Similarly, it is available to obtain the vertical distance h 2 , h 3 . . . h n-1 , and h n from the apexes of the triangles adjacent to the 2 nd to No. n right angle triangles to the parallel line AK. For example, the No. n triangle on one side of the central axle is
tg α = hn n × δ ,
wherein hn is the vertical line made from the apex of the No. n adjacent sectional triangle to the parallel line AK, and H is the height or diameter of the LED bonding die. Usually, hn is equal to H so that the LED bonding die can irradiate the light-receiving marginal surface of each triangle in its height direction via the vertical distance of the apex of the adjacent triangle functioning as the main axle passage of the emitted light beams and provide adequate photon energy.
Refer to FIG. 3 to FIG. 5 . Among them, FIG. 3 a , FIG. 4 a and FIG. 5 a show that there are two terminals 29 equipped with the circular plate lamp and the light-reflecting plate 1 has a receptacle respectively on the end face of the edge 13 outside the lamp groove, wherein the terminals 29 are respectively installed in the receptacles and electrically connected with the leading wire of the strip-type lamp assembly 2 so that external power supply can be connected with the terminals 29 . In fact, FIGS. 3 to 5 illustrate the design of the triangles having identical cross section and symmetrical in the center of the circular plate lamp. First, FIG. 3 a and FIG. 3 b show that the triangle having identical cross section of one of the circular plate lamp is a 45° triangle, wherein the two triangles arranged left and right of the central axis OO′ have respectively outward-going vertical squared edges 15 (from which the LED light irradiates into the edge or surface of the prism) and inward-going inclined edges. These inclined edges face towards the LED irradiation direction (LED optical axis) or are adjacent to the light, and therefore, they are defined as marginal edge (marginal surface) or light-receiving marginal edge (or marginal surface) 16 . For these light-reflecting plates having identical triangular cross sections, the normal line of each right-angled triangular prism body intersects with the extension line of the light-receiving marginal edge and forms an inclusion angle of 45°.
FIG. 4 a and FIG. 4 b show that the triangle having identical cross section of the second circular plate lamp is non-isosceles right-angled triangle, wherein the two right-angled triangles arranged on the right and left of the central axis OO′ are two squared edges facing inward and outward respectively. Among them, the outward-facing edges or surfaces, namely the edges from which the LED light irradiates through the prism, are defined as irradiation squared edge 17 and the facing inward squared edges in the direction of the irradiation direction of LED (LED optical axis) are defined as marginal edges or light-receiving marginal edges 18 . For these light-reflecting plates having non-isosceles right-angled triangles, the normal line F of each right-angled triangular prism body intersects with the extension line of the light-receiving marginal edge 18 and forms an inclusion angle of 45°.
FIG. 5 a and FIG. 5 b show that the triangle having identical cross section of the 3 rd circular plate lamp is non-right-angled triangle, wherein the two triangles arranged on the left and right side of the central plane of the central axis OO′ have two triangular edges 19 and 24 having different length facing inward and outward respectively. These outward-facing short edges face towards the LED irradiation direction and are defined as marginal edges or light-receiving marginal edges 24 . For this kind of light-reflecting plate having identical triangular cross sections, the normal line F of each triangular prism body intersects with the extension line of the light-receiving marginal edge 24 and forms an inclusion angle of 45°.
It can be seen from FIG. 3 to FIG. 5 that how the aforesaid circular plate lamps ensure oriented lighting. If the normal line of each triangular prism body in these kinds of light-reflecting plates having identical triangular cross sections intersects with the extension line of the light-receiving line and forms an inclusion angle of 45°, then the circular plate lamp with triangular prisms having identical cross section generates can emit the light c which is parallel to the normal line of the smooth surface 12 of the circular plate lamp.
The circular plate lamps made of the aforesaid light-reflecting plates having triangles of different cross sections can emit light from the smooth surface at certain angle and can be concentrated to form oriented lighting. Therefore, the term “oriented lighting” refers to the combination of the emitting lights from the light-reflecting plate with triangular prisms having identical cross section and installed with LED, which form inclusion angles with the normal line of the prism plane. Any of the circular plate lamps with triangular prism having identical cross section in FIG. 3 to FIG. 6 can emit light which forms an oriented inclusion angle with the normal line of the smooth surface. Therefore, as one-spot light source, either the LED bonding die 21 or multi-chip LED bonding die can emits lamplight to n triangular prism bodies having identical cross section respectively. Then it forms a strip-type emitting light after being reflected and refracted by the light-receiving marginal edge and smooth surface. A plurality of strip-type emitting light from the LED bonding dies are closely arranged and distributed on the overall surface to form a surface irradiation light having high luminance. This illustrates the main principles why the circular plate lamp of the invention can be used to replace the traditional incandescent and fluorescent lamps.
Please refer to FIG. 6 to FIG. 11 , showing that the common points for the three circular plate lamps with triangular prisms having identical cross section are that the extension lines 16 , 18 and 24 of the light-receiving marginal surfaces or edges all intersect with the normal line of the smooth surface 12 and form an 45° inclusion angle and generate emitting light beams parallel to the normal lines of the smooth surface. Analysis has shown that the inclusion angle between the extension line of the light-receiving marginal surface of the triangular prism having identical cross section shown in these figures and the normal line of the smooth surface of the prism is 45°, which is common to the circular plate lamps with triangular prisms having identical cross section. The light generated by these circular plate lamps is parallel to the normal line of the smooth surface, as shown in FIGS. 3 , 4 and 5 .
FIG. 8 is the partially enlarged drawing of the prism body. In this figure, one of the vertical surface or edge OM ( 15 ) of the triangular prism is the squared edge from which the LED light passes through the prism and the distances of the right-angled triangles are δ1 respectively in their length direction. FIG. 10 shows the squared surface or edge OM′ ( 17 ) from which the LED light from the right-angled triangular prism passes through the prism and the distances of the right-angled triangles are δ2 respectively in their length direction. FIG. 11 shows the squared surface or edge OM″ from which the LED light from the right-angled triangular prism passes through the prism and the distances of the right-angled triangles are δ3 respectively in their length direction. Therefore, it must be noted that among these prism bodies, the distance of the triangles of the light-reflecting plate shown in FIG. 7 in its length direction is δ1 which is the shortest on the light-reflecting plates with same width to ensure that the triangular prisms having identical cross section have the same area, whether they are right-angled or non-right angled triangles. The triangles on the light-reflecting plate shown in FIG. 11 have the longest distance of δ3 in their length direction. However, the right-angled triangles of the light-reflecting plates shown in FIG. 9 have the distance of δ2 in their length direction, which lies between δ1 and δ3. Therefore, a plurality of triangular prism edges can be arranged on the light-reflecting plate of FIG. 7 , while fewer triangular prism edges can be arranged on the light-reflecting panel shown in FIG. 11 . Accordingly, for the light-reflecting sheet with the same width, the more the triangular prism edges are, the more the outgoing light rays and the stronger the light rays will be, and vice versa.
Please also refer to FIGS. 3 b , 4 b and 5 b . It can be seen from these figures that LED bonding die 21 is precisely oriented in the lamp groove 14 and the optical axis of the LED bonding die is parallel to the plane of the circular plate lamp. The parallel light beams emitted from LED bonding die irradiates on the marginal point of the triangular prisms arranged in sequence, which passes out the smooth surface of the prism after total reflection to form an oriented lighting parallel to the normal line of the smooth surface.
In the invention, low-power and low-current LED bonding dies are used. The PN junction of LED generates heat at 80% working current. To ensure long-time LED operation, PN junction must be operated at low temperature and the heat generated by PN junction must be removed promptly. Aluminum alloy with good heat conductivity is used for the edges relative to the outward direction of the lamp groove of the light-reflecting plate (these edges are also the frame of the lighting fixtures). Therefore, heat-dissipating frame 3 made of aluminum alloy is arranged at the edge to ensure good heat conductivity.
Please also refer to FIGS. 1 a , 2 a and 16 , wherein another embodiment of circular plate lamp of the invention is shown, which consists of the heat-dissipating plate 4 and or reflecting back sheet 5 , in addition to the circular light-reflecting plate 1 , a plurality of lamp bodies 2 , and heat-dissipating frame 3 . The said heat-dissipating plate 4 is a circular plate like a cover. Preferably, a plurality of evenly distributed concentric annular heat-dissipating ribs 41 are arranged on the surface of the circular plate, which is connected with the plate edge of the heat-dissipating frame via its edge, including screw 6 and is covered over the light-reflecting plate. The annular heat-dissipating ribs 41 of the heat-dissipating plate 4 conduct the heat emitted from the lamp body 2 . A heat-dissipating groove is formed among the heat-dissipating ribs so as to ensure air circulation and spread the heat from the center. In addition, a plurality of evenly distributed gaps 411 are arranged on each of the annular heat-dissipating ribs 41 of the heat-dissipating plate 4 . Preferably, these gaps are arranged in line so that the heat can be better diffused out of the lamps and the heat-dissipating plate is made of aluminum alloy. The reflecting back sheet 5 has the dimension similar to that of the light-reflecting plate, and can be made by plastic, paper or metal material, and is installed between the light-reflecting plate 1 and the heat-dissipating plate 4 .
Refer to FIGS. 12 and 13 . These figures show the luminance curves of the 4 W circular plate lamp of the invention with the 60 W incandescent lamp at different distances, wherein the black dots and black connection lines are used to indicate the luminance of the 4 W circular plate lamp within certain distance and the grayish black dots and connection lines are used to indicate the luminance of the 60 W incandescent lamps within certain distance. Moreover, the vertex angle of the triangular prism body having identical cross section of the 4 W circular plate lamp is 45° (as shown in FIG. 3 ). Based on the test result, the luminance of 4 W circular plate lamp within 0.3-1.5 m can range from 1350 Lux to 70 Lux, while that for 60 W incandescent lamp within the same distance decreases from 800 Lux to below 70 Lux. The luminance of 4 W circular plate lamp within 1.5-3 m can be from 60 Lux to 20 Lux, while that for 60 W incandescent lamp within the same distance decreases from 30 Lux to 10 Lux. It can be seen that the oriented circular plate lamp with triangular prisms having identical cross sections and with LED of the invention can ensure preferable luminance, and in particular, the luminance at 3 m away from the circular plate lamp can even be 40 Lux. Therefore, the circular plate lamp can be used as a new lighting source so as to substitute the incandescent lamp, and have the advantages of energy conservation, high luminance, low heat dissipation, reasonable structure and easy use.
FIG. 14 and FIG. 15 shows the luminance curves of the two different kinds of 4 W circular plate lamps of the invention with triangular prisms having identical cross section within 0.3-1.5 m and 1.5-3 m, wherein the black dots and black connection lines are used to indicate the luminance of 4 W circular plate lamp made of the light-reflecting plate with the vertex angle of the triangular prism body having identical cross section being 45° (as shown in FIG. 3 ) within certain distance and the grayish black dots and connection lines are used to indicate the luminance of 4 W circular plate lamp made of the light-reflecting plate with the vertex angle of the triangular prism body having identical cross section being 90° (as shown in FIG. 4 ) within certain distance.
Under the same power, the LED-equipped circular plate lamp with triangular prism body having identical cross section with the vertex angle of the prism body being 45° is compared with that with the vertex angle of the prism body being 90° in terms of luminance. From the curves shown in FIGS. 14 and 15 , the luminance of the circular plate lamp with 45° vertex angle is larger than that with 90° vertex angle. In particular, the luminance of 4 W circular plate lamp with 45° vertex angle within 1.5-3 m almost doubles that with 90° vertex angle, the reason for which is that the marginal surfaces of the 4 W circular plate lamp having identical cross section with 45° vertex angle are just double of the marginal surfaces with 90° vertex angle. This also proves that the circular plate lamp of the invention is feasible in terms of the guiding principles for optical design.
Please refer to FIG. 16 . It can be understood that the circular plate lamp of the invention can be used as circular plate lighting fixture for all purposes by equipping with lamp socket, lamp holder, decorative lamp cover, and constant source of power driver like other bulbs or incandescent lamps. The circular plate lamp has simple structure and the oriented lighting fixture can have a 50-500 mm diameter. The embodiment for the circular plate lamp of the invention is a ceiling lamp. The centers of the heat-dissipating plate 4 , reflecting back sheet 5 and light-reflecting plate are equipped with installation holes. Before the circular plate lamp is installed to the ceiling or flat top, a hole is made in advance on the flat top, into which a flat bar with screwed hole is installed to function as the support. Subsequently, a screw is pushed through the installation hole of the circular plate lamp and connected with the screw hole and then the circular plate lamp can be installed on the ceiling. Then, connect the terminal block 29 of the circular plate lamp with the constant current source of the power driver for external power supply to light up the LED bonding dies of the circular plate lamp, i.e. the strip-type LED lighting source so that the light beams emitted as mentioned before pass through the prism bodies and generate lamp light on the smooth surface. In another embodiment, the circular plate lamp of the invention can be made as energy-saving lamps with bayonet or screw sockets. For example, FIG. 17 shows a circular plate lamp with screw socket, wherein the circular plate lamp consists of light-reflecting plate 1 , a plurality of lamp bodies 2 , heat dissipating frame 3 , heat-dissipating plate 4 ′, reflecting back sheet 5 , screw socket 7 and constant current source of power drive 8 . From FIGS. 17 a and 17 b , it can be seen that some basic components of this circular plate lamp are the same with the embodiment illustrated before, except that the heat-dissipating plate 4 ′ is different from the heat-dissipating plate 4 shown in FIG. 16 , which is a conical cover plate, wherein the conical top is arranged on a flat surface and the conical surface is equipped with radiating heat-dissipating ribs 41 ′. The screw socket 7 is installed on the flat surface of the conical top. After the heat-dissipating plate 41 ′ is covered on the light-reflecting plate 1 and the reflecting back sheet 5 , its edge can be connected with the plate edge of the heat-dissipating frame 3 via the screw (not shown in the figure) to integrate the heat-dissipating plate 4 ′ with the heat-dissipating frame 3 . Meanwhile, a conical space is formed between the heat-dissipating plate 4 ′ and the reflecting back sheet 5 , wherein the constant current source for power drive 8 can be installed via the support (not shown in the figure), the input terminal of the later is connected with the screw socket 7 and the output terminal with the terminal block 29 of the LED strip-type lamp bodies 2 (not shown in the figure). Consequently, the circular plate lighting fixture is screwed into the screw socket 7 and connected with the lamp holder of the municipal power supply and then the lamp can be lit up accordingly.
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An oriented circular light-reflecting plate with triangular micro prisms having identical cross sections and a circular plate lamp made therefrom, wherein a plurality of annular micro prism bodies ( 111 ) are arranged on the prism surface ( 11 ) of the light-reflecting plate ( 1 ), the cross sections through the central axis are triangles, which have the same shapes, the same cross sectional areas and the same distances along the diameter direction, the apex of the triangle closest to the central axial line has the shortest distance away from the smooth surface ( 12 ) of the light-reflecting plate, and the apices of the triangles towards the periphery of the light-reflecting plate have the successively increasing distances away from the smooth surface 912 ) of the light-reflecting plate. The circular plate lamp comprises the light-reflecting plate ( 1 ), a heat-dissipating frame ( 3 ), a reflecting back plate ( 5 ), a heat-dissipating plate ( 4 ) and lamp bodies ( 2 ), wherein the heat-dissipating frame ( 3 ) is sleeved around the light-reflecting plate 91 ) so as to form a gap with the cylindrical surface of the light-reflecting plate 91 ) and consequently constitute a lamp groove ( 14 ) to receive the lamp bodies ( 2 ).
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CROSS REFERENCE TO PRIOR APPLICATIONS
This application is a U.S. National Phase application under 35 U.S.C. §371 of International Application No. PCT/EP2013/068158, filed on Sep. 3, 2013 and which claims benefit to German Patent Application No. 10 2012 110 763.7, filed on Nov. 9, 2012. The International Application was published in German on May 15, 2014 as WO 2014/072094 A1 under PCT Article 21(2).
FIELD
The present invention relates to a flap device for an internal combustion engine or an electric vehicle, comprising a flap body, a duct housing in which the flap body is arranged in a rotatable manner, an actuator, and a stub shaft which projects from the actuator through the duct housing to the flap body and is supported in the duct housing via a first bearing.
BACKGROUND
Flap devices of the above type are known in particular as throttle flaps for controlling the air supply to the internal combustion engine. In the process, the flap will be rotated in the duct housing, whereby the available flow cross section will be changed. Other applications for control of a gas flow, particularly of an air or exhaust gas flow, are also, however, known.
Various types of supports and designs of these flaps have been disclosed. In most cases, such flaps, which can be produced from plastic or metal, comprise a throughgoing shaft which is supported on both sides of the flap body in the duct housing. Primarily rolling bearings and, in this case, ball bearings are used for support. While the first shaft end is mostly supported in a blind hole of the duct housing, the opposite end passes through the duct housing. On this shaft end, a toothed wheel of a transmission is normally supported via which a connection to an electric motor is established, the electric motor serving as an actuator to drive the flap body and being connected to the control unit of the internal combustion engine.
Such a throttle body is described, for example, in DE 10 2007 013 937 A1. The rotary shaft, connected to the electric motor via the transmission, is supported in the duct housing by means of two needle bearings which include sealing rings.
DE 44 23 370 A1 describes a throttle flap made of plastic which comprises two opposite receiving openings for two shaft ends which are held in the openings in a form-locking manner. The flap body comprises rotary-bearing sites which are surrounded by a soft plastic sealing. DE 44 23 370 A1 does not disclose how the bearing support in the stub is actually realized.
The known designs have the disadvantage that the assembly process is relatively bothersome and that a high dimensional accuracy or additional measures are required in order the provide an exact position of the flap body when mounting the flap body in the duct in the direction of the axis of rotation. These designs are further vulnerable towards corrosive condensates.
SUMMARY
An aspect of the present invention is to provide a flap device which can be produced and assembled at a favorable cost and which can be precisely located in the duct in a convenient manner without requiring additional measures. An additional aspect of the present invention is that the bearings should be protected from corrosive condensates in the best possible manner.
In an embodiment, the present invention provides a flap device for an internal combustion engine or an electric vehicle which includes a flap body comprising a receiving opening, a duct housing configured to rotate arranged in the flap body, an actuator, a first bearing, a stub shaft arranged to project from the actuator through the duct housing to the flap body, a slide bearing arranged in the receiving opening of the flap body, and an axial pin arranged so as to be fixed in the duct housing on a side of the flap body opposite to the stub shaft. The stub shaft is supported in the duct housing via the first bearing. The axial pin is configured to support the flap body via the slide bearing and to project into the receiving opening.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is described in greater detail below on the basis of embodiments and of the drawings in which:
FIG. 1 shows a three-dimensional representation of a flap device according to the present invention depicting the duct housing in a sectional view at the level of the axis of rotation, and depicting the flap body in a lateral view; and
FIG. 2 shows a plan view onto the flap device in a fully sectional representation.
DETAILED DESCRIPTION
Because an axial pin is fixedly arranged in the duct housing on the side of the flap body opposite the stub shaft, on which pin the flap body is supported via a slide bearing arranged in a receiving opening of the flap body, with the axial pin extending into the receiving opening, there is achieved a particularly simple assembly process because the axial pin and the stub shaft can be inserted into the duct housing from axially opposite sides. The entire arrangement can thus be assembled from the outside in a simple manner. In addition thereto, ingress of condensate in the area of the slide bearing in case of inclined mounting positions is reliably prevented. With this design, the slide bearing cannot only be pressed in at a later time, as has already been common practice, but can also be produced by surrounding injection or be directly formed from the plastic used.
It is advantageous if the axial pin is pressed in internally of the duct housing so that no further sealings need to be provided on the side of the axial pin to provide a sealing tightness toward the outside. By being fastened in the duct housing, the axial pin is not subjected to any alternating bending.
In an embodiment of the present invention, the first bearing can, for example, be a rolling bearing with its axial end extending into the duct and being in abutment on an abutment face of the flap body, said abutment face delimiting a receiving ring having the stub shaft extending through it. During assembly of the stub shaft and the axial pin with the flap, it can thus be avoided that the flap might drop down before insertion of the stub shaft. A high sealing tightness toward the outside is at the same time also provided on the side of the stub shaft. The axial play of the flap in the duct can be adapted through the insertion of the rolling bearing by shifting the rolling bearing to a position which is spaced from the disk, while various disk thicknesses can be used.
It can be advantageous if the rolling bearing is a needle bearing since such a bearing has a particularly high load-bearing capacity and thus has a long operating life at high stress.
In an embodiment of the present invention, a disk can, for example, be arranged between the flap body and the duct housing, the disk radially surrounding the axial pin and being in axial abutment against an abutment face surrounding the receiving opening and against the duct housing. This disk thereby creates a planar abutment face toward the flap body in spite of the cylindrical shape of the duct housing. The flap body can be pressed against this disk by a shift-in of the rolling bearing during the assembly process. The disk serves as a washer disk in the axial direction. The arrangement of the disk around the pin of the bearing arranged in the flap will also lead to a reduction of leakage in the closed position of the flap.
In an embodiment of the present invention, a first axial section of the disk can, for example, be arranged in a recess of the duct housing, and a second axial section can, for example, extend into the duct. This provides the positioning of the disk in the duct and the functioning of the disk as a planar abutment face.
For further simplification of the assembly process and for further enhancement of the sealing tightness of the flap, a respective annular projection extends from the abutment faces to the duct housing. Prior to insertion of the axis and of the stub shaft, the flap body can thus be supported on the disk and the rolling bearing via these projections.
In correspondence thereto, the first annular projection surrounds the section of the rolling bearing extending into the duct, and the second annular projection surrounds the section of the disk extending into the duct. This will also effect an increased resistance against ingress of corrosive liquid into the region of the bearing.
In an embodiment of the present invention, the stub shaft can, for example, comprise a step which is arranged in the receiving ring of the flap body, wherein the section having a smaller diameter faces toward the flap body, thus reliably preventing damage of the seals when passing the stub shaft through the housing.
In an embodiment of the present invention, the flap body can, for example, be made of plastic and can comprise a metal plate having the plastic molded partially around it, and the stub shaft can comprise an axial slot having the metal plate of the flap body extending into it. This makes it possible to obtain a durable fastening of the flap body on the stub shaft. The contour of the flap follows the contour of the shaft in order to prevent leakage within the range of the differences of diameter.
In an embodiment of the present invention, the metal plate can, for example, be formed with a hole in which, for fastening the flap body to the first stub shaft, a screw is attached which extends through the first stub shaft into the hole of the metal plate and engages a thread in the stub shaft beyond the slot.
A further simplification of the assembly process is achieved if, at the end of the stub shaft facing toward the actuator, a tooth segment is attached by molding, which tooth segment is then connected to the further transmission and thus to the actuator.
In an embodiment of the present invention, the slide bearing can, for example, be formed in the flap body geodetically below the rolling bearing, thus excluding ingress of generated condensate into the slide bearing.
It is advantageous if the needle bearing comprises integrated sealing rings. This prevents the ingress of liquid without requiring additional assembly steps.
A flap device is thereby created which allows for a particularly simple assembly process. Possible batch variations during production of the flap body can be compensated by simple means. An exact positioning of the flap body in the duct housing is thus obtained, which leads to a relatively good sealing tightness in the closed state, and to a reduced number of rejected products in the assembly process. The flap device can further be produced at favorable costs and is not sensitive to occurring corrosive liquids.
An embodiment of the flap device of the present invention is illustrated in the drawings and will be described hereunder.
The flap device of the present invention comprises a flap body 12 which is arranged to rotate in a duct housing 10 , wherein the radial dimension of the flap body 12 substantially corresponds to the free diameter of a duct 14 formed in the duct housing 10 . Flap body 12 is fastened in a slot 16 of a stub shaft 18 which on its opposite end has a tooth segment (not shown) molded to it, the tooth segment being connected to a continuing transmission arranged in a transmission housing 20 , while the transmission together with an electric motor forms an actuator 22 driving the flap body 12 .
Duct housing 10 comprises a first bore 24 through which the stub shaft 18 extends from transmission housing 20 into the duct 14 . Arranged in the first bore 24 is a rolling bearing designed as a needle bearing 26 , with sealing rings 28 integrated into it on both sides.
The needle bearing 26 extends by its axial end 30 into duct 14 where it is in axial abutment against an abutment face 32 axially delimiting the flap body 12 . The abutment face 32 forms the axial delimitation of flap body 12 . This axial end 30 of needle bearing 26 is radially surrounded by a first annular projection 36 extending from abutment face 32 of flap body 12 in the direction of duct housing 10 .
In a receiving ring 34 , the stub shaft 18 is arranged which in this region comprises a step 38 so that a slotted section 40 , comprising the slot 16 , of stub shaft 18 facing into the interior of duct 14 has a smaller diameter than the section 42 of stub shaft 18 arranged in first bore 24 .
The thinner slotted section 40 is formed with a hole 44 in which a head 46 of a screw 48 is arranged, the screw 48 clamping a metal plate 52 via the shaft slot and an opposite thread. The metal plate 52 is a part of flap body 12 and, prior to molding, will be inserted in the tool for forming the flap body 12 and then will be enclosed by molding material. The slotted section 40 of stub shaft 18 is arranged in abutment against this metal plate 52 on both sides and thus establishes the fixed connection between flap body 12 and stub shaft 18 .
On the side axially opposite to the receiving ring 34 , the flap body 12 comprises a receiving opening 54 in which a slide bearing 56 is arranged. This slide bearing 56 can either be inserted into the tool prior to the molding of flap body 12 or can be formed by the material itself, or be molded in at a later time. The slide bearing 56 radially surrounds an axial pin 58 whose opposite end is fastened in a second bore 59 , arranged opposite to the first bore 24 , within the duct housing 10 .
A disk 60 is arranged between duct housing 10 and slide bearing 56 , as viewed in the direction of the axis of rotation, whose first axial section 62 is located in a correspondingly shaped recess 64 in the wall of duct housing 10 and whose second axial section 66 extends into duct 14 and is in axial abutment against an abutment face 68 which radially delimits the receiving opening 54 . This second axial section 66 is radially surrounded by a second annular projection 70 extending from the abutment face 68 in the direction of duct housing 10 .
The special advantages of this flap device become clear in the assembly process, particularly if the part of the flap body 12 with the slide bearing 56 is arranged geodetically below the part supported via the needle bearing 26 . After producing the duct housing 10 with the bores 24 , 59 and the molding of the flap body 12 with the metal plate 52 , the slide bearing 56 is first pressed into the receiving opening 54 unless it was already produced along with the molding process for the flap body 12 .
The disk 60 will subsequently be placed in the recess 64 of duct housing 10 , which, due to the geodetic position, is particularly simple. The flap body 12 will be placed in the duct 14 in so that the second annular projection 70 will surround the disk 60 and the abutment surface 68 will be in abutment on disk 60 . The needle bearing 26 will be pressed in at a distance from disk 60 . This distance corresponds to the flap thickness and the temperature-dependent minimum play. The axial pin 58 will then be inserted through the second bore 59 into the receiving opening 54 and through the slide bearing 56 , wherein, by press fit of axial pin 58 within second bore 59 , a sealing effect toward the outside can be generated. From the opposite side, the stub shaft 18 will be shifted through the first bore 24 , and respectively the needle bearing 26 , as well as through the receiving ring 34 , notably so that the metal plate 52 will come to rest in the slot 16 of stub shaft 18 .
The flap body 12 with metal plate 52 as well as the stub shaft 18 can be rotated for this purpose. The flap body 12 will subsequently be screwed by the screw 48 through the hole 44 of the stub shaft 18 and thereby be clamped with the aid of the shaft slot.
By use of favorably priced component parts, there is thus created a flap device which can be assembled with low expenditure. The position of the flap can be optimized in the duct so that batch variations can be compensated for. Particularly in case of an inclined installation position, no condensate will intrude into the slide bearing so that the operating life of the bearings is distinctly increased because, under the effect of gravity, the condensate will run out of both slide bearings.
It should be evident that the scope of protection of the main claim is not delimited to the above described exemplary embodiment but that various constructional modifications can be envisioned; reference should also be had to the appended claims. Connections may in particular be realized in a detachable or non-detachable manner. The design of the individual component parts can of course be adapted to the respective purpose.
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A flap device for an internal combustion engine or an electric vehicle includes a flap body comprising a receiving opening, a duct housing configured to rotate arranged in the flap body, an actuator, a first bearing, a stub shaft arranged to project from the actuator through the duct housing to the flap body, a slide bearing arranged in the receiving opening of the flap body, and an axial pin arranged so as to be fixed in the duct housing on a side of the flap body opposite to the stub shaft. The stub shaft is supported in the duct housing via the first bearing. The axial pin supports the flap body via the slide bearing and projects into the receiving opening.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
Many construction projects result in sloped areas without ground covering such as plants. Agricultural fields also may include sloping areas. These sloped generally bare areas will erode drastically with time and weather unless they are equipped with conservation tools. Various implements have been devised by which a fabric-like fence can be partially inserted in a soil furrow and secures by posts and the like. The fence acts to reduce the erosion of the soil from above the fence and stop it there. Several fences may be required in a single sloped area.
2. Background of the Invention
U.S. Pat. No. 3,182,459 to Grether provides an installer mounted on the side of a tractor and which automatically adds the posts. This installer includes a fabric chute employing at least one rod as a pivotal directions changer for the fabric.
U.S. Pat. No. 5,915,878 to Carpenter provides an installer wherein the fabric is positioned transverse to the direction of travel and is inserted partially in a furrow by a wheel.
U.S. Pat. Nos. D502,470, D504,134, 7,044,689 to McCormick provide a pull-behind installer having a longitudinal frame, a plow element and a fabric chute. The fabric chute is designed to require the fabric to successfully make two turns with the fabric, the second while exiting the leading edge of the chute and turning so the fabric is deposited in the furrow made by the plow element. This design requires the leading edge to be perpendicular to the longitudinal frame and includes a rod at a 45 degree angle from the leading edge around which the fabric makes the first turn so the fabric direction is turned forward, then out the leading edge and a 180 degree second turn to reverse its direction. For threading the fabric, the chute is made of separate plates hinged together on one side so the chute can be opened and closed easily. The direction and position of entry and exit of the fabric are such that the 45 degree angle must be at the trailing edge in order to allow the chute to be opened and threaded and cleaned and the leading edge must be about perpendicular with the ground to provide appropriate alignment of the fabric into the furrow. This arrangement requires a deflector for the front exit slot of the chute to keep dirt out of the chute which may otherwise impede the flow of the fabric. In short, two direction changing rods and two plates hingedly connected on one side are necessary for this installer to function properly. One version of this plow allows the frame to pivot relative to the mounting bracket; another allows a tongue and plow to pivot on the frame steadied by springs.
In addition to dirt lodging in the chute and the necessity of complex structures to allow ease of fabric threading, earlier silt fence installers are plagued with other common problems. Among these problems are a deficit for sharp turns and a lack of versatility for lateral adjustment relative to the mount on the towing vehicle. In addition, the arm upon which the fabric roll rotates is vertically fixed and the deflector adds drag as the installer is moved through the soil. It is therefore one object of the present invention to avoid problems related to dirt in the fabric chute. A second object is to simplify the chute structure and yet increase the ease of threading. A third objective is to structure an installer that is both stronger yet more agile and responsive. A fourth objective is to decrease the drag from that resulting from the use of the regular sized installer and that caused by employing a deflector. The final objective is to provide an installer with a hitch mechanism to allow lateral adjustment.
SUMMARY OF THE INVENTION
The present invention resolves many of the issues present in prior art silt fence installers. First, it provides a simpler fabric chute constructed with fewer pieces which does not require a hinged opening, requires a single change in direction of the fabric, and negates the need for a deflector. This construction also decreases the incidence of fabric tears and tension. Second, the present invention is laterally adjustable relative to the vehicle towing it. Third, this installer follows the turns of the towing vehicle and meets the need for tighter curves while increasing the structural strength of the installer. Fourth, the present invention provides a vertically adjustable fabric roll holder to accommodate varying dimensions of fabric rolls. Fifth, the preferred embodiment is smaller than a typical installer yet it can be used to install fabric 48 inches wide or less.
The installer of the present invention relies on a frame assembly having a main angular frame support affixed to at least one vertically oriented frame member. The vertically oriented frame member has a hitching side for associating with a hitch assembly and a mounting side associated with the angular support. Preferably, the vertically oriented frame member is pivotally associated on its hitching side with a sliding offset assembly which is, in turn, mounted on a sliding offset hitch. Due to the use of rollers in the sliding hitch, no hydraulic power is necessary to adjust the position of the installer on the hitch relative to the vehicle. The hitching side may alternatively be associated with a three point assembly or forklift assembly.
The upper portion of the angular support is associated with the vertically oriented frame member while the lower portion is associated on its leading side with a blade assembly and on its trailing side with a fabric chute assembly. A coulter assembly is attached to a bottom side of the vertically oriented frame member through an association provided by a coulter bracket assembly.
The fabric chute assembly comprises a first and a second vertical plate-like sidewall each joined to the other at the bottom but maintaining a small space therebetween. The first and second sidewalls are affixed to the trailing edge of the blade assembly. The top edges of the first and second sidewalls remain separate forming an entry slot as do the trailing edge of the first and second plates forming an exit slot. The sidewalls may be formed integrally with one another or may be affixed to one another through means known in the art such as welds. In either arrangement, there is no gap between the sidewalls on their leading edges. The leading edge of the chute assembly is generally parallel to the angle of the angular support and associated with the support's lower portion. The trailing edge of the chute assembly is generally vertical. A rod, parallel to the angle of the angular support is positioned near the leading edge of the chute assembly between the first and second plates for a purpose to be described later.
Protruding from the vertically oriented frame member is a roll stand assembly which has a vertical support to which is attached a horizontal fabric roll support. The fabric roll support is oriented along the axis of travel and generally above the fabric chute assembly. A roll of fabric is rotatably associated with the support. The vertical height of the horizontal fabric roll support is adjustable.
To thread the fabric, it is unrolled to extend into the entry slot between the first and second sidewall at their top edges, threaded under the rod near the chute assembly's leading edge which acts to convert the vertical orientation of the fabric's travel to horizontal, and then out the exit slot formed by the trailing edges of sidewalls.
The chute assembly construction relative to the direction of travel negates the need for a deflector because the leading edge of the chute is closed rather than open. Further, because only a single rod is used, the fabric is easily threaded without separating the plates so the first and second sidewalls can be integrally formed or, at the least, require no hinged or pivotal relationships to each other. This greatly simplifies the chute's construction. In addition, this arrangement simplifies threading the fabric and reduces tension on the fabric resulting in fewer tears than other installers.
The angular support coupled with the generally vertically oriented frame member increases the strength of the frame against horizontal moment, further simplifies the overall frame structure and dramatically shortens the installer from leading to trailing edge. Shortening the installer results in making its turns more closely reflective of those of the towing vehicle to which it is attached. In the preferred embodiment, the frame assembly is more clearly described wherein the vertically oriented frame member comprises two parallel planar elements joined at their bottom edges by a horizontal bar and between which is sandwiched the angular support. In this arrangement, the coulter bracket and assembly are affixed to the bottom side of the bar.
The frame assembly is pivotally associated with the hitch assembly on the hitching side of the generally vertically oriented frame member further allowing more responsive turns of the plow. The installer is biased toward a center alignment relative to the hitch by a lateral spring on either side of the means for associating said frame and said hitch.
In operation, the hitch assembly may be associated with a skid steer adaptor and skid loader, a three-point hitch and towing vehicle, a sliding offset hitch and towing vehicle, or other means to associate the installer with a mobile power unit. Preferably, the installer is associated with a sliding offset hitch.
The sliding offset hitch assembly includes an offset frame having an upper lateral support with a rearward side, a bottom side and a forward extending portion to which the top in of a three point hitch can be attached.
The upper lateral support is spaced vertically from two lower lateral supports each having a front side and a rearward side, all positioned between two vertical end plates. A forward plate extends at least partially along the length of each of the lower lateral supports and covers the gap between the two lower lateral supports. The forward plate is associated with a pair of brackets, laterally spaced apart, having openings through which the two bottom pins of a three point hitch will extend.
A sliding offset bracket assembly is associated on one side with the hitch assembly of the installer and on its opposing side with the offset frame. The opposing side of the sliding offset bracket assembly includes a forward extending portion. This forward extending portion is inserted between the first and second lower lateral supports. The forward extending portion is equipped with rollers to turn vertically against the bottom side of the first lower lateral support and the top side of the second lower lateral support and rollers to turn horizontally against the back side of the first lateral support. The positioning of the rollers allows the sliding offset bracket assembly to be slidably associated with the sliding offset hitch assembly such that an operator can adjust the lateral position of the installer by hand and without the need for hydraulic or other powered assistance.
In the preferred embodiment an adjustment bar is proximal the bottom side of the upper lateral support. The adjustment bar includes laterally spaced apart openings. A pin inserted in an opening on the bracket through the bracket and into one of the laterally spaced apart openings secures the offset bracket assembly in position relative to the sliding offset hitch assembly.
Other objects, features, and advantages of the present invention will be readily appreciated from the following description. The description makes reference to the accompanying drawings, which are provided for illustration of the preferred embodiment. However, such embodiment does not represent the full scope of the invention. The subject matter which the inventor does regard as his invention is particularly pointed out and distinctly claimed in the claims at the conclusion of this specification.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective of the installer of the present invention attached to a power and transport source.
FIG. 2 is a side view of the installer of the present invention associated with a sliding offset hitch;
FIG. 2 a perspective of the installer of FIG. 2 ;
FIG. 3 is a front end view of the installer of the present invention associated with a sliding offset hitch;
FIG. 4 is a back end view of the installer of FIG. 3 ;
FIG. 5 is an exploded view of the angular support and chute assembly of the present invention;
FIG. 6 is a close-up perspective of the coulter assembly and coulter bracket;
FIG. 7 is a perspective view of the front of the sliding offset hitch assembly;
FIG. 8 is a perspective view from the back of the sliding offset hitch assembly;
FIG. 9 is an exploded back view of the sliding offset bracket assembly;
FIG. 10 is an exploded front view of the sliding offset bracket assembly; and
FIG. 11 is an exploded, enlarged view of the at least one vertically oriented frame member of the frame assembly of the preferred embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1 , a perspective of the installer 10 of the present invention having a leading edge 11 and a trailing edge 13 is shown hitched to a towing vehicle 12 . Shown in more detail in FIGS. 2-5 , the installer 10 of the present invention relies on a frame assembly 14 having a main angular frame support 16 comprising an upper portion 18 and a lower portion 20 said support 16 is affixed to at least one vertically oriented frame member 22 comprising a hitching side 24 equipped with means for associating a hitch assembly 26 and a mounting side 28 . The vertically oriented frame member 22 is pivotally associated by said means for associating a hitch assembly 26 with a sliding offset bracket assembly 30 which is, in turn, slidably mounted on a sliding offset hitch 32 . Due to the use of rollers 34 and 35 (See FIG. 7 ) in the sliding offset bracket assembly 30 , no hydraulic power is necessary to adjust the position of the installer 10 on the hitch 32 relative to the vehicle 12 . In another embodiment, the at least one vertically oriented frame member 22 is pivotally associated by said means for associating a hitch assembly 26 with a 3-point assembly.
The upper portion 18 of the angular frame support 16 is associated with the at least one vertically oriented frame member 22 while the lower portion 20 further comprises a leading side 40 and a trailing side 42 and is associated on the leading side 40 with a blade assembly 44 having a blade 46 and a tooth 48 and on its trailing side 42 associated with a fabric chute assembly 50 . A coulter assembly 52 is attached to a bottom, generally horizontal side 54 of the at least one vertically oriented frame member 22 through an association provided by a coulter bracket assembly 55 .
The fabric chute assembly 50 comprises a first vertical sidewall 60 having a first top edge 62 , a first bottom edge 64 , and a first trailing edge 65 , and a second vertical sidewall 66 having a second top edge 68 , a second bottom edge 70 and a second trailing edge 72 with a small space 74 between said first sidewall 60 and the second sidewall 66 . In one embodiment, the first and second sidewall 60 , 66 respectively, are joined together by a flange 76 at the bottom edge 64 , 70 respectively, of each sidewall 60 , 66 respectively, and to the trailing edge 42 of the blade assembly 44 . The top edges 62 , 68 respectively of the first 60 and second 66 sidewall remain separate forming an entry slot 80 as do the trailing edge 65 , 70 respectively of the first 60 and second 66 sidewall forming an exit slot 82 . In another embodiment, the sidewalls 60 , 66 and flange 76 may be integral to one another such that the structure is of a single piece or may be affixed to one another through means known in the art such as welds.
A leading edge 84 of the chute assembly 50 is positioned generally parallel to the angle of the angular support 16 and associated with the support's 16 lower portion 20 . The chute assembly 50 further comprises a trailing edge 86 which is generally vertical. A rod 88 , parallel to the angle of the leading edge 84 and the angular support 16 is positioned near the leading edge 84 of the chute assembly 50 between the first 60 and second 66 sidewalls for a purpose to be described later.
Protruding from the at least one vertically oriented frame member 22 is a roll stand assembly 90 comprising a vertical support 92 to which is attached a horizontal fabric roll support 94 . The fabric roll support 94 is oriented along the axis of travel and generally above the fabric chute assembly 50 . A roll of fabric 96 is rotatably associated with the support 94 and fabric 96 is unrolled to extend into the entry slot 80 between the first 60 and second 66 sidewall sides, threaded under the rod 88 which acts to convert the vertical orientation of the fabric's travel to horizontal, and then out the exit slot 82 on the trailing edge 86 .
The chute assembly 50 construction relative to the direction of travel negates the need for a deflector because the leading edge 84 of the chute is closed rather than open. Further, because the fabric 96 is easily threaded without separating the sidewalls 60 , 66 , the first 60 and second 66 sidewalls can be integrally formed or, at the least, require no hinged or pivotal relationships to each other since there is no need to open the sidewalls. The angular support 16 coupled with the generally vertically oriented frame member 22 increases the strength of the frame assembly 14 against horizontal moment, simplifies the construction and dramatically shortens the installer 10 from leading 11 to trailing edge 13 making its turns more closely reflective of those of the towing vehicle 12 to which it is attached. In the preferred embodiment, the frame assembly 14 is more clearly described wherein the at least one generally vertically oriented frame member 22 comprises a first parallel planar elements 100 and a second parallel planar element 102 joined by a horizontal bar 104 . Between the first planar element 100 and the second planar element 102 is sandwiched the angular support 16 . The coulter bracket 52 and coulter assembly 54 are affixed to a bottom side 105 of the bar 104 .
The frame assembly 14 is pivotally associated with the hitch 32 further allowing more responsive turns of the plow. The installer 10 is biased toward a center alignment with said means for associating said assembly 26 by a lateral spring 110 on either side of the means for associating said hitch assembly 26 .
The installer 10 may be removably attached through its means for associating said hitch assembly to a three-point hitch 140 , a skid loader, a sliding offset hitch, or other means allowing the installer to be towed by a power unit. In one preferred embodiment, the sliding offset hitch 32 comprising the sliding offset bracket assembly 30 and an offset frame 150 is associated with said means for associating a hitch assembly 26 on said installer 10 .
The offset frame 150 comprises an upper lateral support 152 with a rearward side 154 , a bottom side 156 , and a forward extending portion 158 to which the top pin 4 - 60 of a three point hitch can be attached.
The upper lateral support 152 is spaced vertically from a first lower lateral support 162 having a first front side 163 and a rearward side 164 and a second lower lateral support 165 having a second front side 166 and a second rearward side 167 . Said first lower 162 and said second lower lateral support 165 are positioned between two vertical end plates 161 , 161 a respectively. A forward plate-like element 168 extends along said first front side 163 and said second front side 166 to at least partially cover a gap 170 between said first lower lateral support 162 and said second lower lateral support 165 . Preferably, the forward plate-like element 168 comprises a pair of brackets 170 , 171 , respectively. These brackets 170 , 171 include elements whereby the bottom two pins 172 , 174 of a three point hitch 140 are associated.
The sliding offset bracket assembly 30 is associated with said means for associating a hitch assembly 26 of the installer 10 and with the offset frame 150 . Said first lower lateral support 162 further comprises an under side 175 ; said second lower lateral support 165 further comprises a top side 176 .
The offset bracket assembly 30 comprises a forward extending portion 180 . The forward extending portion 180 is inserted in the gap 170 and is equipped with at least one roller 34 having a vertical axis and at least one roller 35 having a horizontal axis. Said at least one roller 34 with vertical axes are positioned to roll along said rearward side 164 of said first lower lateral support 162 and said at least one roller 35 having horizontal axes are positioned to roll along between said under side 175 and said top side 176 . At least one roller 177 having a vertical axis is attached to a roller bracket 179 . Said roller bracket 179 is positioned on the opposite side of gap 170 from the forward extending portion 180 and attached thereto such that said at least one roller 177 rolls against the front side 163 of said first lower lateral support 162 further facilitating the sliding of the bracket assembly 30 while keeping its position generally constant in the leading to trailing direction relative to said frame 150 . The forward plate-like element 168 is positioned to act as a dirt guard for the roller bracket 179 and rollers 177 .
The lateral position of the sliding offset bracket assembly 30 may be adjusted by hand. A plurality of openings 180 are spaced apart laterally proximal said rearward side 154 of said upper lateral support 152 . An opening 182 in said bracket assembly 30 is aligned with one of said plurality of openings 180 , a pin 184 is then inserted through said opening 182 and opening 180 to secure the position of the sliding offset bracket assembly on said offset frame. Adjustment of lateral position is simple; the pin is removed, the rollers allow sliding of the installer by hand, the openings 182 and 180 are aligned and the pin is re-inserted.
Thus, the present invention has been described in an illustrative manner. It is to be understood that the terminology that has been used is intended to be in the nature of words of description rather than of limitation.
Many modifications and variations of the present invention are possible in light of the above teachings. For example, a single roller with a horizontal axis may be used although the lateral adjustment of the installer may not be as simple. A single roller may best be used with a track in one or the other lower lateral supports to keep the roller positioned. As another example, the sidewalls of the chute may be integral with one another or they may each be separately attached to the angular support thereby closing any gap that would otherwise occur at their leading edges. The forward plate-like element that covers the gap between the first and second lower lateral supports and protects the roller bracket could be left off completely without significantly changing the invention. However, its presence maximizes protection of the rollers and minimizes what would otherwise be required maintenance. Further, it should be understood that the generally right angle formed with the ground by the trailing edge of the chute assembly is not critical to the operation of the installer; other angles may be used. In addition, although not required, a wind guard may be attached above the chute assembly and below the roller to assist in minimizing any ill effect a strong wind may have on the threading of the fabric and operation of the installer. Therefore, within the scope of the appended claims, the present invention may be practiced otherwise than as specifically described.
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The present invention is a silt fence installer of unique design wherein the frame is angular rather than longitudinal and the fabric chute assembly is oriented parallel with the angular frame. This arrangement results in an installer with a generally perpendicular trailing edge, a fabric chute assembly with a closed leading edge and no need for hinged relationship between the sidewalls, and simple fabric threading with a single directional turn of the fabric. Further, the angular frame results in a shorter installer able to be more responsive to turns. In addition, the invention includes a sliding offset hitch wherein a silt fence installer may be adjusted laterally by hand due to strategic placement of rollers.
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RELATED APPLICATIONS
[0001] The present application is a continuation-in-part of co-pending U.S. patent application Ser. No. 10/406,034, which was filed on Apr. 2, 2003, and which is incorporated by reference herein for all that it contains.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The embodiments of the invention disclosed herein relate to casino gaming, and more particularly, to playing card games and methods of play for a blackjack-type card game.
[0004] 2. Description of the Related Art
[0005] There is a constant demand and need for new or improved games of chance to attract gamblers to gaming establishments.
[0006] A technique that can be used to increase the attraction of blackjack (21) is to allow the player to make a bet in addition to the conventional blackjack bet, whereby the player will win or lose the additional bet after the player's first two cards fall in the predetermined category of “Good Hand” or “Bad Hand.”
[0007] What is needed is a gaming system and method whereby the “Good Hand” is only made up of number totals that most players would consider a “Good Hand.” Conversely, the “Bad Hand” would be made up of only numbers that most players would consider a “Bad Hand.” The listing of “Good Hands” and “Bad Hands” will offer the player every combination of number totals that can result within the first two cards dealt to the player in the conventional game of blackjack.
[0008] If the player bets on the “Good Hand,” the gaming system and method will require that the “Good Hand” is dealt statistically fewer times than the “Bad Hand” in order than an appropriate hold (return) is received by the casino; however, the hold, representing the statistical advantage of the casino over the player, cannot be greater than the maximum percentage allowed by regulators and should not be so large that the player would be discouraged from playing the bet If the player bets on the “Bad Hand” and the first two cards dealt to the relevant player total thirteen (including an Ace and a two—soft thirteen), neither the player nor the casino would win the relevant bet in order to guarantee that an appropriate hold is received by the casino on every bet.
[0009] There is no prior art for such a system.
SUMMARY OF THE INVENTION
[0010] Previous side bets to the game of blackjack or pseudo blackjack games have been limited to exotic payoffs for certain card combinations, large payoffs for consecutive blackjack hands won, the offering of multiple blackjack games played simultaneously and games that trade off more liberal rules for the player, i.e. doubling or surrendering at will, while lowering blackjack payoffs to even money.
[0011] What long has been overdue, is an additional blackjack bet that will win or lose approximately at the same ratio as a blackjack conventional bet. The frequency of the additional bet's payoff, as well as the casino's hold approximating a conventional bet hold, will increase blackjack volume significantly.
[0012] Previous side bets have resulted in nominal increases in total blackjack volume, largely because of the exotic nature and infrequency of side bet payoffs as well as nominal maximum bet totals, because of the large payoff odds established by the casinos due to the infrequency of payoffs.
[0013] The player for the first time may make two bets rather than one bet on the potential of winning and losing hands. The quality of only the player's first two cards will determine the result of the additional bet while both the quality of the dealer's and player's hand will determine the result of the conventional bet.
[0014] In a further aspect of the present invention A method of playing blackjack comprising the steps of: providing a conventional bet receiving region and an additional bet chip receiving region for a “Good Hand—Bad Hand” bet; each player making a conventional bet of a denomination within the denomination range permitted by the rules of the game; and/or each player making a “Good Hand—Bad Hand” bet by placing the bet in said additional bet chip receiving region, the bet being of a denomination permitted by the rules of the game; dealing each player and a dealer two cards each; determining whether the two cards dealt each player represent a winning hand or losing hand according to a posted “Good Hand—Bad Hand” list; and the dealer pays each player having a winning bet an amount equal to the “Good Hand—Bad Hand” bet located in the additional bet chip receiving region for a “Good Hand—Bad Hand” bet, wherein said “Good Hand” playing card values comprise: Blackjack, Two Aces, Twenty, Nineteen, Eighteen, Soft Eighteen, Seventeen, Soft Seventeen, Eleven, Ten, and nine; and wherein said “Bad Hand” playing card values comprise: Sixteen, Fifteen, Fourteen, Twelve, Eight, Seven, Six, Five, Four, and Three.
[0015] In as still further aspect of the present invention a method of playing a blackjack game between at least one player and a dealer using at least one standard deck of playing cards, comprising the steps of: providing each player with a posted list describing an additional bet of either a “Good Hand” bet or a “Bad Hand” bet; providing each player a conventional blackjack bet-receiving region and an additional bet-receiving region; each player placing a first wager, said first wager of each player identified as either a conventional blackjack bet or as said additional bet; each player optionally placing a second wager, differing in identity from said first wager and identified as either said conventional blackjack bet or as said additional bet; dealing each player placing at least said first wager an initial hand of two playing cards and dealing an initial hand of two playing cards to the dealer; evaluating the initial hand of each player placing said additional bet and comparing a playing card point value for said initial hand to said posted list describing a plurality of “Good Hand” bet playing card point values and a plurality of “Bad Hand” bet playing card point values; awarding each player obtaining a winning outcome; continuing play of game for each player placing said conventional blackjack bet under rules of play for conventional blackjack, wherein said plurality of “Good Hand” playing card point values comprise playing card point values of 21, 20, 19, 18, soft eighteen (Ace and seven), soft sixteen (Ace and six), 11, 10, 9, and 2 (two Aces), and wherein said plurality of “Bad Hand” playing card point values comprise playing card point values of 16, 15, 14, 12 (not two Aces), 8 (not using an Ace), 6, 5, 4 or 3.
[0016] It is to be understood that the invention is not limited in its application to the details, manner, and order of play described hereinafter and illustrated in the drawing figures. Those skilled in the art will recognize that various modifications can be made without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The foregoing aspects and other aspects of this disclosure are described in detail below in connection with the accompanying drawing figures in which:
[0018] FIG. 1 is a plan view of a table layout for use in playing live casino versions of a blackjack game in accordance with a preferred embodiment of the present invention;
[0019] FIG. 2 is a partial, enlarged plan view showing a player position in accordance with a preferred embodiment of the present invention;
[0020] FIG. 3 is a first partial flowchart of the play of the game;
[0021] FIG. 4 is a second partial flowchart of the play of the game, continuing game play as initiated in the flowchart of FIG. 3 ; and
[0022] FIG. 5 is a third partial flowchart of the play of the game, completing game play as continued in the flowchart of FIG. 4 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0023] Reference is now made to the drawings wherein like numerals refer to like parts throughout. In FIG. 1 , a playing surface 10 is provided with a plurality of inscribed geometric shapes to assist in the play of a card game described hereinafter.
[0024] A plurality of player positions 16 and a dealer position 18 are spaced opposite one-another on the playing surface 10 . Each of the player positions 16 is provided with a conventional wagering area 22 for placement of wagers relating to the play of conventional Blackjack, and a second wagering area 24 that defines two separate wagers: a “Good Hand” wagering area 26 and a “Bad Hand” wagering area 28 . As will be discussed in greater detail hereinafter, a player may place a wager in only one of the two wagering areas, and by so doing, elects to wager either on a “Good Hand” outcome or a “Bad Hand” outcome.
[0025] A preferred embodiment of the present invention contemplates the use of multiple decks of playing cards placed in a playing card shoe 32 that is used to deal each of the player's hands as well as the dealer's hand. A chip rack 34 is located adjacent the dealer position 18 and holds playing chips of typical gambling denominations. Also preferably inscribed are a plurality of pay tables that include identification of certain playing card point totals, one column identifying “Good Hand” point totals and the other point totals considered as “Bad Hand” totals (also see FIG. 2 ).
[0026] As mentioned above, it is presently contemplated that the game will be played with multiple 52-card decks of playing cards—although it is to be understood and appreciated that play with a single deck also lies within the present invention.
[0027] With reference to FIGS. 3 , 4 , and 5 the play of the game will now be described in accordance with a preferred embodiment of the present invention, a player is provided at 42 with a posted list for an additional bet of either a “Good Hand” bet or a “Bad Hand” bet, as well as providing a conventional Blackjack bet-receiving region and an additional chip bet-receiving region.
[0028] At 44 the player decides to make a conventional bet, to be played under the conventional rules of Blackjack, and/or an additional bet, utilizing the “Good Hand”—“Bad Hand” feature bets provided in accordance with 42 , above.
[0029] Based upon the decision of the player at 44 , three different bet-placing outcomes occur, which are shown and described at 46 . At 48 the player has decided to make only a conventional bet, thus placing the wager in the conventional bet-receiving region. At 52 the player has decided to make only an additional bet, and thus places the wager in either the “Good Hand” or “Bad Hand” additional bet-receiving areas. At 54 the player has decided to make both a conventional bet and an additional bet, so the wagers are placed in both the conventional bet-receiving region and in either the “Good Hand” or “Bad Hand” additional bet-receiving areas.
[0030] With all wagers placed, at 56 the Dealer deals the player and the Dealer two cards each, in accordance with the rules of conventional Blackjack. A decision is then made at 108 as to whether the player did or did not place an additional bet. If an additional bet was not placed, the player waits at 62 for continuation of conventional Blackjack play.
[0031] If an additional bet was placed by the player, at 64 a decision is made regarding whether the player received a winning additional bet hand from the dealer in step 56 or a losing additional bet hand—both as determined by matching the playing card point totals to the posted list. If a winning additional bet hand is made, at 66 the Dealer pays the player an amount equal to the additional bet of the player. If a losing additional bet hand is made, at 68 the Dealer removes the additional bet of the player from the additional bet-receiving region. Upon completion of the additional bet winning/losing evaluation, at 72 play of the game continues under the playing rules of conventional Blackjack, for those players having placed a conventional bet in steps 48 or 54 .
[0032] As may be observed from the foregoing, the wagering system of the present invention can easily be incorporated within a blackjack table in which each player's seating area at the table is provided with a specific additional bet area having marks for receiving the additional bet.
[0033] The player may select or bet value for the additional bet somewhere between the minimum and maximum bet range for the relevant table. The relevant casino may choose to set different minimum-maximum ranges.
[0034] Conventional blackjack bets will continue to be made by placing chips in the conventional betting areas 22 , which are separate from the second wagering area 24 . In the play of each game, the player will make all bets prior to any cards having been dealt face up or face down.
[0035] If the player bets “Good Hands” and the first two cards dealt to the player fall under the list of “Good Hands” listed in the table below, “Good Hands” will be declared as a winning hand to be paid by the dealer immediately after the first two cards are dealt to the player(s) and dealer, and before any further cards are dealt to the player(s) and/or dealer.
[0036] Conversely, if the player has bet on a “Good Hands” and the first two cards dealt to the player fall under the list of “Bad Hands” listed in the table below, the relevant chips will be removed by the dealer from the additional bet mark immediately after the first two cards are dealt to the player(s) and dealer.
[0037] If the player bets “Bad Hand,” the following “Bad Hands” will be considered winning hands to be paid by the dealer immediately after the first two cards are dealt to the player(s) and dealer and before any further cards are dealt to the player(s) and/or dealer.
[0038] Conversely, if the player has bet on a “Bad Hand” and the first two cards dealt to the player fall under the posted list of “Good Hands,” the relevant chips will be removed by the dealer from the additional bet mark immediately after the first two cards are dealt to the player and dealer.
[0039] Additionally, and as previously discussed, if the first two cards dealt to the relevant player total thirteen (13), neither the player nor the casino will win the relevant bet—in order to guarantee than an appropriate hold (return) is received by the casino on every bet.
[0000]
GOOD HAND
Probability
BAD HAND
Probability
Blackjack
4.83
Sixteen
7.70
Two Aces
0.45
Fifteen
8.44
Twenty
10.26
Fourteen
8.90
Nineteen
6.03
*Thirteen
8.45
Eighteen
5.28
Twelve
8.88
Soft Eighteen
1.21
**Eight
2.85
Seventeen
6.05
***Seven
2.42
Soft Seventeen
1.21
Six
1.66
Eleven
4.83
Five
1.21
Ten
4.06
Four
0.45
Nine
3.62
Three
1.21
Total =
47.83
Total =
52.17
*Push (tie)
**Ace-Seven excluded - listed as a soft eighteen (Good Hand)
***Ace-Six excluded - listed as a soft seventeen (Good Hand)
[0040] One presently preferred embodiment of the present invention is depicted in FIGS. 2-4 , showing a method of playing blackjack starting with the step of providing a conventional bet receiving region and an additional bet chip receiving region for the “Good Hand”—“Bad Hand” additional bet (see FIG. 1 ). The player then makes a conventional bet of a denomination range permitted by the relevant casino and regulatory body and/or the player makes a “Good Hand” or “Bad Hand” additional bet by placing the bet in the single betting region for the additional bet, the bet being of a denomination permitted by the relevant casino and regulatory body.
[0041] That is, the player need not participate in the conventional play bet may choose to participate in only the additional bet. Alternatively, the player need not participate in the additional bet—choosing to participate in only the conventional bet. Alternatively, the player may participate in both the conventional bet and the additional bet.
[0042] The dealer then deals the player and dealer two cards each. After the dealing of the two cards, it is determined whether the two cards dealt the player represent a winning hand or a losing hand according to the posted “Good Hand”—“Bad Hand” list and according to the player's bet selection of either a “Good Hand” or a “Bad Hand”.
[0043] After the initial two cards are dealt to the player(s) and the dealer, the dealer pays the player an amount equal to the “Good Hand” or “Bad Hand” winning bet located in the single betting region for the alternative bet. After the determination of the outcome of the additional bet, conventional play continues be keeling the player and dealer additional cards, unless the player determines not to take any additional cards and the dealer has concluded his/her play according to the rules of the game.
[0044] The rules and play of the game are described below in a series of examples.
Example 1
[0045] All Players place their wagers in the conventional betting area, and none in the “Good Hand” or “Bad Hand” betting areas. The cards are dealt by the dealer as in a conventional Blackjack game, with winning wagers paid and losing wagers removed in accordance with the conventional rules of play for Blackjack. At the conclusion of play the dealer removes all cards from the table, placing them in the discard tray prior to starting play of the next game.
Example 2
[0046] Player 1 places a wager in the “Good Hand” betting area. Player 2 places a wager in the “Bad Hand” betting area. Player 3 places a wager in the “Good Hand” betting area. Player 4 places a wager in the “Bad Hand” betting area. Player 1 is dealt two cards, having a point total (under the traditional rules of Blackjack) of 19. In a like manner Player 2 is dealt two cards having a point total of 20; Player 3 is dealt two cards having a point total of 20; and Player 4 is dealt two cards having a point total of 14. The Dealer hand consists of one face-up card and one face-down card—the point total is irrelevant for purposes of evaluating the “Good Hand”/“Bad Hand” wagers.
[0047] Making reference to the payoff table for the “Good Hand”/“Bad Hand” wagers, the Dealer pays Player 1 the amount of the wager placed by Player 1 in the “Good Hand” wagering area, the 19 points being included in a “Good Hand” payoff; the Dealer removes the “Bad Hand” wager of Player 2, since 20 points is in the “Good Hand” listings; the Dealer pays Player 3 the amount of the “Good Hand” wager, 20 points being listed in the “Good Hand” listings; and the Dealer pays Player 4 the amount of the “Good Hand” wager of Player 4, 14 points being listed in the “Good Hand” listings.
[0048] The hands of all players are removed by the Dealer and placed in the discard tray, including the two cards of the Dealer.
Example 3
[0049] Prior to the dealing of the first card, Player 1 places a “Good Hand” wager and a conventional Blackjack wager; and Player 2 places a “Bad Hand” wager and a conventional Blackjack wager. Player 1 is dealt two cards having a point total of 19, and the two cards of Player 2 total 10. The Dealer is dealt two cards, the point totals being irrelevant for the initial evaluation of the “Good Hand” and “Bad Hand” wagers.
[0050] Prior to the dealing of any additional cards, the Dealer pays Player 1 for his winning “Good Hand” wager, the point total being listed as one of the “Good Hands.” The cards of Player 1 are not removed, since Player 1 has also made a conventional Blackjack wager.
[0051] Dealer removes the “Bad Hand” wager of Player 2, since the 10 points of Player 2 is in the “Good Hand” listing of point totals. The Dealer does not remove the playing cards of Player 2 since a conventional Blackjack wager has also been made by Player 2.
[0052] The Dealer then commences the play of a conventional Blackjack game, inquiring first of Player 1 and then of Player 2 whether additional playing cards are desired, and if one or both Players do not bust, the Dealer then obtains additional cards in accordance with house rules. Winning and losing wagers are determined in accordance with the rules of conventional Blackjack.
[0053] The present invention can be incorporated in an electronic gaming device with multiple player video screen and bet selections. Similarly, the present invention can be incorporated in a single play slot machine (video game) device.
[0054] It should be recognized that the numerous descriptional functions and advantages of the subject invention as set forth herein are illustrative only; therefore, change may be made within the general principles of the invention as indicated by the terms expressed within the appended claims listed below.
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A gaming method and system that allows a player to wager varying amounts on whether that player will win or lose an additional bet, contingent on the makeup of the first two cards dealt to a player in the game of blackjack. The first two cards will fall under predetermined, posted category of “Good Hand” or “Bad Hand.” Each category will be made up of playing card combinations that most players would view as good or bad playing card point totals in the game of blackjack. The player will have three wagering options: (1) make only a conventional bet; (2) make only the additional bet by selecting either the “Good Hand” or the “Bad Hand” from the posted categories of “Good Hands” and “Bad Hands”; or (3) Make both a conventional blackjack bet and an additional bet.
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BACKGROUND OF THE INVENTION
This invention relates to the formulation of colloidal slurry used to polish NiP plated substrates. This formulation significantly increases the material removal rate during polishing, reduces polish defects, and improves the polished surface finish.
A metallic magnetic thin film disk used in a computer disk drive typically comprises an aluminum substrate plated with NiP, an underlayer sputtered onto the plated NiP, a magnetic Co alloy sputtered onto the underlayer, a carbon protective overcoat sputtered onto the magnetic layer and a lubricant layer deposited on the carbon.
Before depositing the underlayer, the plated NiP is polished to remove surface defects and to lower surface roughness which strongly affects the flying height of a recording head over the disk. A increasing recording density in computer disk drives. At present, the lowest surface roughness Ra obtained using commercially available slurries for NiP plated substrate polishing is about 0.5 nm. ("Ra" is a well-known measure of surface roughness.) However, polishing defects become severe problems as smaller abrasive particles are used in the slurry to reduce the polished surface roughness. Two kinds of polish defects, micro-scratches and polish pits, are apt to form on the NiP polished surface. In general, micro-scratches are thought to be caused by large agglomerated particles. Polish pits are formed either by chemical attacking or other unknown causes.
Current commercially available slurries used for polishing NiP plated substrates typically comprise two components: alumina abrasive particles and an acidic etchant. The abrasive particle size ranges from 0.1 μm to about 1 μm. The slurry pH ranges from 2 to 6 for various polish process applications. Polishing with these slurries is based on micro-machining, wherein the abrasive has an angular shape and grinds the polished surface. The acidic etchant helps increase the efficiency of the micro-machining and improves the polished surface finish by chemical etching. Although a smoother polished surface can be obtained by using smaller abrasive particles, it is still not possible to make scratch-free polished surfaces. Further, these conventional slurries are apt to cause polish pits. This becomes worse with decreasing abrasive particle size to lower surface roughness. Also, smaller abrasive particles create more numerous polishing pits.
In order to eliminate the above-mentioned problems of conventional slurries, colloidal silica has been considered for polishing NiP plated substrates. Colloidal silica has long been successfully used for polishing various materials, such as silicon, gallium arsenide, indium phosphide and titanium, to form a super-smooth and scratch-free surface finish. Colloidal silica slurries used for chemical-mechanical polishing (CMP) typically include aqueous colloidal silica with an etchant (oxidizer) as a polishing promoter. Various kinds of chemicals are used in colloidal silica slurries for different polishing applications to achieve either a high material removal rate or better polished surface finishes with fewer polish defects. Alkaline chemicals, for instance, are used as etchants in colloidal silica slurries to reduce surface roughness in semiconductor wafer rough polish processes as described in U.S. Pat. No. 5,571,373 issued Nov. 5, 1996 to Krishna et al., incorporated herein by reference. Persulphate, as described in U.S. Pat. No. 5,575,837 issued Nov. 19, 1996 to Kodama et al., is used as an etchant in a colloidal silica slurry for mirror-finishing metal surfaces.
Unfortunately, several problems are encountered when attempting to use these commercially available colloidal silica slurries to polish NiP plated substrates. For example, existing commercial colloidal silica slurries, either with an alkaline etchant or an acidic etchant, exhibit a very low NiP removal rate. Further, these slurries also cause polish pits, which are caused by chemical attacking, and micro-scratches. There is presently no adequate colloidal silica formulation for polishing NiP.
To make a colloidal silica slurry applicable to NiP plated substrate polishing, a new formulation is desired to increase slurry's NiP removal rate and to decrease polish defects. It is known in the art that adding an oxidizer or changing chemistry can increase the material removal rate or remove polish defects. However, the extent to which one can add an oxidizer or change the slurry chemistry is bounded by colloidal chemistry as described by I. Ali et al. in "Charged Particle in Process Liquids", published in Semiconductor Intl., in 1990. The colloidal suspension may be broken or the aqueous colloidal abrasive can jell due to the pH value change caused by oxidizer addition or other chemistry change. On-line hydrogen peroxide addition was used by the inventor to improve the polish performance of colloidal silica slurry. (By "on-line hydrogen peroxide addition," I mean that hydrogen peroxide was added to the slurry shortly before use.) A better polished surface finish was obtained by adding hydrogen peroxide to the slurry. However, the NiP removal rate was not significantly increased by adding hydrogen peroxide. Further, hydrogen peroxide cannot remove polish scratches.
Because of the above-mentioned low NiP removal rate and polish defect problems, it would be desirable to make a new formulation which would increase the NiP removal rate of the colloidal slurry and reduce the number of polish defects, and simultaneously provide a good polished surface finish.
SUMMARY
In one embodiment of my invention, aluminum nitrate, nitric acid and hydrogen peroxide are added to a colloidal silica polishing slurry to significantly increase the material removal rate, reduce the number of polish defects, and decrease polished surface roughness. The slurry is used to polish Ni, Al, NiP, other Ni alloys or Al alloys, or other metals. I have found that aluminum nitrate used with nitric acid significantly increases the NiP removal rate of colloidal slurry. Further, nitric acid helps to stabilize the colloidal suspension, and hydrogen peroxide helps to remove polish pits.
In another embodiment of my invention, aluminum nitrate, nitric acid and hydrogen peroxide are added to a colloidal alumina slurry (or other colloidal aqueous abrasive slurries) to achieve an improved material removal rate and an improved smooth polished surface.
In another embodiment of my invention, the above formulation is used with slurries comprising non-colloidal abrasive particles, e.g. non-colloidal silica or alumina.
In another embodiment of my invention, the above-mentioned formulation is used with colloidal abrasives other than silica or alumina.
A method in accordance with one embodiment of the invention includes the step of polishing a workpiece with a slurry. The slurry comprises abrasive particles and a metal nitrate salt. The slurry has a pH less than about 3.5, and the metal nitrate salt increases the polishing rate of the slurry. The slurry also comprises H 2 O 2 and HNO 3 . The abrasive particles comprise colloidal abrasive particles.
In one embodiment, the metal nitrate salt comprises Al(NO 3 ) 3 .
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B illustrate the results of a polish test performed using a planetary polisher and a colloidal silica slurry with an alkaline etchant having various silica contents. The NiP polish performance was measured in terms of NiP removal rate (FIG. 1A) and polished surface roughness (FIG. 1B).
FIGS. 2A and 2B illustrate the results of polish tests performed using a planetary polisher and various colloidal silica slurry formulations. The polish performance of the various formulations was measured in terms of NiP removal rate (FIG. 2A) and polished surface roughness (FIG. 2B).
FIG. 3 illustrates the polish performance of a colloidal alumina slurry in accordance with an embodiment of my invention compared to a commercial colloidal alumina slurry containing an acidic etchant. The polish performance of the colloidal alumina slurries was measured in terms of NiP removal rate (FIG. 3A) and polished surface roughness (FIG. 3).
FIGS. 4A and 4B schematically show a planetary polishing apparatus in plan view and cross section, respectively.
FIG. 5 schematically shows a single disk polishing apparatus.
FIG. 6 schematically shows a ring polishing apparatus.
DETAILED DESCRIPTION
A colloidal silica slurry in accordance with one embodiment of my invention is made by mixing aqueous colloidal silica with aluminum nitrate, nitric acid and hydrogen peroxide. The slurrv is typically used to polish and etch a metal surface such as NiP, Ni or Al. The silica content is between about 2 and 40 wt. % and typically 11 wt. %. The particle size can be from about 50 to 80 nm although other particle sizes can be used. The pH of the slurry, as measured at 25° C., is between about 1.5 and 3.5. The pH is preferably greater than 2 for safety reasons, and typically about 2.7.
The pH is typically controlled by adding aluminum nitrate (Al (NO 3 ) 3 ). As explained below, I have discovered that adding aluminum nitrate to the slurry increases the polishing rate. In lieu of aluminum nitrate, other acidic metal nitrate salts capable of reducing the pH to 3.5 or less can be used. In one embodiment, ferronitrate is used in lieu of aluminum nitrate.
One example of a slurry in accordance with my invention comprises between 2 and 40 wt. % silica, 0.1 and 2.5 wt. % Al(NO 3 ) 3 , greater than 0 wt. % but less than or equal to 1 wt. % HNO 3 , and between 0.1 and 3 wt. % H 2 O 2 . In one embodiment, the slurry comprises greater than 0 wt. % but less than 0.2 wt. % HNO 3 , and between 0.1 and 2 wt % Al(NO 3 ) 3 . In another embodiment, the slurry contains between 0.02 and 0.1 wt. % HNO 3 and between 0.2 and 1 wt. % Al(NO 3 ) 3 .
I have found that a silica slurry including a high silica content and aluminum nitrate sometimes jells. I have also found that there are at least two ways to avoid this phenomenon: 1) add water to the slurry to dilute it, or 2) add nitric acid (HNO 3 ) to the slurry.
As explained below, depending upon polishing conditions, pits may be formed in the workpiece being polished. I have discovered that hydrogen peroxide (H 2 O 2 ) can be added to the slurry to prevent pit formation.
To prepare the slurry formulation in accordance with one embodiment of my invention, I started with a commercially available silica slurry available from Fujimi America, located in Wilsonville, Oregon. The slurry is sold under the tradename Compol 80. The pH of Compol 80 is about 10. I added to this slurry a solution comprising a solution comprising 30 wt. % Al(NO 3 ) 3 , a solution comprising 70 wt. % HNO 3 , and a solution comprising 30 wt. % H 2 O 2 .
The ratio was 25 parts of the Al(NO 3 ) 3 solution; 1 part of the HNO 3 solution; and 25 parts of the H 2 O 2 solution. A sufficient amount of this mixture was added to reduce the slurry pH to 2.7. (In other embodiments, instead of using 1 part of the HNO 3 solution and 25 parts of the H 2 O 2 solution, other concentrations can be used, e.g. between 0 and 2 parts HNO 3 and between 2 and 50 parts H 2 O 2 .)
A slurry in accordance with my invention is useful for polishing a NiP layer plated onto an Al substrate. (NiP is typically electroless-plated onto Al substrates, e.g. to a thickness between 8 to 10 μm, as part of a magnetic disk manufacturing process.) I have discovered that a slurry in accordance with my invention provides the benefits of:
1) an increased NiP removal rate;
2) improved NiP smoothness; and
3) avoidance of pit formation during polishing.
(In lieu of an Al substrate, other substrate materials may be used in accordance with my invention, e.g. glass, glass ceramic, sputtered carbon, ceramics or other materials having a NiP or other metallic material formed thereon, either by plating, sputtering or other process.)
A set of experiments were performed on NiP-coated Al substrates to evaluate the performance of slurries used to polish the NiP. The polish performance experiments included a) testing NiP removal rate using a planetary polisher; b) evaluating polished NiP surface roughness on a texture measurement system; c) evaluating polish scratches under a high intensity light; and d) testing the polish pitting propensity using a single-disk polisher. The polish performance of the colloidal silica slurry in accordance with one embodiment of my invention was compared with a commercial colloidal silica slurry which comprised the same colloidal silica abrasive (and the same silica content) and an alkaline etchant. The commercial slurry was the above-mentioned Compol 80.
The NiP removal rate test was performed by measuring the NiP thickness of NiP plated substrates before and after a polish test, and dividing the difference in these two measurements by polish time. Two polish runs (forty-two disks per run) were performed with the planetary polisher using each tested slurry, and seven disks were measured from each test run. The polishing machine was model no. 9B-14, available from SpeedFam International Corp. of Chandler, Ariz. The average of the NiP removal rate calculated from the measurements of the two runs (fourteen measurements) of each slurry were taken as the final result. The slurry flow rate was 500 ml/minute, the ring gear RPM (revolutions per minute) was 8.9, the sun gear RPM was 3.6, the bottom plate RPM was 16.5 and the top plate RPM was 5.5. The normal load was 230 kg.
FIGS. 1A and 1B show the NiP polish performance of Compol 80 colloidal silica slurry with the alkaline etchant and various silica contents. The silica content was varied by diluting the slurry with water. The NiP removal rate decreased with increasing water dilution. Also, polish pits were observed with increased water dilution. The polished surface roughness was increased by the presence of the pits.
FIGS. 2A and 2B show the NiP polish performance of a slurry in accordance with one embodiment of my invention having an 11 wt. % silica content (composition 5) compared with a slurry including the 11 wt. % silica and an alkaline etchant (composition 1) the slurry of composition 1 combined with hydrogen peroxide (composition 2), the slurry of composition 1 combined with aluminum nitrate (composition 3), and the slurry of composition 1 combined with nitric acid (composition 4).
The slurries tested in FIGS. 2A and 2B were prepared as follows:
No. Slurry Composition
1. The slurry formed by adding 1 part Compol 80 to 3 parts water. The pH was about 9.7 to 9.8.
2. The slurry was 1 part Compol 80, 3 parts water, and 0.2 parts 30 wt. % H 2 O 2 solution.
3. The slurry was 1 part Compol 80, 3 parts water, and 0.1 parts of a 30 wt. % Al(NO 3 ) 3 solution; no H 2 O 2 .
4. The slurry was 1 part Compol 80, 3 parts water, and 0.008 part 70 wt. % HNO 3 solution.
5. The slurry was 1 part Compol 80, 3 parts water, 0.1 parts of a 30 wt. % Al(NO 3 ) 3 solution, 0.1 parts of a 30 wt. % H 2 O 2 solution, and 0.004 parts of a 70 wt. % HNO 3 solution.
Bar 1 in FIG. 2A shows the NiP removal rate of the commercial colloidal silica slurry with the alkaline etchant. The removal rate was about 0.4 μ"/min (0.01 μm/min). The polished surface roughness with this slurry was about 0.31 nm RMS as shown by the clear circle in FIG. 2B.
Bar 2 shows the removal rate for a slurry containing H 2 O 2 . The material removal rate was increased to about 0.5 μ"/min (0.0127 μm/min) and the polished surface roughness decreased to about 0.23 nm as shown by bar 2 in FIG. 2A and the clear triangle in FIG. 2B.
The formulation of slurry no. 1 was changed by adding aluminum nitrate as an etchant to form slurry no. 3. The pH of slurry no. 3 was about 3.1. The NiP removal rate increased significantly to about 1.7 μ"/min (0.043 μm/min) and the polished surface roughness decreased to 0.18 nm. This is shown by bar 3 and the clear diamond in FIGS. 2A and 2B , respectively.
Using nitric acid as etchant in the colloidal silica slurry (the pH was about 3.0), the NiP removal rate was 0.9 μ"/min (0.023 μm/min), and the polished surface roughness was about 0.18 nm as shown by bar 4 and the clear square in FIGS. 2A and 2B. As can be seen, a large gain in the NiP removal rate (compared to the commercial slurry no. 1) was not obtained when the slurry pH value was decreased to about 2 by adding nitric acid.
Bar 5 represents the NiP removal rate of a colloidal silica slurry in accordance with an embodiment of my invention. The removal rate was 3.8 μ"/min (0.1 μm/min)--about ten times higher than the colloidal silica with the same silica content and the alkaline etchant. The polished surface finish roughness was about 0.2 nm RMS as shown by the solid circle in FIG. 2B.
The results of polish pitting evaluation and polish scratch evaluation for the colloidal silica slurries of FIG. 2 are shown in Table 1. The commercial colloidal silica with the alkaline etchant showed a large pitting propensity during NiP polishing caused scratches on the NiP surface. Both aluminum rate and nitric acid worked well to removal polish atches. However, aluminum nitrate and nitric acid cause polish pits depending on polishing ditions. Although hydrogen peroxide did not remove ish scratches significantly, it substantially vented pitting during the NiP polish process with loidal silica slurry. The formulation with the odiment of my invention combined the benefits from se three chemicals as follows:
TABLE 1______________________________________Barchart Polish PolishNo. in scratches pittingFIG. 2A Slurry formulation observed propensity______________________________________1 Commercial colloidal Many High silica with an alkaline etchant2 Commercial colloidal Many No silica with an alkaline etchant and hydrogen peroxide addition3 The colloidal silica No Low with aluminum nitrate etchant4 The colloidal silica No Low with nitric acid etchant5 The colloidal silica Very few No in accordance with one embodiment of my invention______________________________________
To summarize:
1) Hydrogen peroxide can significantly remove pitting caused when polishing with a colloidal silica slurry. Hydrogen peroxide also provides a minor contribution in removing polish scratches and increasing the NiP removal rate of the colloidal silica slurry.
2) Aluminum nitrate can significantly increase the NiP removal rate of a colloidal silica slurry and remove polish scratches. However, aluminum nitrate may cause polish pits and cause the slurry to jell. The jelling time depends on the amount of water and nitrate added. More water helps to break the jell.
3) Nitric acid can increase the NiP removal rate of a colloidal silica slurry, but not as much as aluminum nitrate if the nitric acid is used alone. Nitric acid also causes polish pits. However, nitric acid can prevent the colloidal silica from jelling, which would result from nitrate addition. Nitric acid can also effectively increase the material removal rate when used with nitrate.
As mentioned above, my invention is also applicable to colloidal alumina slurry. FIGS. 3A and 3B show the NiP polish performance of colloidal alumina slurry in accordance witn one embodiment of my invention (slurry no. 7) compared to that of a conventional alumina colloidal slurry with an acidic etchant (slurry no. 6). Slurry no. 6 was EP1000, provided by Cabot Corp. of Aurora, Ill. The particle size was about 100 nm, and the pH of the slurry was about 4. Slurry no. 7 was formed by providing a mixture of 25 parts of a 30 wt. % aluminum nitrate solution, 1 part of a 70 wt. % nitric acid solution, and 25 parts of a hydrogen peroxide solution. This mixture was added to slurry no. 6 (8% by volume of the resulting slurry was the aluminum nitrate/nitric acid/hydrogen peroxide mixture). The pH of the resulting slurry was about 3.0.
The material removal rate for the EP1000 slurry was 1.1 μ"/min (0.028 μm/min) (bar 6 in FIG. 3A). The removal rate was increased to 3.3 μ"/min (0.084 μm/min) (bar 7 in FIG. 3A) by adding aluminum nitrate, nitric acid and hydrogen peroxide to the slurry. The polished surface roughness was lowered from 0.38 nm (the clear circle in FIG. 3B) to 0.33 nm (the solid circle in FIG. 3B). The results of polish scratch and polish pitting evaluation are shown in Table 2. Both polish scratches and polish pitting propensity were decreased with the embodiment of my invention.
TABLE 2______________________________________BarChart Polish PolishNo. in scratches pittingFIG. 3A Slurry formulation observed propensity______________________________________6 A commercial Many High colloidal alumina slurry with an acidic etchant7 The colloidal Less Very Low alumina slurry in accordance with one embodiment of my invention______________________________________
Industrial Application
In one embodiment, the slurry is used to polish an NiP layer plated onto an Al substrate as part of a magnetic disk manufacturing process. In one embodiment, the polishing apparatus is a planetary polisher, such as the above-mentioned SpeedFam polisher. The polishing parameters may be the same as for the experiments described in the tables and figures discussed above. However, it may be desirable to increase the normal loading force to increase through-put. In one embodiment, a normal loading force of 390 kg is used. (The SpeedFam apparatus polishes 42 disks at a time, which means a force of about 9.2 kg/disk is applied.) Larger normal loading forces can be used. I have not encountered an increase in defects when using a high normal force. Also, I have found that aluminum nitrate decreases friction during polishing, which facilitates use of a higher normal loading force.
FIGS. 4A and 4B schematically show a planetary polisher 100 including a circular disk holder 102 which holds disks 104, 106 and 108 during polishing. Although only three disks 104, 106, 108 are held by one holder 102 as shown in FIG. 4, the above-mentioned SpeedFam polisher simultaneously polishes 42 disks.
During polishing, a gear 110 rotates in the direction of arrow A around a central circular member 112, causing holder 102 to move around member 112 in a direction B. Simultaneously, central circular member 112 rotates in a direction C, and holder 102 rotates around its central axis in direction a D.
Simultaneously stationary top lap surface 116 and bottom lap surface 118 rub against and polish disks 104, 106 and 108. The slurry is applied to the regions between the lapping pads 116, 118 and disks 104, 106 and 108 via channels 120.
In another embodiment, a single-disk type polisher is used to polish the NiP plated layer. Such a single disk polisher can have a structure similar to the Strasbaugh 6DEDC-25P2 texturing apparatus. FIG. 5 schematically shows a single disk polishing apparatus 130 for polishing a disk 132 with a polishing pad 134. During polishing, disk 132 rotates in a direction E while pad 134 presses against disk 132 and rotates in a direction F. One side of disk 132 is polished at a time. The slurry of the present invention is introduced between pad 134 and disk 132.
In yet another embodiment, a ring type polisher is used to polish the NiP layer. In one embodiment, the ring type polisher can be an MDS ring polisher available from SpeedFam.
FIG. 6 schematically shows a ring polisher 160 for polishing disks 162. During polishing, disks 160 are rotated in a direction G by the motion of a center driving ring 164 in direction H. Disks 162 are urged against ring 164 by pivoting stanchions 166. (Pivoting stanchions 166 are mounted to stanchion assemblies 168. During use, stanchions 166 are caused to rotate in direction I by the motion of disks 162.)
During use, while disks 162 are rotated by center driving ring 164, a lower polishing platen 170 presses against disks 162 to thereby polish the lower surface of disks 162. Simultaneously, an upper platen (not shown, but having the same lateral extent as lower platen 170) pushes down on disks 162 to thereby polish the upper surface of disks 162. A slurry in accordance with my invention is introduced into the space between the platens and disks 162.
After polishing, the NiP is typically textured. After texturing, the magnetic disk is completed by sputtering an underlayer (typically NiP or Cr), a magnetic Co alloy and a hydrogenated carbon overcoat onto the substrate in that order. A liquid lubricant is then deposited onto the carbon. Details concerning these steps are disclosed in U.S. Pat. No. 5,658,659, issued on Aug. 19, 1997 to Chen et al., incorporated herein by reference.
Although the slurry can be used to manufacture magnetic disks, it can also be used to manufacture other products, and to polish materials other than NiP, e.g. Ni, Al, or other metals or alloys thereof.
While the invention has been described with respect to a specific embodiment, those skilled in the art will recognize that changes can be made in form and detail without departing from the spirit and scope of the invention. For example, as mentioned above, instead of using aluminum nitrate as main NiP removal promoter in a colloidal silica slurry, other nitrates, such as ferronitrate, can be used. A nitrate etchant in accordance with my invention can also be used with aqueous colloidal abrasive solids other than aqueous colloidal silica or alumina. In addition, my invention can be used with a slurry having colloidal silica and alumina combined. Accordingly, all such changes come within the invention.
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A novel colloidal silica slurry including additives for enhancing the removal rate of a metallic workpiece, preventing etch pits, and enhancing smoothness. These additives include HNO 3 , H 2 O 2 and Al(NO 3 ) 3 . In lieu of colloidal silica, colloidal alumina can be used. The metallic workpiece can be NiP, Ni, Al or other appropriate materials.
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RELATED APPLICATION
[0001] This patent application claims priority to U.S. Provisional Application Ser. No. 61/490,403, filed on May 26, 2011, and to U.S. Provisional Application Ser. No. 61/452,570, filed on Mar. 14, 2011, the contents of each are hereby incorporated by reference in their entirety.
FIELD
[0002] Disclosed herein is a light wavelength converting material for taggant applications and quantitative diagnostics.
Environment
[0003] In the processing and packaging of various consumer products, oils, greases and lubricants may come into contact with the product.
[0004] Typically, lubricants can come into contact with consumer products due to leakage of lubricants through gaskets or seals, from sliding mechanisms, from drum systems, from gear boxes, from pumps, from sealed rolling bearing units, from chains and belts, and the like. For example, lubricants are used in a variety of machines commonly used in the preparation and packaging of produce for market.
[0005] Since lubricants of similar compositions are used throughout the various stages of produce treatment and packaging, it is often difficult for the manufacturer to locate the source of a particular lubricant. As such, the manufacturer is forced to conduct a time consuming search for the source of the lubricant which is lowering the quality of the manufactured products.
[0006] One possible way to detect the presence of undesired lubricants would be to add a taggant to the lubricant that could be readily detected on-line and at production speeds. However, suitable oil soluble taggants are not known to exist.
[0007] Therefore, it would be advantageous if an oil-soluble taggant could be developed that would enable inspection to be conducted on-line, in real time, during the production process.
SUMMARY
[0008] In one form, disclosed is a fluorescent taggant composition, comprising a Stokes-shifting taggant, which absorbs radiation at a first wavelength and emits radiation at a second wavelength, different from said first wavelength; and an oil or lubricant.
[0009] In another form, disclosed is a taggant composition, comprising an oil-soluble fluorescent taggant and an oil or lubricant.
[0010] In yet another form, disclosed is a compound comprising a tetrabutylammonium chloride complex of Indocyanine Green (ICG).
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The forms disclosed herein are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar elements and in which:
[0012] FIG. 1 is a representation of the infrared absorption and emission peaks of the Indocyanine Green (ICG) complex taggant, illustrating the Stokes-shift;
[0013] FIG. 2 is a representation of the infrared absorption and emission peaks of a modified ICG-complex, illustrating a secondary emission peak;
[0014] FIG. 3 is a representation of the infrared absorption peak for the modified ICG-complex of Example 1;
[0015] FIG. 4 is a representation of the infrared excitation and emission peaks for the modified ICG-complex of Example 1; and
[0016] FIG. 5 is an H-nuclear magnetic resonance scan of the ICG-complex according to this invention.
DETAILED DESCRIPTION
[0017] Various aspects will now be described with reference to specific forms selected for purposes of illustration. It will be appreciated that the spirit and scope of the apparatus, system and methods disclosed herein are not limited to the selected forms. Moreover, it is to be noted that the figures provided herein are not drawn to any particular proportion or scale, and that many variations can be made to the illustrated forms. Reference is now made to FIGS. 1-5 , wherein like numerals are used to designate like elements throughout.
[0018] Each of the following terms written in singular grammatical form: “a,” “an,” and “the,” as used herein, may also refer to, and encompass, a plurality of the stated entity or object, unless otherwise specifically defined or stated herein, or, unless the context clearly dictates otherwise. For example, the phrases “a device,” “an assembly,” “a mechanism,” “a component,” and “an element,” as used herein, may also refer to, and encompass, a plurality of devices, a plurality of assemblies, a plurality of mechanisms, a plurality of components, and a plurality of elements, respectively.
[0019] Each of the following terms: “includes,” “including,” “has,” “‘having,” “comprises,” and “comprising,” and, their linguistic or grammatical variants, derivatives, and/or conjugates, as used herein, means “including, but not limited to.”
[0020] Throughout the illustrative description, the examples, and the appended claims, a numerical value of a parameter, feature, object, or dimension, may be stated or described in terms of a numerical range format. It is to be fully understood that the stated numerical range format is provided for illustrating implementation of the forms disclosed herein, and is not to be understood or construed as inflexibly limiting the scope of the forms disclosed herein.
[0021] Moreover, for stating or describing a numerical range, the phrase “in a range of between about a first numerical value and about a second numerical value,” is considered equivalent to, and means the same as, the phrase “in a range of from about a first numerical value to about a second numerical value,” and, thus, the two equivalently meaning phrases may be used interchangeably.
[0022] It is to be understood that the various forms disclosed herein are not limited in their application to the details of the order or sequence, and number, of steps or procedures, and sub-steps or sub-procedures, of operation or implementation of forms of the method or to the details of type, composition, construction, arrangement, order and number of the system, system sub-units, devices, assemblies, sub-assemblies, mechanisms, structures, components, elements, and configurations, and, peripheral equipment, utilities, accessories, and materials of forms of the system, set forth in the following illustrative description, accompanying drawings, and examples, unless otherwise specifically stated herein. The apparatus, systems and methods disclosed herein can be practiced or implemented according to various other alternative forms and in various other alternative ways.
[0023] It is also to be understood that all technical and scientific words, terms, and/or phrases, used herein throughout the present disclosure have either the identical or similar meaning as commonly understood by one of ordinary skill in the art, unless otherwise specifically defined or stated herein. Phraseology, terminology, and, notation, employed herein throughout the present disclosure are for the purpose of description and should not be regarded as limiting.
[0024] Provided are new oil soluble, light wavelength-converting, preferably upconverting, compositions for taggant applications and quantitative diagnostics in connection with lubricants, such as by way of non-limiting example, the detection of errant lubricants on product that comes into contact with lubricated machinery. Other taggant applications are contemplated, including, but not limited to, anti-counterfeiting, brand protection, or verification that a machine contains a correct lubricant, and other possible applications. A detection system enables the development of near real time, low cost, compact, portable and highly sensitive detection, monitoring and diagnostics of modifications to manufacturing process systems in real world environments. It is the unique process (e.g. the conversion of visible light to infrared light, infrared to visible light and the upconversion of infrared to higher energy infrared) that enables high sensitivity detection against almost any sample or environmental background.
[0025] Using the system, theoretical particle detection (10 23 mol) of molecules added to analytic mixtures can be achieved through the use of on-line verification methods and even handheld detection applications. Detection sensitivity of 10 −20 mol is possible in a variety of detection schemes, and even direct visual detection of 10 −14 mol sensitivity has been demonstrated using a hand held 3.0 to 9.0 volt laser diode system against backgrounds of various colors and compositions. The narrow emission bandwidths and small particle size of these materials enable the simultaneous detection of multiple analytes (i.e. multiplexed assays).
[0026] According to the present invention, a detectable taggant compound is added to the various lubricants used in manufacturing and processing machinery, and advantageously taggant compounds having different characteristics are added into the lubricants at different processing locations, such that detection of one or more of these taggant compounds can enable rapid identification of the location of the source of lubricant contamination in the manufactured product.
[0027] Advantageously, the taggant compound is one which is detectable by fluorescence when it is exposed to particular wavelengths of light. In particular, a suitable taggant is one which absorbs energy at one wavelength and fluoresces/emits at a different wavelength. Such materials are well-known in the art as Stokes-shifting materials, and have recently found increasing use in inks for security marking of documents, such as banknotes and the like, to render such documents less susceptible to counterfeiting or copying.
[0028] However, most conventional Stokes-shifting and anti-Stokes shifting materials are composed of inorganic compounds, such as doped rare earth metal particles as described in U.S. Published Patent Application No. 2010/0219377, which are insoluble in lubricants. It would be advantageous if taggant compounds could be formulated to be soluble or dispersible in oils or lubricants.
[0029] According to the present invention, the taggant may be an organic compound comprised of purified crystals from naturally occurring chlorophyll. Suitable naturally-occurring chlorophyll crystals include Chlorophyll A (CAS number 1406-65-1) and Chlorophyll B (CAS number 519-62-0). These taggants are known as being down-converting or fluorescent, and are sensitive to excitation at a particular narrow bandwidth of IR light (680 nanometers). The taggant emits light at a different wavelength (715 nanometers). A similar compound may be a benze-indolium perchlorate or a benze-indolium tosolyate. Such materials absorb at around 670 nanometers and emit at a wavelength of about 713 nanometers. The chemical structure for Chlorophyll A is provided below.
[0000]
[0000] Since this compound is an organic chemical, it is readily dissolved in oils and lubricants.
[0030] In another form, an oil-soluble fluorescent material has been developed based on Indocyanine Green (ICG), the chemical structure of which is provided below.
[0000]
[0031] ICG is sodium 4-[2-[(1E,3E,5E,7Z)-7-[1,1-dimethyl-3-(4-sulfonatobutyl)-benzo[e]indol-2-ylidene]hepta-1,3,5-trienyl]-1,1-dimethyl-benzo[e]indol-3-ium-3-yl]butane-1-sulfonate, an infrared fluorescing compound currently used in the medical industry for imaging cells and blood flows in the human body, which in its conventional form is water-soluble.
[0032] The newly developed taggant is an ICG-complex available from Persis Science LLC, Andreas Pa. The chemical structure for a tetrabutylammonium chloride complexation of ICG is provided below and analytical structural information is provided in FIG. 5 .
[0000]
[0033] The new ICG-complex is sensitive to a particular narrow absorption band of IR light between about 760 to about 810 nanometers ( FIG. 3 ), and emits light at a different band between about 810 to about 840 nanometers ( FIG. 4 ), with discrete absorbance peaks at about 785 nanometers ( FIGS. 4 ) and 805 nanometers ( FIG. 1 ), and a discrete emission peak at about 840 nanometers ( FIG. 1 ).
[0034] The ICG complex can be added to oils or lubricants in the amounts of approximately 1 ppb to 5%, preferably a range of 1 ppm to 2000 ppm, based on the weight of the lubricant.
[0035] Additionally, the nature of the ICG complexing agent can be modified to impart one or more secondary NIR reflectance wavelengths adjacent to the major emission peak at 840 nanometers. By utilizing such variations in the complexing agent, and adding differently complexed ICG compounds in lubricants at differing locations in the overall process, a single detector can be located at the end of the process, and when contamination is detected, the contaminated product can be removed from the process and further analyzed for said secondary NIR reflectance peaks, to determine the location of the source of contamination. FIG. 2 is an illustration of the absorption and emission peaks of a modified ICG-complex, showing a secondary emission peak of a longer wavelength on the shoulder of the primary emission peak.
[0036] The detection system of the present invention can be used in many processes and for consumer products which are susceptible to lubricant contamination during the manufacturing process, such as for example in the growing, collection, processing and/or packaging of packaged consumer goods, such as food products, beverages, tipped and non-tipped cigars, cigarillos, snus and other smokeless tobacco products, smoking articles, electronic cigarettes, distilled products, pharmaceuticals, frozen foods and other comestibles, and the like. Further applications could include clothing, furniture, finished wood or lumber or any other manufactured or packaged product wherein an absence of oil spotting is desired.
[0037] The taggant can be added to process machinery lubricants in minor amounts, so as to obtain ultimate concentrations in the oil/lubricant as low as between about 10 ppm and 100 ppm, typically at a concentration of about 50 ppm. At these taggant concentration levels the detection system can detect as little as 10 microliters of oil, or even as little as 1 microliter of tagged oil.
[0038] However, in order to provide for easier treatment of oils or lubricants already in place within various machines, it can be more convenient to formulate a master batch of the taggant in any particular oil, wherein the taggant is mixed at higher concentrations in the base oil/lubricant, such as from about 0.1 to about 5 wt % taggant, or even from about 0.2 to about 2 wt % taggant, in a balance of the base oil/lubricant. A portion of such tagged master batch is then easily transported and added to oils/lubricants which are already in place in the machines to be treated, for example by adding a small amount of the tagged master batch to the oil sump of the machine.
[0039] When the taggant is not an oil-soluble taggant, such as when it is an inorganic particle, an optional surfactant or dispersant additive can be added in an amount effective to facilitate dispersion of the taggant particles in the base oil. Such surfactants/dispersants are well-known in the art and their identities need not be repeated herein.
[0040] Specific forms will now be described further by way of example. While the following examples demonstrate certain forms of the subject matter disclosed herein, they are not to be interpreted as limiting the scope thereof, but rather as contributing to a complete description.
EXAMPLES
Example 1
[0041] 500 mg of complexed ICG (Product No. OT-1013, available from Persis Science LLC of Andreas Pa.) is dispersed into 1.0 kg of Klüberoil 68 using a speedmixer. Klüberoil 68 is available from Klüber Lubrication North America L.P., Londonderry, N.H. The material is mixed for 10.0 minutes at a speed of 2100 RPM. The resulting master batch concentrate is slowly added to an additional 100.0 kg of Kluberoil 68 while stirring under high speed dispersion. A sample of the material is placed into a Shimadzu 5301 Fluorometer and the excitation and emission spectrographs are recorded. When excited at a wavelength of 785, a strong infrared emission is noted from 810 nanometers to 960 nanometers. See FIG. 3 for a representation of the infrared absorption peak for the ICG-complex of Example 1 and FIG. 4 for a representation of the infrared excitation and emission peaks for the ICG-complex of Example 1.
Example 2
[0042] The above example is modified slightly using a tetrabutylammonium bromide complexation of an Infrared dye IR830, available from Sigma-Aldrich of St. Louis, Mo. After mixing, it is noted that the material will produce fluorescence around 833 nanometers when excited with approximately 0.5 mW of 785 light.
Example 3
[0043] Upconverting nanoparticles, MED C-19 (Yb 2 O 3 :Er 3+ ), were obtained from Persis Science, LLC in a slurry format in DMSO. The DMSO was dialyzed from the aqueous phase leaving the particles in aqueous phase. The particles were dried and dispersed into Kluberoil 68 using a Speedmixer. The dispersion was measured optically using a Spex Fluorolog-3. The oil suspension was excited at 970 nm and the detection occurred in the visible from 400 to 700 nm to determine the presence of the tagged oil.
Example 4
[0044] 0.5 wt % of a europium chelate, available from Honeywell Corporation under the trade name of CD-335, was incorporated into 99.5 wt % of Lubriplate 220 oil using a horizontal media mill. Adequate detection was achieved using UV LED's at a wavelength of 363 nm and an APD detector with a 600 nm-700 nm notch filter.
Example 5
[0045] 1.0 wt % of an infrared absorbing dithiolene dye commercially available from Epolin, Inc—358 Adams St. Newark N.J. 07105, was dissolved via mixing with 99 parts of Kluber Oil 220 under nitrogen with a stir bar for 5 hours. The resulting mixture was analyzed for infrared absorption. The absorption occurred from 800 nm to 1200 nm with a peak at around 1060 nm. The detection was achieved by contrast imaging with a Cognex In-Sight vision system and using a Monster LED light system with a wavelength of 850 nm. A Midwest optical filter 850 bandpass was used to isolate the absorption.
[0046] While the present invention has been described and illustrated by reference to particular forms, those of ordinary skill in the art will appreciate that the invention lends itself to variations not necessarily illustrated herein. For this reason, then, reference should be made solely to the appended claims for purposes of determining the true scope of the present invention.
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A process for detecting oil or lubricant contamination in the production of an article by adding a Stokes-shifting taggant to an oil or lubricant of a machine utilized to produce the article or a component thereof, irradiating the articles produced with a first wavelength of radiation, and monitoring the articles for emission of radiation at a second wavelength. The taggant can be in the form of a composition containing a Stokes-shifting taggant, which absorbs radiation at a first wavelength and emits radiation at a second wavelength, different from said first wavelength, dissolved or dispersed in an oil or lubricant.
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SPECIFIC DATA RELATED TO INVENTION
[0001] This application claims the benefit of U.S. Provisional Patent Application No. 60/450,049 filed Feb. 27, 2003, and U.S. Provisional Patent Application No. 60/417,413 filed Oct. 10, 2002, incorporated herein by reference.
FIELD OF INVENTION
[0002] This application relates generally to optical signal processing, and more particularly, to polarization control devices.
SUMMARY DESCRIPTION OF THE INVENTION
[0003] Electronically agile optical filtering modules are used for manipulating optical and electrical signals. The modules use optical polarization rotation devices that may include acousto-optic tunable filter (AOTF) devices, liquid crystal devices, and magneto-optic devices. The AOTF acts as a wavelength sensitive polarization rotation element where diffracted and undiffracted beam optical wavelength, power levels, and polarization state are controlled by selection of bulk AOTF device radio frequency (RF) drive power and frequency position. Although such devices may be subject to polarization dispersion losses (PDL) and polarization mode dispersion (PMD) that may be different for when light travel along different light paths through the device, redirecting light beams back along a different bi-directional path through the device, PDL and PMD, such as may be induced in polarization control devices having non-uniform performance across orthogonal polarizations, may be reduced.
DESCRIPTION OF THE DRAWINGS
[0004] [0004]FIG. 1 shows a Prior Art pair of Self-Imaging Fiber Grin Lenses.
[0005] [0005]FIG. 2A shows a top view of a filtering system wherein the optical beams from a beam displacement prism (BDP) are horizontally displaced.
[0006] [0006]FIG. 2B shows a Side View of the system of FIG. 2A where the optical beams from the BDP are vertically displaced.
[0007] [0007]FIG. 3A shows a top view of a filtering system wherein the optical beams from a beam displacement prism (BDP) are horizontally displaced.
[0008] [0008]FIG. 3B shows a Side View of the system of FIG. 3A where the optical beams from the BDP are vertically displaced.
[0009] [0009]FIG. 4A shows a Top View of Liquid Crystal (LC) Variable Optical Attenuator (VOA) using a total internal reflection prism.
[0010] [0010]FIG. 4A shows a Side View of a Liquid Crystal (LC) Variable Optical Attenuator (VOA) using a lens and mirror combination.
[0011] [0011]FIG. 5A shows a Polarization Independent Notch filter.
[0012] [0012]FIG. 5A shows a Polarization Independent Drop filter.
[0013] [0013]FIG. 6A shows a Reconfigurable Add-Drop Filter.
[0014] [0014]FIG. 6B shows a Polarization Independent Band Pass filter.
DETAILED DESCRIPTION OF THE INVENTION
[0015] A module for reducing PDL and PMD may include a self-aligning optical loop using optical components, such as a beam splitter, or beam displacing polarizer, a circulator, a total internal reflection prism (retro-reflective) or a lens-mirror combination, and a half-wave plate (HWP). Accordingly, for a polarization device that may perform non-uniformly for orthogonal polarizations, the overall polarization dependent loss and polarization-mode dispersion of the structure may be reduced or eliminated. Such a module may be used, for instance, in applications in WDM networks, microwave signal processing, and array radar controls wherein optical or electrical signal filtering is required. In another aspect of the invention, the retro-reflective prism or the mirror-lens combination may be replaced with a mirror and a path length compensator (PLC) to provide PLD compensation when the active device has a polarization balanced performance for both beams passing through the active device, such as an AOTF.
[0016] [0016]FIG. 1 illustrates a pair of self-imaging fiber grin lenses 10 , 12 characterized by a working distance 14 . FIGS. 2, 3, 5 , and 6 illustrate polarization rotation devices using a collinear geometry bulk acousto-optic tunable filter (AOTF) device that operates, for example, on horizontal or p-polarized input light, giving high diffraction at a given wavelength for a given RF drive frequency. For example, the input p-light is deflected and diffracted into an output s-, or vertical, light. However, when using an AOTF device, at the two different physical locations of the two beam light interaction in the AOTF, it is possible to have different polarization performance, i.e, different diffraction efficiencies for the beams. This leads to large (e.g., >1 dB) PDL in the filter. The innovative loop structure described herein reduces this PDL and also reduces PMD, or relative time delay, between the two beams originally separated, for example, by the BDP at the input to the filter.
[0017] FIGS. 2 - 6 show optical beam directions and polarizations for the illustrated embodiments. Important aspects of the illustrated embodiments include (a) use of circulator in loop geometry (b) Use of HWP (or Faraday rotator) with BDP, and (c) use of TIR prism or lens/mirror to cause light looping. Note that using AOTF's with multiple RF frequencies, complex optical and electrical signal processing can be performed using wavelength sensitive manipulations of the optical carrier as they pass through the proposed modules. Finally note that non-collinear AOTF devices plus other polarization control devices (rotation or diffraction based) can also be used in the proposed architectures with minor optical path modifications. The self-imaging technique shown in FIG. 1 may be used to reduce structure loss in the modules (see, for example, Martin van Buren and N. A. Riza, “Foundations for low loss fiber gradient-index lens pair coupling with the self-imaging mechanism,” Applied Optics, LP, Vo.42, No.3, Jan. 20, 2003).
[0018] [0018]FIG. 2A shows a top view of a filtering system 16 wherein the optical beams from the BDP are horizontally displaced along respective light paths 18 , 20 . The system 16 includes a beam displacement prism (BDP) 22 with a half wave plate (HWP) 24 placed in at least one light path between the AOTF 28 and the BDP 22 . A total internal reflection prism (TIR) reflects light back through the AOTF 28 . The filter may include blocks 30 , 32 for blocking diffracted light. A circulator 34 may be provided with SMF connections to direct an input beam through a grin lens L to the AOTF 28 and redirect a filtered beam received from the AOTF 28 . FIG. 2B shows a side view of a filtering system of FIG. 2A wherein the optical beams from the BDP 22 are vertically displaced.
[0019] [0019]FIG. 3A shows a top view of a filtering system 42 wherein the optical beams from the BDP 22 are horizontally displaced. The embodiment depicted in FIG. 3A employs a lens 40 and mirror 38 arrangement instead of the TIR prism 26 of FIG. 2A. The lens, S, may be positioned a focal length, f, from the mirror 38 and a focal length, f, from a diffraction point within the AOTF 28 . FIG. 3B shows a side view of the filtering system 42 of FIG. 3A wherein the optical beams from the BDP 22 are vertically displaced.
[0020] [0020]FIG. 4A shows a top view of Liquid Crystal (LC) Variable Optical Attenuator (VOA) 44 . The system includes a BDP 22 with a HWP 24 placed in at least one light path 18 , 20 between the TIR 26 and the BDP 22 . A LC 46 may be placed in at least one light path 18 , 20 , such as a different light path 18 , 20 than the light path 18 , 20 in which HWP 24 is placed, to perform a desired attenuation function. The TIR 26 reflects light back along light paths 18 , 20 different from the light path 18 , 20 from which light arrived at the TIR 26 . A circulator 34 may be provided with SMF connections to direct an input beam through a grin lens L and redirect an attenuated beam received from the grin lens L. FIG. 4B shows a top view of the VOA 44 of FIG. 4B wherein the TIR 26 is replaced with mirror 38 and lens 40 arrangement.
[0021] [0021]FIGS. 5 and 6 show alternate embodiments of the invention when an active device, such as the AOTF, has minimal PDL, but may still require PMD compensation. The preferred embodiment using the loop geometry with a prism or the mirror plus lens combination can be used within these alternate embodiments (instead of mirror plus PLC) to eliminate PDL along with PMD if needed. FIGS. 5 and 6 show optical beam directions and polarizations for the illustrated embodiments. Important aspects of the illustrated embodiments include (a) use of circulators in retroreflective geometry off either the undiffracted (or DC beam) or the diffracted (+1 and/or −1) order beam, (b) Use of PBSs, HWPS, Spatial filters, and polarizers to route and clean beams, (c) Use of two diffractions via an AOTF to improve filter wavelength characteristics. Also note that because freespace beams are used, special spatial filters (e.g., on-axis pin hole) can be placed throughout the beam paths to eliminate spatial/wavelength noise; this is a unique feature of the proposed freespace-type bulk-AOTF module based designs.
[0022] [0022]FIG. 5A is a polarization independent notch filter 48 including an AOTF 28 controllable by an RF signal 29 . The filter 48 includes a BDP 22 with an HWP 24 placed in at least one light path between the AOTF 28 and the BDP 22 . A mirror 38 reflects light back through the AOTF 28 and may include a path length compensator (PLC) 50 placed in at least one light path between the AOTF 28 and the BDP 22 . The filter 48 may include blocks 30 , 32 for blocking diffracted light. A circulator 34 may be provided with SMF connections to direct an input beam to the AOTF 28 and redirect a filtered beam received from the AOTF 28 . A fiber lens (FL) 27 may be provided to direct light propagating in an SMF into freespace.
[0023] [0023]FIG. 5B is a drop filter 56 including an AOTF 28 controllable by an RF signal 29 . The filter 56 includes a BDP 22 with a HWP 24 placed in at least one light path 18 , 20 between the AOTF 28 and the BDP 22 . A mirror 38 reflects light back through the AOTF 28 and may include PLC 50 placed in at least one light path 18 , 20 between the AOTF 28 and the BDP 22 . The filter 56 may include block 32 for blocking diffracted light. A circulator 34 may be provided with SMF connections to direct an input beam to the AOTF 28 and redirect a filtered beam received from the AOTF 28 . A FL 27 may be provided to direct light propagating in an SMF into freespace. In an aspect of the invention, a second BDP 52 with an HWP 54 placed in at least one diffracted light path 19 , 21 between the AOTF 28 and the BDP 28 may be provided to drop a portion of the light beam. With the addition of a circulator 60 the drop filter 56 of FIG. 5B may be used as reconfigurable Add-Drop filter 58 as shown in FIG. 6A.
[0024] [0024]FIG. 6B depicts a polarization independent band pass filter 62 , for example, configured by reflecting, with mirror 38 , a diffracted light portion 23 and blocking, with block 30 , a non-diffracted light portion 25 from the AOTF 28 . A PLC 50 may be placed in at least one diffracted light path 19 , 21 between the AOTF 28 and the mirror 38 .
[0025] The embodiment depicted in FIG. 5B (the drop filter 56 ) may be used as scanning optical spectrum analyzers or variable tap filters. In this case, to make a spectrum analyzer, the drop port out fiber 51 and BDP 52 can be replaced with a large area detector that measures the power in the chosen wavelength, adding the powers for the two diffracted polarizations. Since the detector measures this power for a given wavelength at a given RF drive frequency, the RF can be swept to take power readings across the entire input light wavelength band. Generally, the AOTF drive power is kept low to tap only say 5% of the light from the input main beam. This way, smooth interruption free monitoring of the optical WDM signal is maintained. In the case the structures is used as a tap filter, in this case the output fiber 51 and BDP 52 at the output drop port are retained and again the AOTF 28 is weakly driven to tap the correct wavelength or wavelengths with their correct moderate to low power levels. Finally note that non-collinear AOTF devices can also be used in the proposed architectures with minor optical path modifications.
[0026] While the preferred embodiments of the present invention have been shown and described herein, it will be obvious that such embodiments are provided by way of example only. Numerous variations, changes and substitutions will occur to those of skill in the art without departing from the invention herein. Accordingly, it is intended that the invention be limited only by the spirit and scope of the appended claims.
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Electronically agile optical filtering modules for equalizing light propagation differences in at least two spaced optical beam pathways in the modules. The modules use optical polarization rotation devices that may include acousto-optic tunable filter (AOTF) devices, liquid crystal devices, and magneto-optic devices. Such devices may be subject to polarization dispersion losses (PDL) and polarization mode dispersion (PMD) that may be different for when light travel along different light paths through the device. By redirecting light beams back along a different bi-directional path through the devices which may exhibit non-uniform performance across orthogonal polarizations, PDL and PMD may be reduced.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from U.S. Provisional Application Ser. No. 60/723,065 filed Oct. 1, 2005, and from U.S. Provisional Application Ser. No. 60/636,256 filed Dec. 14, 2004, and from U.S. Provisional Application Ser. No. ______ (not yet allotted), filed Oct. 24, 2005.
FIELD OF INVENTION
[0002] This invention concerns pumps and, more specifically, is directed to a programmable actuator pump system for moving a fluid at a determined rate and in a determined flow path.
BACKGROUND
[0003] Many kinds of pumps are known in the art and adaptations have been made for specific applications. Pumps for moving fluids are powered by motors that drive moving components, usually pistons and valves, to produce a force on a fluid that causes it to flow. Valves in such pump systems are generally activated by electromechanical devices such as solenoids and other mechanical components. As one of skill in the art will appreciate, there are countless versions of pumps for many different applications. In the medical device field, e.g., there are peristaltic pumps, diaphragm pumps and centrifuge pumps for delivering blood and other biological fluids for specific purposes. Pumps used in many of today's modern chemical processes, including oil or petroleum refining, food and drug manufacturing and electric generation, rely extensively on a complex interconnection of pumps, piping and valves to effect a particular chemical conversion or mixture. The reliance on multiple dedicated pumps or redundant valve configurations results in complex, expensive systems that require high maintenance and manufacturing costs.
[0004] Polymer actuators, requiring no moving parts, are often used in these complex systems to simplify valve operation. A class of actuators, electroactive polymers (EAP—known as artificial muscles), has recently been developed. See, e.g., “Electroactive Polymer (EAP) Activators as an Artificial Muscles” Yoseph ar-Cohen Ed., Society of Photo-Optical Instrumentation Engineers, Publisher (2001). Electroactived polymers reversibly swell or change form when activated. The mechanical force exerted by activated EAP is captured to move components in actuator devices.
[0005] U.S. Pat. No. 6,664,718 describes monolithic electroactive polymers that act as transducers and convert electrical energy to mechanical energy. The EAP are used to generate mechanical forces to move components of robots or pumps.
[0006] U.S. Pat. No. 6,682,500 describes a diaphragm pump powered by EAP. In this pump, an EAP is positioned beneath a flexible membrane termed a “diaphragm”. As the EAP is activated, it swells and contracts and thereby reversibly moves the diaphragm which in turn displaces liquid in which it is in contact. The diaphragm pump uses check-flow valves to control liquid flow.
[0007] U.S. Pat. No. 6,685,442 discloses a valve actuator based on a conductive elastomeric polymer gel. In operation, the conductive gel polymer is activated by an electrolyte solution. By manipulating the potential across the gel, the motion of an elastomeric membrane over the expanding gel and the electrolyte solution can be controlled to act as a “gate” to open or close a fluid channel as a check-valve for that channel.
[0008] The use of actuators in pump systems reduces the complexity of system operation. Yet each of the disclosed pumps that incorporate polymeric actuators still requires moving parts and valves. The mechanical complexity, maintenance expense, large size and weight, sterility problems, fluid-contaminating erosion products, chemical incompatibility with certain fluids and often noisy operation, make most pump systems unsuitable for certain purposes.
[0009] The foregoing background discussion derives from my published PCT application PCT/US2004/005922 which is incorporated in its entirety, by reference, in which I describe an actuator pumping system that utilizes the force of expanding or deflecting actuators inside a housing of fixed volume to displace liquid through the housing. No moving parts or valves are required. The timed activation of individual actuators causes the actuators to change dimensions at a determined time and sequence and thereby cause the fluid to flow at a certain time and path. More particularly, as described in my aforesaid PCT application, a pump system for moving a fluid comprises an actuator housing having a chamber for housing the fluid, a plurality of contiguous actuators located in the chamber, and activating means for sequentially activating individual actuators. Each actuator, when activated, changes dimensions and exerts a displacing force on the housed fluid.
[0010] In preferred embodiments of the invention of my aforesaid PCT application, the actuator housing comprises two or more chambers in fluid connection. In certain instances, the separate chambers may be programmed to displace different segments of fluid at individualized rates and flow paths. The separate chambers may, e.g., be used to modify flow rates of fluids that change viscosity while moving through the housing. In other instances, coordination of flow rate through the separate chambers may be used to subdue any pulsing flow patterns from individual chambers into a smooth continuous fluid flow pattern downstream from the chambers.
[0011] The pump may comprise a means for controlling the actuator activating means whereby individual actuators are activated at a determined time. The controller in preferred embodiments is a programmable microprocessor in electrical connection with the activating means. Also, in certain instances, the pump may comprise a sensor means for determining physical properties of the fluid. The sensor is in electrical connection with the controlling means and provides feed-back about the physical state of the fluid to the controlling means. The sensor may, for example, measure changes in pH, viscosity, ionic strength, velocity, pressure or chemical composition of fluid. This feed-back allows the pump to interactively alter fluid flow rate and direction.
[0012] In preferred embodiments of the invention of my aforesaid PCT application, the pump moves a fluid at a controlled rate. In these embodiments, the activating means sequentially activates individual contiguous actuators at a selected time. The rate at which the fluid flows depends on the rate of actuator activation and volume displaced by each actuator. Thus, in certain preferred instances, the individual actuators are repeatedly pulsed sequentially at rapid intervals, and liquid is essentially spurted from the housing. In other instances, a first group of contiguous actuators is activated at a certain time and then, while the first group return to their original dimensions, a second group of contiguous actuators is sequentially activated. Repetition of this activation pattern for several times or with more groups of actuators along the fluid flow path causes a volume of fluid to be displaced and eventually to be ejected from the housing. The amount of fluid displaced in a given time is determined by the difference in volume between activated actuators restored activators.
[0013] As taught in my aforesaid PCT application, the chamber in the actuator housing should be sufficiently rigid to prevent it being deformed by the force exerted by activated actuators, since the displacing force of the activated actuators requires the chamber to maintain an essentially constant volume. In certain instances, however, as when the pump is to be placed into a small cavity, the actuator housing may be slightly deformable while being inserted.
[0014] Other activated pump systems described in the art include Harting in U.S. Pat. No. 6,955,923, who describes a device and method for investigating the flowability of a physiological fluid sample. This claims a device that measures various components of the blood through a pump that comprises an uptake passage for the fluid sample, an actuator device for providing cyclic change in orientation of measuring particles in the fluid sample, and a detector device for detecting the change in orientation of the measuring particles. This device also describes the movement of the fluid through the actuator in a back and forth motion. Systems for moving fluid and measuring components of the blood can be combined with molecule delivery systems within the pumping device. Westberg and Vishnoi described blood processes systems and methods using an actuated and programmable in U.S. Pat. No. 6,949,079 describes a pump system where blood is analyzed and a control and analysis system can make various programmed responses in relation to the blood components. Wilson describes an injection pump and combinatorial reactor method in U.S. Pat. No. 6,902,704 where a pathway in a plurality of injectors move to ingest, store, and discharge fluid. Multifaceted actuators will aid in the flexibility and dynamics of such pumping devices because of their varying physical properties can be manipulated to achieve a wide range of applications.
[0015] Most actuator systems described in the prior art comprise Electro Active Polymers (EAPs). Electricity can be used as an activating method for causing the material composing the actuator housing to change shape. The completion of an electrical circuit causes delivery of electrons to the shape changing material, which makes the actuator housing unit move. Once electrically activated, the material will also expand and exert force on the matter being moved through the actuator housing or will contract, relax, and relieve force or pressure from the matter and will keep it in the actuator housing.
[0016] Many actuator pumps and devices have described the use of EAPs in their composition. Pelrine, Kornbluh, and Pei described a system of electrocute polymers transducers and actuators in U.S. Pat. No. 6,940,211. The actuator system described a system composed of EAPs where one transducer moved a fluid in one direction as part of a pumping system that might be composed of many transducers. Urano and Kitahara described an EAP actuator and diaphragm pump in U.S. Pat. No. 6,960,864 where a pump is composed of several EAP tubular layers that are connected by a continuity of peripheral surfaces. Pelrine and Kornbluh used master and slave EAPs in U.S. Pat. No. 6,876,135 for a device that converts electrical to mechanical energy, where the device is composed one or two active areas.
[0017] Calvert and Liu described the “Freeform Fabrication of Hydrogels” in Acta Materialia (1998), where new kinds of hydrogels that contains multiple layers are able to exhibit multiple properties that will aid in the development of EAP actuators. They outlined a process in which novel hydrogels combine the usage of their structure to obtain certain functionalities with both chemical and thermal materials. They also described “Multilayer Hydrogels as Muscle-like Actuators” in the Journal Advanced Materials (2000) where An actuator was constructed using a combination of cross-linked polyacrylic acid and polyacrylamide hydrogels. The advantage of this particular stacking of polymers resulted in a linear rather than bent motion, which allowed control of water flow through the chamber.
[0018] Chemical methods can be used to activate the autonomous pumping and processing actuator system. The material that composes the actuator housing system changes shape upon activation involving a chemical reaction. Processing, mixing, and other reactions and chemical synthesis methods can be accomplished with the addition of heating or cooling elements, allowing temperature sensitive processes and chemical reactions to actuator housing systems. The housing actuator systems can also be used in combination with catalysts and other materials such as oxides or metals to obtain specifically desired chemical results.
[0019] Light and other photoactive elements may also be used as the activating method. Using one or more different wavelengths can produce photochemical reactions and processes. This lighted method of activation also causes a physical change in the material composing the actuator housing. These and additional energy sources may also be utilized together to generate the desired chemical or biological reactions and chemistry coupled with sensors to allow process and reaction control feedback and autonomous abilities to the system.
[0020] A specific example of an actuator composed of a light activated substance would be an epoxy based formulation of a water soluble amine such as Jeffamine and Poly Ethylene Glycol or EGDE in aqueous solution, by adding a light emitting dopant, dye or photo initiator such as Methylene Blue. The initial aqueous solution in the dye is suspended or polymerized into the epoxy. After the curing process is complete, the polymer is hydrated and swollen with aqueous solution and photo irradiation of the material, which creates a pH change within the hydrated polymer to acid. The acids swell the amines further, and the amount of swelling is tunable by changing ratios and concentrations of the epoxy components and the dye. When the irradiation is stopped, the reaction stops and the polymer relaxes back to its neutral hydrated state, thereby creating an effective photo switch mechanism for a polymer actuator.
[0021] To further refine or reverse the switching mechanism a chelator or quenching molecule can be used to reverse or rebalance the polymer at a different wavelength of light. An example of this is the use of Titanium Dioxide in the polymer to oxidize the aqueous solution, and when irradiated it produces oxygen, which can then quench the fluorescence of a dye such as a Tris (4,7-diphenyl-1,10-phenanthroline)ruthenium(II) bis(hexafluorophosphate) complex. There are many additional chemicals and compound molecules that can be used for the switching process such as functionalized dendrimers with amino or other surface groups, chemiluminescent dyes, laser dyes, photochromic dyes, phthalocyanines, porphyrins, fluoropolymers and monomers. This method is also applicable to changing the polymer ions selectivity, allowing the control of the polymers hydrophilic and hydrophobic properties in order to control the polymer swelling.
[0022] The various forms of energizing may be visible and non visible light, electrical, chemical, photochemical, electromagnetic, electrochemical, radiation, radio frequency, ultrasonic, temperature can be used in combination to allow various combinations of simultaneous functions. These functions include actuation, chemistry, application, sensing and feed back control, and processing. This allows programmed or autonomous sensing for the alteration or processing of matter in or through the system. Additional non-activated materials such as non activated hydro gels may also be encapsulated in the actuator and may perform functions or store biological fluids, chemical molecules, or cells.
SUMMARY OF THE INVENTION
[0023] The present invention is able to conduct sequential isolation, testing, and introduction of a droplet or portion of a chemical or biological fluid being passed through an actuator system, wherein one or more actuators performing different processes or reactions work in conjunction as a whole system, such as an artificial organ, an autonomous fluid processor or bio reactor to produce antibodies or cellular proliferation.
[0024] More particularly, the present invention provides many potential and possible variations of an actuator pump system. Such variations are regarded as the major benefit of this invention, where a combination of differentially activated materials can be used in various ways to move matter through the actuator housing by the transfer of momentum from the activated and shape changing substance to the matter moving through the housing. Alternatively, the momentum transfer between the actuated material and matter can be removed to keep the matter within the housing unit.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Further features and advantages of the present invention will be seen from the following description taken in conjunction with the accompanying drawings, wherein:
[0026] FIG. 1 is a perspective view of an array pump made in accordance with the present invention;
[0027] FIGS. 2 and 3 are cross-sectional views showing an individual pump chamber at the various stages of activations; and
[0028] FIG. 4 diagrammatically illustrates a multi-function activator and pump system made in accordance with the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0029] The system actuators of the present invention can be constructed to perform multiple functions by combining energy sources or frequencies that start, maintain and end various processes and reactions within the actuator and additionally stimulate a physical or chemical phase change at the same time.
[0030] Referring to the drawings, an actuator array pump in accordance with the present invention, when sequentially activated can move materials through connecting chambers ( 2 ) with openings ( 3 ) or ports allowing fluid connection and closing of fluid connection to predetermined locations of array. The method of activation can be electrical, hydraulic, magnetic, electromagnetic, hydrostatic, electrostatic, chemical, thermal, compressed air/gas or other mechanical actuation methods.
[0031] The pump includes an array housing ( 4 ) which holds and aligns actuators ( 6 ) that have contact with or are attached to a reversibly deformable member ( 5 ) (See FIG. 2 ). When activated the actuator moves or applies pressure to the reversibly deformable member which in turn comes in contact with the opposing housing wall ( 7 ). The deformable member upon contact with the chamber wall distorts ( FIG. 3 ) so that as it compresses in one or more directions it distorts or expands in other directions and forces the material in the chamber through the port openings until it compresses/deforms and displaces to the point of closing or blocking the chamber port.
[0032] The deformable members may be manufactured in a sheet form to match the array, such as an elastomeric flexible gasket type material such as Nylon, Teflon, rubber, polymer composites, etc. then assembled in between the top ( 1 ) (chamber) and bottom ( 4 ) (actuator housing) of the pump. In other embodiments deformable member may be individually attached, formed, molded to the housing or to the actuator or to the opposing wall of the chamber. The single or multiple deformable members may be solid, hollow or filled with a gas, liquid, gel or viscous material to allow for the properties and efficient locomotion of the material being processed/pumped.
[0033] Further processing and reaction or chemical synthesis can be accomplished with the addition of heating or cooling elements to allow for temperature sensitive processes and chemical reactions.
[0034] Light may also be used as the activating and/or by using one or more different wavelengths can produce photochemical reactions and processes in the pump chamber or actuators or both. These and additional energy sources may also be utilized together to generate the desired chemical or biological reactions and chemistry coupled with sensors to allow process and reaction control feedback and autonomous abilities to the system.
[0035] The system actuators can be construed to perform multiple functions by combining energy sources or frequencies that start, maintain and end various processes and reactions within the actuator and additionally stimulate a physical or chemical phase change at the same time. An example of one possible actuator is an Electro Activated Polymer gel that swells when electrically charged. This gel can be encapsulated on at least one side or surface with a membrane that can also be altered upon application of energy to allow flow of a certain size molecule. The swelling is caused by absorption of a liquid, electrolyte or biological fluid into the gel. Using a light source to create a photo chemical change between the absorbed solution and chemicals or molecules suspended in the gel. The light wavelength can then be changed to create another reaction to the membrane that allows the altered chemical fluid or molecule to travel through the membrane when the electric current to the actuator is altered or stopped. Another example is the actuator could store a medication in concentration and release diluted portions at predetermined rates or in reaction to a test of another fluid.
[0036] The various forms of energizing may be visible and non visible light, electrical, chemical, photochemical, electromagnetic, radiation, temperature etc. and can be combined in various combinations to allow simultaneous functions to be performed such as actuation, chemistry, application, sensing and feed back to the controller of the processor to allow for programmed or autonomous sensing and altering or processing in or through the system.
[0037] This system would be able to conduct sequential isolation, testing, and introduction of a droplet or portion of a chemical or biological fluid being passed through the system. It is envisioned that one or more actuators performing different processes or reactions would work in conjunction as a whole system, such as an artificial organ, an autonomous fluid processor or bio reactor to produce antibodies or other cellular growth.
[0038] Referring to FIG. 4 there is illustrated a preferred example of actuator made in accordance with the present invention, comprises a photo activated polymer gel 10 that swells when irradiated 15 from a light source 12 such as an LED. The light is transmitted to the gel from the light sources via fiber optic 16 cable or light channel. This gel can be encapsulated on at least one side or surface with a membrane 13 that can also be altered upon application of energy or irradiation to allow flow of a certain size molecule. The swelling is caused by absorption of an aqueous solution 14 , liquid, electrolyte or biological fluid into the gel, using a light source of different wavelength 17 to create a photo chemical change 18 between the absorbed solution and chemicals or molecules suspended in the gel. The light wavelength can then be changed to create another reaction to the membrane that allows the altered chemical fluid or molecule to travel through the membrane when photo irradiation to the actuator is altered or stopped. Alternatively, the actuator could store a medication in concentration and release diluted portions at predetermined rates or in reaction to a test of another fluid.
[0039] Methods which use various, activated materials, arranged in order to obtain linear motion through the properties of a polymer actuator system, can be used for a number of different purposes. The present invention provides a system which incorporates different routes of activation, in which the material responds dependently to an applied stimulus. A segmental means of various activated surfaces combines to form a system in which mechanical energy is transferred in variously activated means to control the flow of matter through the actuator housing system.
[0040] The system impedes or permits fluid within a chamber via an autonomous system that drives the activation of the material that results in the matter being expelled or retained within the actuator housing. Subsequent activation of adjacent materials is carried out by the ability of different material activation by different methods. Combinations of activated and non-activated materials can be used in the actuator housing system. A myriad of activated and non-activated materials work in concert to form a particularly desired system of movement of the matter inside of the actuator housing unit system. Thus, the system minimizes the use of materials that compose mechanically moving parts, which reduces manufacturing costs.
[0041] In one aspect, the present invention provides a design of an actuator device that utilizes the unique properties of specifically responsive materials. A physical force is obtained by the interaction of connecting two or more chambers, allowing alternate sources of activation or stimulation to occur by incorporating different energy sources that will change the morphology of the actuator housing. The actuator housing, where the matter is pushed through or retained, consists of a well that is capable of retaining fluid and capable of altering the chemical or other physical properties of any adjacent material. By inducing alternate means of activation or stimulation such as a photo, electrical, and chemical induction within the well, transferred and altered matter travels down the polymer pathway in a manner that is predetermined by the autonomous system and performed by the mechanical properties that the activated materials possess.
[0042] Chemical, electrical, and light activations or stimulations are used throughout the actuator housing system in order to achieve the preferred movement or containment of matter through the system. These alternative energy sources form a system that is scaleable for a wide range of uses. The delivery or retention of matter by isolating specific materials entrapped within the system and being able to further manipulate its structure by the introduction of various activations or stimulations allows the system to be quite versatile.
[0043] The actuator systems of the present invention can be constructed to perform multiple functions by integrating a coordinate pathway that adheres to directional flow of cardinal directions left, right, up and down. This process is mediated by combining energy sources that start and maintain processes of the characteristics of the materials that will cause reactions within the actuator well, and additionally stimulate a physical or chemical change at the same time within the an adjacent material.
[0044] The movement of the material facilitates displacement of fluid between neighboring chambers permitting a multi-flow pathway that is caused by the material reacting to a stimulus that can be interchanged to allow increasing flow control flexibility of the system. Proper material arrangement and placement within the system is dependent on the manner in which it may be activated, allowing adjacent wells to directly alter the flow of matter by other surrounding wells, such that the chambers are exchanging chemical information with each other through the addition of sequential energy sources.
[0045] As will be appreciated from the foregoing description, the polymer and mechanical actuator systems of the present invention allows programmable and autonomous pumping/processing in single or multiple paths and axis's. This includes designed and non designed options available based upon system needs and feedback from sensors such as pressure, composition, temperature, particle size or other sensing needs to process, test and evaluate material being processed, pumped or moved. The system is scaleable for a wide range of uses and industries. Further system options include modular stackability to allow for increased flexibility of system use.
[0046] Various other changes may be made in the foregoing without departing from the spirit and scope of the current invention.
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An actuator housing unit for a system of layered surfaces, comprising an activated primary surface having a physical shape capable of change when activated by an electrical, chemical, or light stimulus, to expand and exert force or pressure or contract and remove force or pressure, upon activation or deactivation, to move or keep matter within the housing by direct or indirect contact.
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FIELD
[0001] The present invention relates generally to a pinion shaft and bearing assembly, and more particularly to a pinion shaft and bearing assembly using an adhesive for improved bearing location and retention of an inner race of a rolling element bearing.
BACKGROUND
[0002] The statements in this section merely provide background information related to the present disclosure and may or may not constitute prior art.
[0003] A typical pinion shaft and bearing assembly uses various mechanisms to maintain sufficient friction between the pinion shaft and the bearing to prevent the bearing from spinning free from or walking off the pinion shaft. These mechanisms include various mechanical methods of coupling the bearing to the pinion shaft such as, for example, press-fitting the bearing to the pinion shaft. The effectiveness of these mechanisms may be enhanced by the addition of an anaerobic adhesive between the pinion shaft and the bearing.
[0004] Typically, the anaerobic adhesive is applied to the pinion shaft or bearing prior to assembly and is cured in situ. The adhesive fits within gaps formed on the surfaces due to surface roughness. In general applications the cure time for the anaerobic adhesive is a function of the gap between the pinion shaft and the bearing. The cure times are shorter when the anaerobic adhesive is applied to a smaller gap. Also, the relationship between retention strength of the adhesive and surface roughness is integral in the robustness of the assembly where the rougher the surface finish the higher the retention strength achieved.
[0005] However, the location accuracy (i.e., the radial and axial position) of the bearing on the pinion shaft improves when tight dimensional controls are employed. One result of tight dimensional controls is smooth surface finish. In balancing the needs for tight location accuracy and high bearing retention strength, location accuracy is typically favored. Alternative solutions for preventing bearing spin or walk while maintaining location accuracy include integrated bearing sleeves or mechanical retention of the bearing. However, these alternative solutions may increase cost and may not be practical due to packaging restraints. Accordingly, there is a need in the art for a pinion shaft and bearing assembly that increases the effectiveness of anaerobic adhesives without increasing cure time and without decreasing locational accuracy.
SUMMARY
[0006] A pinion shaft and bearing combination is provided including a pinion shaft with at least two outer regions each having a different surface finish and a pinion bearing with at least two inner regions each having a different surface finish.
[0007] An embodiment of a pinion shaft and bearing combination is provided having a pinion shaft having a first outer region with a first surface treatment and a second outer region with a second surface treatment. A pinion bearing is disposed on the pinion shaft with the pinion bearing having a first inner region with a third surface treatment and a second inner region with a fourth surface treatment. An adhesive is applied to one or both of the second outer region and the second inner region. The first surface treatment and the third surface treatment cooperate to locate the pinion bearing on the pinion shaft and the second surface treatment and the fourth surface treatment cooperate to improve a performance of the adhesive.
[0008] In another embodiment of the present invention, the pinion shaft defines a longitudinal axis and includes a first pinion end and a second pinion end disposed opposite the first pinion end along the longitudinal axis.
[0009] In yet another embodiment of the present invention, the first outer region is located on an outer surface of the pinion shaft and extends from the first pinion end a first distance along the longitudinal axis.
[0010] In yet another embodiment of the present invention, the second outer region is located on the outer surface of the pinion shaft and extends from the first outer region a second distance along the longitudinal axis.
[0011] In yet another embodiment of the present invention, the pinion shaft includes a third outer region on the outer surface of the pinion shaft, the third outer region having the first surface treatment and extending from the second outer region a third distance along the longitudinal axis to the second pinion end.
[0012] In yet another embodiment of the present invention, the first distance is approximately equal to the third distance, and the second distance is greater than the first and third distances.
[0013] In yet another embodiment of the present invention, the pinion bearing is concentric with the pinion shaft and includes a first bearing end and a second bearing end disposed opposite the first bearing end along the longitudinal axis.
[0014] In yet another embodiment of the present invention, the first inner region is located on an inner surface of the pinion bearing and extends from the first bearing end a fourth distance along the longitudinal axis.
[0015] In yet another embodiment of the present invention, the second inner region is located on the inner surface of the pinion bearing and extends from the first inner region a fifth distance along the longitudinal axis.
[0016] In yet another embodiment of the present invention, the pinion bearing includes a third inner region on the inner surface of the pinion bearing, the third inner region having the third surface treatment and extending from the second inner region a sixth distance along the longitudinal axis to the second bearing end.
[0017] In yet another embodiment of the present invention, the fourth distance is approximately equal to the sixth distance, and the fifth distance is greater than the fourth and sixth distances.
[0018] In yet another embodiment of the present invention, the first and third surface treatments result in a surface finish from about 0.10 to about 0.35 μm Ra.
[0019] In yet another embodiment of the present invention, the second and fourth surface treatments result in a surface having a plurality of indentations about 0.025 mm deep and have a surface finish of about 1.0 to about 3.2 μm Ra.
[0020] In yet another embodiment of the present invention, the first inner region of the pinion bearing is disposed opposing the first outer region of the pinion shaft and the second inner region of the pinion bearing is disposed opposing the second outer region of the pinion shaft.
[0021] In yet another embodiment of the present invention, the first inner region is press fit to the first outer region.
[0022] In yet another embodiment of the present invention, the second surface treatment of the second outer region and the second surface treatment of the second inner region cooperate to define a plurality of gaps between the pinion bearing and the pinion shaft.
[0023] In yet another embodiment of the present invention, the adhesive is disposed within the gaps.
[0024] In yet another embodiment of the present invention, the gaps are comprised of at least one of continuous elongated divots, round pockets, diamond pockets, and square pockets.
[0025] In yet another embodiment of the present invention, the gaps are continuous channels.
[0026] Further objects, aspects and advantages of the present invention will become apparent by reference to the following description and appended drawings wherein like reference numbers refer to the same component, element or feature.
DRAWINGS
[0027] The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way.
[0028] FIG. 1 is a side view of a gear and shaft assembly including an embodiment of a pinion shaft and bearing assembly according to the principles of the present invention;
[0029] FIG. 2 is a side view of an embodiment of a pinion according to the principles of the present invention;
[0030] FIG. 3 is a cross-sectional view of an embodiment of a bearing according to the principles of the present invention;
[0031] FIG. 4 is a cross-sectional view of an embodiment of a bearing installed on a pinion according to the principles of the present invention;
[0032] FIG. 5 is an enlarged cross-sectional view of an embodiment of a bearing installed on a pinion detailing the surface finishes;
[0033] FIG. 6 is a magnified view of an exemplary surface structure showing a continuous feature;
[0034] FIG. 7 is a magnified view of an exemplary surface structure showing a pocket surface structure; and
[0035] FIG. 8 is a further magnified view of an exemplary surface structure showing another pocket surface structure.
DETAILED DESCRIPTION
[0036] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses.
[0037] Referring to FIG. 1 , a side view of an exemplary gear and shaft assembly is generally indicated by reference number 10 . The gear and shaft assembly 10 is preferably located in a transmission (not shown) and is supported by at least one member 12 . The member 12 may take various forms, such as a non-rotational housing member, a radial rolling element bearing, or a rotating sleeve shaft without departing from the scope of the present invention. The gear and shaft assembly 10 includes a gear 11 , a shaft 13 , and at least one pinion shaft and bearing assembly 14 according to the principles of the present invention. The gear 11 intermeshes with a second gear (not shown) providing torque and rotation to the gear and shaft assembly 10 . The gear 11 is drivingly mounted to the shaft 13 which integrates the pinion shaft and bearing assembly 14 . The pinion shaft and bearing assembly 14 generally includes a pinion shaft 20 integrated with the shaft 13 and a bearing 40 coupled to the pinion shaft 20 , as will be described in greater detail below. The bearing 40 provides a material more suitable for improving the durability and performance of the pinion shaft 20 than the shaft 13 material alone.
[0038] Referring to FIG. 2 , a side view of the pinion shaft 20 proximate to the bearing 40 is illustrated and will now be described in detail. The pinion shaft 20 is generally cylindrical with an approximately circular cross-section, although other cross-sectional shapes may be employed without departing from the scope of the present invention. The pinion shaft 20 has a diameter D 1 and includes a base end 22 and a distal end 24 located opposite the base end 22 . The pinion shaft 20 further includes an outer surface 26 that has a first outer region 28 , a second outer region 30 , and a third outer region 32 . Each of the outer regions 28 , 30 , 32 are circumferentially continuous on the pinion shaft 20 . The first outer region 28 extends axially from the base end 22 of the pinion shaft 20 a distance of X 1 . The second outer region 30 extends axially from the first outer region 28 a distance of Y 1 . The third outer region 32 extends axially from the second outer region 24 a distance of Z 1 to the distal end 24 of the pinion shaft 20 . In the example provided, the first and third outer regions 28 , 32 have a surface with a microfinish below about 0.25 μm Ra. The second outer region 30 has a surface that is treated to create a plurality of features or indentations 31 reaching about 0.025 mm in depth where the surface of the indentations 31 have a microfinish of about 1.0 μm to 3.2 μm Ra. However, it should be appreciated that other microfinishes may be used without departing from the scope of the present invention. The surface finish of the second outer region 30 is greater than or equal to the surface finish of the first outer region 28 and less than the surface finish of the indentations 31 . Additionally, the distances X 1 , Y 1 , Z 1 may be adjusted depending upon the application. In the embodiment provided, distances X 1 and Z 1 are approximately equal and the distance Y 1 is greater than the distances X 1 and Z 1 . However, the distance Y 1 is directly related to a retention force of the bearing 40 on the pinion shaft 20 required for a particular application.
[0039] Turning now to FIG. 3 , a cross-sectional view of the bearing 40 is illustrated and will now be described. The bearing 40 is generally cylindrical and includes an inner race or surface 42 that defines a central bore 44 . The central bore 44 has a diameter D 2 . The bearing 40 further includes a first end 46 and a second end 48 opposite the first end 46 . The inner surface 42 includes a first inner region 48 , a second inner region 50 , and a third inner region 52 . The first inner region 48 extends axially from the first end 46 of the bearing 40 a distance of X 2 . The second inner region 50 extends axially from the first inner region 48 a distance of Y 2 . The third inner region 52 extends axially from the second inner region 48 a distance of Z 2 to the second end 48 of the bearing 40 . In the example provided, the first and third inner regions 48 , 52 have a microfinish below about 0.25 μm Ra. The second inner region 50 has a surface that is treated to create a plurality of features or indentations 51 reaching about 0.025 mm in depth where the surface of the indentations 51 have a microfinish of about 1.0 μm to 3.2 μm Ra. However, it should be appreciated that other microfinishes may be used without departing from the scope of the present invention. The surface finish of the second inner region 50 is greater than or equal to the surface finish of the first inner region 48 and less than the surface finish of the indentations 51 . Additionally, the distances X 2 , Y 2 , Z 2 may be adjusted depending upon the application. In the embodiment provided, distances X 2 and Z 2 are approximately equal and the distance Y 2 is greater than the distances X 2 and Z 2 . However, the distance Y 2 is directly related to a retention force of the bearing 40 on the pinion shaft 20 required for a particular application. Furthermore, the distances X 2 , Y 2 , Z 2 are approximately equal to the distances X 1 , Y 1 , Z 1 respectively.
[0040] Referring now to FIG. 4 , a cross-sectional view of the pinion and bearing assembly 14 with the bearing 40 installed on the pinion shaft 20 is illustrated and will now be described. The pinion bearing 40 is installed onto the pinion shaft 20 such that the pinion shaft 20 is located within the central bore 44 . As installed, the first inner region 48 opposes the first outer region 28 , the second inner region 50 opposes the second outer region 30 , and the third inner region 52 opposes the third outer region 32 . Where the first inner region 48 and first outer region 28 contact, the diameters D 1 and D 2 create a first press fit region 60 . The contact between the third inner region 52 and third outer region 32 creates a second press fit region 64 . The press fit is accomplished by providing that diameter D 2 is smaller or equal to the diameter D 1 . The overlap in diameters D 1 and D 2 ensures that there is no space between the pinion bearing 40 and the pinion shaft 20 for the pinion bearing 40 to move once installed on the pinion shaft 20 . Thus the press fit regions 60 , 64 allow the pinion bearing 40 to be accurately located on the pinion shaft 20 by minimizing relative movement between the parts.
[0041] As the pinion bearing 40 is installed on the pinion shaft 20 , the second inner region 50 opposes second outer region 30 each having a surface pattern of features or indentations 31 , 51 . The depth of the indentations 82 is around 0.025 mm thus providing a gap 61 , as shown in FIG. 5 , of at most around 0.05 mm when two indentations 31 , 51 are stacked on top of one another. The gap 61 provides a volume 81 for depositing an anaerobic adhesive 80 into the adhesive region 62 by applying it to one of or both of the outer surface 26 of the pinion shaft 20 and the inner surface 42 of the bearing 40 prior to installation. A preferred anaerobic adhesive 80 , for example, Loctite® 609 or 680 Retaining Compound or Loctite® Sleeve Retainer 640 manufactured by Henkel Corporation of Warren, Mich., although various other adhesives may be employed without departing from the scope of the present invention. One result of the surface treatment is that the inner surface 83 of the indentations 82 has a surface roughness of about 1.0 μm to about 3.2 μm Ra. As noted above, the press fit region 60 is accomplished by providing that diameter D 2 is smaller or equal to the diameter D 1 and is used to precisely locate the bearing 40 on the pinion shaft 20 . The press fit also provides an initial retention force resulting from stretching the pinion bearing 40 material and compressing the pinion shaft 20 material.
[0042] Referring now to FIGS. 6-8 , magnified views of various embodiments of the indentations 82 in the second outer region 30 of the outer surface 26 of the pinion shaft 20 resulting from various stages of processing are shown and will now be described. Initially the outer surface 26 is honed or ground to slightly larger finished size. Next, laser processing creates the indentations 82 , for example, as continuous elongated channels 82 , shown in FIG. 6 . When the material is removed from the outer surface 26 , displaced material (not shown) is formed near the indentations 82 . Finally, the outer surface is finished honed producing the surface finish. Any displaced material remaining on the outer surface 26 but outside of the specified diameter is removed. The indentations 82 may also have shapes other than a continuous channel without departing from the scope of the present invention. For example, FIG. 6 shows the embodiment wherein the indentations 82 take the form of a pattern of continuous, elongated pockets 100 . FIG. 7 shows another embodiment of the finished surface wherein the indentations 82 form a pattern of round pockets 102 . FIG. 8 shows still another embodiment of the finished surface wherein the indentations 82 form a pattern of pattern of diamond or square pockets 104 . These surface features described in FIGS. 6-8 cooperate to form the pockets 82 , as described above. It should be appreciated that other surface features may be employed without departing from the scope of the present invention. FIGS. 6-8 may also represent the second inner surface 50 of the inner surface 48 of the bearing 40 without departing from the scope of this invention.
[0043] The description of the invention is merely exemplary in nature and variations that do not depart from the gist of the invention are intended to be within the scope of the invention. Such variations are not to be regarded as a departure from the spirit and scope of the invention.
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A pinion shaft and bearing assembly is provided having two different surface finish interfaces. A first surface finish functions to locate the bearing to the pinion. A second surface finish functions to improve the cure time of an adhesive used to retain the bearing to the pinion.
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FIELD OF THE INVENTION
The present invention relates generally to communication systems; and, more particularly, to an improved method and apparatus for decoding serially concatenated block- and convolutional-coded data.
BACKGROUND OF THE INVENTION
Wireless communication systems are often limited in terms of transmitter power and spectrum availability. Broadband communication services often must fit within a limited if narrowband spectrum on an air interface network. Additionally, wireless transmission is significantly more error prone than broadband hard-wired networks. This tends to further reduce data capacity due to the necessity to transmit and process error control protocols.
For these and, other reasons, it is often a goal of digital communications design to maximize the transmission bit rate R and minimize the probability of bit error, or Bit Error Rate (BER) and system power S. The minimum bandwidth (BW) required to transmit at rate (R) is known to be Rs/2, where Rs is the symbol rate. A limit on the transmission rate, called the system capacity, is based on the channel BW and the signal to noise ratio (SNR). This limit theorem, also called the Shannon Noisy Channel Coding Theorem, states that every channel has a channel capacity C which is given by the formula, C=BW log 2 (1+SNR), and that for any rate R<C, there exist codes of rate R c which can have an arbitrarily small decoding BER.
For some time, the digital communications art has sought a coding/decoding algorithm which would reach the Shannon limit. Recently, coding/decoding schemes, called “Turbo Codes,” have been determined to achieve fairly reliable data communication at an SNR which is very close to the Shannon Limit.
One form of turbo decoding operates upon serial concatenated codes. As an example, a serial concatenation of an outer, block code—such as a Reed Solomon code—and an inner, convolutional code, can be found in many communications and data storage applications requiring very low bit error rates. This type of serial concatenation is used, for example, in DBS (Direct Broadcast Satellite) standards.
One such serial concatenated system 100 is illustrated in FIG. 1 . The serial concatenated system 100 includes a transmitter portion 102 for communicating encoded information to a receiver portion 104 via a communication channel 106 . The transmitter portion 102 uses an outer code encoder or block encoder 108 (e.g., a Reed-Solomon encoder) to encode input bits. The output of the outer code encoder 108 is then provided to an interleaver 110 wherein the signal is shuffled in a predetermined manner. Next, the output of the interleaver is provided to an inner code encoder (e.g., convolutional encoder) 112 . The output of the inner code encoder 112 is then modulated by modulator 114 and transmitted over the communication channel 106 to the receiver portion 104 for decoding and processing.
Once demodulated by demodulator 116 , the classical approach for decoding a serial concatenated system 100 is to apply a soft-decision inner code decoder (e.g., Viterbi decoder) 118 that receives as inputs soft symbols and outputs hard bit estimates for the inner block code. The outputs of the inner code decoder 118 are then byte-deinterleaved by deinterleaver 120 and provided to an outer code decoder 122 (generally a block decoder such as a Reed-Solomon decoder) that can correct multiple byte errors in a block. If the outer code decoder 122 indicates that the number of errors is beyond its correction capability, it may indicate so and no corrections are made.
In effect, this classical approach to concatenated decoding decomposes the task into two independent procedures: one for the inner code, and another for the outer code. An “optimal” decoder is then selected and applied for each of these procedures. However, although each decoder may be optimal for its specific task, the overall composite system may not be optimal for a given concatenated code. This is because (1) the Reed-Solomon decoder uses hard—rather than soft-decision data, and (2) the Viterbi decoder performance could be improved in a second pass decoding operation. In particular, error bursts, which are observed in the first-pass decoding, could be broken up by using the bit decisions from blocks which were successfully decoded by a Reed-Solomon decoder. This operation would, in turn, impact a second-pass Reed-Solomon decoding of the data, perhaps enabling the Reed-Solomon decoder to correct another block that previously was considered uncorrectable. In principle, the sharing of outer-to-inner code decoding information could be re-iterated, resulting in even further improvements. In fact, this technique is similar to turbo decoding in a parallel or serial concatenated code context, with bit-by-bit maximum a posteriori probability (MAP) decoding.
Various iterative (turbo-like) decoding approaches have been used in simulation to decode serial concatenations of convolutional and Reed-Solomon codes. One problem in such decoding processes is determining how the Viterbi algorithm is to be modified to accommodate inputs from Reed-Solomon decoded blocks that are correct. No known technique has been developed for efficiently forcing a Viterbi encoder to constrain certain locations in a data record to desired output logic levels.
SUMMARY OF THE INVENTION
Briefly, the present invention uses a pipelined process to accelerate signal decoding and improve receiver performance in a serial concatenated coding environment. As compared with a conventional non-pipelined approach, the resulting coding gain is substantially greater with a decrease in BER. A system according to the present invention is particularly applicable to DBS communications and like applications.
In a disclosed embodiment of the present invention, demodulated serial concatenated data is provided to a first decoder (e.g., a convolutional or Trellis Coded Modulation (TCM) decoder). The decoder output is then deinterleaved and decoded by a second decoder (e.g., an algebraic and/or block decoder). In addition to providing decoded data, the outer decoder also provides at least one decode status signal indicative of the success of second decoder operations. Both the decoder data and decode status signals are provided as inputs to a pipeline decoder unit.
The pipeline decoder unit interleaves the data outputs of the second decoder, as well as the decode status signals. Interleaved data signals are then convolutionally encoded with the same type of convolutional encoder that was used to generate encoded data at the transmitter. The resulting binary “hard-decision” data may then be mapped into highly reliable soft-decision data. In one embodiment, for example, a logic level “0” may be mapped to a minimum-scale soft-decision value (e.g., 0000 with 4-bit quantization), and a logic level “1” mapped to a maximum-scale soft-decision value (e.g., 1111 with 4-bit quantization). In this embodiment, the output of the convolutional encoder 216 (FIG. 2) is not punctured regardless of whether the convolutionally encoded data at the transmitter was punctured. Instead, the “mapped” datastream is time-aligned with a buffered version of the original demodulated soft-symbol input sequence (with erasures inserted at punctured locations), and these datastreams are provided to the parallel inputs of multiplexing circuitry. The multiplexing circuitry is responsive to the interleaved decode status signals to selectively provide data to a third decoder.
In an exemplary embodiment of the invention, the third decoder is a Viterbi decoder configured to function in a similar manner to a MAP sequence decoder when provided with high-reliability hard-decision data from successfully decoded Reed-Solomon blocks. More particularly, when a “mapped” data element from a successfully decoded Reed-Solomon block is available, the multiplexing circuitry passes that data to the third decoder. When the incumbent “mapped” data element is from a failed Reed-Solomon block, then the multiplexer passes the buffered soft-decision input to the third decoder. Performing a second pass of Viterbi decoding results in a much smaller bit error rate than seen with a first Viterbi decoding pass, in that the third decoder benefits from the entire concatenated coding gain of the first decoding pass. Employing additional pipelined decoding units/operations provides even further improvements in bit error rates.
In an alternate embodiment of the invention, the third decoder is a Viterbi decoder having rescaled path metrics. In this embodiment, the interleaved data outputs of the second decoder are passed directly to the third decoder as forced a-priori values. The interleaved decode status signals are also provided to the third decoder to selectively constrain the output of the third decoder to be based on either the forced a-priori values or a delayed version of the demodulated serially concatenated code data.
A decoder according to the present invention thus provides improved decoding performance as compared to prior solutions, and is suitable for VLSI implementation and operation at relatively high data rates. In addition, with the disclosed pipelined approach, the processing speed of elements in the pipelined data path may be no different from those found in a classical concatenated decoder. Moreover, the present invention does not require a change to existing standards, and provides enhanced performance for communication systems that employ punctured encoding schemes.
BRIEF DESCRIPTION OF THE DRAWINGS
A better understanding of the present invention can be obtained when the following detailed description of an exemplary embodiment is considered in conjunction with the following drawings, in which:
FIG. 1 is a schematic diagram of a conventional Serial Concatenated Coding system;
FIG. 2 is a schematic diagram of an exemplary communications system according to the present invention;
FIG. 3 provides exemplary details of a convolutional encoder for encoding data in the communication system of FIG. 2;
FIG. 4 provides exemplary details of a modified encoder for encoding data status information for use by the communication system of FIG. 2; and
FIG. 5 is a schematic diagram of an alternate embodiment of a pipelined communications system according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 2 is a schematic diagram of an exemplary communications system according to the present invention. The communications system includes a receiver 200 comprising at least one pipeline decoder unit 201 . As will be appreciated, the pipeline decoder unit 201 includes decoding functionality that efficiently utilizes inputs from previously decoded blocks to improve receiver performance and coding gain.
One obstacle to direct VLSI implementations of iterative concatenated decoding is the required processing speed. For example, if serial data is input at 20 Msymbols/sec, and four iterations are desired, the Viterbi and Reed-Solomon decoders must operate at four times the symbol rate (80 Msymbols/sec)—if the streaming data is to be processed in real time. With the disclosed pipeline approach, however, the processing speed of elements in the pipelined datapaths does not need to be increased with respect to those found in a classical concatenated decoder.
Referring more particularly to FIG. 2, received data is first demodulated by a demodulator 202 to produce quantized data at the channel symbol rate. The quantized data/demodulated serial concatenated code data may then be provided to an erasure insertion circuit 204 , in which an erasure is inserted, before the first decoding pass, at the point where the symbol was punctured by the transmitter. Puncturing coded outputs is acceptable for transmission purposes because of the redundancy of information which is created within typical encoders. As discussed in greater detail below, the pipeline decoder units 201 may be advantageously isolated from puncture-specific procedures.
The soft-decision symbols provided by the erasure insertion circuitry 204 are first decoded by an inner or first decoder 206 (e.g., a Viterbi or other convolutional decoder, or a TCM decoder), to produce first decoded data. The first decoded data is then deinterleaved by a deinterleaver 208 prior to provision to an outer or second decoder 210 (e.g., an algebraic and/or block decoder such as a Reed-Solomon decoder).
The Reed-Solomon decoder 210 has two outputs, which are provided to the first pipeline decoder unit 201 : the actual bits of a decoded Reed-Solomon block, and a decode status signal output that indicates whether an associated Reed-Solomon block was decoded without error. The Reed-Solomon decoding status signal is replicated for each Reed-Solomon bit, forming a stream of status bits. In the disclosed embodiment, the Reed-Solomon data bits are provided to a data interleaver 212 of the first pipeline decoder unit 201 , while the decode status bits are interleaved by a control interleaver 214 . The data interleaver 212 and control interleaver 214 function to spread the status and data bits over multiple Reed-Solomon blocks of data. The data interleaver 212 preferably functions in a manner similar to the interleaver used by the transmitter to generate the serial concatenated data received by the receiver 200 .
After interleaving, the Reed-Solomon data bits are re-encoded by convolutional encoder 216 to form encoded outputs. Again, the convolutional encoder 216 preferably functions in a like manner to the inner decoder used by the transmitter to produce the serial concatenated code data. As discussed more fully below in conjunction with FIG. 4, a similar encoding process is performed on the interleaved status bits by a “modified encoder” 220 , such that a Viterbi or third decoder 226 can determine whether or not data bits produced by the convolutional encoder 216 evolved entirely from reliable Reed-Solomon-decoded blocks.
The Viterbi decoder 226 of the pipeline decoder unit 201 of the disclosed embodiment of the invention is configured to behave in a like manner to a MAP sequence decoder when provided with high-reliability data from successfully decoded Reed-Solomon blocks. In particular, the binary “hard-decision” data provided by the convolutional encoder 216 is provided to a soft-decision minimum-/maximum-scale level mapper 218 , which functions to produce highly reliable soft-decision data. For example, a logic level “0” may be mapped to a minimum-scale soft-decision value (e.g., 0000 with 4-bit quantization), and a logic level “1” mapped to the maximum-scale soft-decision value (e.g., 1111 with 4-bit quantization). Next, the “mapped” datastream (or Reed-Solomon-forced decision symbol data) is time-aligned with the soft-decision symbol data produced by the erasure insertion circuitry 204 . The temporal alignment is provided by delay circuitry 224 . The time-aligned datastreams are then provided to the parallel inputs of multiplexing circuitry 222 .
The multiplexing circuitry 222 receives the output of the modified encoder 220 as a control signal to selectively determine which of the datastreams to provide to the third decoder 226 . When Reed-Solomon forced-decision symbol data is available from a successfully decoded Reed-Solomon block, the multiplexing circuitry 222 passes that data to the third decoder 226 . When the incumbent “mapped” element is from a failed Reed-Solomon block, the multiplexing circuitry instead passes the delayed soft-decision symbol data from block 224 to the third decoder 226 . The third decoder 226 decodes the output of the multiplexing circuitry 222 to provide “pipelined” decoded data characterized by having a smaller bit error rate than the decoded data provided by the first decoder 206 . In particular, the third decoder 226 benefits from the entire concatenated coding gain of the first decoding pass.
The output of the third decoder 226 is next deinterleaved by deinterleaver 228 , whose output is provided to a fourth/Reed-Solomon decoder 230 . As with the Reed-Solomon decoder 210 , the Reed-Solomon decoder 230 of the pipeline decoder unit 201 may include both a decoded data datastream, as well as a decode status signal datastream. These datastreams, as well as the output of the delay circuitry 224 , may be provided to an additional pipeline decoder unit 201 .
It is contemplated that any number of additional pipeline decoder units 201 may be similarly utilized until the desired coding gains and BER is achieved. In another contemplated embodiment of the invention, the clock rate for the decoder 200 could be increased and additional multiplexing circuitry provided such that the first decoder 206 could be leveraged to perform the function of the third decoder 226 . Similarly, the second decoder 210 could be reused to perform the function of the fourth decoder 230 . By using an appropriate clocking scheme, additional “pipelined” iterations could be performed by the first decoder 206 and the second decoder 210 . In this manner, the hardware overhead associated with the disclosed received 200 may be reduced.
Although the illustrated receiver 200 makes use of a convolutional inner code and an algebraic or Reed-Solomon outer code, it is contemplated that a decoder according to the present invention may be adapted to utilize TCM codes and/or other types of block codes.
FIG. 3 provides exemplary details of a convolutional encoder 216 for encoding data in the communication system of FIG. 2 . The convolutional encoder 216 receives a continuous sequence of data input bits that are mapped into a continuous sequence of encoder data bit outputs. The convolutional encoder 216 comprises a finite state shift register formed of series-connected flip-flops 300 and 302 . In accordance with conventional encoder architectures, the data inputs bits, as well as the outputs of each of the flip-flops 300 and 302 are provided to a first exclusive OR (XOR) gate 304 . The XOR gate 304 produces a first data bit output. The data bit inputs are likewise provided to a second XOR gate 306 , which also receives the output of the flip-flop 302 . The second exclusive OR gate 306 produces a second data output bit. As will be appreciated, the first and second outputs of the convolutional encoder 216 relate to a rate ½ code, and may be converted from a parallel format to a serial format via a converter (not shown).
FIG. 4 provides exemplary details of a modified encoder 220 for encoding decode status signals generated by an outer decoder 210 . The modified encoder 220 structurally resembles the convolutional encoder 216 , with the exception that the XOR gates 304 and 306 in the convolutional encoder 216 are replaced by AND gates 404 and 406 . The incoming decode status signal/control bits, as well as the outputs of flip-flops 400 and 402 are provided to the three input AND gate 404 , which produces a first control bit. The decode status signals and the output of the flip-flop 402 are provided to the two input AND gate 406 , which produces a second control bit. This arrangement is advantageous because when the output of the convolutional encoder 216 has no dependency on input data that is invalid, the modified encoder 220 signals that the output is valid. This is true even if the code in question may have shift register entries which are invalid but not accessed, as is the case for the control bit produced by AND gate 406 . As previously discussed, the outputs of the modified encoder 220 may be used to control the multiplexing circuitry 222 , which determines whether the re-encoded data is used.
As illustrated in the disclosed embodiment of the invention, the symbols erased by puncturing (at the transmitter) are inserted before the first decoding pass. Thus, decoding operations performed by the pipeline decoder unit(s) 201 need not perform puncture-specific procedures. Instead, the pipelined decoder unit(s) 201 can be configured to operate as fixed-rate devices (with the possible exception that the trace back length in the Viterbi decoder(s) 216 may be lengthened for optimal decoding performance when punctured data is present). It is also noted that in secondary decoding passes, the erased data that was re-inserted does not necessarily remain indeterminate (i.e., somewhere between a logic level “1” and “0”) as it was when initially inserted. If the re-inserted data arises from a bit that was correctly decoded in a Reed-Solomon block evaluation, then its value is known with very high probability. Thus, it is possible to correctly infer the value of untransmitted punctured bits and use this information in all subsequent decoding passes. This enhances the performance of the receiver 200 in high data rate applications involving puncturing.
In the disclosed embodiment of the invention, the Viterbi or third decoder 226 of the pipeline decoder unit 201 is described as utilizing forced decision data, which forces the third decoder 226 to behave much like a MAP sequence processor. Although not precisely a MAP solution, the approximation is such that there is no discernible difference in the disclosed implementation. The actual MAP solution is to not allow any transition from trellis states which would result in a Viterbi decoder outputting a result which is contrary to what a Reed-Solomon decoder has indicated as the desired output. In one contemplated alternate embodiment, if the number of memory elements in a code is m (resulting in 2 m states), and it is desired to force a logic level “0” at the output of the third decoder 226 for a given node, then the top 2 m−1 states are not altered, while the bottom 2 m−1 states are set to the most unfavorable path metric. In this manner, the next state at the output of the third decoder 226 will be a logic level “0”. Similarly, to force a logic level “1”, the top 2 −1 states are set to the most unfavorable path metric. This procedure describes the decoding of rate 1/n non-systematic convolutional codes. As will be appreciated, in this embodiment it is not necessary to reinsert erasures into punctured data positions. Analogous techniques (e.g., a look-up table) using the same concept of path re-normalization can be devised for other codes without departing from the spirit of the invention.
In one contemplated embodiment of the invention, the described approximation functions in part because of an implementation of a four-bit soft-decision Viterbi or third decoder 226 requiring only five-bit path metrics for minimal implementation loss. For a rate ½ code, two 4-bit symbols are used to form a branch metric, and these in turn are added to a previous path metric to form an updated path metric. The two maximum-scale four-bit inputs (which are forced using the disclosed mapping approach) add up to five bits, and this in turn is added to a previous path metric. So long as the path metric registers saturate, encoder “forcing” is equivalent to forcing the, unfavored path metrics to extreme five-bit worse case values, ala a MAP processor.
FIG. 5 is a schematic diagram of an alternate embodiment of a pipeline communication system according to the present invention. In this embodiment of the invention, a receiver 500 includes demodulation and decoding elements 502 - 510 functioning in a like manner to demodulation and decoding elements 202 - 210 of FIG. 2 . The receiver 500 also includes at least one pipeline decoder unit 501 employing a data interleaver 512 and a control interleaver 514 (functioning in a like manner to data interleaver 212 and control interleaver 214 described above).
In this embodiment of the invention, the outputs of the data interleaver 512 are provided directly to a Viterbi decoder 516 as forced a-priori values. The Viterbi decoder 516 includes rescaled path metrics for utilizing the forced a-priori values. The decode status signals provided by the control interleaver 214 are also passed directly to the Viterbi decoder 516 to selectively constrain the output of the Viterbi decoder 516 to be based on either the forced a-priori values or a delayed version of the demodulated serially concatenated code data provided by delay circuitry 518 . The output of the Viterbi decoder 516 is provided to a deinterleaver 520 and second outer decoder 522 operating in an analogous manner to deinterleaver 228 and fourth decoder 230 of FIG. 2 .
Thus, a communication system has been described for accelerating signal decoding and increasing receiver performance in a serial concatenated coding environment. The communication system utilizes a pipelined architecture to provide recognizable increases coding gains, even at high data rates, without increasing the speed of decoding elements in pipelined datapaths.
In view of the above detailed description of the present invention and associated drawings, other modifications and variations will now become apparent to those skilled in the art. It should also be apparent that such other modifications and variations may be effected without departing from the spirit and scope of the present invention.
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A decoder having a first decoder providing first decoded data. A deinterleaver is included for deinterleaving the first decoded data. A second decoder provides second decoded data based on the deinterleaved first decoded data. The second decoder provides at least one decode status signal indicative of second decoder operations. A pipeline decoder unit is included that is coupled to the second decoder. The pipeline decoder unit includes an encoder that receives the second decoded data and provides forced decision data, a multiplexer, and a third decoder that provides pipelined decoded data. The multiplexer is responsive to the at least one decode status signal to selectively constrain the pipelined decoded data to be at least partially dependent on the forced decision data.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is based on Japanese Patent Applications No. 2006-163877 filed on Jun. 13, 2006, and No. 2007-60596 filed on Mar. 9, 2007, the disclosures of which are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to a physical quantity sensor.
BACKGROUND OF THE INVENTION
As technical ideas capable of combining pressure sensors with other dynamic amount (i.e., physical quantity) detecting sensors in module forms, one technical idea is disclosed in JP-A-2002-286571, and another technical idea is described in Japanese magazine “DEMPA-SHINBUN HIGH TECHNOLOGY” issued by DEMPA-SHINBUN newspaper publisher on May 13, 2004.
The technical idea disclosed in JP-A-2002-286571 is related to the pressure speed sensor equipped with the pressure detecting function for detecting the air pressure of the tire and the speed detecting function for detecting the rotation speed of the tire. The pressure speed sensor is equipped with the diaphragm which receives pressure, the movable electrode and the fixed electrode which detect pressure, and the movable electrode and the fixed electrode which detect speeds. These pressure detecting movable and fixed electrodes, and the speed detecting movable and fixed electrodes are provided within the reference pressure chamber which has been hermetically closed by the housing. Both pressure and speeds are detected based upon changes in electrostatic capacitances between the movable electrodes and the fixed electrodes. Then, since the respective movable and fixed electrodes of this pressure/speed sensor are provided within the reference pressure chamber, it is possible to avoid that these movable and fixed electrodes are corroded by adhering dust and by applying acids to these electrodes.
The Japanese magazine “DEMPA-SHINBUN HIGH TECHNOLOGY” describes the tire air pressure sensor in which the pressure detecting sensor equipped with the pressure detecting function and the acceleration sensor equipped with the acceleration detecting function have been integrated in the same die. In the tire air pressure sensor, the pressure sensor (piezoelectric resistor) is equipped on the plane of the pressure film on the side of the reference pressure chamber so as to detect deformations of this pressure film, and thus, the tire air pressure is sensed based upon the detected deformations of the pressure film which separates the hermetically-closed reference pressure chamber from the air inside the tire. Also, the acceleration sensor has been provided within another hermetically-closed space which is different from the reference pressure chamber. As previously explained, since the pressure sensor and the acceleration sensor are provided within the hermetically-closed space, both the pressure and acceleration sensors can be protected from various sorts of chemical substances (remaining substances, soap, water, and the like in tire hardening process) which are present within tires.
Also, JP-A-6-347475 discloses such a structure that the acceleration sensor having the movable portion and the fixed portion, and the signal processing circuit for processing the output signal of the acceleration sensor have been stored in the package.
The technical idea disclosed in JP-A-2002-286571 has the following problems: That is, not only the structure of the sensor is made complex, but also the large number of structural members are required. Furthermore, since there are many joined portions, the air tight characteristic may be deteriorated. In addition, since these sensors must be separately manufactured, characteristic aspects of these sensors may be readily fluctuated. As a result, the technical idea disclosed in JP-A-2002-286571 has another problem that a large number of sensors having high precision can be hardly manufactured. On the other hand, the apparatus described in the Japanese magazine “DEMPA-SHINBUN HIGH TECHNOLOGY” has the following problem. That is, since the pressure sensor and the acceleration sensor are arrayed side by side to be integrated within the same die, the area occupied by these sensors becomes bulky. Furthermore, as explained in JP-A-6-347475, in the case where the sensor portion and the signal processing circuit are arranged on the same plane, there is another problem that the sensor area defined by combining the sensor unit with the signal processing circuit becomes bulky.
Thus, it is required for a physical quantity sensor to correctly sense physical quantity (i.e., dynamic amounts), and to have a structure by which an area occupied by a sensor is not made bulky.
SUMMARY OF THE INVENTION
In view of the above-described problem, it is an object of the present disclosure to provide a physical quantity sensor.
According to a first aspect of the present disclosure, a physical quantity sensor for detecting a physical quantity includes: a first substrate having a first physical quantity detection element; a second substrate having a second physical quantity detection element, wherein the second substrate contacts the first substrate; and an accommodation space disposed between the first substrate and the second substrate. The first physical quantity detection element is disposed in the accommodation space.
Since the first physical quantity detection element is accommodated in the accommodation space, the first physical quantity detection element is protected.
Alternatively, the first physical quantity detection element may face the second physical quantity detection element. In this case, the sensor is minimized, compared with a sensor in which a first element and a second element are arranged laterally.
Alternatively, the first substrate may further include a support layer, an insulation layer, a conductive layer and a lower wiring. The support layer, the insulation layer and the conductive layer are stacked in this order. The first physical quantity detection element is disposed in the conductive layer. The lower wiring is sandwiched between the insulation layer and the conductive layer. The first physical quantity detection element is coupled with the second substrate through the lower wiring. This lower wiring provides strong construction, compared with a wire bonding sensor.
According to a second aspect of the present disclosure, a physical quantity sensor for detecting a physical quantity includes: a first substrate having a first physical quantity detection element; and a second substrate having at least a processing circuit for processing an output signal from the first physical quantity detection element. The second substrate faces and contacts the first substrate so that an accommodation space is provided between the first substrate and the second substrate.
In this case, the dimensions of the sensor are minimized.
Alternatively, the processing circuit on the second substrate is opposite to the first substrate. In this case, the output signal from the processing circuit is easily retrieved. For example, a part of the protection film for covering an output wiring from the processing circuit is removed so that the output wiring is exposed from the protection film. Thus, the output signal from the processing circuit is easily retrieved.
Further, the second substrate may further include a concavity, which is disposed opposite to the processing circuit. The accommodation space is provided between the concavity and the first substrate. In this case, the accommodation space is provided without a spacer between the first and second substrates. Further, even when a spacer is formed between the first and second substrates, the accommodation space becomes larger than a case where the second substrate includes no concavity.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description made with reference to the accompanying drawings. In the drawings:
FIG. 1A to FIG. 1C are diagrams for showing a composite type dynamic amount sensor according to a first embodiment, FIG. 1A is a plan view of the composite type dynamic amount sensor, FIG. 1B is a sectional view of the sensor taken along a line IB-IB of FIG. 1A , and FIG. 1C is a sectional view thereof taken along a line IC-IC of FIG. 1A ;
FIG. 2 is a sectional view for showing the sensor taken along a line II-II of FIG. 1B and FIG. 1C ;
FIG. 3A to FIG. 3H are diagrams for representing manufacturing steps of a piezoelectric type pressure sensor for indicating the first embodiment;
FIG. 4A to FIG. 4D are diagrams for showing setting steps of fixed portion-purpose wiring lines employed in the first embodiment;
FIG. 5A and FIG. 5B are diagrams for showing steps for manufacturing a fixed portion and a movable portion employed in the first embodiment, which correspond to FIG. 1B before being manufactured;
FIG. 6A and FIG. 6B are diagrams for showing steps for manufacturing a fixed portion and a movable portion employed in the first embodiment, which correspond to FIG. 1C before being manufactured;
FIG. 7A and FIG. 7B are diagrams for representing steps for stacking the piezoelectric type pressure sensor employed in the first embodiment on a capacitance type acceleration sensor, which correspond to FIG. 1B before being manufactured;
FIG. 8A and FIG. 8B are diagrams for representing steps for stacking the piezoelectric type pressure sensor employed in the first embodiment on a capacitance type acceleration sensor, which correspond to FIG. 1C before being manufactured;
FIG. 9A to FIG. 9C are diagrams for showing a composite type dynamic amount sensor indicated in a second embodiment, FIG. 9A is a sectional view of the sensor taken along a line IXA-IXA of FIGS. 9B and 9C , FIG. 9 B is a sectional view thereof taken along a line IXB-IXB of FIG. 9A , and FIG. 9C is a sectional view thereof taken along a line IXC-IXC of FIG. 9A ;
FIG. 10A to FIG. 10C are diagrams for showing a composite type dynamic amount sensor indicated in a third embodiment, FIG. 10A is a sectional view of the sensor taken along a line XA-XA of FIGS. 10B and 10C , FIG. 10B is a sectional view thereof taken along a line XB-XB of FIG. 10A , and FIG. 10C is a sectional view thereof taken along a line XC-XC of FIG. 10A ;
FIG. 11 is a diagram for indicating a composite type dynamic amount sensor which shows a fourth embodiment;
FIG. 12 is a diagram for showing a composite type dynamic amount sensor which indicates a fifth embodiment;
FIG. 13 is a diagram for indicating a composite type dynamic amount sensor which shows a sixth embodiment;
FIG. 14 is a diagram for showing a composite type dynamic amount sensor which indicates a seventh embodiment;
FIGS. 15A and 15B are sectional views for indicating a composite type dynamic amount sensor which shows an eighth embodiment;
FIG. 16 is a sectional view for showing a composite type dynamic amount sensor which indicates a ninth embodiment;
FIG. 17 is a diagram for illustratively showing a wafer substrate on which a plurality of composite type dynamic amount sensors have been integrated, which is represented in a tenth embodiment;
FIG. 18 is a sectional view of the wafer substrate taken along a line XVIII-XVIII of FIG. 17 ;
FIG. 19 is a diagram for showing a composite type dynamic amount sensor which indicates an eleventh embodiment;
FIG. 20A to FIG. 20C represent steps for stacking a pressure sensor-sided wafer substrate on an acceleration sensor-sided wafer substrate, which are employed in the eleventh embodiment;
FIG. 21 is a plan view for indicating a stacked layer type dynamic amount sensor which represents a twelfth embodiment;
FIG. 22A to FIG. 22B are diagrams of a stacked layer type dynamic amount sensor used in the twelfth embodiment, FIG. 22A is a sectional view of the sensor taken along a line XXIIA-XXIIA of FIG. 21 , and FIG. 22B is a sectional view thereof taken along a line XXIIB-XXIIB of FIG. 21 ;
FIG. 23A to FIG. 23F are diagram for showing manufacturing steps of the stacked layer type dynamic amount sensor of FIG. 22A , which is provided in the twelfth embodiment;
FIG. 24 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates a thirteenth embodiment;
FIG. 25A to FIG. 25B are diagrams for indicating a stacked layer type dynamic amount sensor which shows a fourteenth embodiment;
FIG. 26 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates a fifteenth embodiment;
FIG. 27 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates a sixteenth embodiment;
FIG. 28A to FIG. 28E are diagram for showing manufacturing steps of the stacked layer type dynamic amount sensor of FIG. 27 , which is provided in the sixteenth embodiment;
FIG. 29 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates a seventeenth embodiment;
FIG. 30 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates an eighteenth embodiment;
FIG. 31 is a diagram for representing a stacked layer type dynamic amount sensor, which shows a nineteenth embodiment;
FIG. 32 is a diagram for showing a stacked layer type dynamic amount sensor, which indicates a twentieth embodiment;
FIG. 33A to FIG. 33B are diagrams for indicating a stacked layer type dynamic amount sensor which shows a twenty-first embodiment;
FIG. 34 is a diagram for representing a dicing cut line when stacked layer type dynamic amount sensors are integrated so as to be manufactured, which shows the twenty-first embodiment;
FIG. 35 is a sectional view for showing a composite type dynamic amount sensor represented in a modification of embodiments; and
FIG. 36 shows a detailed diagram of the capacitance type acceleration sensor indicated in the first embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
First Embodiment
In a first embodiment, a description is made of a composite type dynamic amount sensor 1 by employing FIG. 1A to FIG. 8B and FIG. 36 .
FIG. 1A is a plan view of the composite type dynamic amount sensor 1 ; FIG. 1B is a sectional view of the sensor 1 taken along a line IB-IB of FIG. 1A ; and FIG. 1C is a sectional view thereof taken along a line IC-IC of FIG. 1A . FIG. 2 is a sectional view for showing the sensor 1 taken along a line II-II of FIG. 1B and FIG. 1C .
As indicated in FIG. 1A to FIG. 1C and FIG. 2 , the composite type dynamic amount sensor 1 is constructed in such a way that a piezoelectric type pressure sensor 30 has been stacked on an N type silicon substrate 21 where a capacitance type acceleration sensor 20 has been formed in such a manner that the capacitance type acceleration sensor 20 is sealed. Also, the composite type dynamic amount sensor 1 has been mounted in the same package 50 for packaging a processing circuit 40 which processes an output of the composite type dynamic amount sensor 1 .
A first description is made of the piezoelectric type pressure sensor 30 with reference to FIG. 1A to FIG. 1C . The piezoelectric type pressure sensor 30 is constituted by a diaphragm 31 having a concave shape, 4 pieces of piezoelectric resistors 32 in total, 4 pieces of pressure sensor-purpose wiring lines 33 , 4 pieces of pressure sensor-purpose pads 34 , and a surface protection film 35 for protecting surfaces of the pressure sensor-purpose wiring lines 33 . The diaphragm 31 has been formed by etching an N type silicon substrate 31 c . The piezoelectric resistors 32 are provided in a deforming portion 31 a of the diaphragm 31 , and detect deformation of the deforming portion 31 a along a direction perpendicular to an elongation direction of the deforming portion 31 a so as to output the detected deformation. The pressure sensor-purpose wiring lines 33 transfer the outputs of the respective piezoelectric resistors 32 . The pressure sensor-purpose pads 34 have been connected to the respective pressure sensor-purpose wiring lines 33 . This deforming portion 31 a constitutes a concave button plane of the diaphragm 31 , and if pressure is applied to the deforming portion 31 a , then the deforming portion 31 a is deformed. While the deforming portion 31 a has a structure surrounded by a ground frame 31 b , the diaphragm 31 has been constructed of the deforming portion 31 a and the ground frame 31 b.
Four pieces of the piezoelectric resistors 32 are internally provided on a plane located opposite to the concave bottom plane of the deforming portion 31 a . Although not shown in the drawings, these piezoelectric resistors 32 have constituted a bridge circuit. The pressure sensor-purpose wiring lines 33 , the pressure sensor-purpose pads 34 , and the surface protection film 35 have been set on the plane on the side where the piezoelectric resistors 32 are internally provided. Then, the respective pressure sensor-purpose pads 34 are electrically connected to the respective processing circuit-purpose pads 41 coupled to the processing circuit 40 by employing a wire bonding. It should be understood that the diaphragm 31 has such a dimension capable of sealing the capacitance type acceleration sensor 20 within a sealing space formed by the diaphragm 31 and an outer frame 22 (will be explained later). Then, the above-described sealing space constitutes a reference pressure chamber 37 of the pressure sensor.
Next, the capacitance type acceleration sensor 20 will now be described with reference to FIG. 1B , FIG. 1C , and FIG. 2 . It should be understood that although the diagrams shown in FIG. 1B , FIG. 1C and FIG. 2 exemplify a basic idea of the capacitance type acceleration sensor 20 , namely, a cantilever, a double camber beam and a multiple camber beam may be alternatively employed. One example of actual concrete structures is indicated in FIG. 36 .
The capacitance type acceleration sensor 20 has been formed by a movable portion 23 and a fixed portion 24 , while an entire circumference of the capacitance type acceleration sensor 20 has been surrounded by an outer frame 22 by separating a gap. As will be described later with reference to FIG. 5A , FIG. 5B , FIG. 6A and FIG. 6B , the outer frame 22 , the movable portion 23 , and the fixed portion 24 have been formed by etching the N type silicon substrate 21 .
As shown in FIG. 2 , the movable portion 23 has been constituted by 2 pieces of movable electrodes 23 a , a weight 23 b which joins these movable electrodes 23 a , a pillar 23 d to which a movable portion-purpose wiring line 23 c is connected, and a beam 23 e which joins the weight 23 b and the pillar 23 d . As indicated in FIG. 1B , the movable electrode 23 a has a gap between a supporting substrate 25 and the own movable electrode 23 a . Similarly to the movable electrode 23 a , the weight 23 b and the beam 23 e have a gap between the supporting substrate 25 and the weight 23 b and the beam 23 e although not shown in the figure. On the other hand, the pillar 23 d has been fixed on an insulating film 26 stacked on the supporting substrate 25 . Since the capacitance type acceleration sensor 20 is equipped with such a structure, the beam 23 e causes the pillar 23 d to be distorted along a direction “IIC” of FIG. 2 , so that both the weight 23 b and the movable electrode 23 a are displaced along the direction “IIC.”
Also, the movable portion-purpose wiring line 23 c connected to the pillar 23 d has joined the movable portion-purpose pad 23 f provided on the outer frame 22 to the pillar 23 d under bridging condition. Then, while a predetermined voltage (or predetermined current) is applied to the movable portion-purpose pad 23 f , the same voltage (or same current) as that of the movable portion-purpose pad 23 f is applied also to the movable electrode 23 a via the movable portion-purpose wiring line 23 c.
On the other hand, as shown in FIG. 2 , the fixed portion 24 is made of 2 pieces of fixed electrodes 24 a , a coupling portion 24 b , and a fixed portion-purpose wiring line 24 c . These two fixed electrodes 24 a are located opposite to the above-described respective movable electrodes 23 a . The coupling portion 24 b joins these fixed electrodes 24 a . The two fixed electrodes 24 a and the coupling portion 24 b have been constructed on the insulating film 26 . The fixed portion-purpose wiring line 24 c has joined the fixed portion-purpose pad 24 d provided on the outer frame 22 to the coupling portion 24 b under bridging condition. Then, while a predetermined voltage (or predetermined current) is applied to the fixed portion-purpose pad 24 d , the same voltage (or same current) as that of the fixed portion-purpose pad 24 d is applied also to the fixed electrode 24 a via the fixed portion-purpose wiring line 24 c.
Since such a structure is provided, if acceleration is applied to the capacitance type acceleration sensor 20 along the direction “IIC”, then the movable electrode 23 a is displaced along the direction “IIC” to approach the fixed electrode 24 a , while the pillar 23 d of the movable portion 23 is set to a fulcrum. At this time, an electrostatic capacitance between the movable electrode 23 a and the fixed electrode 24 a is changed with respect to an electrostatic capacitance of such a condition that acceleration is not applied. Concretely speaking, in such a case where acceleration is applied along a direction “IIC 1 ” of FIG. 2 , the fixed electrode 24 a is separated from the movable electrode 23 a , so that the electrostatic capacitance is decreased. Conversely, in such a case where acceleration is applied along a direction “IIC 2 ” of FIG. 2 , the fixed electrode 24 a approaches to the movable electrode 23 a , so that the electrostatic capacitance is increased. In other words, magnitudes of the applied acceleration may correspond to the increase/decrease of the electrostatic capacitances.
Then, a change in the electrostatic capacitances is detected by comparing a voltage (or current) transferred to the movable portion-purpose pad 23 f via the movable portion-purpose wiring line 23 c which joins the movable portion 23 and the outer frame 22 with another voltage (or current) transferred to the fixed portion-purpose pad 24 d via the fixed portion-purpose wiring line 24 c which joins the fixed portion 24 and the outer frame 22 by the processing circuit 40 . Concretely speaking, as shown in FIG. 1A , FIG. 1C , and FIG. 2 , while the movable portion-purpose pad 23 f and the fixed portion-purpose 24 d are connected to the corresponding processing circuit-purpose pads 41 by the wire bonding manner, the voltages (currents) which are inputted from the respective processing circuit-purpose pads 41 are compared with each other by the processing circuit 40 so as to detect the applied acceleration.
Also, a frame “IID” indicated in FIG. 2 shows an outer fence of the ground frame 31 b of the diaphragm 31 in such a case where the piezoelectric type pressure sensor 30 is stacked on the outer frame 22 which surrounds the capacitance type acceleration sensor 20 . As represented in FIG. 2 , both the movable portion 23 and the fixed portion 24 have been sealed inside a sealing space which is formed by the outer frame 22 and the diaphragm 31 .
It should be noted that in order to prevent from being short-circuited between the movable portion-purpose wiring line 23 c and the fixed portion-purpose wiring line 24 c , the movable portion-purpose wiring line 23 c and the fixed portion-purpose wiring line 24 c have been set via an SiN film 27 on the outer frame 22 , and have been covered by the surface protection film 28 except for such portions which will constitute the movable portion-purpose pad 23 f and the fixed portion-purpose pad 24 d.
Referring now to FIG. 3A to FIG. 3H , a description is made of steps for manufacturing the piezoelectric type pressure sensor 30 . In the beginning, as indicated in FIG. 3A , an N type silicon substrate 31 c is prepared, and then, an insulating film (SiO 2 ) 31 d is formed on both planes of this N type silicon substrate 31 c . It is desirable that a thickness of the N type silicon substrate 31 c is approximately 400 μm.
Next, a photo-resist mask is formed on the insulating film (SiO 2 ) 31 d of FIG. 3A , and an etching process is further carried out so as to remove a portion of the insulating film 31 d . Then, in the N type silicon substrate 31 c , an impurity is diffused from a vapor phase in a portion from which the insulating film 31 d has been removed and which has been exposed. Alternatively, ions of P type boron may be implanted so as to form a P type region containing the piezoelectric resistors 32 as indicated in FIG. 3B , while a depth of this P type region is made in approximately 0.5 μm to 1.0 μm.
Next, after the photo-resist mask and the insulating film 31 d formed on the plane of the N type silicon substrate 31 c on the piezoelectric resistor forming side are once removed, an insulating film 36 is once formed on one plane, and both a photo-resist mask is formed and an etching process is carried out so as to form a contact hole 31 e as an oxide film, as shown in FIG. 3C . This contact hole 31 e is provided at such a position that this contact hole 31 e becomes the ground frame 31 b when the piezoelectric type pressure sensor 30 is accomplished.
Then, as shown in FIG. 3D , both a pressure sensor-purpose wiring line 33 and a pressure sensor-purpose pad 34 are provided in and on the contact hole 31 e and the insulating film 36 by vapor-depositing either aluminum or poly-silicon.
Next, as shown in FIG. 3E , an SiN film which constitutes the surface protection film 35 is provided on the side where the pressure sensor-purpose wiring line 33 and the pressure sensor-purpose pad 34 of FIG. 3D have been provided.
Then, as shown in FIG. 3F , the surface protection film 35 of such a portion is removed which constitutes the pressure sensor-purpose pad 34 when the piezoelectric type pressure sensor 30 is accomplished, in order that either aluminum or poly-silicon of the under layer is exposed.
Next, as shown in FIG. 3G , in the N type silicon substrate 31 c , a portion of the insulating film 36 is removed which has been formed on the plane located opposite to the plane on the piezoelectric resistor forming side. The region of the insulating film 36 to be removed corresponds to such a portion which becomes a concave portion when a diaphragm is completed, namely a portion which constitutes the deforming portion 31 a.
Finally, as indicated in FIG. 3H , since the region from which the insulating film 31 d has been removed in FIG. 3G is etched, a portion of the N type silicon substrate 31 is removed so as to form the concave portion. Since the above-described manufacturing steps are carried out, the piezoelectric type pressure sensor 30 is accomplished.
Next, a description is made of steps for manufacturing the capacitance type acceleration sensor 20 with reference to FIG. 4A to FIG. 4D , FIG. 5A to FIG. 5B , and FIG. 6A to FIG. 6B .
Referring now to FIG. 4A to FIG. 4D , a description is made of steps for manufacturing the fixed portion-purpose wiring line 24 c.
In the beginning, a high concentration N type silicon substrate 21 is prepared, the resistivity of which is 0.1 to 0.001 Ω·cm, and then, an insulating film 26 is formed on one plane of the N type silicon substrate 21 by executing a thermal oxidation. Then, another silicon substrate (supporting substrate 25 ) is directly joined to the N type silicon substrate 21 where the insulating film 26 has been formed on one plane thereof in a furnace whose temperature is approximately 1000° C., so that a structure shown in FIG. 4A is obtained.
Further, a SiN film 27 (insulating film) is formed on the structure of FIG. 4A , and a photo-resist etching process is carried out so as to form a contact hole 27 a in a portion of this SiN film 27 . It should also be noted that this contact hole 27 a is formed in such a portion which will become a fixed portion 24 when the capacitance type acceleration sensor 20 is accomplished, and to which the fixed portion-purpose wiring line 24 c is connected. Then, an ion implantation is carried out via the contact hole 27 a so as to form an N + region 24 e , so that such a structure as indicated in FIG. 4B is obtained. It should also be understood that when concentration of a high concentration N type silicon substrate is sufficiently high, an ion implantation may be omitted.
Next, either aluminum or poly-silicon is vapor-deposited on the contact hole 27 a and the SiN film 27 of FIG. 4B in order to set either a fixed portion-purpose wiring line 24 c or a fixed portion-purpose pad 24 d as indicated in FIG. 4C . At this time, the N + region 24 e is being ohmic-contacted to the fixed portion-purpose wiring line 24 c.
Next, an SiN film which will constitute the surface protection film 28 is formed on the side where the fixed portion-purpose wiring line 24 c and the fixed portion-purpose pad 24 d have been formed, and as shown in FIG. 4D , the surface protection film 28 of such a portion which will constitute the fixed portion-purpose pad 24 d when the fixed portion-purpose wiring line 24 c is accomplished is removed.
Since the above-described manufacturing steps are carried out, the fixed portion-purpose wiring line 24 c is completed. It should also be noted that since the movable portion-purpose wiring line 23 c may be manufactured by the substantially same steps as those of the fixed portion-purpose wiring line 24 c , an explanation thereof is omitted.
Subsequently, a method for manufacturing a fixed portion 24 and a movable portion 23 will now be described with reference to FIG. 5A , FIG. 5B , and FIG. 6A , FIG. 6B . It should also be noted that FIG. 5A and FIG. 5B correspond to FIG. 1B before these fixed and movable portions 24 and 23 are manufactured, and also, FIG. 6A and FIG. 6B correspond to FIG. 1C before these fixed and movable portions 24 and 23 are manufactured.
Firstly, the N type silicon substrate 21 on which the fixed portion-purpose wiring line 24 c of FIG. 4D has been accomplished is prepared, and then, as indicated in FIG. 5A and FIG. 6A , a portion of the surface protection films 27 , and 28 of the side where the fixed portion-purpose wiring line 24 c has been formed is removed. The portion of the surface protection films to be removed corresponds to such a portion which will not constitute the outer frame 22 , the movable portion 23 , and fixed portion 24 when the fixed and movable portions 24 and 23 are completed.
Next, as shown in FIG. 5B and FIG. 6B , the N type silicon substrate 21 at such a portion from which the surface protection films 27 and 28 have been removed is etched in a sacrifice layer etching manner, while the insulating film 26 is employed as a sacrifice layer, in order to form the fixed portion 24 , the movable portion 23 , and the outer frame 22 . The fixed portion 24 has been fixed on the insulating film 26 . Only the pillar 23 d of the movable portion 23 has been fixed on the insulating film 26 . The outer frame 22 surrounds the movable portion 23 and the fixed portion 24 . As a result, such a capacitance type acceleration sensor 20 shown in FIG. 2 is accomplished.
Referring now to FIG. 7A , FIG. 7B , FIG. 8A , and FIG. 8B , a description is made of steps for stacking the piezoelectric type pressure sensor 30 on the outer frame 22 which surrounds the capacitance type acceleration sensor 20 . It should be understood that FIG. 7A and FIG. 7B correspond to FIG. 1B before the manufacture thereof, and FIG. 8A and FIG. 8B correspond to FIG. 1 c before the manufacture thereof.
As represented in FIG. 7A and FIG. 8A , low melting point glass 60 having an insulating characteristic and which constitutes an adhesive agent is coated on an edge plane of the deforming portion 31 a of the ground frame 31 b , which is located on the side of the elongation direction.
Next, as shown in FIG. 7B and FIG. 8B , the low melting point glass 60 coated on the ground frame 31 b is adhered to the outer frame 22 so as to be fixed thereon under vacuum condition. As a result, a sealing space (namely, reference pressure chamber 37 ) is produced by the diaphragm 31 of the piezoelectric type pressure sensor 30 , the outer frame 22 , and the insulating film 26 , so that both the fixed portion 24 and the movable portion 23 are sealed with this sealing space.
As previously described, the steps for manufacturing the piezoelectric type pressure sensor 30 shown in FIG. 3A to FIG. 3H ; the steps for manufacturing the capacitance type acceleration sensor 20 represented in FIG. 4A to FIG. 4D , FIG. 5A to FIG. 5B , and FIG. 6A to FIG. 6B ; and also the stacking steps shown in FIG. 7A to FIG. 7B and FIG. 8A to FIG. 8B are sequentially carried out, so that the composite type dynamic amount sensor 1 shown in FIG. 1A to FIG. 1C and FIG. 2 may be constructed.
Subsequently, a description is made of effects of the above-described composite type dynamic amount sensor 1 .
As to a first effect, since the capacitance type acceleration sensor 20 is stacked on the piezoelectric type pressure sensor 30 , the occupied area of the sensors 20 and the 30 can be reduced, as compared with the conventional structure that the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 are separately provided.
A description is made of a second effect. In the conventional capacitance type acceleration sensor, in order to avoid that contaminations (particles etc.) are entered to the movable portion, the cap made of glass and the like have been employed so as to seal the movable portion. However, in the case of the composite type dynamic amount sensor 1 of the first embodiment, the movable portion 23 is sealed by the diaphragm 31 of the piezoelectric type pressure sensor 30 . As previously explained, the movable portion 23 can be sealed without separately employing the cap.
A third effect is described. As previously described, the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 have been separately manufactured, and have been stacked on each other, as indicated in FIG. 7A , FIG. 7B , FIG. 8A , and FIG. 8B . As a result, the capacitance type acceleration sensor 20 and the piezoelectric pressure sensor 30 may be employed which are substantially identical to the conventional acceleration and pressure sensors. In other words, the conventional detecting performance can be maintained and these acceleration and pressure sensors 20 and 30 can be stacked on each other, so that the structure thereof need not be made complex, as compared with the conventional sensors. Also, since the joining portion constitutes the joining portion between the ground frame 31 b of the diaphragm 31 and the outer frame 22 , the air tight characteristic of the joining portion is high.
Also, in the first embodiment, such a case that the reference pressure chamber 37 becomes vacuum has been exemplified. In the case where the reference pressure chamber 37 is not vacuum, such an effect capable of suppressing air dumping may be achieved. Concretely speaking, since the deformation direction of the deforming portion 31 a of the diaphragm 31 is directed along such a direction perpendicular to the movable direction of the movable portion 23 , even in such a case where the deforming portion 31 a is deformed and thus the internal pressure of the reference pressure chamber 37 is increased, the movable portion 23 can be hardly depressed against the fixed portion 24 by receiving this internal pressure. In other words, the internal pressure can hardly give an adverse influence to the distance between the movable portion 23 and the fixed portion 24 . As a result, the acceleration can be detected in higher precision.
It should also be noted that it is desirable that in order to suppress the air dumping, the deformation direction of the deforming portion 31 a is located perpendicular to the movable direction of the movable portion 23 . However, even when the deformation direction is made coincident with the movable direction, it is possible to suppress the air dumping, although the detection precision is slightly lowered.
Second Embodiment
Referring now to FIG. 9A to FIG. 9C , a description is made of a composite type dynamic amount sensor 1 according to a second embodiment. This embodiment is different from the above-described first embodiment as to the following technical point: That is, a piezoelectric type pressure sensor 30 is adhered to a capacitance type acceleration sensor 20 by employing solder 91 and 92 , and an air tight characteristic of a reference pressure chamber 37 is secured by an air tight annular ring 93 . It should also be noted that the same reference numerals shown in the first embodiment will be employed as those for denoting the same, or similar structures indicated in the second embodiment, and explanations in this embodiment are omitted.
FIG. 9A is a sectional view for indicating the composite type dynamic amount sensor 1 according to the second embodiment, namely such a sectional view, taken along a line IXA-IXA of FIG. 9B and FIG. 9C . Also, FIG. 9B corresponds to FIG. 1B in the first embodiment, and FIG. 9C corresponds to FIG. 1C in the first embodiment.
As shown in FIG. 9B and FIG. 9C , the capacitance type acceleration sensor 20 has been fixed to the piezoelectric type pressure sensor 30 via conducting-purpose solder 91 , coupling-purpose solder 92 , and the air tight annular ring 93 . The air tight annular ring 93 is made of rubber (namely, elastic member) having an annular shape, and is provided in a region “IXE” of FIG. 9A . Alternatively, the air tight annular ring 93 may be formed by solder similar to the above-described conducting-purpose solder 91 and coupling-purpose solder 92 . Since air tight connecting and sealing of these sensor 20 and 30 are realized by the solder, the resulting air tight characteristic may be further improved. Then, lumps of the conducting-purpose solder 91 and the coupling-purpose solder 92 are present within the annular shape of this air tight annular ring 93 . Both the conducting-purpose solder 91 and the coupling-purpose solder 92 may couple the capacitance type acceleration sensor 20 to the piezoelectric type pressure sensor 30 , and also, may depress the air tight annular ring 93 between the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 so as to sandwich the air tight annular ring 93 so as to maintain the air tight characteristic of the reference pressure chamber 37 .
Also, in the first embodiment, the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c have been provided by employing aluminum, and the like. In this embodiment, as represented in FIG. 9A to FIG. 9C , a portion of the outer frame 22 is insulating-processed so as to form the fixed portion-purpose wiring line 24 c , the movable portion-purpose wiring line 23 c , and a pressure sensor-purpose wiring line 94 . Concretely speaking, as indicated in FIG. 9A , the pressure sensor-purpose wiring line 94 provided at a portion of the outer frame 22 in order to transfer an output signal of the piezoelectric type pressure sensor 30 has been insulated from the outer frame 22 by employing an insulating film 95 such as SiO 2 . Furthermore, as indicated in FIG. 9B , this pressure sensor-purpose wiring line 94 is electrically conducted via the conducting-purpose solder 91 to the pressure sensor-purpose wiring line 33 provided inside the piezoelectric type pressure sensor 30 . In other words, the conducting-purpose solder 91 may achieve two actions: That is, the piezoelectric type pressure sensor 30 is coupled to the capacitance type acceleration sensor 20 under a condition that the air tight annual ring 93 is pushed into; and the output signals of the piezoelectric resistors 32 are transferred to the pressure sensor-purpose wiring line 94 . In the pressure sensor-purpose wiring line 94 , a terminal portion thereof on the side where the conducting-purpose solder 91 is not set becomes a pressure sensor-purpose pad 34 which is wire-bonded to the processing circuit-purpose pad 41 of the processing circuit 40 .
On the other hand, as shown in FIG. 9A , the fixed portion-purpose wiring line 24 c constitutes a portion of a coupling portion 24 b of the fixed portion 24 , and has been electrically insulated from the outer frame 22 by employing the insulating film 95 such as SiO 2 . It should also be understood that as indicated in FIG. 9A and FIG. 9C , an insulating film 27 has been provided on an entire plane of the fixed portion-purpose wiring line 24 c except for a terminal portion of the edge plane on the side of the piezoelectric type pressure sensor 30 . Then, in the terminal portion of the fixed portion-purpose wiring line 24 c , such a portion where the insulating film 27 is not provided constitutes the fixed portion-purpose pad 24 d , while this fixed portion-purpose pad 24 d has been connected to the processing circuit purpose pad 41 by a wire bonding manner.
Also, as indicated in FIG. 9A , the movable portion-purpose wiring line 23 c elongated to the pillar 23 d in an integral body has a substantially same structure as that of the fixed portion-purpose wiring line 24 c . Under such a condition that this movable portion-purpose wiring line 23 c is insulated from the outer frame 22 , a terminal portion of the movable portion-purpose wiring line 23 c is exposed and constitutes the movable portion-purpose pad 23 f.
As previously described, both the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c have been electrically insulated from the outer frame 22 and the piezoelectric type pressure sensor 30 , and the pressure sensor-purpose wiring line 94 has been electrically insulated from the capacitance type acceleration sensor 20 .
Although not shown in the drawing, the coupling-purpose solder 92 has coupled a coupling pad provided in the piezoelectric type pressure sensor 30 to another coupling-purpose pad provided on the outer frame 22 . The first-mentioned coupling-purpose pad has been provided in order not to give an adverse influence to an output signal of the piezoelectric type pressure sensor 30 , whereas the last-mentioned coupling-purpose pad has been provided in order not to give an adverse influence to an output result obtained from the capacitance type acceleration sensor 20 .
Since the above-described structure is employed, the pressure sensor-purpose pad 34 , the fixed portion-purpose pad 24 d , and the movable portion-purpose pad 23 f may be provided to be closed to each other. Furthermore, similar to the first embodiment, the piezoelectric resistors 32 and the pressure sensor-purpose wiring line 33 are sealed in the sealing space of the reference pressure chamber 37 , so that both the piezoelectric resistor 32 and the pressure sensor-purpose wiring line 33 can be protected from particles, and the like.
In this embodiment, although the conducting-purpose solder 91 and the coupling-purpose solder 92 are set within the annular shape of the air tight ring 93 , the setting places of the conducting-purpose solder 91 and the coupling-purpose solder 92 may be alternatively located outside the annular shape of the air tight ring 93 . Furthermore, a total setting number as to the conducting-purpose solder 91 and the coupling-purpose solder 92 may not be alternatively selected to be 6 portions as indicated in FIG. 9A . It is desirable as the setting places of the solder 91 and 92 , the setting intervals of the solder become equal to each other, and/or the solder 91 and 92 is set in the vicinity of the corners of the air tight ring 93 . However, if the air tight ring 93 can seal the reference pressure chamber 37 constituted by the diaphragm 31 and the outer frame 22 , then there is no limitation in the setting numbers and the setting places of the solder.
Also, since the shape of the air tight ring 93 may be merely made in an annular shape, such a substantially rectangular shape as shown in FIG. 9A need not be employed as this shape of the air tight ring 93 . Alternatively, a toroidal shape may be employed.
Third Embodiment
Referring now to FIG. 10A to FIG. 10C , a description is made of a composite type dynamic amount sensor 1 according to a third embodiment. This embodiment is different from the above-described second embodiment as to the following technical point: That is, the air tight characteristic of the reference pressure chamber 37 is secured by employing an NCF (Non-Conductive Film) 101 . It should also be noted that the same reference numerals shown in the first embodiment, or the second embodiment will be employed as those for denoting the same, or similar structures indicated in the third embodiment, and explanations in this embodiment are omitted.
FIG. 10A is a sectional view for indicating the composite type dynamic amount sensor 1 according to the third embodiment, namely such a sectional view, taken along a line XA-XA of FIG. 10B and FIG. 10C . Also, FIG. 10B corresponds to FIG. 1B in the first embodiment, and FIG. 10C corresponds to FIG. 1C in the first embodiment.
As shown in FIG. 10B and FIG. 10C , the capacitance type acceleration sensor 20 has been fixed to the piezoelectric type pressure sensor 30 via the conducting-purpose solder 91 , the coupling-purpose solder 92 , and the NCF 101 . This NCF 101 is made of a resin film having a non-conductive characteristic, and the NCF 101 may be joined by way of a crimping manner, a thermal crimping manner, or an adhesive manner. Alternatively, the NCF 101 may be manufactured by a screen printing method, or an ink jet printing method. Since the material of the NCF 101 is made of a resin having an electric insulating characteristic, for example, an epoxy resin, or a polyimide resin, this resin material is softened by receiving heat. Then, heat is continuously applied to this resin material under softened condition, so that the softened resin material may be hardened.
As indicated in a region “XF” of FIG. 10A , this NCF 101 has an annular shape which is located in the vicinity of an inner diameter of the outer frame 22 , and which surrounds a region containing a terminal portion of the pressure sensor-purpose wiring line 94 on the side of the reference pressure chamber 37 . Then, lumps of the conducting-purpose solder 91 and the coupling-purpose solder 92 are present within the NCF 101 .
Next, a description is made of steps for stacking the capacitance type acceleration sensor 20 on the piezoelectric type pressure sensor 30 via the NCF 101 .
At a time instant when the piezoelectric type pressure sensor 30 is completed, for example, in FIG. 3H , the above-described conducting-purpose solder 91 is provided as a bump on an exposed portion (namely, pressure sensor-purpose pad in the first embodiment) of the pressure sensor-purpose wiring line 33 . If the pressure sensor-purpose wiring line 33 is made of an aluminum material, Ti, Ni, Au are stacked in this order on the pressure sensor-purpose wiring line 33 , and then, the conducting-purpose solder 91 is provided on this Au. Similarly, the coupling-purpose solder 92 is provided within the region “XF” (namely, setting scheduled region of NCF 101 ). Thereafter, the NCF 101 is set by employing a crimping method, or a printing method within the region “XF” in such a manner that the NCF 101 seals the conducting-purpose solder 91 and the coupling-purpose solder 92 .
On the other hand, after the fixed portion 24 and the movable portion 23 which constitute the capacitance type acceleration sensor 20 , the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c which have been insulated by the insulating film 95 such as SiO 2 from the outer frame 22 , and also, the pressure sensor-purpose wiring line 94 have been completed, the conducting-purpose solder 91 is provided as a bump on the pressure sensor-purpose pad 34 . Similarly, the coupling-purpose solder 92 is set within the region “XF” (setting scheduled region of NCF 101 ).
As previously explained, after the NCF 101 , the conducting-purpose solder 91 , and also the coupling-purpose solder 92 have been set to both the piezoelectric type pressure sensor 30 and the capacitance type acceleration sensor 20 , the piezoelectric type pressure sensor 30 is located opposite to the capacitance type acceleration sensor 20 , and the NCF 101 is heated at a temperature of approximately 150° C. A positioning operation is carried out in such a manner that the conducting-purpose solder 91 and the coupling-purpose solder 92 of the piezoelectric type pressure sensor 30 are located opposite to the corresponding conducting-purpose solder 91 and the corresponding coupling-purpose solder 92 of the capacitance type acceleration sensor 20 , and then, the piezoelectric type pressure sensor 30 is depressed against the capacitance type acceleration sensor 20 . As a result, the NCF 101 is broken through by the conducting-purpose solder 91 and the coupling-purpose solder 92 on the side of the capacitance type acceleration sensor 20 , so that the both the conducting-purpose solder 91 and the coupling-purpose solder 92 on the side of the capacitance type acceleration sensor 20 are contacted to the corresponding conducting-purpose solder 91 and the corresponding coupling-purpose solder 92 of the piezoelectric type pressure sensor 30 . After these solders contact, ultrasonic joining is performed with respect to the respective conducting-purpose solder 91 and the respective coupling-purpose solder 92 so as to be electrically connected to each other.
With employment of the above-described structure, similar operation and effects to those of the second embodiment can be achieved in the third embodiment.
Fourth Embodiment
Referring now to FIG. 11 , a description is made of a composite type dynamic amount sensor 1 according to a fourth embodiment. The fourth embodiment has the below-mentioned technical different points from those of the first embodiment. That is, in this embodiment, while a penetration electrode 111 is provided on a diaphragm 31 , a signal of a capacitance type acceleration sensor 20 can be derived from the diaphragm 31 through the penetration electrode 111 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the fourth embodiment, and descriptions thereof are omitted.
FIG. 11 is a sectional view for showing the composite type dynamic amount sensor 1 according to the fourth embodiment, and corresponds to FIG. 1C in the first embodiment.
As indicated in FIG. 11 , the penetration electrode 111 and an insulating film 112 have been formed on the ground frame 31 b of the diaphragm 31 . The penetration electrode 111 is located parallel to the deforming direction of the deforming portion 31 a . The insulating film 112 insulates the penetration electrode 111 from the diaphragm 31 . It should also be noted that the place where the penetration electrode 111 is provided is such a place that when the capacitance type acceleration sensor 20 is adhered to the piezoelectric type pressure sensor 30 , this place is located opposite to both the exposed portion (namely, fixed portion-purpose pad of the first embodiment) of the fixed portion-purpose wiring line 24 c , and the exposed portion (namely, movable portion-purpose pad of the first embodiment) of the movable portion-purpose wiring line 23 c.
Then, the penetration electrode 111 has been connected to the exposed portion of the fixed portion-purpose wiring line 24 c , or the exposed portion of the movable portion-purpose wiring line 23 c by the conducting-purpose solder 91 . Furthermore, in addition to the above-described conducting-purpose solder 91 , the coupling-purpose solder 92 employed in the above-explained third embodiment has been provided at such a portion between the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 , which gives a less electrically adverse influence.
Also, similar to the third embodiment, the NCF 101 having the annular shape has been provided between the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 so as to maintain the air tight characteristic of the reference pressure chamber 37 . Alternatively, as shown in the second embodiment, a ring for the air tight sealing may be formed by a ring of solder on either the outer side or the inner side of the penetration electrode 111 .
A terminal edge of the penetration electrode 111 , which is not connected to either the fixed portion-purpose wiring line 24 c or the movable portion-purpose wiring line 23 c , has been constituted as either the fixed portion-purpose pad 24 d or the movable portion-purpose pad 23 f , which is wire-bonded to the processing circuit-purpose pad 41 of the processing circuit 40 . It should also be noted that these pads 23 f and 24 d may also function as the terminal portion of the penetration electrode 111 as shown in FIG. 11 , or may be formed as an enlarged portion which is manufactured by vapor-depositing aluminum on the terminal portion in order to be easily wire-bonded.
In this case, a step for forming this penetration electrode 111 is constructed of the following 3 forming steps, a step in which while the ground frame 31 b is masked, a reactive ion etching process is carried out so as to form a penetration hole; a step in which this penetration hole is further thermally oxidized in order to form an insulating film 112 ; and a step in which poly-silicon is grown on the penetration hole reduced by the thermal oxidation, so that the penetration electrode 111 is accomplished. Alternatively, instead of this poly-silicon, such a metal as tungsten, copper, aluminum may be employed.
It should also be understood that the structure of the piezoelectric type pressure sensor 30 is manufactured in such a manner that 2 pieces of the penetration electrodes 111 , and the insulating film 112 for insulating these penetration electrodes 111 are additionally provided in the piezoelectric type pressure sensor 30 of the first embodiment, whereas positions of the pressure sensor-purpose wiring line 33 and the pressure sensor-purpose pad 34 are similar to those of the first embodiment.
As previously described, while the penetration electrodes 111 are provided on the diaphragm 31 , the penetration electrodes 111 , the fixed portion-purpose wiring line 24 c , and the movable portion-purpose wiring line 23 c are electrically connected to each other. As a result, as represented in FIG. 11 , the setting positions as to the fixed portion-purpose pad 24 d , and the movable portion-purpose pad (not shown) can be located on the diaphragm 31 . As a consequently, while the operation and effects similar to those of the first embodiment may be achieved, the pressure sensor-purpose pad 34 , the fixed portion-purpose pad 24 d , and the movable portion-purpose pad can be formed on the diaphragm 31 . In addition, if gold balls, solder balls, and the like are formed on the pad portions over this pressure sensor, then connection pads for so-called “ball bonding” may be alternatively formed.
Fifth Embodiment
Referring now to FIG. 12 , a description is made of a composite type dynamic amount sensor 1 according to a fifth embodiment. The fifth embodiment has the below-mentioned technical different points from those of the fourth embodiment. That is, in this embodiment, while a fixed portion-purpose wiring line 24 c and a movable portion-purpose wiring line 23 c have been provided on an insulating film 26 , the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c have been connected via a poly-silicon film 121 to the penetration electrodes 111 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the fifth embodiment, and descriptions thereof are omitted.
FIG. 12 is a sectional view for showing the composite type dynamic amount sensor 1 according to the fifth embodiment, and corresponds to FIG. 1C in the first embodiment.
As indicated in FIG. 12 , the coupling portion 24 b of the fixed portion 24 has been connected to the fixed portion-purpose wiring line 24 c on the side of the supporting substrate 25 . Then, a surface except for the coupling portion 24 b of the fixed portion 24 has been covered by the insulating film 27 such as SiO 2 . Also, the fixed portion-purpose wiring line 24 c has been electrically connected to the poly-silicon film 121 provided on the outer frame 22 , and has been insulated from the outer frame 22 and the movable portion 23 by an insulating film 122 . Also, this poly-silicon film 121 has been insulated from the outer frame 22 by the insulating film 122 . Similar to the above-described fourth embodiment, the poly-silicon film 121 has been connected by the conducting-purpose solder 91 to the penetration electrodes 111 formed on the ground frame 31 b of the diaphragm 31 . The fixed portion-purpose pad 24 d has been provided on a terminal portion of this penetration electrode 111 , which is not connected to the poly-silicon film 121 . Then, this fixed portion-purpose pad 24 d is connected to the processing circuit-purpose pad 41 of the processing circuit 40 by a wire bonding.
Also, with respect to a movable portion (not shown), a supporting substrate side of the pillar has been connected to the movable portion-purpose wiring line 23 c , and furthermore, this movable portion-purpose wiring line 23 c has been electrically connected to the poly-silicon film 121 formed on the outer frame 22 . This movable portion-purpose wiring line 23 c has been insulated from the outer frame 22 and the fixed portion 24 by the insulating film 122 . Further, the poly-silicon film 121 has been connected by the conducting-purpose solder 91 to the penetration electrodes 111 formed on the ground frame 31 b of the diaphragm 31 . The movable portion-purpose pad has been provided on a terminal portion of this penetration electrode 111 . Then, this movable portion-purpose pad is connected to the processing circuit-purpose pad 41 of the processing circuit 40 by a wire bonding. Also, the movable electrode, the beam, and the weight have gaps with respect to the insulating film 26 , and can be displaced along the elongation direction of the supporting substrate 25 similar to the first embodiment.
It should also be noted that as to a step for forming both the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c between the fixed portion 24 and the movable portion 23 , and the supporting substrate 25 , the manufacturing method described in JP-A-H06-1236285 may be employed. With employment of the above-described structure, similar operation and effects to those of the fourth embodiment may be achieved. In addition, since a penetration electrode is formed on the supporting substrate 25 of the acceleration sensor 20 by the same method as that described above, an electrode may be derived from the lower portion of the supporting substrate 25 of the acceleration sensor 20 .
Sixth Embodiment
Referring now to FIG. 13 , a description is made of a composite type dynamic amount sensor 1 according to a sixth embodiment. The sixth embodiment has the below-mentioned technical different points from those of the third embodiment. That is, in this embodiment, a capacitance type pressure sensor 130 is stacked on the capacitance Type acceleration sensor 20 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the sixth embodiment, and descriptions thereof are omitted.
FIG. 13 is a sectional view for showing the composite type dynamic amount sensor 1 according to the sixth embodiment, and corresponds to FIG. 1B in the first embodiment.
As represented in FIG. 13 , the capacitance type pressure sensor 130 is constituted by a base portion 131 , a lower electrode 132 , an insulating film 134 , and a lower electrode pierced wiring line 136 . The base portion 131 is provided with an opening portion having a tapered form at a center. The lower electrode 132 corresponds to a circular-shaped diaphragm 31 which is deformed when pressure is applied, while the lower electrode 132 covers the opening portion of the base portion 131 . The insulating film 134 insulates the lower electrode 132 from the base portion 131 . The lower electrode pierced wiring line 136 is pierced in the base portion 131 and is connected to the lower electrode 132 . Although not shown in the drawing, the lower electrode pierced wiring line 136 has been insulated from the base portion 131 .
Also, a switch circuit for switching an applied signal (voltage, or current) has been connected to the lower electrode 132 and the movable portion 23 and the fixed portion 24 of the capacitance type acceleration sensor 20 . Since this switch current is employed, a first time and a second time are set in a periodic manner. In the first time, signals different from each other are inputted to the movable portion 23 and the fixed portion 24 , whereas no signal is inputted to the lower electrode 132 . In the second time, the same signals are inputted to the movable portion 23 and the fixed portion 24 , and a signal is inputted to the lower electrode 132 .
In synchronism with this time period, an A/D converting circuit (not shown) switches input ports so as to acquire a potential difference (current difference) between the movable portion 23 and the fixed portion 24 in the first time, and also to acquire a potential difference (current difference) between the lower electrode 132 , and both the movable portion 23 and the fixed portion 24 in the second time.
Generally speaking, since an A/D converter and a D/A converter are operated in response to the same timer pulse, an input port for acquiring an output signal is synchronized with an output port for outputting an applied signal, so that the input port and the output port may be switched.
Since such a structure is equipped with the composite type dynamic amount sensor 1 , acceleration may be calculated based upon a change in electrostatic capacitances between the movable portion 23 and the fixed portion 24 in the first time. On the other hand, pressure applied to the lower electrode 132 may be calculated based upon an electrostatic capacitance between the movable portion 23 and the fixed portion 24 , and the lower electrode 132 in the second time.
Seventh Embodiment
Referring now to FIG. 14 , a description is made of a composite type dynamic amount sensor 1 according to a seventh embodiment. The seventh embodiment has the below-mentioned technical different points from those of the sixth embodiment. That is, in this embodiment, the capacitance type pressure sensor 130 is equipped with an upper electrode. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the seventh embodiment, and descriptions thereof are omitted.
FIG. 14 is a sectional view for showing the composite type dynamic amount sensor 1 according to the seventh embodiment, and corresponds to FIG. 1B in the first embodiment.
As represented in FIG. 14 , the capacitance type pressure sensor 130 is constituted by a base portion 131 , a lower electrode 132 , an upper electrode 133 , an insulating film 134 , an upper electrode pierced wiring line 135 , and also a lower electrode pieced wiring line 136 . The base portion 131 is provided with an opening portion having a tapered form at a center. The lower electrode 132 corresponds to a circular-shaped diaphragm 31 which is deformed when pressure is applied, while the lower electrode 132 covers the opening portion of the base portion 131 . The upper electrode 133 has an annular shape which is not deformed by pressure, and is provided within the base portion 131 in such a manner that this upper electrode 133 is located opposite to the lower electrode 132 . The insulating film 134 insulates both the upper electrode 133 and the lower electrode 132 . The upper electrode pierced wiring line 135 is pierced in the base portion 131 , and is connected to the upper electrode 133 . The lower electrode pierced wiring line 136 is pierced in the base portion 131 , and is connected to the lower electrode 132 . It should also be noted that although not shown, the lower electrode 132 and the lower electrode pierced wiring line 136 have been insulated from the base portion 131 , the upper electrode 133 and the upper electrode pierced wiring line 135 connected to the upper electrode 133 . The lower electrode pierced wiring line 136 is connected to the lower electrode 132 .
Also, the respective pierced wiring lines 135 and 136 have been connected via the conducting-purpose solder 91 to the pressure sensor-purpose wiring lines 94 respectively provided on a portion of the outer frame 22 . Also, similar to the structure of the third embodiment in which the NCF 101 has been sandwiched between the ground frame 31 and the outer frame 22 , the NCF 101 has been sandwiched between the base portion 131 and the outer frame 22 even in this embodiment.
Next, a description is made of effects achieved in the seventh embodiment. When positive pressure is applied to the opening portion of the base portion 131 , the lower electrode 132 corresponding to the diaphragm 31 is deformed, so that a distance between the lower electrode 132 and the upper electrode 133 is separated. At this time, since either the voltage or the current is applied between the upper electrode 133 and the lower electrode 132 , the distance between the upper and lower electrodes 133 and 132 is separated, so that the electrostatic capacitance between these lower and upper electrodes 132 and 133 is decreased. Also, at this time, since such a sealing space has been formed by the lower electrode 132 , the capacitance type acceleration sensor 20 (concretely speaking, both outer frame 22 and insulating film 134 ), and the NCF 101 , this sealing space may constitute the reference pressure chamber 37 so as to improve the detection precision of the capacitance type pressure sensor 130 .
As previously explained, even in such a case that the capacitance type pressure sensor 130 is employed, similar operation and effects to those of the third embodiment may be achieved.
Eighth Embodiment
Referring now to FIG. 15A and FIG. 15B , a description is made of a composite type dynamic amount sensor 1 according to an eighth embodiment. The eighth embodiment has the below-mentioned technical different points from those of the respective embodiments described above. That is, in this embodiment, a pressure sensor processing circuit 40 a of a piezoelectric type pressure sensor 30 has been provided on a pressure sensor substrate 151 of the piezoelectric type pressure sensor 30 ; and an acceleration sensor processing circuit 40 b has been provided on an outer frame of a capacitance type acceleration sensor 20 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the eighth embodiment, and descriptions thereof are omitted.
FIG. 15A is a sectional view for showing the composite type dynamic amount sensor 1 according to the eighth embodiment, and corresponds to FIG. 1B in the first embodiment; and FIG. 15B corresponds to FIG. 1C in the first embodiment.
The piezoelectric type pressure sensor 30 will now be described with reference to FIG. 15A . The piezoelectric type pressure sensor 30 is constituted by a diaphragm 31 , a piezoelectric resistor 32 , a pressure sensor-purpose wiring line 33 , a pressure sensor processing circuit 40 a , and a penetration electrode 111 . The diaphragm 31 has been formed by removing a portion of a pressure sensor substrate 151 . The piezoelectric resistor 32 has been provided on the diaphragm 31 . The pressure sensor-purpose wiring line 33 is connected to the piezoelectric resistor 32 and the pressure sensor processing circuit 40 a . The pressure sensor processing circuit 40 a has been formed within the pressure sensor substrate 151 and processes a signal of the pressure sensor-purpose wiring line 33 . The penetration electrode 111 transfers a processed signal of the pressure sensor processing circuit 40 a over the pressure sensor substrate 151 . It should also be noted that the pressure sensor processing circuit 40 a has been formed on an opposite plane of the diaphragm 31 on the opening side in the pressure sensor substrate 151 . The pressure sensor-purpose wiring line 33 has been connected to an input terminal of the pressure sensor processing circuit 40 a . Also, an output terminal of the pressure sensor processing circuit 40 a has been connected to the penetration electrode 111 . It should also be understood that this penetration electrode 111 has been insulated from the pressure sensor substrate 151 by the insulating film 112 .
Referring now to FIG. 15A and FIG. 15B , the capacitance type acceleration sensor 20 will be described. When the piezoelectric type pressure sensor 30 is stacked on the capacitance type acceleration sensor 20 , in the outer frame 22 , the acceleration sensor processing circuit 40 b has been formed at a place located opposite to the diaphragm 31 . Also, both the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c have been connected to an input terminal of the acceleration sensor processing circuit 40 b , whereas an acceleration sensor output wiring line 152 has been connected to an output terminal thereof. This acceleration sensor output wiring line 152 implies such a wiring line which outputs a result obtained by the acceleration sensor processing circuit 40 b for processing signals entered from the fixed portion-purpose wiring line 24 c and the movable portion-purpose wiring line 23 c . As this acceleration sensor output wiring line 152 , such a portion which is not covered by the pressure sensor substrate 151 is exposed from the oxide film 28 to become a pad.
Also, as shown in FIG. 15A and FIG. 15B , the piezoelectric type pressure sensor 30 has been coupled to the capacitance type acceleration sensor 20 by the coupling-purpose solder 92 under such a condition that these sensors 30 and 20 depress a first air tight ring 93 a and a second air tight ring 93 b so as to sandwich therebetween these rings 93 a and 93 b . In other words, both the movable portion 23 and the fixed portion 24 are sealed within the sealing space by the first air tight ring 93 a . Furthermore, the reference pressure chamber 37 is formed by the second air tight ring 93 b , the diaphragm 31 , and the insulating film 28 .
Since the above-explained structure is employed in the composite type dynamic amount sensor 1 , while similar operation and effects to these of the first embodiment may be achieved, the processing circuits 40 a and 40 b can be sealed, so that processing circuits 40 a and 40 b can be protected.
Ninth Embodiment
Referring now to FIG. 16 , a description is made of a composite type dynamic amount sensor 1 according to a ninth embodiment. The ninth embodiment has the below-mentioned technical different points from those of the eighth embodiment. That is, in this embodiment, a sensor which senses pressure corresponds to a capacitance type pressure sensor. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the ninth embodiment, and descriptions thereof are omitted.
FIG. 16 is a sectional view for showing the composite type dynamic amount sensor 1 according to the ninth embodiment, and corresponds to FIG. 15B in the eighth embodiment.
As indicated in FIG. 16 , the capacitance type pressure sensor is constituted by an upper electrode 133 provided on a diaphragm 35 , and a lower electrode 132 which is located opposite to the upper electrode 133 and is upwardly formed on a supporting substrate via an insulating film 26 . Then, an output signal of the upper electrode 133 and an output signal of the lower electrode 132 are inputted to the processing circuit 40 via wiring lines (not shown, for example, penetration electrodes). The processing circuit 40 compares the output signal of the upper electrode 133 with the output signal of the lower electrode 132 so as to detect an electrostatic capacitance between the upper electrode 133 and the lower electrode 132 , and then, calculates pressure applied to the diaphragm 35 based upon a change amount of the detected electrostatic capacitances. It should also be noted that as the lower electrode 132 of this embodiment, this lower electrode 132 is not formed by being substituted by the movable portion 23 and the fixed portion 24 as shown in FIG. 13 , but a single silicon member having a rectangular shape may be employed.
On the other hand, the capacitance type acceleration sensor 20 is made of a substantially same structure as that of the above-described capacitance type acceleration sensor 20 of FIG. 11 . However, although the penetration electrode 111 which transfers the output signal of the capacitance type acceleration sensor 20 has been provided on the diaphragm 31 in FIG. 11 , the penetration electrode 111 has been provided on a place of the pressure sensor substrate 151 , which is not the diaphragm 35 in this embodiment. Then, in the pressure sensor substrate 151 , the processing circuit 40 has been provided on an edge plane of this substrate 151 , which is located opposite to the side of the supporting substrate. As indicated in FIG. 16 , an output signal of the fixed portion 24 is entered via the penetration electrode 111 and the wiring line 161 to the processing circuit 40 , and furthermore, an output signal of a movable portion (not shown), and also output signals of the lower electrode 132 and the upper electrode 133 are entered to this processing circuit 40 . The processing circuit 40 further executes an amplifying process and a calculating process based upon these input signals in order to output calculation results by employing an acceleration sensor output wiring line 152 and another wiring line (not shown). As shown in the acceleration sensor output wiring line 152 of FIG. 16 , pads have been provided on edge portions of these wiring lines.
Since the above-described structure is constructed in the composite type dynamic amount sensor 1 , even when such a capacitance type pressure sensor is employed, similar operation and effects as those of the above-described eighth embodiment can be achieved.
It should also be understood that although the lower electrode 132 is made of the electrode having the plate-shaped member in the ninth embodiment, such a structure may be alternatively employed instead of the lower electrode 132 that both the fixed portion and the movable portion of FIG. 13 are located opposite to the upper electrode 133 . In this alternative case, it is so assumed that while the capacitance type acceleration sensor 20 located opposite to the processing circuit 40 is defined as a first acceleration sensor, and both the fixed portion and the movable portion are defined as a second acceleration sensor, which are located opposite to the upper electrode 133 and are substituted as the lower electrode; and both a detecting direction (displace direction of movable portion) of the first accelerator sensor and a detecting direction of the second acceleration sensor are made different from each other (for instance, orthogonal direction). At this time, similar to the sixth embodiment, timing (first time) for detecting acceleration and timing (second time) for detecting pressure are set to both the fixed portion and the movable portion of the second acceleration sensor in a periodic manner. As a result, acceleration may be detected by the second acceleration sensor in the first time, whereas pressure may be detected by the second acceleration sensor and the upper electrode 133 in the second time.
Since the above-described alternative structure is constructed, the acceleration of the 2 axes may be detected by the first acceleration sensor and the second acceleration sensor, and further, the pressure may be detected by employing the fixed portion and the movable portion of the second acceleration sensor, and the upper electrode 133 .
Tenth Embodiment
Referring now to FIG. 17 and FIG. 18 , a description is made of a composite type dynamic amount sensor 1 according to a tenth embodiment. This embodiment is such an embodiment that a plurality of the above-explained composite type dynamic amount sensors 1 of the first embodiment are manufactured at the same time by employing a semiconductor process. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the tenth embodiment, and descriptions thereof are omitted.
FIG. 17 is a bird's eye view for representing a wafer substrate 171 in which a plurality of the above-described composite type dynamic amount sensors 1 of the first embodiment shown in FIG. 1A to FIG. 1C have been integrated. Furthermore, FIG. 18 is an enlarged sectional view of the wafer substrate 171 , taken along a line XVIII-XVIII in FIG. 17 . As represented in FIG. 18 , the piezoelectric type pressure sensors 30 of FIG. 1A to FIG. 1C are stacked on each other in order to correspond to the respective capacitance type acceleration sensors 20 of the acceleration sensor-sided wafer substrate where the plural pieces of capacitance type acceleration sensor 20 of FIG. 1A to FIG. 1C are stacked. As a result, such a wafer substrate 171 that the plural pieces of composite type dynamic amount sensors 1 shown in FIG. 17 have been stacked is formed. Then, this wafer substrate 171 is dicing-cut along dot lines shown in FIG. 17 and FIG. 18 , so that a plurality of the composite type dynamic amount sensors 1 of FIG. 1A to FIG. 1C can be obtained.
Under such a condition that the piezoelectric type pressure sensors 30 have been stacked on the capacitance type acceleration sensors 20 , the fixed portion-purpose pads 24 d and the movable portion-purpose pads 23 f of the capacitance type acceleration sensors 20 are exposed, so that an energizing test may be carried out before the wafer substrate 171 is dicing-cut. Alternatively, a wafer substrate 1 where a plurality of acceleration sensors have been formed, and another wafer substrate 2 where a plurality of pressure sensors have been formed may be stacked each other under wafer statuses, and thereafter, the stacked wafer substrates may be dicing-cut. In this alternative case, either a penetration groove or a penetration hole has been formed in the wafer substrate 2 on which the pressure sensors of the upper area portion have been formed, which are wired-bonded with the acceleration sensors in order to be equivalent to, for example, FIG. 18 , and thereafter, the wafer substrates are stacked on each other.
Eleventh Embodiment
Referring now to FIG. 19A and FIG. 20A to FIG. 20C , a description is made of a composite type dynamic amount sensor 1 according to an eleventh embodiment. The eleventh embodiment has the below-mentioned technical different points from those of the above-described tenth embodiment. That is, in this embodiment, a piezoelectric type pressure sensor 30 which is stacked on an acceleration sensor-sided wafer substrate 171 is stacked under a condition of a pressure sensor-sided wafer substrate 172 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the eleventh embodiment, and descriptions thereof are omitted.
FIG. 19 is a sectional view for showing the composite type dynamic amount sensor 1 according to the eleventh embodiment. As a structure of the composite type dynamic amount sensor 1 , with respect to FIG. 11 of the fourth embodiment, a side plane (namely, plane of direction perpendicular to pressure applied direction) of the ground frame 31 b of the piezoelectric type pressure sensor 30 is made coincident with a side plane (namely, plane of acceleration applied direction) of the capacitance type acceleration sensor 20 .
Next, a description is made of a method for manufacturing the composite type dynamic amount sensor 1 of the eleventh embodiment with reference to FIG. 20A to FIG. 20C .
Firstly, as shown in FIG. 20A , such a pressure sensor-sided wafer substrate 172 is prepared in which a plurality of the above-explained piezoelectric type pressure sensors 30 shown in FIG. 19 have been stacked. This pressure sensor-sided wafer substrate 172 is such a pressure sensor-sided wafer substrate into which the piezoelectric resistor 32 and the penetration electrode 111 (which are not shown) have been processed in the above-described forming step in the fourth embodiment and then have already been formed.
In a step of FIG. 20B subsequent to the step of FIG. 20A , after the conducting-purpose solder 91 is set to an exposed portion of the penetration electrode 111 of the pressure sensor-sided wafer substrate 172 , and the NCF 101 is set to a predetermined portion, the pressure sensor-sided wafer substrate 172 is stacked with respect to the acceleration sensor-sided wafer substrate 171 .
In a step of FIG. 20C subsequent to the step of FIG. 20B , the stacked substrate manufactured in FIG. 20B is dicing-cut along dot lines, so that such a composite type dynamic amount sensor 1 of FIG. 19 can be obtained.
In the eleventh embodiment, after the pressure sensor-sided wafer substrate 172 and the acceleration sensor-sided wafer substrate 171 have been stacked to each other, the stacked wafer substrate is dicing-cut. As a result, in accordance with the manufacturing method of the eleventh embodiment, total numbers of the dicing-cut process and of the stacking process are smaller than those of the below-mentioned case: That is, the pressure sensor-sided wafer substrate 172 is dicing-cut to form the piezoelectric type pressure sensor 30 , and further, the acceleration sensor-sided wafer substrate 171 is dicing-cut to form the capacitance type acceleration sensor 1 , and then, these sensors 172 and 171 are separately stacked to each other.
On the other hand, in the present embodiment, the composite type dynamic amount sensor 1 having the substantially same structure as that of the above-described fourth embodiment shown in FIG. 11 has been manufactured by stacking the pressure sensor-sided wafer substrate 172 on the acceleration sensor-sided wafer substrate 171 . However, a structure of a composite type dynamic amount sensor manufactured by a stacking manner is not limited only to that shown in FIG. 11 . For example, as represented in FIG. 1A to FIG. 1C of the first embodiment, even when the piezoelectric type pressure sensor 30 is employed which has the pressure sensor-purpose pad 34 on the plane of the ground frame 31 b of the deforming portion 31 a , which is located opposite to the concave bottom plane, such a pressure sensor-sided wafer substrate on which the above-described piezoelectric type pressure sensor 30 has been integrated is prepared. Then, this pressure sensor-sided wafer substrate may be stacked on an acceleration sensor-sided wafer substrate. In this alternative case, it is preferable to form a penetration hole in the pressure sensor-sided wafer substrate before the piezoelectric type pressure sensor 30 is stacked in order that the fixed portion-purpose pad is not covered by the ground frame 31 b of the piezoelectric type pressure sensor 30 .
In addition to the structure shown in FIG. 1A to FIG. 1C , even in the structure of FIG. 9A to FIG. 9C , the structure of FIG. 10A to FIG. 10C , the structure of FIG. 11 , and the structure of FIG. 12 , the pressure sensor-sided wafer substrates may be stacked on the acceleration sensor-sided wafer substrates, and then, the stacked wafer substrates may be dicing-cut. Also, in the structure of FIG. 35 , the first acceleration sensor-sided wafer substrate may be stacked on the second acceleration sensor-sided wafer substrate, and then, the stacked wafer substrate may be dicing-cut.
Twelfth Embodiment
Referring now to FIG. 21 , FIG. 22A to FIG. 22B , and FIG. 23A to FIG. 23F , a description is made of a stacked layer type dynamic amount sensor 201 according to a twelfth embodiment. The twelfth embodiment has the below-mentioned technical different points from those of the first embodiment. That is, in this embodiment, a piezoelectric type pressure sensor 30 has been stacked on a circuit board 240 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the twelfth embodiment, and descriptions thereof are omitted.
FIG. 21 is a plan view for showing the stacked layer type dynamic amount sensor 201 according to the twelfth embodiment. In FIG. 21 , although piezoelectric resistors 32 are not exposed from a surface of the stacked layer type dynamic amount sensor 201 , setting positions are indicated by using dot lines, for the sake of explanations. The penetration electrodes 111 exposed in FIG. 21 are employed so as to supply electric power for driving the processing circuit 40 and the piezoelectric type pressure sensor 30 , and are used as the ground, and also are employed to derive output signals from the processing circuit 40 and the piezoelectric type pressure sensor 30 . A sectional view, taken along a line XXIIA-XXIIA of FIG. 21 is shown in FIG. 22A , and another sectional view, taken along a line XXIIB-XXIIB of FIG. 21 is indicated in FIG. 22B .
As indicated in FIG. 22A , the stacked layer type dynamic amount sensor 201 has such a structure that the piezoelectric type pressure sensor 30 has been stacked on the circuit board 240 . An output signal of the piezoelectric type pressure sensor 30 is entered via the penetration electrode 111 and a wiring line 161 to the processing circuit 40 of the circuit board 24 , and thus, is processed in this processing circuit 40 . Then, a signal processed result of the processing circuit 40 is derived from a surface of the diaphragm 31 by the processing circuit 40 and the penetration electrode 111 which penetrates the surface of the diaphragm 31 . Also, the reference pressure chamber 37 of the piezoelectric type pressure sensor 30 is realized by diverting a space which is formed between a surface protection film 241 of the circuit board 240 and the diaphragm 31 . Also, as indicated in FIG. 22B , another penetration electrode 111 for supply the drive power to the processing circuit 40 has been provided.
Referring now to FIG. 23A to FIG. 23F , a description is made of a method for manufacturing the stacked layer type dynamic amount sensor 201 according to this embodiment.
Firstly, as shown in FIG. 23A , the diaphragm 31 into which the piezoelectric resistors 32 have been internally formed, and the circuit board 240 are prepared, and then are adhered to each other. In the circuit board 240 , the processing circuit 40 and the wiring line 161 made of aluminum are provided on a silicon substrate. As one example as to the adhering methods, both the diaphragm 31 and the circuit board 240 may be surface-processed in a vacuum atmosphere, and may be joined to each other by a surface activating method (direct joining at room temperature). If the direct joining method at the room temperature is conducted, then the following merit may be obtained: That is, the diaphragm 31 can be joined to the circuit board 240 at a temperature lower than a melting point of aluminum which constitutes the wiring line 161 . Alternatively, an anode joining method and a glass joining method using low melting point glass may be employed.
In a step of FIG. 23B subsequent to FIG. 23A , a photo-resist mask forming operation and a reactive ion etching process (will be referred to as “RIE” process hereinafter) are carried out with respect to the insulating film 36 formed on the piezoelectric resistors 32 of the diaphragm 31 so as to form a contact hole 243 in the ground frame 31 b . This RIE process is performed until the wiring line 161 of the circuit board 240 is exposed. In other words, since the wiring line 161 is made of aluminum, this wiring line 161 may function as a stopper when the RIE process is performed.
In a step of FIG. 23C subsequent to FIG. 23B , an oxide film (SiO 2 ) 242 is deposited by way of a CVD (chemical vapor deposition) method on the wall plane of the contact hole 243 . At this time, the oxide film 242 is also deposited even on the wiring line 161 on the bottom plane of the contact hole 243 .
In a step of FIG. 23D subsequent to FIG. 23C , the RIE process is further performed so as to expose the wiring line 161 , and also to form a contact hole 31 e in a portion of the insulating film 36 which covers the piezoelectric resistors 32 .
In a step of FIG. 23E subsequent to FIG. 23D , aluminum is deposited by the CVD method on the contact hole 243 and the contact hole 31 e formed in the oxide film 36 which covers the piezoelectric resistors 32 . At this time, aluminum is also deposited on a space between a portion of the contact hole 243 and the contact hole 31 e formed in the oxide film 36 in order to electrically connect these contact holes 243 and 31 e to each other, so that a pressure sensor-purpose wiring line 33 is formed. It should also be noted that a substance to be deposited is not limited only to aluminum, but may be selected from other metals such as tungsten, and poly-silicon. In a step of FIG. 23F subsequent to FIG. 23E , the surface protection film 35 is deposited in such a manner that this surface protection film 35 covers the pressure sensor-purpose wiring line 33 formed in the preceding step of FIG. 23E . Thereafter, the RIE process is carried out in order to provide a contact hole in the surface protection film 35 , so that such a stacked layer type dynamic amount sensor 201 as shown in FIG. 21 and FIG. 22A to FIG. 22B is accomplished. This contact hole is formed in order to derive a signal of the processing circuit 40 outside this sensor 201 .
Next, a description is made of effects achieved by the stacked layer type dynamic amount sensor 201 of the twelfth embodiment. As a first effect, since the piezoelectric type pressure sensor 30 is stacked on the circuit board 240 , the area occupied by the sensor can be reduced, as compared with such a structure that a piezoelectric type pressure sensor and a circuit board are separately provided.
Also, as a second effect, the penetration electrodes 111 are provided on the ground frame 31 b for supporting the diaphragm 31 so as to connect the piezoelectric resistors 32 to the processing circuit 40 , so that higher reliability can be achieved, as compared with such a structure that the piezoelectric resistor 32 and the processing circuit 40 are not stacked, but are electrically connected to each other by using wires.
As a third effect, the processing circuit 40 is arranged behind the diaphragm 31 with respect to the pressure applied direction, namely arranged via the reference pressure chamber 37 . As a result, the processing circuit 40 can be protected. More specifically, since transistor elements which construct the processing circuit 40 may be readily and adversely influenced by contaminations (for example, contaminations caused by fluid and gas, whose pressure should be detected), it is desirable to arrange that the processing circuit 40 is separated apart from the diaphragm 31 having risks of such contaminations.
It should also be noted that the stacking layer steps need not be carried out in the chip unit as represented in FIG. 23A to FIG. 23F . That is, as explained in the above tenth embodiment, one structural component (for example, piezoelectric type pressure sensor 30 ) may be subdivided in the chip unit, and thereafter, the divided sensor may be stacked on the other structural component (circuit board 240 ) under wafer substrate condition. Also, as described in the above eleventh embodiment, both the structural components (namely, piezoelectric type pressure sensor 30 and circuit board 240 ) may be alternatively stacked to each other under wafer substrate condition.
Thirteenth Embodiment
Referring now to FIG. 24 , a description is made of a stacked layer type dynamic amount sensor 201 according to a thirteenth embodiment. The thirteenth embodiment has the below-mentioned technical different points from those of the twelfth embodiment. That is, in this embodiment a concave portion of a diaphragm 31 of a piezoelectric type pressure sensor 30 is present on the side of a pressure application. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the thirteenth embodiment, and descriptions thereof are omitted.
FIG. 24 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the thirteenth embodiment. As indicated in FIG. 24 , the concave portion of the diaphragm 31 of the piezoelectric type pressure sensor 30 is present on the pressure application side. Then, the piezoelectric resistors 32 have been arranged via a silicon layer which constitutes the diaphragm 31 on an inner side of a bottom plane of the concave portion.
Also, a concave 244 has been formed in a place of the circuit board 240 , which is located opposite to the deforming portion 31 a of the diaphragm 31 in order to become the reference pressure chamber 37 when the piezoelectric type pressure sensor 30 is stacked on the circuit board 240 . This concave 244 is formed in such a plane of the silicon substrate, which is located opposite to a plane thereof into which the processing circuit 40 has been formed. Concretely speaking, after the processing circuit 40 has been formed in the silicon substrate, a portion of the oxide film 242 provided on the plane of this silicon substrate is removed, which is located opposite to the plane thereof where the processing circuit 40 has been formed. Furthermore, while the oxide film 242 which has not been removed is employed as a mask, the silicon substrate is etched so as to form the concave 244 . Then, with respect to the circuit board 240 under such a condition that the concave 244 has been formed, such a piezoelectric type pressure sensor 30 is stacked by the direct joining process. In this piezoelectric type pressure sensor 30 , the piezoelectric resistors 32 , the pressure sensor-purpose wiring 33 , and the deforming portion 31 a have been formed in the silicon substrate. After the direct joining process, the processing circuit 40 is electrically connected to the piezoelectric resistors 32 by utilizing the above-described method for forming the penetration electrodes 111 with reference to FIG. 23A to FIG. 23F , and furthermore, the protection film 241 for protecting the circuit board 240 is provided on the side of the processing circuit 40 .
Also, a signal deriving electrode 245 may be formed on the protection film 241 for protecting the processing circuit 40 , and this signal driving electrode 245 may be connected by a bump, so that the stacked layer type dynamic amount sensor 201 may be formed as a flip chip.
Effects of this embodiment will now be described. As a first effect, since the sensor 201 is formed in the flip chip, a total number of wiring lines exposed at portions which are exposed to the open air can be decreased (in particular, total number should be preferably decreased to zero). As a second effect, while the concave 244 is formed at the rear plane of the processing circuit 40 where no element is formed, this concave 244 is utilized as the reference pressure chamber 37 , so that the capacity of the reference pressure chamber 37 can be secured. As a consequence, in order to secure the capacity of the reference pressure chamber 37 , either a spacer or an insulating film is no longer provided between the piezoelectric type pressure sensor 30 and the circuit board 240 (otherwise, may be provided).
Fourteenth Embodiment
Referring now to FIG. 25A to FIG. 25B , a description is made of a stacked layer type dynamic amount sensor 201 according to a fourteenth embodiment. This embodiment is different from the above-described twelfth embodiment as to the following technical point: That is, the processing circuit 40 has been formed on such a side of the circuit board 240 , which is located opposite to the reference pressure chamber 37 .
It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the fourteenth embodiment, and descriptions thereof are omitted.
FIG. 25A and FIG. 25B are sectional views for indicating the stacked layer type dynamic amount sensor 201 according to the fourteenth embodiment. Also, FIG. 25A corresponds to FIG. 22A in the twelfth embodiment, and FIG. 25B corresponds to FIG. 22B in the twelfth embodiment. As shown in FIG. 25A and FIG. 25B , the processing circuit 40 has been formed on a plane of the circuit board 240 , which is located opposite to the reference pressure chamber 37 , namely, has been formed on the plane of this circuit board 240 along a direction opposite to the pressure applied direction of the diaphragm 31 .
Firstly, a detailed description is made of FIG. 25A . The pressure sensor-purpose wiring line 33 has been provided within the surface protection film 35 provided on the pressure applied side of the diaphragm 31 . The pressure sensor-purpose wiring line 33 electrically connects the piezoelectric resistors 32 to the penetration electrodes 111 within the ground frame 31 b . Furthermore, the penetration electrodes 111 have been electrically connected to wiring lines 161 formed inside the protection film 241 which is provided on the surface of the circuit board 240 where the processing circuit 40 is present. Since the wiring lines 161 are set in the above-described manner, the piezoelectric resistors 32 have been electrically connected to the processing circuit 40 .
Next, a description is made of FIG. 25B . In FIG. 25B , one wiring line 161 is partially exposed from the protection film 241 , and constitutes a processing circuit-purpose pad 41 for a bonding process. This wiring line 161 is different from the wiring line of FIG. 25A , and passes through the inner portion of the protection film 241 provided on the surface of the circuit board 240 . Also, the other wiring line 161 which passes through the protection film 241 has been electrically connected to a penetration electrode 111 which is different from that of FIG. 22A and has been provided in the ground frame 31 b . Then, an edge portion of this penetration electrode 111 is exposed from the surface protection film 35 provided on the pressure applied side of the diaphragm 31 , and then constitutes the processing circuit-purpose pad 41 .
Since the above-described structure is employed, in accordance with the stacked layer type dynamic amount sensor 201 of the fourteenth embodiment, the output signals of the processing circuit 40 may be derived not only from the edge plane of the diaphragm 31 on the pressure applied side, but also from the edge plane of the circuit board 240 , which is located opposite side from the pressure applied side.
It should be noted that in this embodiment, the stacked layer type dynamic amount sensor 201 has been made of such a structure that the piezoelectric pressure sensor 30 is stacked on the circuit board 240 , and the signals are derived from both planes of the stacked elements. However, this structure is merely one example. For instance, in the structure of FIG. 1A to FIG. 1C , if such a penetration electrode which penetrates both the N type silicon substrate 21 and the insulating film 26 is provided on the supporting substrate 25 of the capacitance type acceleration sensor 20 , then signals may be inputted and outputted from both the planes of the composite type dynamic amount sensor 1 as explained in this embodiment. In other words, the gist of this embodiment is given as follows: While the penetration electrode is provided, the signals are inputted and outputted from both the planes of either the composite type dynamic amount sensor 1 or the stacked layer type dynamic amount sensor 201 . As a consequence, the structure of the sensor 1 , or 201 is not limited only to the structures shown in FIG. 22A and FIG. 22B .
Fifteenth Embodiment
Referring now to FIG. 26 , a description is made of a stacked layer type dynamic amount sensor 201 according to a fifteenth embodiment. The fifteenth embodiment has the below-mentioned technical different points from those of the above-described embodiments. That is, in this embodiment, a pressure sensor-purpose wiring line 33 has been formed by an impurity diffusion layer. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the fifteenth embodiment, and descriptions thereof are omitted.
FIG. 26 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the fifteenth embodiment. As shown in FIG. 26 , the piezoelectric resistors 32 have been formed on such a plane of the diaphragm 31 , which is located opposite to the side thereof to which pressure is applied. Furthermore, an impurity diffusion layer formed by diffusing an impurity into the silicon substrate is located adjacent to the diaphragm 31 in such a manner that this impurity diffusion layer is electrically connected to these piezoelectric registers 32 . Then, the pressure sensor-purpose wiring line 33 made of this impurity diffusion layer has been electrically connected via the penetration electrode 111 provided on the circuit board 240 to this circuit board 240 .
Also, as shown in FIG. 26 , the plane of the circuit board 240 , in which the processing circuit 40 has been formed, is faced to the reference pressure chamber 37 .
Although not shown in the drawing, a method for manufacturing the above-described stacked layer type dynamic amount sensor 201 will now be described. As a first step, such a piezoelectric type pressure sensor 30 is prepared on which the diaphragm 31 , the piezoelectric resistors 32 , and the pressure sensor-purpose wiring line 33 made of the impurity diffusion layer have been formed. Also, such a circuit board 240 is prepared which contains the processing circuit 40 , the protection film 241 for protecting the processing circuit 40 , and the wiring line 161 which is provided within this protection film 241 and is electrically connected to the processing circuit 40 .
As a second step, an edge plane of the diaphragm 31 on the side where the pressure sensor-purpose wiring line 33 made of the impurity diffusion layer is present is directly joined to such a plane of the circuit board 240 on the side where the processing circuit 40 is present.
As a third step, a contact hole is formed in such a plane of the circuit board 240 on the side where the processing circuit 40 is not present, while this contact hole is connected to the pressure sensor-purpose wiring line 33 made of the impurity diffusion layer. Furthermore, another contact hole which is connected to the wiring line 161 is formed in the above-described plane of the circuit board 240 .
As a fourth step, poly-silicon, or the like is deposited by the CVD method in such a manner that the contact holes formed in the third step are electrically connected to each other. With executions of the above-described steps, the stacked layer type dynamic amount sensor 201 of FIG. 26 can be manufactured.
As an effect achieved by the stacked layer type dynamic amount sensor 201 of the fifteenth embodiment, since not only the processing circuit 40 but also the piezoelectric resistors 32 are present on the side of the reference pressure chamber 27 , these processing circuit 40 and piezoelectric resistors 32 can be hardly contacted to the open air. In other words, the environmental resistance characteristic of this stacked layer type dynamic amount sensor 201 can be increased, as compared with such a case that these processing circuit 40 and piezoelectric resistors 32 are exposed to the open air.
Sixteenth Embodiment
Referring now to FIG. 27 and FIG. 28A to FIG. 28E , a description is made of a stacked layer type dynamic amount sensor 201 according to a sixteenth embodiment. The sixteenth embodiment has the below-mentioned technical different points from those of the above-described twelfth embodiment. That is, in this embodiment, the circuit board 240 has been stacked on the capacitance type acceleration sensor 20 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the sixteenth embodiment, and descriptions thereof are omitted.
FIG. 27 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the sixteenth embodiment. As indicated in FIG. 27 , a plane of the circuit board 240 on the side thereof where the processing circuit 40 is present is stacked with respect to such plane of the capacitance type acceleration sensor 20 on the side thereof where the fixed portion 24 and the movable portion 23 are present. Also, an output signal of the fixed portion 24 is once derived via one penetration electrode 111 provided on the circuit board 240 to another plane of the circuit board 240 on the side thereof where the processing circuit 40 is not present. Furthermore, this derived output signal is electrically connected via another penetration electrode 111 to the wiring line 161 present on the plane of the circuit board 240 on the side thereof where the processing circuit 40 is not present. Then, this wiring line 161 has been connected to the input terminal of the processing circuit 40 .
As another feature, as represented in FIG. 27 , the SiN film 27 is not present on at least the movable portion 23 , or the thickness of this SiN film 27 is made thinner, as compared with thickness of the SiN films 27 of the outer frame 22 and the fixed portion 24 . As a consequence, the movable portion 23 has a clearance with respect to the circuit board 240 , and such a structure which is movable along the same direction as the elongation direction of the supporting substrate 25 . On the other hand, in order that the circuit board 240 can be stacked under stable condition, the SiN films 27 are present on either portions or entire portions of the fixed portion 24 and the outer frame 22 . In the case shown in FIG. 27 , in order to simplify the step for removing the SiN films 27 , while the SiN film 27 is provided on the outer frame 22 , the clearance between the movable portion 23 and the circuit board 240 may be secured by this SiN film 27 .
Referring now to FIG. 28A to FIG. 28E , a method for manufacturing the above-described stacked layer type dynamic amount sensor 201 will now be described. As a first step, such a circuit board 240 is prepared which contains the processing circuit 40 , the protection film 241 for protecting the processing circuit 40 , and the wiring line 161 which is provided within this protection film 241 and is electrically connected to the processing circuit 40 . Also, the capacitance type acceleration sensor 20 is prepared which has been formed in the above-described steps of FIG. 5 and FIG. 6 .
As a second step shown in FIG. 28A , the SiN films 27 formed on the movable portion 23 and the fixed portion 24 of the capacitance type acceleration sensor 20 of FIG. 5B are made thin, or are removed. It should be understood that although the SiN film 27 formed on the fixed portion 24 is not always made thin, or not always removed, since there are many possibilities that the movable portion 23 is located close to the fixed portion 24 , if all of these SiN films 27 are removed, then the film removing process can be carried out in a higher efficiency.
As a third step shown in FIG. 28B , the SiN film 27 of the capacitance type acceleration sensor 20 is directly joined to the plane of the circuit board 240 on the side thereof where the processing circuit 40 is present at the room temperature.
As a fourth step of FIG. 28C , similar to each of the respective embodiments, contact holes 243 are provided by the RIE process. Concretely speaking, one contact hole 243 is formed which passes through the circuit board 240 and is reached to the silicon layer of the fixed portion 24 (and/or movable portion 23 ) of the capacitance type acceleration sensor 20 , and another contact hole 243 is formed which is reached to the wiring line 161 within the circuit board 240 .
As a fifth step shown in FIG. 28D , an oxide film 242 is deposited on a surface of the contact hole 243 by the CVD method.
As a sixth step shown in FIG. 28E , after the oxide film 242 is removed which is deposited on the surface of the silicon layer whose potential is equal to that of either the wiring line 161 or the fixed portion 24 (and/or movable portion 23 ) of the capacitance type acceleration sensor 20 , aluminum is deposited on a region which couples the contact hole 243 to the contact hole 243 . As a result, either the fixed portion-purpose wiring line 24 c (and/or movable portion-purpose wiring line 23 c ) or the fixed portion 24 (and/or movable portion 23 ) of the capacitance type acceleration sensor 20 is electrically connected to the processing circuit 40 , and also, the output signal of the processing circuit 40 can be derived from the plane of the circuit board 240 on the side thereof where the processing circuit 40 is not formed. Deriving of this output signal of the processing circuit 40 may be carried out by a wire bonding, or by a flip-chip connection. Furthermore, the substance to be deposited is not limited only to aluminum, but also may be made of other metals such as tungsten, or poly-silicon.
With employment of the above-described structure, in accordance with the stacked layer type dynamic amount sensor 201 of the sixteenth embodiment, both the movable portion 23 and the fixed portion 24 can be sealed in the sealing space 246 which is formed by the circuit board 240 and the capacitance type acceleration sensor 20 . As a result, such a cap is no longer required which is employed so as to protect both a movable portion and a fixed portion of a capacitance type acceleration sensor, which is not a stacked layer type acceleration sensor. Also, since the processing circuit 40 is similarly present on the side of the above-described sealing space 246 , the stacked layer type dynamic amount sensor 201 can have a not-easily-broken structure, and also have such a structure which can be hardly and adversely influenced by contaminations from external environments.
Seventeenth Embodiment
Referring now to FIG. 29 , a description is made of a stacked layer type dynamic amount sensor 201 according to a seventeenth embodiment. The seventeenth embodiment has the below-mentioned technical different points from those of the sixteenth embodiment. That is, in this embodiment, a plane of the circuit board 240 , on which the processing circuit 40 has been formed, is largely different from the opposite side of the above-described sixteenth embodiment. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the seventeenth embodiment, and descriptions thereof are omitted.
FIG. 29 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the seventeenth embodiment. As indicated in FIG. 29 , the processing circuit 40 has been formed on a plane of the circuit board 240 , which is located opposite to another plane thereof on which the movable portion 23 and the fixed portion 24 of the capacitance type acceleration sensor are present. In other words, the processing circuit 40 has been formed on such a plane which is located opposite to the stacked plane which stacks the capacitance type acceleration sensor on the circuit board 240 .
As previously explained, since the processing circuit 40 is provided on the plane opposite to the stacked plane, a total number of the penetration electrodes 111 can be reduced and the sensor structure can be made simpler, as compared with the sensor structure shown in FIG. 27 . Concretely speaking, in such a case where the processing circuit 40 is present on the side of the capacitance type acceleration sensor and the capacitance type acceleration sensor is electrically connected to the processing circuit 40 , a signal must be once derived by the penetration electrode 111 to the surface of the circuit board 240 , and furthermore, the signal must be inputted to the processing circuit 40 of the circuit board 240 on the side of the sealing space by employing another penetration electrode 111 . However, in accordance with the sensor structure of this embodiment, when the capacitance type acceleration sensor is electrically connected to the processing circuit 40 , the signal is once derived by the penetration electrode 111 to the surface of the circuit board 240 , and may be directly conducted to the processing circuit 40 .
Eighteenth Embodiment
Referring now to FIG. 30 , a description is made of a stacked layer type dynamic amount sensor 201 according to an eighteenth embodiment. The eighteenth embodiment has the below-mentioned technical different points from those of the respective embodiments. That is, in this embodiment, piezoelectric type pressure sensor 30 , a capacitance type acceleration sensor 20 , and a circuit board 240 have been stacked with each other. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the eighteenth embodiment, and descriptions thereof are omitted.
FIG. 30 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the eighteenth embodiment. As indicated in FIG. 30 , the capacitance type acceleration sensor 20 has been stacked on the circuit board 240 , and furthermore, the piezoelectric type pressure sensor 30 has been stacked on the capacitance type acceleration sensor 20 . It should also be understood that structures as to the circuit board 240 , the capacitance type acceleration sensor 20 , and the piezoelectric type pressure sensor 30 are substantially identical to the structures employed in the above-explained respective embodiments.
Subsequently, a method for manufacturing the above-described stacked layer type dynamic amount sensor 201 will now be described. As a first step, such a circuit board 240 is prepared which contains the processing circuit 40 , the protection film 241 for protecting the processing circuit 40 , and the wiring line 161 which is provided within this protection film 241 and is electrically connected to the processing circuit 40 . Also, a capacitance type acceleration sensor 20 is prepared.
In a second step subsequent to the first step, the supporting substrate side of the capacitance type acceleration sensor 20 is directly joined to the protection film 241 on the circuit board 240 on the side thereof where the processing circuit 40 is present at the room temperature. It should also be noted that this joining process may be replaced by a glass adhesive method, or an anode joining process.
In a third step subsequent to the second step, similar to the above-described respective embodiments, a contact hole is formed until the silicon layer of the movable portion 23 (and fixed portion 24 ) present under the insulating film 27 (SiN film etc.) of the capacitance type acceleration sensor 20 is exposed by employing the RIE process. Also, another contact hole is similarly formed until the input wiring line 247 of the circuit board 240 is exposed.
In a fourth step subsequent to the third step, aluminum is deposited so as to embed the contact holes formed in the above-described third step, and also, in order that the contact holes are electrically connected to each other by the CVD method, so that the fixed portion-purpose wiring line 24 c is produced. It should be noted that the substance to be deposited is not limited only to aluminum, but may be selected from other metals such as tungsten, and poly-silicon.
In a fifth step subsequent to the fourth step, a surface protection film 28 is formed in such a manner that the SiN film 27 of the capacitance type acceleration sensor 20 and the fixed portion-purpose wiring line 24 c formed in the third step are covered. Thereafter, both the movable portion and the fixed portion shown in FIG. 5 and FIG. 6 are formed.
In a sixth step subsequent to the fifth step, the diaphragm 31 in which the piezoelectric resistors 32 have been internally provided is prepared, and the ground frame 31 b is directly joined to the surface protection film 28 of the capacitance type acceleration sensor 20 .
In a seventh step subsequent to the sixth step, a photo-resist mask forming process and a reactive ion etching process (will be referred to as “RIE” process hereinafter) are carried out with respect to the insulating film 36 formed on the piezoelectric resistors 32 of the diaphragm 31 so that a plurality of contact holes are formed in the ground frame 31 b . This RIE process is carried out until both an input wiring line 247 and an output wiring line 248 of the circuit board 240 are exposed. In other words, the contact holes correspond to such holes which pass through the ground frame 31 b , the surface protection film 28 of the capacitance type acceleration sensor 20 , the SiN film 27 of the capacitance type acceleration sensor 20 , the N type silicon substrate 21 of the capacitance type acceleration sensor 20 , the insulating film 26 of the capacitance type acceleration sensor 20 , and the supporting substrate 25 of the capacitance type acceleration sensor 20 , and then, are reached to the input wiring line 247 of the circuit board 240 .
In an eighth step subsequent to the seventh step, aluminum is deposited in such a manner that the plural contact holes formed in the seventh step are embedded and are electrically connected to each other by executing the CVD process. At this time, the contact hole communicated with the input wiring line 247 of the processing circuit 40 is electrically connected to the contact holes communicated with the piezoelectric resistors 32 by aluminum. Also, poly-silicon is simply deposited in the contact hole communicated with the output wiring line 248 , which constitutes the penetration electrodes 111 .
In a ninth step subsequent to the eighth step, a surface protection film 35 is provided in such a manner that the surface protection film 35 covers the aluminum and the insulating film 36 on the diaphragm 31 formed in the eighth step. Furthermore, an opening portion is formed in this surface protection film 35 so as to expose an edge portion of the penetration electrode 111 communicated with the output wiring line 248 , so that such a pad 249 used to derive an output signal of the processing circuit 40 is formed. It should be noted that the substances to be deposited in the eighth step and the ninth step are not limited only to aluminum, but may be selected from other metals such as tungsten, and poly-silicon.
Subsequently, a description is made of effects achieved by the stacked layer type dynamic amount sensor 201 of the eighteenth embodiment. As a first effect, since the piezoelectric type pressure sensor 30 , the capacitance type acceleration sensor 20 , and the circuit board 240 are stacked with each other, an area occupied by the sensors can be reduced, as compared with a sensor occupied area of such a structure that a piezoelectric type pressure sensor, a capacitance type acceleration sensor, and a circuit board are separately provided.
Also, as a second effect, under such a condition before the piezoelectric type pressure sensor 30 is adhered to the capacitance type acceleration sensor 20 , namely under such a condition that the capacitance type acceleration sensor 20 has been adhered to the circuit board 240 , the penetration electrodes 111 are provided, and the output of the capacitance type acceleration sensor 20 can be entered to the processing circuit 40 . As a result, the simple structure can be made. Concretely speaking, the structure of this embodiment can reduce a total number of the penetration electrodes 111 , as compared with the below-mentioned structure: That is, an output of a capacitance type acceleration sensor is derived up to a diaphragm by a first penetration electrode, and furthermore, the output of the capacitance type acceleration sensor derived up to the diaphragm is entered to a processing circuit by a second penetration electrode which electrically connects the first penetration electrode to the processing circuit.
Nineteenth Embodiment
Referring now to FIG. 31 , a description is made of a stacked layer type dynamic amount sensor 201 according to an nineteenth embodiment. The nineteenth embodiment has the below-mentioned technical different points from those of the eighteenth embodiment. That is, in this embodiment, after the piezoelectric type pressure sensor 30 , the capacitance type acceleration sensor 20 , and the circuit board 240 have been stacked with each other, all of the penetration electrodes 111 are formed. It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the nineteenth embodiment, and descriptions thereof are omitted.
FIG. 31 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the nineteenth embodiment. As indicated in FIG. 31 , the capacitance type acceleration sensor 20 has been stacked on the circuit board 240 , and further, the piezoelectric type pressure sensor 30 has been stacked on the capacitance acceleration sensor 20 . It should also be noted that the circuit board 240 , the capacitance type acceleration sensor 20 , and the piezoelectric type pressure sensor 30 have the substantially same structures as those of these structural members employed in the above-described respective embodiments.
A technical different point between the above-described eighteenth embodiment shown in FIG. 30 and the present embodiment is given as follows: That is, the plurality of penetration electrodes 111 formed on the diaphragm 31 , and the fixed portion wiring line 24 c for electrically connecting these penetration electrodes 111 are present. Precisely speaking, one penetration electrode 111 passes through the ground frame 31 b from the N type silicon substrate 21 of the capacitance type acceleration sensor 20 , and is communicated to the upper portion of the diaphragm 31 . The other penetration electrode 111 penetrates the ground frame 31 b and the capacitance acceleration sensor 20 from the upper portion of the diaphragm 31 , and is communicated to the input wiring line 247 of the processing circuit 40 .
Next, a method for manufacturing the above-described stacked layer type dynamic amount sensor 201 of the nineteenth embodiment will now be described. As a first step, such a circuit board 240 is prepared which contains the processing circuit 40 , the protection film 241 for protecting the processing circuit 40 , and wiring lines 247 and 248 which are provided within this protection film 241 and are electrically connected to the processing circuit 40 . Also, the capacitance type acceleration sensor 20 is prepared which has been formed in the above-described steps of FIG. 5 and FIG. 6 , and further, the diaphragm 31 is prepared into which the piezoelectric resistors 32 have been internally provided. Then, these circuit board 240 , the capacitance type acceleration sensor 20 , and diaphragm 31 are adhered to each other by executing the direct joining process at the room temperature.
In a second step subsequent to the first step, a photo-resist mask forming process and a reactive ion etching process (will be referred to as “RIE” process hereinafter) are carried out with respect to the oxide film 36 formed on the piezo electric resistors 32 of the diaphragm 31 so that a plurality of contact holes are formed in the ground frame 31 b . This RIE process is carried out until a silicon substrate plane which is electrically connected to the fixed portion 24 of the capacitance type acceleration sensor 20 is exposed, and also another silicon substrate plane which is electrically connected to the movable portion 23 thereof is exposed.
In a third step subsequent to the second step, a photo-resist mask forming process and a reactive ion etching process (will be referred to as “RIE” process hereinafter) are carried out with respect to the oxide film 36 formed on the piezoelectric resistors 32 of the diaphragm 31 so that a plurality of contact holes are formed in the ground frame 31 b . This RIE process is carried out until both the input wiring line 247 and the output wiring line 248 of the circuit board 240 are exposed. In other words, the contact holes correspond to such holes which pass through the ground frame 31 b , the surface protection film 28 of the capacitance type acceleration sensor 20 , the SiN film 27 of the capacitance type acceleration sensor 20 , the N type silicon substrate 21 of the capacitance type acceleration sensor 20 , the insulating film 26 of the capacitance type acceleration sensor 20 , and the supporting substrate 25 of the capacitance type acceleration sensor 20 , and then, are reached to the input and output wiring liens 247 and 248 of the circuit board 240 .
In a fourth step subsequent to the third step, aluminum is deposited in such a manner that the plural contact holes formed in the second step and the third step are embedded and are electrically connected to each other by executing the CVD process. At this time, the contact hole communicated with the input wiring lien 247 of the processing circuit 40 is electrically connected to the contact holes communicated with the piezoelectric resistors 32 by aluminum so as to constitute the pressure sensor-purpose wiring line 33 . Similarly, the contact hole communicated with the input wiring line 247 of the processing circuit 40 is electrically connected to the contact hole communicated with such a silicon layer whose potential is equal to that of the movable portion 23 (and fixed portion 24 ) of the capacitance type acceleration sensor 20 by aluminum so as to constitute the fixed portion-purpose wiring line 24 c . Also, poly-silicon is merely deposited on the contact hole communicated with the output wiring line 248 of the processing circuit 40 so as to constitute the penetration electrode 111 . It should also be noted that the substance to be deposited is not limited only to aluminum, but may be selected from other metals such as tungsten, and poly-silicon.
In a fifth step subsequent to the fourth step, the surface protection film 35 is provided in such a manner that the surface protection film 35 covers the poly-silicon and the oxide film 36 on the diaphragm 31 formed in the fourth step. Furthermore, an opening portion is formed in this surface protection film 35 so as to expose the edge portion of the penetration electrode 111 communicated with the output wiring line 248 , so that such a pad 249 used to derive an output signal of the processing circuit 40 is formed. As a result, the stacked layer type dynamic amount sensor 201 of FIG. 31 can be manufactured.
Since the above-described structure is provided and the manufacturing method is carried out, the stacked layer type dynamic amount sensor 201 of this embodiment can have the below-mentioned effects: That is, as a first effect, the piezoelectric type pressure sensor 30 , the capacitance type acceleration sensor 20 , and the circuit board 240 are stacked with each other, and all of the penetration electrodes 111 are formed under such a condition that the movable portion 23 has been sealed in the reference pressure chamber 37 . As a result, there is no risk that particles and cleaning water produced when the penetration electrodes 111 are formed enter spaces between the movable portion 23 and the fixed portion 24 , which may cause the sticking phenomenon.
As a second effect, the output signal of the capacitance type acceleration sensor 20 is once derived above the diaphragm 31 . In this case, for example, if a portion of the surface protection film 35 covered on the diaphragm 31 is removed so as to expose the pressure sensor-purpose wiring line 33 which connects the penetration electrode 111 to the penetration electrode 111 , then the capacitance type acceleration sensor 20 can be checked.
Twentieth Embodiment
Referring now to FIG. 32 , a description is made of a stacked layer type dynamic amount sensor 201 according to a twentieth embodiment. The twentieth embodiment has the below-mentioned technical different points from those of the eighteenth embodiment. That is, in this embodiment, a ceramic chip 250 where a wiring line 251 has been provided is sandwiched between the capacitance type acceleration sensor 20 and the circuit board 240 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the twentieth embodiment, and descriptions thereof are omitted.
FIG. 32 is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the twentieth embodiment. As indicated in FIG. 32 , the ceramic chip 250 where the wiring line 251 has been provided is sandwiched between the capacitance type acceleration sensor 20 and the circuit board 240 . While this ceramic chip 250 contains such a structure manufactured by combining an oxide film with the wiring line 251 , a peripheral edge portion of the wiring line 251 has been exposed from a predetermined portion (namely, place where wiring line 251 is contacted with below-mentioned penetration electrodes 111 ). Then, as an entire structure of the stacked layer type dynamic amount sensor 201 , the piezoelectric type pressure sensor 30 , the capacitance type acceleration sensor 20 , the ceramic chip 250 , and the circuit board 240 have been sequentially stacked with each other in this order from the pressure application side.
Next, a description is made of a method for manufacturing the stacked layer type dynamic amount sensor 201 of the twentieth embodiment. Firstly, as a first step, such a circuit board 240 , the capacitance type acceleration sensor 20 manufactured by the steps shown in FIGS. 5A to 6B described above and the ceramic chip 250 are prepared. The circuit board 240 contains the processing circuit 40 and the protection film 241 which protects the processing unit 40 . In the ceramic chip 250 , the peripheral edge portion of the wiring line 251 has been exposed at the predetermined portion (place where wiring line 251 is contacted with below-mentioned penetration electrode 111 ). These circuit board 240 , the sensor 20 and ceramic chip 250 are joined to each other by the direct joining process at the room temperature. At this time, the wiring line 251 is electrically connected to the processing circuit 40 . It should also be noted that as the substance which constitutes the wiring line 251 , metals such as aluminum, copper and tungsten may be employed.
In a second step subsequent to the first step, one penetration electrode 111 is formed in such a manner that the peripheral edge portion of the wiring line 251 is electrically connected to the fixed portion 24 (otherwise, movable portion 23 ) of the capacitance type acceleration sensor 20 . The wiring line 251 has been connected to such a place which is used to process an output signal of the capacitance type acceleration sensor 20 in the processing circuit 40 .
In a third step subsequent to the second step, the piezoelectric type pressure sensor 30 is directly joined to the capacitance type acceleration sensor 20 .
In a fourth step subsequent to the third step, another penetration electrode 111 is formed in such a manner that the peripheral edge portion of the wiring line 251 is connected to the piezoelectric resistors 32 . The wiring line 251 has been connected to such a place which is used to process an output signal of the piezoelectric type pressure sensor 30 in the processing circuit 40 . Also, another penetration electrode 111 is formed which is communicated with the peripheral edge portion of the wiring line 251 connected to an output place of an output signal in the processing circuit 40 , and drives this output signal above the diaphragm 31 . These penetration electrodes 111 have passed through the capacitance type acceleration sensor 20 so as to be connected to the wiring line 251 of the ceramic chip 250 .
Since the stacked layer type dynamic amount sensor 201 of this embodiment, which has such a structure, employs the above-described ceramic chip 250 , the following effect may be achieved. That is, there is a high freedom degree when the wiring lines are routed. It should also be noted that the present embodiment has exemplified the stacked layer type dynamic amount sensor 201 in the unit of chip. Alternatively, while a plurality of such stacked layer type dynamic amount sensors 201 are integrated on a wafer, these stacked layer type dynamic amount sensors 201 may be manufactured under wafer condition.
Twenty-first Embodiment
Referring now to FIG. 33A to FIG. 33B and FIG. 34 , a description is made of a stacked layer type dynamic amount sensor 201 according to a twenty-first embodiment. The twenty-first embodiment has the below-mentioned technical different points from those of the above-described twentieth embodiment. That is, in this embodiment, a deriving electrode 245 has been provided on a side plane of the ceramic chip 250 . It should be understood that the same reference numerals shown in the above-described respective embodiments will be employed as those for denoting the same, or similar structural elements in the twenty-first embodiment, and descriptions thereof are omitted.
FIG. 33A is a sectional view for showing the stacked layer type dynamic amount sensor 201 according to the twenty-first embodiment. FIG. 33B is a sectional view of the sensor 201 , taken along a line XXXIIIB-XXXIIIB of FIG. 33A . As shown in FIG. 33A , the deriving electrode 245 has been provided on the side plane of the ceramic chip 250 , namely, along a direction perpendicular to a stacking direction of the capacitance type acceleration sensor 20 and the piezoelectric type pressure sensor 30 . This deriving electrode 245 has been connected to the wiring line 251 which connects the capacitance type acceleration sensor 20 to the processing circuit 40 . In other words, an output signal of the capacitance type acceleration sensor 20 may be derived from this deriving electrode 245 . As represented in FIG. 33B , a plurality of such deriving electrodes 245 have been formed on the side plane of the ceramic chip 250 . Concretely speaking, various sorts of output signals from the movable portion 23 , the fixed portion 24 , the piezoelectric resistors 32 , and the processing circuit 40 are derived from these deriving electrodes 245 formed on the side plane of the ceramic chip 250 . As shown in FIG. 33A , these deriving electrodes 245 have been fixed by a bump joining 252 with respect to lead frames of the package 253 , and have been electrically connected thereto. Also, these deriving electrodes 245 have been alternately arranged with respect to the stacking direction. The substance for constructing the wiring line 251 may be selected from metals such as aluminum, copper, and tungsten.
In such a case that a plurality of stacked layer type dynamic amount sensors 201 of this embodiment are manufactured in an integral manner, as represented in FIG. 34 , if one deriving electrode 245 and the other deriving electrode 245 are formed by being faced with each other, then the formed deriving electrodes 245 are dicing-cut along a dot line, and thus, one deriving electrode 245 may be divided from the other deriving electrode 245 . As other methods than the above-described dicing-cut method, after the structure of FIG. 32 has been formed, the deriving electrodes 245 may be formed by employing the CVD process, or the like. Alternatively, as shown in FIG. 33A , a spacer 254 having a height substantially equal to the height of the bump join 252 is set among the insulating film 26 , the SiN film 27 , and the package 253 , so that the stacked layer type dynamic amount sensor 201 is horizontally supported with respect to the package 253 .
Next, a description is made of effects achieved by the stacked layer type dynamic amount sensor 201 of the twenty-first embodiment. As a first effect, the output signals of the respective sensors can be derived from the deriving electrodes 245 formed on the side plane of the ceramic chip 250 , so that the stacked layer type dynamic amount sensor 201 can be vertically installed with respect to the bottom plane of the package 253 . Also, as a second effect, in addition to the above-described merit that the output signals of the respective sensors can be derived from the deriving electrodes 245 formed on the side plane of the ceramic chip 250 , similar to the above-described twentieth embodiment, the output signal of the processing circuit 40 may be derived from the upper portion of the diaphragm 31 . In other words, the output signals may be derived from at least 2 planes which have no parallel relationship with each other.
Other Embodiments
In the above-described first to tenth embodiments, either the piezoelectric type pressure sensor or the capacitance type pressure sensor has been stacked with respect to the capacitance type acceleration sensor. However, combinations of these sensors to be stacked are not limited only to the above examples. For example, a capacitance type acceleration sensor may be stacked with respect to a capacitance type angular velocity (yaw rate) sensor, or a pressure sensor may be alternatively be stacked on the capacitance type angular velocity sensor. Also, a piezoelectric resistor type pressure sensor may be alternatively stacked on a piezoelectric resistor type acceleration sensor. Furthermore, acceleration sensors whose detection directions are different from each other may be alternatively stacked with each other in such a manner that these acceleration sensors are located opposite to each other. Also, acceleration sensors for 3 axes may be alternatively formed in such a way that the acceleration sensors for X-axis and Y-axis directions are formed on one substrate, whereas the acceleration sensor for a Z-axis direction is formed on another substrate. Moreover, although the detecting directions are equal to each other, as represented in FIG. 19 , acceleration sensors whose sensitivities are different from each other may be alternatively stacked with each other.
In the above-described eleventh to seventeenth embodiments, either the capacitance type acceleration sensor or the piezoelectric type pressure sensor has been stacked on the circuit board. However, combinations of these sensors to be stacked are not limited only to the above example. For instance, a capacitance type angular velocity (yaw rate) sensor may be alternatively stacked on a circuit board, or a capacitance type pressure sensor may be alternatively stacked on the circuit board.
The composite type dynamic amount sensor 1 shown in the above-explained embodiments first to ninth, and the stacked layer type dynamic amount sensor 201 indicated in the twelfth to twenty-first embodiments may be alternatively manufactured in accordance with such a manufacturing method that semiconductor wafer substrates are stacked with each other, and thereafter, the stacked semiconductor wafer substrate may be dicing-cut to obtain the respective chips. Also, as to stacking methods for semiconductor wafer substrates with each other, when no NCF is interposed between the substrates, a direct joining method at the room temperature, a direct joining method at a high temperature, a glass adhering method, and an anode joining method may be arbitrarily selected.
While the invention has been described with reference to preferred embodiments thereof, it is to be understood that the invention is not limited to the preferred embodiments and constructions. The invention is intended to cover various modification and equivalent arrangements. In addition, while the various combinations and configurations, which are preferred, other combinations and configurations, including more, less or only a single element, are also within the spirit and scope of the invention.
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A physical quantity sensor for detecting a physical quantity includes: a first substrate having a first physical quantity detection element; a second substrate having a second physical quantity detection element, wherein the second substrate contacts the first substrate; and an accommodation space disposed between the first substrate and the second substrate. The first physical quantity detection element is disposed in the accommodation space. The first physical quantity detection element is protected with the first substrate and the second substrate since the first physical quantity detection element is sealed in the accommodation space.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 14/210,987 filed Mar. 14, 2014, which claims the benefit of U.S. Provisional Patent Application Nos. 61/794,064 filed Mar. 15, 2013, and 61/793,712 filed Mar. 15, 2013, the entire disclosures of which are incorporated by reference herein.
FIELD OF THE INVENTION
[0002] Embodiments of the present invention are generally related to a tapered line production device and method and, in particular, to a device and method for efficient production of tapered fishing line through the use of heat transfer media.
BACKGROUND OF THE INVENTION
[0003] Drawing Polyethylene (PE) fiber (a process where a thermoplastic yarn is heated and elongated to result in a stronger but thinner yarn) is a well-known process, and has been used to increase strength of fibrous materials. Drawing PE fiber allows tremendous flexibility in final product sizing, oftentimes producing different products from the same feeder stock.
[0004] By changing the draw ratio during a production run, it is possible to create a tapered line that has a thick section (lower draw ratio, e.g. 1.1×) and a thinner section (higher draw ratio, e.g. 2.0×). In one example, the thick portion of the taper is 50% stronger than the thin portion.
[0005] The purpose of the thicker, stronger section is to have enough strength to offset the reduction due to making a knot. A good knot in 80 lb line breaks around 50 lbs. By creating a line with 80 lbs in a thicker section (designated for knot tying), and then tapering down to 50 lbs in the thinner section, one creates a line that has the same load carrying performance as an all 80 lb line, yet with increased capacity on the reel (and reduced drag in the water) because the line is not all at the thicker diameter. The thick/thin section may repeat, for example, every 25 feet to allow anglers to cut off only 25 feet each time they exhaust the thicker knot section of the line.
[0006] Production rates are affected by dwell time in heat transfer media. For example, if it takes 20 seconds to heat and draw braid to a desired ratio, the longer the “oven” (or heat transfer device) the faster the output. Here, the word “oven” indicates an intuitive concept of any heat transfer media. A double length of oven will allow double output speed at a given temperature. However, the draw happens throughout the length of the oven, so as long as one is making a constant diameter product there is no production penalty.
[0007] In the specific case of a tapered line of the invention, it is desired to taper from the thin portion to the thicker portion of the line within a short period or length. This requires a short oven to localize the taper. However, the throughput cost of such a short oven may be 10× slower than the regular process due to long dwell time, thus resulting in a cost-prohibitive process. With the invention herein disclosed, a reduced processing time to between 2× to 3× is achieved.
[0008] Therefore, there is a long-felt need for a production device and method that can efficiently and effectively yield a tapered line of varying thickness. The present device and method of operation addresses and solves these needs. The present invention relates to a device and method for efficient production of tapered fishing line through the use of heat transfer media. The device and method allow, among other things, a means to create tapered fishing line with minimal transitional distances between tapered sections and may operate at higher rates of production than conventionally provided.
[0009] By way of providing additional background and context, the following reference is incorporated by reference in its entirety for the purpose of explaining various methods of tapering fishing lines: U.S. Pat. No. 7,081,298 to Nakanishi.
SUMMARY OF THE PREFERRED EMBODIMENTS
[0010] It is one aspect of the present invention to provide a programmable, movable trolley assembly that allows for relatively quick and drastic draw ratio changes in line, such as braided superline, without negatively impacting processing speeds is disclosed. The trolley interfaces with the line at the point of entry into the heat transfer media. Nominal thickness line is produced at a nominal draw ratio by passing line through a heat transfer media. The line enters the upper portion of a trolley device positioned proximal the heat transfer media. The line then is routed to a lower portion of the trolley where it is immersed in the heat transfer media. The line exits the heat transfer media having been stretched or drawn to a thinner diameter. During this process, the trolley is stationary at a first or entry end of the heat transfer media. To produce a line portion which is relatively thicker than the nominal thickness line, the trolley moves with the line from the first or entry end of the heat transfer media toward the second or exit end of the heat transfer media. The trolley travels down all or some of the length of the heat transfer media with the line at the desired point of draw ratio decrease to delay entry of any new length of braid into the heat transfer media. The trolley also allows the length of braid already in the tank to continue to be drawn to its maximum length. The trolley then stops at a pre-determined point along the heat transfer media length (which may include the second or exit end of the heat transfer media) to allow un-drawn material to enter a shorter length of heat transfer media, thus experiencing a shorter draw rate (and thus produce a relatively thicker diameter line). The trolley then returns to its original location to repeat the process. In this way, a line with variable thickness is produced.
[0011] Stated another way:
Step 1: The braided line running on the machine is run through the full length of heat transfer media and stretched to the maximum desired elongation ratio at the maximum preferred input speed. Step 2: When the point of the braid where the desired decreased draw ratio length is located begins to pass through the trolley device and into the heat transfer media (located at the input end of the heat transfer media), the trolley begins to move through the heat transfer media at the exact input speed of the braid until it reaches the desired location along the heat transfer media length. At the same time, the output speed of the rollers retrieving the braid out of the heat transfer media begins to decrease to the desired low-draw ratio speed at a rate equal to that of the travel time of the interface device. Step 3: A length of braid enters the heat transfer media and is exposed to a shorter length of heat transfer media and drawn to its desired smaller draw ratio using the same preferred input speed as in Step 1. Step 4: When the point of the braid where the desired draw ratio increase is located begins to pass through the trolley (now located toward the output side of the heat transfer media), the trolley begins to move through the heat transfer media at the maximum speed possible to its original position at the input end of the heat transfer media. At the same time, the output speed of the rollers retrieving the braid out of the heat transfer media begins to increase up to the original maximum-draw speed at a rate equal to that of the travel time of the interface device. Step 5: Repeat, i.e. return to Step 1.
[0017] In one embodiment of the invention, a tapered line production device is disclosed, the tapered line production device comprising: a body having a first side, a second side, and a heat transfer assembly positioned therein, the heat transfer assembly adapted to selectively provide thermal energy to a line passing through the heat transfer assembly from the first side to the second side; an input roller operating at a first rate that delivers line to the first side; an output roller operating at a nominal second rate that receives line from the second side; and a moveable trolley assembly engaged with the body, the trolley assembly configured to controllably position the line to selectively engage or not engage with the heat transfer assembly.
[0018] In another embodiment of the invention, a method of producing tapered line is disclosed, the method comprising: providing a device having a body with a first side, a second side, and a heat transfer assembly positioned therein, the heat transfer assembly adapted to selectively provide thermal energy to a line passing through the heat transfer assembly between the first side to the second side; providing a moveable trolley assembly engaged with the body, the trolley assembly configured to controllably position the line to selectively engage or not engage with the heat transfer assembly; receiving the line at the first side by an input roller operating at a first rate; passing the line through the heat transfer assembly so as to elongate the line; outputting a first portion of the line from the second side by an output roller operating at a nominal second rate wherein the first portion of the line has a first diameter; moving the trolley assembly from the first side to the second side at a first speed approximately equal to the first rate wherein the line does not pass through the heat transfer assembly; operating the output roller at a decreasing rate from the nominal second rate to approximately the first rate as the trolley traverses the length of the body from the first side to the second side; outputting a second portion of the line from the second side wherein the second portion of the line has a second diameter larger than the first diameter; wherein a tapered line is produced.
[0019] In one aspect of the invention, the device and/or method further comprises a controller, which may comprise a Programmable Logic Controller, which controls at least one of the input roller, output roller and trolley. In one embodiment of the invention, the nominal second rate of the output roller is greater than the first rate of the first roller. In another aspect of the invention, the trolley is configured to traverse at least a portion of the length of the body from the first side to the second side at a first speed, and/or wherein the first speed may be approximately the speed of the line delivered to the first side, and/or wherein as the trolley traverses the length of the body from the first side to the second side, the output roller decreases from the nominal second rate to approximately the first rate and/or wherein the trolley is configured to traverse the length of the body from the second side to the first side at a second speed, and/or a plurality of lines are delivered to the first side. In another aspect of the invention, the line comprises polyethylene, and/or the heat transfer media is a resin bath, and/or the first speed is selectable by a user. In one embodiment of the invention, as the trolley traverses the length of the body from the first side to the second side, the nominal second rate of the output roller remains constant while the first rate of the input roller varies. In another embodiment of the invention, as the trolley traverses the length of the body from the first side to the second side, the nominal second rate of the output roller varies and the first rate of the input roller varies.
[0020] In another embodiment of the invention, a tapered line production system is disclosed, the method comprising: a body having a first side, a second side, and a heat transfer assembly positioned therein, the heat transfer assembly adapted to selectively provide thermal energy to a line passing through the heat transfer assembly from the first side to the second side; an input roller operating at a first rate that delivers line to the first side; an output roller operating at a nominal second rate that receives line from the second side, the nominal second rate greater than the first rate; a moveable trolley assembly engaged with the body, the trolley assembly configured to controllably position the line to selectively engage or not engage with the heat transfer assembly while the trolley traverses at least a portion of the body from the first side to the second side at a first speed; and a controller which controls at least one of the input roller, output roller and trolley; wherein the first speed is approximately the speed of the line delivered to the first side; wherein as the trolley traverses the length of the body from the first side to the second side, the output roller decreases from the nominal second rate to approximately the first rate; wherein the line comprises polyethylene, fluorocarbon, nylon, olefins, polyester, and thermoplastic and is configured as at least one of monofilament, co-filament, multi-filament, twisted, braided, thermally-fused and chemically-fused line; and wherein the heat transfer media is a resin bath.
[0021] The term “automatic” and variations thereof, as used herein, refers to any process or operation done without material human input when the process or operation is performed. However, a process or operation can be automatic, even though performance of the process or operation uses material or immaterial human input, if the input is received before performance of the process or operation. Human input is deemed to be material if such input influences how the process or operation will be performed. Human input that consents to the performance of the process or operation is not deemed to be “material.”
[0022] The terms “determine”, “calculate” and “compute,” and variations thereof, as used herein, are used interchangeably and include any type of methodology, process, mathematical operation or technique.
[0023] The term “line” or “braided line” shall mean any cord that has elastic properties and may be stretched, without breaking, such as by a source of thermal energy. Line shall include, without limitation, fishing lines and lines comprising polyethylene, fluorocarbon, nylon, olefins, polyester, and other thermoplastic materials in multi-filament or monofilament forms. Line shall include, without limitation, twisted, braided, co-filament, monofilament and thermally-fused or chemically-fused lines (also known as “superlines”).
[0024] The term “resin” shall mean any liquid substance that will set into a solid substance, to include, without limitation, synthetic or natural or organic resins.
[0025] It shall be understood that the term “means” as used herein shall be given its broadest possible interpretation in accordance with 35 U.S.C., Section 112, Paragraph 6. Accordingly, a claim incorporating the term “means” shall cover all structures, materials, or acts set forth herein, and all of the equivalents thereof. Further, the structures, materials or acts and the equivalents thereof shall include all those described in the summary of the invention, brief description of the drawings, detailed description, abstract, and claims themselves.
[0026] It is important to note that the transition length from long draw ratio to short draw ratio or short draw ratio to long draw ratio is directly related to the length of braid in the heat transfer media at the time of draw ratio transition. To achieve a short transition length the braid length exposed in the heat transfer media must be short. Alternately, the shorter the braid length in the heat transfer media, the lower the processing speed. The movable trolley allows one to maximize processing speed and minimize the transition lengths by adjusting the braid length in the heat transfer media depending on process step.
[0027] One of ordinary skill in the art will appreciate that embodiments of the present disclosure may be constructed of materials known to provide, or predictably manufactured to provide the various aspects of the present disclosure. These materials may include, for example, stainless steel, titanium alloy, aluminum alloy, chromium alloy, and other metals or metal alloys. These materials may also include, for example, carbon fiber, ABS plastic, polyurethane, and other fiber-encased resinous materials, synthetic materials, polymers, and natural materials.
[0028] This Summary of the Invention is neither intended nor should it be construed as being representative of the full extent and scope of the present disclosure. The present disclosure is set forth in various levels of detail in the Summary of the Invention as well as in the attached drawings and the Detailed Description of the Invention, and no limitation as to the scope of the present disclosure is intended by either the inclusion or non-inclusion of elements, components, etc. in this Summary of the Invention. Additional aspects of the present disclosure will become more readily apparent from the Detailed Description, particularly when taken together with the drawings.
[0029] The above-described benefits, embodiments, and/or characterizations are not necessarily complete or exhaustive, and in particular, as to the patentable subject matter disclosed herein. Other benefits, embodiments, and/or characterizations of the present disclosure are possible utilizing, alone or in combination, as set forth above and/or described in the accompanying figures and/or in the description herein below. However, the Detailed Description of the Invention, the drawing figures, and the exemplary claims set forth herein, taken in conjunction with this Summary, define the invention.
[0030] As used herein, “at least one”, “one or more”, and “and/or” are open-ended expressions that are both conjunctive and disjunctive in operation. For example, each of the expressions “at least one of A, B and C”, “at least one of A, B, or C”, “one or more of A, B, and C”, “one or more of A, B, or C” and “A, B, and/or C” means A alone, B alone, C alone, A and B together, A and C together, B and C together, or A, B and C together.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention and together with the general description of the invention given above, and the detailed description of the drawings given below, serve to explain the principals of this invention.
[0032] FIG. 1 depicts a schematic representation of the device of the invention in one preferred embodiment;
[0033] FIG. 2 is a cut-away side-view of a representation of a portion of the device in one preferred embodiment;
[0034] FIGS. 3A-H are schematic representations of various states of the device in one embodiment;
[0035] FIGS. 4A-C are an example construction of a portion of the device in one preferred embodiment; and
[0036] FIG. 5 is an example construction of a portion of the device in one preferred embodiment. This figure is to scale.
[0037] It should be understood that the drawings are not necessarily to scale. In certain instances, details that are not necessary for an understanding of the invention or that render other details difficult to perceive may have been omitted. It should be understood, of course, that the invention is not necessarily limited to the particular embodiments illustrated herein.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0038] FIGS. 1-5 show various embodiments of the Device 100 of the present invention.
[0039] FIGS. 1 and 2 depict schematic representations of the Device 100 of the invention in one preferred embodiment. Generally, the Device 100 comprises a Feeder Stock Spool 110 , which provides raw braid Line 102 to the Device 100 . The Line 102 unwinds and travels along the direction of the arrows shown, i.e. generally right to left. The Line 102 travels through two consecutive Loop One 112 and Loop Two 114 . In other embodiments of the invention, no such loops are employed, or a different number of such loops are employed, such as one or a plurality of loops. The Line 102 then travels to Input Roller 120 which is in communication with Controller 200 . The Controller 200 also may be in communication with one or more of the Output Roller 180 , Trolley 160 , and Heat Transfer Assembly 140 . The Controller 200 may be a Programmable Logic Control (PLC) or any controller known to those skilled in the art. For example, any digital or analog control that may, among other things, comprise controlling the speed (RPM) of the Input Roller 120 , the speed (RPM) of the Output Roller 180 , positioning (to include speed) of the Trolley 160 , and thermal parameters (such as temperature) of the Heat Transfer Assembly 140 . After engaging the Input Roller 120 , the Line 102 engages Roller One 122 , Roller Two 124 and Roller Three 126 . In other embodiments of the invention, no such rollers are employed, or a different number of such rollers are employed, such as one or a plurality of rollers.
[0040] Line 102 continues in a generally right to left direction to optionally engage one or more inking stations. FIG. 1 depicts Line 102 engaging a sequence of Inking Station One 132 , Inking Station Two 134 and Inking Station 136 . The Line 102 is colored or inked during engagement with the one or more inking stations.
[0041] The Line 102 then enters the Heat Transfer Assembly 140 , comprising a Heat Transfer Assembly First End 141 with Heat Transfer Assembly Line Input End 142 (where Line 102 enters the Heat Transfer Assembly 140 ), and Heat Transfer Assembly Second End 143 with Heat Transfer Assembly Line Output End 144 (where Line 102 exits the Heat Transfer Assembly 140 ). Within the Heat Transfer Assembly 140 the Line 102 engages the Trolley 160 and may pass through a portion of the Heat Transfer Volume 150 comprising a Heat Transfer Volume Upper End 152 .
[0042] Upon exiting the Heat Transfer Assembly 140 , the former Line 102 , having passed through the Heat Transfer Assembly 140 , is deemed Finished Line 104 . The Finished Line 104 optionally engages Roller Four 174 before engaging Output Roller 180 . Output Roller 180 , by adjusting its rotational speed (that is RPM), generally determines the amount of time a particular portion of Line 102 will remain within Heat Transfer Assembly 140 , which determines the diametrical thickness of Finished Line 104 . A tapered product will have Finished Line 104 of varying thickness, e.g. thick to thin to thick.
[0043] After engaging Output Roller 180 , Finished Line 104 may optionally engage one or more of Roller Five 182 , Roller Six 184 and Loop Three 186 before engaging Take-up Reel or Spool 190 . The Finished Line 104 is gathered at Take-up Reel 190 . In one embodiment, the Take-up Reel 190 comprises a clutch mechanism.
[0044] In one embodiment, the Input Roller 120 and Roller One 122 are an integrated assembly in which Line 102 winds around both elements before continuing downstream of the Device 100 (i.e. generally right to left and toward the Heat Transfer Assembly 140 ). More specifically, the Input Roller 120 and Roller One 122 are an integrated assembly commonly called a Godet Roller by one skilled in the art. A Godet Roller enables, among other things, tension to be applied to the assembly of Input Roller 120 and Roller One 122 without imparting tension upstream, e.g. to the Stock Spool 110 . Similarly, in one embodiment, the Output Roller 180 and Roller Five 182 are an integrated assembly in which Line 104 winds around both elements before continuing downstream of the Device 100 (i.e. generally right to left and toward the Take-up Reel 190 ). More specifically, the Output Roller 180 and Roller Five 182 are an integrated assembly such as a Godet Roller.
[0045] The device 100 comprises a Controller Display 210 and a Motor 220 . In one embodiment, the Motor 220 is a DC motor, although any means of driving one or more of the Input Roller 120 , Output Roller 180 , and Trolley 160 may be employed.
[0046] Specifically as depicted in FIG. 2 , Trolley 160 comprises a Trolley Upper Wheel 162 which receives Line 102 through Heat Transfer Assembly Line Input End 142 and routes the line to Trolley Lower Wheel 164 before directing the line out of Heat Transfer Assembly 140 via Heat Transfer Assembly Line Output End 144 . Note that the line leaving Trolley Lower Wheel 164 is below the Heat Transfer Volume Upper End 152 and therefore is contained within the Heat Transfer Volume 150 .
[0047] Trolley 160 may be driven within the Heat Transfer Assembly 140 by any means known to those skilled in the art, to include one or more rails. For example, two linear rails may be employed as shown in FIG. 2 as Trolley Lower Rail Assembly 166 and Trolley Lower Rail Assembly 167 .
[0048] The Heat Transfer Assembly 140 may be any means known to those skilled in the art to provide thermal transfer, to include ovens such as convection ovens, liquids, and gases to include heated air. In one embodiment, the Heat Transfer Assembly 140 may comprise heated surfaces, such as heated rollers, which engage the line.
[0049] In one preferred embodiment, the Heat Transfer Assembly 140 operates between approximately 120 degree and 180 degree Celsius. In a more preferred embodiment, Heat Transfer Assembly 140 operates between approximately 130 degree and 170 degree Celsius.
[0050] In another preferred embodiment, the Heat Transfer Assembly 140 operates at approximately 150 degree Celsius.
[0051] In one embodiment, the Heat Transfer Assembly 140 comprises a plurality of individually-controlled heat or temperature zones. The temperature zones may be any combination of multiple horizontally-spaced or separated temperature zones or vertically-spaced or separated temperature zones. Such zones, among other things, create different draw ratios for line immersed therein, thereby creating different relative line thicknesses.
[0052] In one embodiment, the Heat Transfer Assembly 140 is a resin bath, such as a wax bath or wax resin bath.
[0053] Referring to FIGS. 3A-H , a schematic representation of various states of the Device 100 is provided. Generally, Line 102 travels from Input Roller 120 into Heat Transfer Assembly 140 and to Output Roller 180 . Within the Heat Transfer Assembly 140 , Line 102 engages Trolley 160 and may engage (i.e. pass through) a portion of Heat Transfer Volume 150 .
[0054] The amount of time a given portion of Line 102 engages the Heat Transfer Volume 150 (i.e. the “dwell time) determines the potential relative thickness of the diameter of Line 102 . A portion of Line 102 engaging a greater amount of Heat Transfer Volume 150 (i.e. a Line 102 with a relatively longer or greater dwell time) may become more elongated (drawn farther) and thus thinner than a portion of Line 102 that engages the same Heat Transfer Volume 150 for a shorter amount of time (ie. a shorter or smaller dwell time with less draw potential).
[0055] The device 100 allows a given input Line 102 to receive differing dwell times and therefore result in a Line 102 of differing elongation or diametrical thickness. A sequence of sequential states D N of the Device 100 is provided in FIGS. 3A-H , where N=1 through 8. Also shown in FIGS. 3A-H are states T N of the Trolley 160 and states O N of the Output Roller 180 . Input Roller 120 typically operates at a constant speed.
Device State D 1 (FIG. 3 A)
[0000]
T 1 : Trolley 160 stationary at Heat Transfer Assembly First End 141
O 1 : Output Roller 180 operating at a constant, maximum preferred speed (e.g. O MAX )
Line Engaged with Heat Transfer Assembly 102 ′ being elongated to maximum elongation (thus becoming thinner relative to input Line 102 upstream of Heat Transfer Assembly 140 )
Device State D 2 (FIG. 3 B)
[0000]
T 2 : Trolley 160 departs from Heat Transfer Assembly First End 141 at speed T SET (i.e. begins to move from right to left)
O 2 : Output Roller 180 begins to decrease in rotational speed (i.e. RPM) from the maximum preferred speed (i.e. O MAX ); rate of speed decrease is approximately determined by Trolley travel time from Heat Transfer Assembly First End 141 to Heat Transfer Assembly Second End 143
Line Engaged with Heat Transfer Assembly 102 ′ being elongated to maximum elongation (thus becoming relatively thinner)
Device State D 3 (FIG. 3 C)
[0000]
T 3 : Trolley 160 continues away from Heat Transfer Assembly First End 141 at speed T SET
O 3 : Output Roller 180 continues to decrease in speed from the maximum preferred speed (i.e. O MAX ); rate of speed decrease is approximately determined by Trolley travel time from Heat Transfer Assembly First End 141 to Heat Transfer Assembly Second End 143
Line Engaged with Heat Transfer Assembly 102 ′ being elongated to maximum elongation (thus becoming relatively thinner)
Line Affixed Atop Trolley 102 ″ is not engaged with Heat Transfer Assembly 140 and thus is not undergoing elongation (thus remaining at its nominal diameter and thus relatively thicker with respect to Line Engaged with Heat Transfer Assembly 102 ′)
Device State D 4 (FIG. 3 D)
[0000]
T 4 : Trolley 160 reaches Heat Transfer Assembly Second End 143
O 4 : Output Roller 180 reaches minimum preferred speed (i.e. O MIN )
All of Line Affixed Atop Trolley 102 ″, spanning length of Heat Transfer Assembly 140 , remains atop Trolley 160 and none of Line Atop Trolley 102 ″ has engaged with Heat Transfer Assembly 140 and thus is not elongated (thus remaining at its nominal diameter and thus relatively thicker with respect to Line Engaged with Heat Transfer Assembly 102 ′)
Device State D 5 (FIG. 3 E)
[0000]
T 5 : Trolley 160 momentarily stops at Heat Transfer Assembly Second End 143
O 5 : Output Roller 180 now operating at steady minimum preferred speed (i.e. O MIN )
All of Line Affixed Atop Trolley 102 ″, spanning length of Heat Transfer Assembly 140 , remains atop Trolley 150 and none of Line Atop Trolley 102 ″ has engaged with Heat Transfer Assembly 140 and thus is not elongated (thus remaining at its nominal diameter and thus relatively thicker with respect to Line Engaged with Heat Transfer Assembly 102 ′)
Device State D 6 (FIG. 3 F)
[0000]
T 6 : Trolley 160 departs Heat Transfer Assembly Second End 143 at speed T RETURN toward Heat Transfer Assembly First End 141 (i.e. begins to move left to right)
O 6 : Output Roller 180 begins to accelerate from minimum preferred speed (i.e. O MIN )
Former Line Affixed Atop Trolley 102 ′″ begins to engage with Heat Transfer Assembly 140 and thus begins to undergo elongation proportional to dwell time of particular portion of Former Line Atop Trolley 102 ′″
Device State D 7 (FIG. 3 G)
[0000]
T 7 : Trolley 160 continues toward Heat Transfer Assembly First End 141 at speed T RETURN
O 7 : Output Roller 180 continues to accelerate from minimum preferred speed (i.e. O MIN ) to maximum preferred speed (i.e. O MAX )
Former Line Atop Trolley 102 ′″ continues to engage with Heat Transfer Assembly 140 and continues to undergo elongation proportional to dwell time of particular portion of Former Line Atop Trolley 102 ′″
Device State D 8 (FIG. 3 H)
[0000]
T 8 : Trolley 160 arrives at Heat Transfer Assembly First End 141
O 8 : Output Roller 180 reaches maximum preferred speed (i.e. O MAX )
End of Former Line Atop Trolley 102 ′″ reaches Heat Transfer Assembly Second End 143 ; all line upstream (i.e. to the right) of Former Line Affixed Atop Trolley 102 ′″ will be Line Engaged with Heat Transfer Assembly 102 ′
(Trolley 160 idles, i.e. remains stationary, at Heat Transfer Assembly First End 141 for Trolley Idle Time T IDLE —this is Device State 1 —thus beginning a new cycle of Device States D 1→8 )
[0082] FIGS. 4A-C are an example construction of a portion of the device in one preferred embodiment. This figure is to scale; all dimensions are in inches.
[0083] FIG. 5 is an example construction of a portion of the device in one preferred embodiment. This figure is to scale.
[0084] The invention may use other than polyethylene (PE) fiber as a line. For example, any linearly oriented polymeric structure, braided, twisted or otherwise constructed linear fibrous assembly, thermally fused line, monofilament and those lines known to one skilled in the art that may be manipulated through application of thermal energy, to include manipulation such as tapering, may be used.
[0085] In another embodiment, rather than decreasing the rate of the output roller from the nominal second rate to approximately the first rate as the trolley traverses the length of the body from the first side to the second side, the same relative change in rate (and thus yielding the same tapered effect) between the input and output rollers is achieved by varying one or both of the input and output rollers. That is, in one embodiment of the invention, when the Trolley 160 traverses the length of the Heat Transfer Assembly 140 from the first side to the second side, the second rate of the Output Roller 180 remains constant while the first rate of the Input Roller 120 varies. In another embodiment of the invention, when the Trolley 160 traverses the length of the Heat Transfer Assembly 140 from the first side to the second side, the second rate of the Output Roller 180 varies and the first rate of the Input Roller 120 also varies.
[0086] In one embodiment, one or more computers are used to control, among other things, the RPM (rate) of the input roller, the RPM (rate) of the output roller, the movement and positioning of the trolley, the temperature of the heat transfer assembly, and the RPM (rate) of the stock spool. In one embodiment, a user selectively inputs one or more of the RPM of the input roller, the RPM of the output roller, the movement and positioning of the trolley, the temperature of the heat transfer assembly, and the RPM of the stock spool.
[0087] The user may engage with device and/or controller through a display. The term “display” refers to a portion of one or more screens used to display the output of a computer to a user. A display may be a single-screen display or a multi-screen display, referred to as a composite display. A composite display can encompass the touch sensitive display of one or more screens. A single physical screen can include multiple displays that are managed as separate logical displays. Thus, different content can be displayed on the separate displays although part of the same physical screen. A display may have the capability to record and/or print display presentations and display content, such as reports.
[0088] In one embodiment, the user interacts with the computer through any means known to those skilled in the art, to include a keyboard and/or display to include a touch-screen display. The term “computer-readable medium” as used herein refers to any tangible storage and/or transmission medium that participate in providing instructions to a processor for execution. Such a medium may take many forms, including but not limited to, non-volatile media, volatile media, and transmission media. Non-volatile media includes, for example, NVRAM, or magnetic or optical disks. Volatile media includes dynamic memory, such as main memory. Common forms of computer-readable media include, for example, a floppy disk, a flexible disk, hard disk, magnetic tape, or any other magnetic medium, magneto-optical medium, a CD-ROM, any other optical medium, punch cards, paper tape, any other physical medium with patterns of holes, a RAM, a PROM, and EPROM, a FLASH-EPROM, a solid state medium like a memory card, any other memory chip or cartridge, a carrier wave as described hereinafter, or any other medium from which a computer can read. A digital file attachment to e-mail or other self-contained information archive or set of archives is considered a distribution medium equivalent to a tangible storage medium. When the computer-readable media is configured as a database, it is to be understood that the database may be any type of database, such as relational, hierarchical, object-oriented, and/or the like. Accordingly, the disclosure is considered to include a tangible storage medium or distribution medium and prior art-recognized equivalents and successor media, in which the software implementations of the present disclosure are stored.
[0089] Computer processing may include any known to those skilled in the art, to include desktop personal computers, laptops, mainframe computers, mobile devices and other computational devices.
[0090] In yet another embodiment, the disclosed systems and methods may be partially implemented in software that can be stored on a storage medium to include a computer-readable medium, executed on programmed general-purpose computer with the cooperation of a controller and memory, a special purpose computer, a microprocessor, or the like. In these instances, the systems and methods of this disclosure can be implemented as program embedded on personal computer such as an applet, JAVA® or CGI script, as a resource residing on a server or computer workstation, as a routine embedded in a dedicated measurement system, system component, or the like. The system can also be implemented by physically incorporating the system and/or method into a software and/or hardware system.
[0091] Communications means and protocols, such as those used to communicate between a user display and controller, may include any known to those skilled in the art, to include cellular telephony, internet and other data network means such as satellite communications and local area networks. As examples, the cellular telephony can comprise a GSM, CDMA, FDMA and/or analog cellular telephony transceiver capable of supporting voice, multimedia and/or data transfers over a cellular network. Alternatively or in addition, other wireless communications means may comprise a Wi-Fi, BLUETOOTH™, WiMax, infrared, or other wireless communications link. Cellular telephony and the other wireless communications can each be associated with a shared or a dedicated antenna. Data input/output and associated ports may be included to support communications over wired networks or links, for example with other communication devices, server devices, and/or peripheral devices. Examples of input/output means include an Ethernet port, a Universal Serial Bus (USB) port, Institute of Electrical and Electronics Engineers (IEEE) 1394, or other interface. Communications between various components can be carried by one or more buses.
[0092] As will be appreciated, it would be possible to provide for some features of the inventions without providing others.
[0093] The present invention, in various embodiments, includes components, methods, processes, systems and/or apparatus substantially as depicted and described herein, including various embodiments, sub-combinations, and subsets thereof. Those of skill in the art will understand how to make and use the present invention after understanding the present disclosure. The present invention, in various embodiments, includes providing devices and processes in the absence of items not depicted and/or described herein or in various embodiments hereof, including in the absence of such items as may have been used in previous devices or processes, for example for improving performance, achieving ease and/or reducing cost of implementation.
[0094] The foregoing discussion of the invention has been presented for purposes of illustration and description. The foregoing is not intended to limit the invention to the form or forms disclosed herein. In the foregoing Detailed Description for example, various features of the invention are grouped together in one or more embodiments for the purpose of streamlining the disclosure. This method of disclosure is not to be interpreted as reflecting an intention that the claimed invention requires more features than are expressly recited in each claim. Rather, as the following claims reflect, inventive aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the following claims are hereby incorporated into this Detailed Description, with each claim standing on its own as a separate preferred embodiment of the invention.
[0095] Moreover though the description of the invention has included description of one or more embodiments and certain variations and modifications, other variations and modifications are within the scope of the invention, e.g., as may be within the skill and knowledge of those in the art, after understanding the present disclosure. It is intended to obtain rights which include alternative embodiments to the extent permitted, including alternate, interchangeable and/or equivalent structures, functions, ranges or steps to those claimed, whether or not such alternate, interchangeable and/or equivalent structures, functions, ranges or steps are disclosed herein, and without intending to publicly dedicate any patentable subject matter. For example, the steps may be performed in any order and are not limited to the particular ordering discussed herein.
[0000]
Reference No.
Component
100
Device
102
Line
102′
Line Engaged with Heat Transfer Assembly
102″
Line Affixed Atop Trolley
102′″
Former Line Affixed Atop Trolley
104
Finished Line
110
Feeder Stock Spool
112
Loop One
114
Loop Two
120
Input Roller
122
Roller One
124
Roller Two
126
Roller Three
132
Inking Station One
134
Inking Station Two
136
Inking Station Three
140
Heat Transfer Assembly
141
Heat Transfer Assembly First End
142
Heat Transfer Assembly Line Input End
143
Heat Transfer Assembly Second End
144
Heat Transfer Assembly Line Output End
150
Heat Transfer Volume
152
Heat Transfer Volume Upper End
160
Trolley
162
Trolley Upper Wheel
164
Trolley Lower Wheel
166
Trolley Upper Rail Assembly
167
Trolley Lower Rail Assembly
174
Roller Four
180
Output Roller
182
Roller Five
184
Roller Six
186
Loop Three
190
Take-up Reel
200
Controller
210
Controller Display
220
Motor
D N
Device State N
T IDLE
Trolley Idle Time
T N
Trolley State N
T RETURN
Trolley Return Speed
T SET
Trolley Set Speed
O N
Output Roller State N
O MIN
Output Roller Minimum Speed
O MAX
Output Roller Maximum Speed
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The present invention provides a tapered line production device and method for efficiently producing line of varying thickness. An additional aspect of the present invention is to employ a heat transfer media to provide a tapered fishing line production device and method that operates at high rates of production. Further, the device may be configured to create tapered fishing line with minimal transitional distances between tapered sections.
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FIELD OF THE INVENTION
The present invention relates to a centrifugal separator for the separation of two liquids having different densities from a mixture thereof. The centrifugal separator is of the kind comprising a rotor body having a separation chamber, having a stack of conical separation discs arranged coaxially with the rotor in the separation chamber with their base portions facing one end and their apex portions facing the other end of the separation chamber, a central inlet chamber, inlet passages connecting the inlet chamber with the separation chamber at the end of the latter towards which the apices of the separation discs face and separate outlets for relatively light and relatively heavy separated liquid, which two outlets are situated at one and the same axial outlet end of the rotor, said inlet passages having substantially the same inclination relative to the rotor axis as the separation discs. A centrifugal separator of this kind is shown e.g. in the Swedish Patent No. 19666 from the year 1904. It is unknown whether a centrifugal separator of this kind has been produced and used in practice.
The term "conical separation discs" refers to the type of completely conical or frusto-conical plates employed in centrifugal separators since von Bechtolsheim's invention, disclosed in German Patent No. 48615 of 19 Sept. 1889. The term "conical", used to describe these discs, is employed in its common geometric sense to mean the surface generated by the whole or part of the hypoteneuse of a right triangle when the triangle is rotated about one leg. The "apex" end of the conical surface is the narrow end and the "base" end is the broad end.
BACKGROUND OF THE INVENTION
From the turn of the century and onwards centrifugal separators have normally not been designed in the manner described. Instead, the inlet of the separation chamber has been situated at the end of the separation chamber, towards which the base portions of the separation discs face. A conventional centrifugal separator of this kind is shown e.g. in U.S Pat. No. 3,986,663. However, even centrifugal separators of the latter kind have a rotor with outlets for the two separated liquids situated at one and the same axial end of the rotor. This has several advantages. Among other things the outlet members of the rotor, which may have to be adjusted, are more easily accesible. Furthermore, use of stationary so called paring members for the discharge of the separated liquids from the rotor is facilitated.
A principle advantage of a centrifugal separator of the first kind, into which a mixture is introduced in the separation chamber at the end, towards which the apices of the separation discs face, is that a pre-separation, which takes place in the inlet passages before the mixture enters the separation chamber, can be taken advantage of to the maximum. Thus, part of the relatively heavy liquid component and possibly solids in the liquid mixture, may be separated, even as the mixture, is on its way through said inlet passages between the central inlet chamber and the inlet of the separation chamber. Relatively heavy component of the supplied mixture, separated in the inlet passages, may slide along the outer walls of the inlet passages directly out into the outermost part of the separation chamber radially outside the separation discs without being disturbed by or disturbing the rest of the mixture when this flows into the separation chamber.
In a conventional centrifugal separator, in which the liquid mixture is introduced through inlet passages at the end of the separation chamber, towards which the base portions of the separation discs face, (see e.g. U.S. Pat. No. 3,986,663), a relatively heavy component of the mixture, separated in the inlet passages, is forced to cross the flow of the rest of the mixture as the latter enters the separation chamber. This is a consequence of the fact that the inlet passages have an inclination relative to the rotor axis just about the same as that of the conical separation discs. Thereby, the result of the pre-separation in the inlet passages is spoiled wholly or partly. This undesired effect of the cross flow will be greatest when the entire mixture is introduced into the separation chamber at the outer edge of the separation disc situated closest to the inlet passages.
The object of the present invention is to provide a centrifugal separator, whose rotor in the first place has the arrangement, known at least since 1904, for introducing a liquid mixture into the separation chamber and, in the second place, has both the outlets for the separated liquids available at one and the same end of the rotor. The centrifugal separator has an improved design enabling more effective separation of two liquids having different densities than a centrifugal separator of the kind shown in the above mentioned Swedish Patent No. 19666.
SUMMARY OF THE INVENTION
In accordance with the invention this object is achieved by means of a centrifugal separator of the initially defined kind, characterized in that at least one outlet channel extends from a radially outer part of the separation chamber towards the rotor center at the end of the separation chamber towards which the base portions of the separation discs face and that this outlet channel communicates with the rotor outlet for separated heavy liquid at said outlet end of the rotor.
In a centrifugal separator according to the invention pre-separation in said inlet passages may be taken advantage of to its maximum extent as the relatively heavy liquid component of the mixture is given a long axial flow path in the separation chamber. Thereby relatively heavy liquid may be separated effectively from relatively light liquid and simultanteously freed from solids present in the mixture, which are heavier than the relatively heavy liquid. Furthermore, both the separated liquids are available for discharge from the rotor at one and the same end thereof.
Within the scope of the invention it is possible to locate both the rotor outlets for the separated liquids at either of the rotor ends, the rotor being connected with a driving shaft at its opposite end. However, in a preferred embodiment of the invention the two rotor outlets are situated at the end of the rotor, towards which the apex portions of the separation discs face, outlet means having at least one through channel being arranged to conduct relatively heavy separated liquid from said outlet channel axially through the separation chamber to the rotor outlet for the separated heavy liquid. Thereby, the rotor can be connected with the driving shaft so that its point of gravity will be located as close as possible to the drive and its bearings, viewed axially.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be described more fully with reference to the accompanying drawings in which:
FIG. 1. is a schematic view partly in vertical section of a centrifugal separator according to a preferred embodiment of the invention;
FIG. 2, is a plan view of an element of the centrifugal separator of FIG. 1;
FIG. 3. is a view in vertical section of a somewhat modified element of the centrifugal separator shown in FIG. 1;
FIG. 4. shows a modified embodiment of an element of the separator shown in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a centrifugal separator having a rotor 1, a vertical drive shaft 2 supporting the rotor, a driving device 3 in engagement with the drive shaft, a lower housing 4 for the driving device 3 and an upper housing 5 for the rotor.
The upper housing 5 forms an inlet tube 6 for a mixture of two liquids having different densities and particles suspended therein. Further, the housing 5 forms a receiving chamber 7 having an outlet 8 for separated relatively light liquid and a receiving chamber 9 having an outlet 10 for a separated relatively heavy liquid.
The rotor comprises two rotor parts 11 and 12, which are kept axially pressed against each other and which surround a separation chamber 13. The rotor part 11, which forms the bottom of the separation chamber 13 and is connected with the driving shaft 2, has a central column 14, the upper part of which holds the rotor part 12 by means of an annular locking member 15. The rotor part 12 forms a substantially cylindrical surrounding wall and a substantially conical upper end wall of the rotor.
A narrow end portion of the inlet tube 6 extends axially through the locking member 15 into a central inlet chamber 16 formed in a tubular upper portion of the central column 14. This tubular portion of the column 14 has several openings 17 in its surrounding wall. The locking member 15 forms an upper annular end wall in the inlet chamber 16.
Around the central column 14 there is arranged a partition member having a sleeve formed part 18 and a conical part 19. The sleeve formed part 18 surrounds the column 14 below said openings 17. An annular gasket seals between the sleeve formed part 18 and the column 14. The conical part 19 abuts against said upper end wall of the rotor. Radial recesses in the conical part 19 form between this and the rotor end wall several passages 20, which connect the openings 17 with the separation chamber 13.
Between the conical part 19 and the lower rotor part 11 there is arranged in the separation chamber 13 coaxially with the rotor axis a set of frusto-conical separation discs 21. The outer edges of the separation discs 21 are situated substantially at the same radial level as the outer edge of the previously mentioned conical part 19. The inner edges of the separation discs 21 are situated at some radial distance outside the sleeve formed part 18, so that a central space is formed in the separation chamber 13 radially inside of the separation discs 21. This space is divided in parallel axial channels by radially and axially extending wings supported by the sleeve formed part 18.
The conical part 19 has a number of, for instance three, axial throug-channels 22 and supports on its upper side an equal number of tubular members 23, the interior of which communicates with the channels 22. Also the rotor part 12 has an equal number of axial through-channels 24, which are situated such that they communicate through the tubular members 23 with the respective channels 22. An annular gasket is arranged to seal between the tubular members 23 and the rotor part 12 around the channels communicating with each other.
On the top of the rotor part 12 there is arranged an annular member 25, which together with the rotor part 12 forms a chamber 26, in which the channels 24 through the rotor part 12 are opening. The chamber 26 has one or several peripheral outlets 27.
In the lower part of the separation chamber 13 there is placed an annular member 28, which axially inwards and axially down wards seals against the rotor part 11 and extends radially outwards into the separation chamber 13 a distance longer than the separation discs 21. On its under side the annular member 28 has a number or radial grooves, which form channels 29 extending between the separation chamber 13 and an equal number of central radial channels 30 in the rotor part 11. The radial channels 30 communicate with a number of axial channels 31, in which axial tubes 32 are inserted.
The tubes 32 extend through aligned holes in the separation discs 21 and further through holes in the previously mentioned conical part 19, holes in the rotor part 12 and holes in the annular member 25. Sealing gaskets are arranged around said holes and around the tubes 32 between the rotor part 12 and the conical part 9 and the annular member 25, respectively.
The interior of the tubes 32, which through the channels 29-31 communicates with the separation chamber 13, opens into a radially inwards open groove 33 in the annular member 25. The upper edge of the groove 33 forms an overflow outlet 34 therefrom.
From the radially innermost part of each channel 30 a draining channel 35 extends through the rotor part 11 to the outside of the rotor. A shielding member 36 is connected with the driving shaft 2 and is arranged to prevent liquid leaving the rotor through the draining channels 35 from flowing down into the housing 4 of the driving device. The rotor housing 5 has a separate outlet 37 for such liquid.
FIG. 2 shows from above the partition member that comprises the conical part 19. Apart from the three previously mentioned tubular members 23 three futher tubular members 38 are shown, through the openings of which the tubes 32 (FIG. 1) are intended to be inserted. As can be best seen from FIG. 2 the tubular members 38 are situated at a greater radius than the tubular members 23. Radially and axially extending ridges 39 on the upper side of the conical part 19 form between themselves the previously mentioned recesses which together with the rotor part 12 form the passages 20 in FIG. 1.
Around its circumference the conical part 19 has a number of recesses 40, the function of which is to be described later. Corresponding recesses axially aligned with the recesses 40 are present in all of the separation disc 21 in the separation chamber 13.
FIG. 3 shows a section through a somewhat modified partition member comprising a conical part 19a, a sleeve formed part 18a and tubular members 23a and 38a. The partition member shown in FIG. 3 is intended to be made entirely of plastic, and as can be seen the tubular members 23a and 38a have been shaped in a way enabling a firm connection between these and the rotor part 12. Sleeve formed extensions 41 and 42 having small external annular end flanges 43 and 44, respectively, are dimensioned such that they are resilient when they are inserted in the holes in the rotor part 12 intended therefor.
FIG. 4 shows the upper part of a rotor according to FIG. 1, comprising a partition member according to FIG. 3. The tubular members 23a and 38a are inserted into through-channels in the rotor part 12a. The walls of these channels have annular grooves for receiving the annular end flanges 43 and 44 (FIG. 3). The partition member is thus connected with the rotor part 12a by means of a so called snap-lock connection.
A further so called snap-lock connection is present between the rotor part 12a and the annular member 25a. The latter has an internal annular flange 45 which engages in an external groove in the rotor part 12a.
Instead of a fixed end wall the annular member 25a has a removable and thus exchangeable annular end wall 46, the inner edge of which forms an overflow outlet corresponding to the overflow outlet 34 in FIG. 1. Even the end wall 46 is kept in place at the annular member 25a by means of a so called snap-lock connection.
The centrifugal separator in FIG. 1 is intended to operate in the following manner after the rotor 1 has been put in rotation by means of the driving device 3.
Through the tube 6 a mixture of two liquids having different densities and solids suspended therein are introduced into the central inlet chamber 16. The mixture flows through the openings 17 and the passages 20 to the separation chamber 13. Mainly through the recesses 40 in the conical part 19 and corresponding recesses in the separation discs 21 the mixture is distributed between the separation discs.
Even in the passages 20 a pre-separation of the three components forming the supplied mixture takes place. A large part of the suspended solids and part of the heavier of the liquids move along the rotor part 12 out of the surrounding wall of the separation chamber 13 without interfering with the continued flow of the liquid mixture into the separation chamber. The liquid mixture together with possibly remaining solids is then distributed between the separation discs 21. Between the separation discs the two liquids of different densities are separated, the lightest liquid flowing radially inwards and being conducted through the channels 22 and 24 to the chamber 26, whereas the heaviest liquid flows radially outwards. Outside the separation discs 21 the latter liquid flows axially downwards in the separation chamber and out thereof through the channels 29. It is conducted further through the channels 30 and 31 and by the tube 32 to the annular groove 33.
While the separated heavy liquid leaves over the overflow outlet 34 the separated light liquid leaves through the outlet 27 of the chamber 26. The outlet 27 is so large that the chamber 26 during normal operation is only partly filled. This means that the tubular members 23 and the radially outer limiting walls of the channels 22 and 24 form overflow outlets from the separation chamber 13 for the separated light liquid. The position of the interface layer formed between the two separated liquids in the separation chamber during operation is determined by the position of the two overflow outlets of the separation chamber. The position of the interface layer may be changed by exchange of the annular member 25 for one, whose overflow outlet 34 is situated at a different radial level. As an alternative, of course, an exchangeable so called gravity disc may be arranged in the chamber 26 or the groove 33.
If desired, conventional distribution channels extending axially through the separation discs 21 and the conical part 19 may be situated at any desired distance from the rotor axis.
Upon need the annular member 28 at the bottom of the separation chamber may be exchanged for one having a larger or smaller radial extension.
To remove separated solids from the separation chamber the locking member 15 has to be removed and the rotor parts 11 and 12 have to be separated.
Since the channels 22 and 24 will serve during operation as overflow outlets of the separation chamber 13, a free liquid surface will be formed in the separation chamber radially outside the sleeve formed part 18 around the central column 14. Possible liquid leakage past the gasket between the column 14 and the sleeve formed part 18 therefore will be directed away from the inlet chamber 16 to the separation chamber 13. Since the lower portion of the sleeve formed part 18 is situated at a substantial axial distance from the overflow outlet 24 for separated light liquid, any possible leakage will be of such small magnitude, that it will not influence the separation in the rotor.
In a preferred embodiment of the invention the elements 11, 12 and 32 are made of metal, whereas the elements 18, 19, 25 and 28 are made of plastic. Thereby, instead of separate sealing members such as gaskets placed between the tubular members 23, 38 and the rotor part 12, the tubular members 23 and 38 made of plastic will accomplish sealing by themselves. Preferably this is achieved by shaping the members in question to provide a firm connection, for instance a so called snap-lock connection, between these and the rotor part 12 (FIG. 4). Thus one avoids breaking the important sealing between the tubular members 23, 38 and the rotar part 12 each time the rotor is to be disassembled; in other words the sealing function will be more safe and will not be jeopardized by wear or damage. Furthermore, the disassembling and mounting of the rotor is facilitated by the fact that the latter will consist of a smaller number of parts. Also the uppermost annular member 25 may be formed so that a firm connection may be obtained between this and the rotor part 12 (FIG. 4).
The tubes 32 preferably are fixed to the rotar part 11, so that they can keep the separation discs 21 in unchanges positions when the rotor part 12 is removed. The tubes 32 thus serve as guiding members for the separation discs 21 and prevent them from being turned relative to each other during rotation of the rotor.
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In a centrifuge rotor for separation of two liquids having different densities from a mixture thereof a stack of conical separation discs (21) is arranged in the separation chamber (13) with the base portions of the separation discs turned towards one end and with the apex portions of the separation discs turned towards the other end of the separation chamber. According to the invention the separation chamber (13) has an inlet for mixture situated at the end, towards which the separation discs turn their apex portions, and an outlet for separated relatively heavy liquid situated at the opposite end. The inlet for liquid mixture as well as both outlets for the separated liquids are situated at the same axial end wall of the centrifuge rotor.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a divisional of U.S. patent application Ser. No. 13/361,699, filed Jan. 30, 2012, the contents of which are incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to the field of women's hosiery, such as stockings or tights, and in particular, to a stocking or tights construction, which may be converted from a footed to a footless configuration, or vice versa.
SUMMARY OF THE INVENTION
[0003] The present invention is directed to a women's hosiery construction, which may be easily converted from a footed stocking or tights to a footless hosiery, similar to leggings, wherein the foot portion is turned under when worn in a footless configuration.
[0004] In one embodiment, the end portion of a tubular knitted foot portion for an article of hosiery has a turned welt knitted in around about one half of the perimeter of the end portion, leaving about half of the perimeter unattached such that an opening is formed in the end portion, so that the unattached portion of the end portion may be pulled forward and extended over the wearer's toes and sole of the foot, or alternatively wherein the unattached portion may be folded inwardly into the end portion to form a footless configuration.
[0005] Another embodiment of the present invention is directed to an article of hosiery, comprising a pair of circularly knitted tubular portions, each tubular portion comprising a panty portion, leg portion, and an integrally knitted foot portion as described above.
[0006] Other aspects of the present invention are directed to alternate methods for forming the tubular knitted foot portion and the article of hosiery including the integrally knitted foot portion. In one method, the turned welt is knitted only about one half of the circumference of the end portion, and in an alternate method the turned welt is knitted around the entire circumference, and the unattached portion may be formed by cutting half of the circumference.
[0007] Various features and aspects of the invention will become apparent upon review of the detailed description set forth below when taken in conjunction with the accompanying drawings, which are briefly described as follows.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a front perspective, environmental view of an embodiment of the convertible tights formed according to the present invention, illustrating the tights when worn in a footless configuration.
[0009] FIG. 2 is a close-up perspective view of the convertible tights of FIG. 1 , illustrating the tights when worn in a footed configuration.
[0010] FIG. 3 is a top view of the foot portion of the convertible tights of FIG. 1 , illustrating the tights when worn in a footed configuration.
[0011] FIG. 4 is a rear view of the convertible tights of FIG. 1 , illustrating the tights when worn in a footless configuration.
[0012] FIG. 5 is a cross-sectional view of the foot portion of the convertible tights of FIG. 3 , illustrating the tights when worn in a footed configuration.
[0013] FIG. 6 is a cross-sectional view of the foot portion of the convertible tights of FIG. 4 , illustrating the tights when worn in a footless configuration.
DETAILED DESCRIPTION
[0014] Certain exemplary embodiments of the present invention are described below and illustrated in the accompanying figures. The embodiments described are only for purposes of illustrating the present invention and should not be interpreted as limiting the scope of the invention, which, of course, is limited only by the claims below. Other embodiments of the invention, and certain modifications and improvements of the described embodiments, will occur to those skilled in the art, and all such alternate embodiments, modifications, and improvements are within the scope of the present invention.
[0015] Referring to the Figures in general, and to FIG. 1 , in particular, the present invention is directed to an article of women's hosiery, shown generally as 100 , such as tights. As used herein, “hosiery” refers to any article of apparel that covers some or all of a wearer's legs and/or feet, such as, stockings, tights, socks, etc.
[0016] As shown in FIG. 1 , which is a front perspective, environmental view of an embodiment of the convertible tights formed according to the present invention, illustrating the tights when worn in a footless configuration, the tights 100 comprise a pair of continuously knitted tubes 110 , each tube comprising a panty portion 120 , a leg portion 130 , and an integrally knitted foot portion (shown as 140 in FIG. 2 ). A waistband 122 may be integrally knitted to the top of the panty portion 120 during the formation of the tubes 110 . In forming a complete pair of tights 100 , the panty portions 120 may be each cut and seamed together along seams 124 a and 124 b. A separately-formed crotch piece 126 , formed of similar knitted material, and which may include a liner, may be separately attached to complete the tights. As will be appreciated, the tights may then be dyed a selected color.
[0017] As shown in FIG. 2 , which is a close-up perspective view of the convertible tights of FIG. 1 , illustrating the tights when worn in a footed configuration, each foot portion 140 comprises an upper portion 142 and an end portion 144 , or toe pocket. In one embodiment, as illustrated in FIGS. 2 and 3 , during the knitting process, and as explained in greater detail below, the end portion may be turned back inside the tube 110 and the edge adjoined to the outer layer of the tube 110 to complete the turned welt. As explained in greater detail below, this may be done in one of two manners, which include either adjoining the edge of the end portion around approximately one-half of the perimeter of the end portion, or alternatively, by adjoining the edge of the end portion around the entire perimeter of the end portion, and subsequently separating the turned welt around approximately half of the perimeter of the end portion in a manual operation. The turned-in part of the end portion 144 , which is in contact with the bottom (sole) of the foot when worn, extends circumferentially around approximately half of the perimeter of the end portion 144 .
[0018] Referring to FIG. 3 , which a top view of the foot portion of the convertible tights of FIG. 1 , illustrating the tights when worn in a footed configuration, the turned-in portion of end portion 144 ( FIG. 4 ) may be folded back at or near the line created by a turned welt 145 , as that term is commonly known in the knitting arts, where the turned-in portion of a knitted fabric is folded in to create a double layer of fabric and then adjoined along the edge of the end portion with transfer loops, as they are commonly known in the art.
[0019] As shown in FIG. 4 , which is a bottom view (when worn) of foot portion 144 ( FIG. 3 ), the turned welt 145 may generally separate the upper portion 142 from the end portion 144 .
[0020] In an exemplary embodiment, the knitted tubes 110 of tights 100 are formed on a commercially-available Lonati, Model 400 circular knitting machine. This particular knitting machine comprises a standard four inch knitting head having 200 dial jacks, or bits, 400 needles, and 4 yarn feeds; however, other models or brands, including different sizes of knitting heads may be used to form the same tights 100 .
[0021] The knitting process may begin with the toe pocket 144 . One-half, or 100 of the dial jacks on the knitting machine are programmed to knit the end portion 144 to create the turned welt 145 . More specifically, the machine is programmed to knit about one half of the end portion 144 , hold the fabric so folioed, and then complete the turned welt 145 with transfer loops. As will be understood, by knitting with only one half of the dial jacks, the turned welt 145 is completed around approximately half of the perimeter of the end portion 144 , with the remaining unattached portion of the perimeter thus forming the toe pocket and a portion of the bottom (sole) part of the foot when worn.
[0022] In the embodiment shown in the Figures, three yarns are fed from each of the four yarn feeds, each of the yarns comprising 20 denier spandex plaited with a 40 denier, 34 filament nylon; however, the selection of yarn types, materials, and deniers is not critical to the present invention and may be varied according to the type of hosiery desired. As will be appreciated, tights typically include an elastomeric component.
[0023] Alternatively, the circular knitting machine may be programmed to take yarn on all 200 of the dial jacks and complete a turned welt 145 around the entire perimeter of the end portion 144 . In this embodiment, the machine is programmed to knit in “puckers” (not shown) approximately 180 degrees apart along the turned welt 145 . As used herein, puckers are simply raised portions, or markers. In this embodiment, in a subsequent step, a bar tack is applied manually by an operator over the puckers. A bar tack may be stitched to a fabric to prevent unraveling. In this particular embodiment, subsequent to applying the bar tacks, an operator will manually cut one half of the perimeter along the line 147 forming the turned welt to create the end portion 144 .
[0024] Referring now to FIG. 5 , a cross-section of the convertible tights 100 in the footed position is illustrated (the scale and thickness of the layers has been exaggerated to better illustrate the configuration of the cross section). To wear the tights in the footed configuration, the wearer's foot ‘F’ is inserted through the leg opening and is then inserted into the opening 146 of the folded back end portion 144 . As shown in FIG. 5 , below the wearer's foot F are a first layer 144 a and a second layer 144 b of the bottom (sole) side of the end portion 144 . The first layer 144 a and second layer 144 b are adjoined along line 147 . Also, below the wearer's foot F, but above layers 144 a and 144 b, is a third layer 144 c, which forms the folded back portion, or toe pocket 144 . Above the wearer's foot F is a top layer 144 d, which is simply a continuation of third layer 144 c. As illustrated in FIG. 5 , layers 144 c and layers 144 a and 144 b, are unattached.
[0025] Turning lastly to FIG. 6 , a cross-section of the convertible tights 100 is illustrated in the footless configuration (again, the scale and thickness of layers has been exaggerated to better illustrate the configuration of the cross-section). To wear the tights in the footless configuration, the wearer's foot F is removed from the opening 146 of end portion 144 and inserted between the first and second layers 144 a and 144 b, which are adjoined by the turned welt 145 , and the third layer 144 c, which is folded inwardly beneath top layer 144 d. Because the first and second layers 144 a and 144 b are joined by the turned welt 145 , there is no substantially visible seam or bulge when the tights 100 are worn in this footless configuration. As also can be seen in FIG. 6 , layers 144 c and 144 d are positioned generally in front of the wearer's leg.
[0026] With respect to the remaining portions of the convertible tights 100 , once the turned welt 145 is formed, the knitting machine is programmed to transfer the yarns from the dial jacks to all 400 needles to knit the leg portion 120 and panty portion 130 . Lastly, the yarns are transferred back to the 200 dial jacks, wherein the waistband 122 is also formed having a turned welt 143 , as explained above.
[0027] Although the present invention has been described with an exemplary embodiment, it is to be understood that modifications and variations may be utilized without departing from the spirit and scope of the invention, as those skilled in the art will readily understand. Such modifications and variations are considered to be within the purview and scope of the appended claims and their equivalents.
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A method of forming an article of hosiery for being worn by a wearer in a footed or footless configuration includes forming a foot portion, leg portion, and panty portion, where the foot portion is formed by turning in an end portion of a circularly knitted fabric tube and connecting a first portion of an end edge to the fabric tube using transfer loops to form a turned welt around only a first portion of the perimeter of the fabric tube. A second portion of the end edge remains unattached and defines an opening between the second portion of the end edge and the fabric tube. The opening is dimensioned to receive toes of the wearer.
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This invention relates in general to a process for adhering precious metal to vitreous objects, and in particular to a process in which the outer skin of the vitreous object is made plastic and caused to bond to applied precious metal.
BACKGROUND OF THE INVENTION
Precious metal adhesion to glass is involved in a number of industrial and aesthetic applications. Optical and infrared reflectors and lenses can be made to reflect and/or transmit different wavelengths depending upon the particular precious metal film applied. Often such films are also applied in patterns utilizing their ability to conduct electricity. Finally, precious metals, especially gold, have many decorative uses in glass and crystal objects.
U.S. Pat. No. 3,266,912, assigned to Engelhard Corporation, describes a family of products known as “liquid bright golds”. These are varnish-like precious metal preparations containing organic compounds combined with flux components which are based on organic metal compounds. The flux components act as an adhesion promoter. On a smooth glass ceramic surface, a high gloss metal film forms after firing in a high temperature oven or annealer. This film has a gold or other precious metal content of 6 to 15%. Such compounds are used in a number of aesthetic and industrial applications in a relatively straightforward application of precious metal to glass. However, the products have some disadvantages. The organic compounds and flux agents essential to such solutions are environmentally toxic. Moreover, the presence of such agents in the fired film or coating compromise the aesthetic and physical properties of such films. The fluxes discolor when applied to certain types of glasses. This causes the color of the precious metal coating to have two tones; depending upon whether one is viewing the film from the surface of the vitreous substrate or through the actual substance the film is applied to. Furthermore, the liquid bright films have a distinct plated look as the gold is formed on the top and not absorbed or melted into the surface of the vitreous substances. From a material efficiency viewpoint, the relatively low precious metal content of such films degrades the electrical, thermal, and optical properties of the films.
U.S. Pat. No. 4,837,052 describes a technology which involves sandwiching a layer of deposited gold between an inner coating of gold-chromium and an outer protective polymer overcoat. In this process, adhesion to the vitreous substrate is achieved through the application first of gold-chromium. Pure gold is then applied to the layer of gold coating but is very complex, requiring three applications. Moreover, successful adhesion is only achieved through the application of a polymer foreign substance.
A third approach to achieving precious metal adhesion is; described in U.S. Pat. No. 2,950,996. This technology involves; combining gold resinates and vitreous substances together in one compound. This mixture is applied to the vitreous surface. Upon firing, the mixture forms a combination gold/vitreous compound which adheres to the vitreous surface as well as to the gold particles suspended in the composition. This technique is effective for many technical applications but also has shortcomings. Particularly, the film is never 100% gold. Moreover, only gold resinates may be used, these compounds limiting the appearance and physical characteristics of the adhered precious metal. Finally, the vitreous substances must have low melting points relative to the glasses they are coated upon, in order that the contour of the coated glass does not distort. Currently, such low melting glasses contain lead. This prevents the use of such coatings in functional glassware.
SUMMARY OF THE INVENTION
The present invention involves the adhesion of precious metal to glass without the use of any foreign material or substances. After the substrate is coated or otherwise contacted with precious metal, the substrate itself is utilized as the means of permanently adhering the precious metal. In particular, the outer or peripheral skin of the coated glass substrate in contact with the metal is superheated to a temperature at which the skin is in a plastic state. A change in viscosity then takes place, allowing a molecular bond to form between the precious metal and the substrate. The superheating phase is accomplished by rapidly applying high-intensity heat to the surface of the precious metal. By conduction through the metal, heat is transmitted to the peripheral surface or skin of the substrate, until lowering of the viscosity of the skin effects adhesion between the metal and the substrate. This superheating process is completed relatively quickly in order to prevent overeating of the entire cross-section of the substrate and resultant change in shape and contour as well as to avoid negatively affecting the state of the precious metal through melting or vaporization.
This process allows precious metal to glass adhesion without additional fluxes or other chemical agents, allowing the formation of a 100% pure coating of precious metal. Gold in any mesh size or composition may be adhered to glass including gold powder, chips, and/or sheets. Moreover, the molecular bond created is quite strong and wear-resistant.
The vitreous substrate may be any one of a variety of substances, including ceramic, quartz, soda-lime qlasses, lead glasses, and boro-silicate and potasium-based glasses. The metal may be any one of several such as gold, silver, platinum, palladium or alloys containing gold, silver, platinum or palladium.
BRIEF DESCRIPTION OF DRAWING
For a better understanding of the invention, reference should be made to the following description of preferred embodiments which should be read in connection with the appended drawings in which:
FIG. 1 is a schematic showing of the process of the invention as practiced with a generally flat product, and
FIG. 2 is a schematic illustrating the invention as used with a curved surface.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the practice of this invention, the chosen precious metal is first placed in contact with a vitreous substance. With a glass substrate, coating may be achieved through conventional vacuum or electrostatic metal deposition, or other techniques known in the art. These techniques may include, for example, placing gold powder within an evaporative substance such as toluene and then brushing or spraying the coating directly a plate. Alternatively, the substrate can be wetted with an evaporative substance such as toluene or methylethylketone and coated with gold leaf or foil.
After the plate is coated, it is preheated in an oven to its annealing point, which may be about 950° F. for soda-lime type glass. Preheating of other glasses, such as lead crystal glasses, which have lower annealing points, is done at lower temperatures.
Still other glasses having higher annealing points are preheated at higher temperatures. This step prepares the glass substrate for the superheating phase. Most glasses will explode and crack if they are superheated directly from room temperature. Successful superheating is enhanced if preceded by a heating to the annealing temperature. On the other hand, thin lead glasses of the order of ⅛″ or less in thickness are quite shock-resistant and may be superheated without need for preheating.
Next, the plate is then to within a quarter to a half-inch of a silicon carbide heating element 13 having a watt density of at least 50 watts per inch. Alternatively, heat sources such as quartz infra-red or oxy-gas heating units could be used. Whatever heat source is used, it must have sufficient capacity that superheating of the substrate takes place. Such superheating is defined as heating to a stage at which the body of the substrate remains undistorted but the surface or skin of the substrate becomes plastic and tacky. The skin of the substrate as viewed through the metal has a shiny, continuous appearance when it has reached the stage where it can serve as an adherent by superheating in this fashion. After the superheating phase is completed, the plate is placed within an annealing oven to cool. Glasses with higher melting points may require extended heating phases and possibly higher power densities (depending upon the gauge and type of precious metal and specific melting point of the glass). With a fixed power density, lead glasses will adhere precious metal significantly faster than higher melting point glasses such as a soda-lime type glass.
Alternatively, the heat source may consist of any other high intensity heat creator. In particular, Moly-D resistance elements, quartz infrared heat lamps, and oxy/fuel burner systems all produce power densities needed to change the viscosity of the surface layer of the coated glass. In addition to a high power concentration, the heat source must also be precisely controlled in order to achieve and maintain consistent and thorough adhesion. Temperatures are monitored with the use of optical pyrometers and/or other sensors and power inputs are adjusted in order to achieve this. In the case of electrical power sources, voltage and amperage may be controlled in order to achieve a consistent element temperature. Oxy/fuel systems require precise control of the gas inputs with accurate gas regulators and flow controllers. Thus, any type of heat source with the proper power density may be used. In the case of adhering patterned gold, oxy/gas or other equivalent convective heat source is preferred to an infrared heat source. This is due to the highly reflective or emissive quality of gold. This reflective property can create substantial temperature gradients between uncoated and coated sections; the uncoated areas absorbing most of the infrared spectrum while the coated areas reflecting the same. In this instance, the uncoated substrate may deform excessively before the patterned areas are successfully adhered. Superheating with a convective heat source will prevent this.
Another concern with the described process is the melting temperature of the precious metal. Sustained heating of the precious metal coating can cause the coating to degrade quite rapidly. The temperature of the heat source is typically higher than the melting point of the precious metal. This places an additional constraint on the superheating phase, as prolonged heating will cause the precious metal coating to degrade and ultimately vaporize.
EXAMPLE I
In FIG. 1 of the appended drawing, there is shown a lead-crystal plate 11 having a thickness of about ¼″. A layer of gold leaf 12 which may have a thickness of about 0.032″ may be adhered by any of the several methods described above, but preferably in this example with the use of an evaporative solvent. The plate 11 is then preheated in an oven to its annealing point of about 840° F.
Following the preheating step, high intensity heat is applied to the surface of the metal layer 12 . The heat is generated by a source 13 which has a watt-density of at least 50 watts per inch. This is achieved by placing the metal surface 12 at a point ¼ to ½″ from the source 13 . Superheating continues until the skin of the plate 11 is liquefied and the glass becomes shiny in appearance as viewed through the metal layer. This may occur when the melting point of the lead crystal glass is reached and should not be maintained long enough for the entire plate to soften and lose its contours. Also, the superheating phase should be discontinued before degradation of the metal coating occurs. The rate of such distorting of the substrate and degradation of the metal coating may be reduced by directing a stream of cooling air upon the uncoated lower surface of the substrate 11 from a source 15 .
EXAMPLE II
Precious metal may be adhered to a curved surface of a vitreous body in accordance with the invention in the following manner as shown in FIG. 2. A high temperature furnace 25 is heated by a high-intensity heat source having the approximate shape and contour of the object 33 being coated with precious metal. The heat source may be any one of those previously mentioned such as curved electrical elements or an oxy-gas burner configured in a curved shape as at source 26 on a high-temperature furnace 26 . The source 26 is controlled by a controller 27 which receives feedback from a thermocouple 28 . The floor 29 of the furnace may be constituted by a highly conductive shell case, preferably from sintered silicon carbide. The silicon carbide may be cast in any shape to match that of the object 33 being coated. As in the embodiment of FIG. 1, cooling air may be provided from a source 35 beneath the substrate of the object 33 to prevent thin substrates from distorting. The object 33 may be lifted by a pneumatic lifter 34 to within a ¼″ of the floor shell 29 . The object 33 is held in such proximity to the shell 29 briefly to superheat and melt the skin of the substrate immediately adjacent to the layer of precious metal only until the metal coating becomes shiny to reveal its plastic and viscous adherent state.
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There is provided a method for adhering precious metal to vitreous substances or bodies. Precious metal (including but not limited to, gold, palladium or platinum) is deposited or applied to the surface of the vitreous body. After such initial application, which may include a preheating step, the outer skin or membrane of the glass is made plastic and sticky by superheating. This change in viscosity allows the glass to bond to the deposited precious metal. The superheating process is completed quickly before distortion of the contour of the vitreous object and unwanted vaporization of the deposited metal take place. After the superheating process is completed, the object is annealed conventionally to room temperature.
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FIELD OF THE INVENTION
[0001] The present invention relates to an eavestrough cover and more particularly, relates to an eavestrough cover or screen which permits the flow of water into a gutter while preventing debris from collecting in the gutter or eavestrough.
BACKGROUND OF THE INVENTION
[0002] The use of eavestrough covers (also known as gutter guards) is well known in the art. These eavestrough covers have gained popularity as the problem of clogged gutters is almost universal. Irrespective of the climate, leaves and other debris find their way into the eavestrough. These can lead to clogging of the eavestrough, either at the downspout or elsewhere. This in turn can lead to water back up into adjacent structures. Wood rot and other problems can then occur.
[0003] In order to overcome this problem, the use of eavestrough covers is widely practiced. These eavestrough covers permit the passage of water into the eavestrough or gutter while preventing extraneous matter from entering the eavestrough. Various mounting systems have been employed in order to secure the eavestrough cover in place. The success of the mounting system will frequently depend on the place of installation and the design of the eavestrough cover.
SUMMARY OF THE INVENTION
[0004] It is an object of the present invention to provide an eavestrough cover which is designed to prevent extraneous matter from entering the eavestrough while also efficiently allowing the passage of water through the cover into the eavestrough.
[0005] It is a further object of the present invention to provide an eavestrough cover having sufficient rigidity to be easily secured in place.
[0006] According to one aspect of the present invention, there is provided an eavestrough cover comprising a front longitudinally extending portion, a rear longitudinally extending portion, a central portion extending between and secured to both of the front longitudinally extending portion and the rear longitudinally extending portion, the central portion being formed of a woven material, and the woven material being embossed in a generally transverse direction so as to improve the rigidity of the woven material.
[0007] According to a further aspect of the present invention, there is provided in combination, an eavestrough cover comprising a front longitudinally extending portion, a rear longitudinally extending portion, a central portion extending between and secured to both of the front longitudinally extending portion and the rear longitudinally extending portion, the central portion being formed of a woven material, the woven material being embossed in a generally transverse direction so as to improve the rigidity of the woven material, and an eavestrough, the eavestrough having a rear wall, a bottom wall, a front wall, a vertical segment formed at an upper portion of the front wall, a top wall and a downwardly extending diagonal segment.
[0008] As aforementioned, the eavestrough cover has a front longitudinally extending portion and a rear longitudinally extending portion. Intermediate the front longitudinally extending portion and the rear longitudinally extending portion is a central portion. This central portion is formed of a woven material as is known in the art. Embossed areas are provided in the woven material with the embossed areas extending in the traverse direction (i.e. between the front longitudinally extending portion and the rear longitudinally extending portion.
[0009] The woven material may be selected from any suitable material (i.e. an aluminum material, a stainless steel material, plastic material, etc.) and is preferably a woven wire mesh known as a micro mesh.
[0010] The embossments are arranged such that they extend upwardly to form generally transversely extending ridges between the front longitudinally extending portion and the rear longitudinally extending portion. The embossments, in a preferred embodiment, extend from the front longitudinally extending portion and the rear longitudinally extending portion. It will be understood that modifications to such an arrangement may be provided; in other words, some of the embossments may not extend completely transversely of the woven material and/or may extend at somewhat of an angle with respect thereto such as an S or Z shape.
[0011] The front longitudinally extending portion is preferably formed of a metallic material such as aluminum and it is arranged to grip one side of the woven material. To this end, the arrangement is such that the aluminum material is folded back on itself and pressed together to retain the woven material.
[0012] Preferably, the arrangement is such that there is provided an upwardly extending portion which forms a wall to direct any excess water back towards the center of the eavestrough cover. In this arrangement, the woven material is gripped firstly by the portion forming the wall and also by a further horizontal portion extending frontwardly from the wall.
[0013] In this arrangement, the front longitudinally extending portion also preferably includes a member which will engage with the eavestrough to assist in retention of the eavestrough cover.
[0014] The rear longitudinally extending portion is also preferably formed of a metallic material such as aluminum. Again, the rear longitudinally extending portion is arranged to grip the woven material. Also, preferably the rear longitudinally extending portion has an upwardly sloping segment which assists in retaining water and directing the same towards the central portion.
[0015] A rearwardly extending flange forms a portion of the rear longitudinally extending portion. This flange is provided to fit under the tiles of a roof.
[0016] Preferably, the flange is of a substantial transverse length to reach between the eavestrough and the roof. In one embodiment, the flange is provided with a line of demarcation or fold line above which the flange may be folded if it is used in other situations. The line of demarcation may comprise a longitudinally extending groove formed in the flange portion.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Having thus generally described the invention, reference will be made to the accompanying drawings illustrating an embodiment thereof, in which:
[0018] FIG. 1 is perspective view of a portion of an eavestrough cover according to the present invention;
[0019] FIG. 2 is a further perspective view thereof;
[0020] FIG. 3 is a bottom perspective view thereof;
[0021] FIG. 4 is a further bottom perspective view thereof;
[0022] FIG. 5 is a cross-sectional view thereof;
[0023] FIG. 6 is an enlarged cross-sectional view of the left hand side portion of the eavestrough cover shown in FIG. 5 ;
[0024] FIG. 7 is an enlarged view of the right hand side of the eavestrough cover seen in FIG. 5 ; and
[0025] FIG. 8 is a cross-sectional view of the eavestrough cover mounted on an eavestrough.
DETAILED DESCRIPTION OF THE INVENTION
[0026] Referring to the drawings in greater detail and by reference characters thereto, there is illustrated an eavestrough cover which is generally designated by reference numeral 10 .
[0027] Eavestrough cover 10 has a front longitudinally extending portion generally designated by reference numeral 12 and a rear longitudinally extending portion generally designated by reference numeral 14 . A central portion generally designated by reference numeral 16 is formed of a suitable woven material as is known in the art. Central portion 16 has a plurality of longitudinally extending filaments 18 and transversely extending filaments 20 which together form the woven material.
[0028] Formed in the woven material are a plurality of transversely extending embossments 22 . As may be seen, embossments 22 extend upwardly—i.e. the embossed portion is on the upper surface of the woven material with reference to the normal placement of the eavestrough cover 10 .
[0029] Front longitudinally extending portion 12 includes, proximate the central portion 16 , a vertical upwardly extending segment 26 . A vertical downwardly extending segment 28 lies substantially parallel to vertical upwardly extending segment 26 to thereby retain a crimped portion 38 of central portion 16 therebetween. Extending from the lower portion of vertical downwardly extending portion 28 is an upper horizontal segment 32 . Lying underneath is a lower horizontal segment 34 which again is arranged such that there is a crimped portion 36 therebetween. Lower horizontal segment 34 terminates in a diagonally and downwardly extending segment 38 designed to engage with the eavestrough.
[0030] Rear longitudinally extending portion 14 has a lower horizontal segment 42 and a parallel intermediate horizontal segment 44 . Retained therebetween is central portion 16 which is a crimped relationship therewith. An upper horizontally extending segment extends rearwardly and is provided with a diagonally upwardly extending segment 47 . A flange 48 extends rearwardly to fit underneath the tiles of a roof.
[0031] It will be noted that rearwardly extending flange 48 terminates in a folded under segment 50 . There is also formed a fold line 52 comprising a groove which extends longitudinally of flange 48 such that flange 48 may be bent thereabout in situations where the length of flange 48 is not required. If desired, a plurality of fold lines could be provided therein to form a desired length of flange 48 .
[0032] The eavestrough cover 10 is shown mounted on an eavestrough generally designated by reference numeral 56 . Eavestrough 56 includes a rear wall 58 , a bottom wall 60 and a front wall generally designated by reference numeral 62 . An upper segment 64 of front wall 62 extends substantially vertically and joins with a top wall 66 . In turn, top wall 66 terminates in a diagonally and downwardly extending segment 68 .
[0033] As may be seen, eavestrough cover 10 engages with top wall 66 and diagonal segment 68 . Flange 48 extends rearwardly and is adapted to fit under the shingles of an adjacent roof.
[0034] It will be understood that the above described embodiment is for purposes of illustration only and that changes and modifications may be made thereto without departing from the spirit and scope of the invention.
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An eavestrough cover which has a central portion formed of a woven material and a front longitudinally extending portion and a rear longitudinally extending portion, the woven material being embossed in a generally transverse direction so as to improve the rigidity of the woven material.
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BACKGROUND OF THE INVENTION
The background of the invention will be set forth in two parts.
FIELD OF THE INVENTION
This invention relates to ignition systems for internal combustion engines and more particularly to solid state internal combustion ignition systems.
DESCRIPTION OF THE PRIOR ART
Conventional combustion engines require some means for igniting a combustible gaseous or vapor mixture in each cylinder at the proper time for efficient engine operation. The ignition is usually accomplished by a high voltage pulse provided at the center electrode of a spark plug extending into the engine's combustion chamber, causing a spark to bridge the gap between the center electrode and the plug's grounded frame.
For many years, the high potential energy delivered to the spark plugs in an ignition system has been generated in an electrical circuit comprising a relatively low potential storage battery connected to one side of a primary winding of a step up transformer. An engine-actuated switch, which temporarily grounds the other side of the primary winding to complete the primary circuit, induces a high potential across the secondary winding of the ignition transformer which is connected through a distributor and appropriate high tension electrical cable to the spark plugs in a sequence determined by the distributor in accordance with the engine's design.
It has been found that at relatively high engine speeds, the spark plug potential available at each spark plug is markedly less than that available at lower speeds. This is because the relatively large magnetic flux changes in the transformer, which are necessary to generate the high potential, are not obtainable when the period between each pulse of energy is shortened to the extent necessitated by high engine speed. With lower spark potential, the problem arises of having insufficient ignition of the combustible materials which lessens engine efficiency and increases the exhausting of hydrocarbon emissions from the engine. In order to overcome this problem, much effort has been directed to develop several types of solid state or transistorized ignition systems.
Most of the popular transistorized systems do overcome the aforementioned problem related to high speed operation in that the spark plug potential is maintained at a relatively high level over most of the engine's speed operating range. However, the duration of the spark is relatively short, and a higher than desirable amount of the combustible material is still not completely burned.
One technique that has been proposed is to employ a Jensen type oscillator having a control winding which acts to saturate a magnetic core of a multi-winding transformer. Spark energy is provided by this system when the current flow through the control winding is cut off to allow the feedback windings of the transformer to become effective and thereby instigate oscillation.
It should therefore be evident that an electronic ignition system that provides relatively high potential, high frequency, optimum constant amplitude ignition energy would constitute a significant advancement in the art.
SUMMARY OF THE INVENTION
In view of the foregoing factors and conditions of the prior art, it is a primary object of the present invention to provide a new and improved electronic ignition system.
Another object of the present invention is to provide a highly efficient electronic ignition system that produces a relatively high constant potential, high frequency pulse ignition energy over a wide range of d.c. input potential.
Still another object of the present invention is to provide a highly reliable electronic ignition system, the output of which is relatively unaffected by the heavy power drain of a storage battery during the period an engine's starting motor is energized.
Yet another object of the present invention is to provide an electronic ignition system that includes a safety turn-off feature when the system is energized but the engine is not operating.
Still a further object of the present invention is to provide an electronic ignition system which rectifies high frequency pulse ignition energy and applies the rectified energy across a capacitor that stores such energy until discharged by a spark generated across the points of a spark plug connected across the capacitor.
In accordance with the present invention, an electronic ignition system for use with an internal combustion engine includes a triggered oscillator circuit having a relatively high frequency energy generator portion providing pulses of oscillator energy in response to ignition timing signals. A constant current pulse circuit is coupled to the oscillator circuit for providing constant current pulses of energy in response to the pulses of oscillator energy. The invention also includes an output circuit coupled to the constant current pulse circuit for providing relatively high potential, high frequency, constant current combustion initiating pulses of output energy in direct relationship to and over the engine frequency operating range of the ignition timing signals. Still another embodiment of the invention rectifies high frequency pulse ignition energy from an electronic ignition system and applies this energy across a capacitor that is connected in parallel (through a distributor) with the spark plugs in the ignition system. Thus, the capacitor stores the energy until it is discharged when the potential across the spark plug points is great enough to cause a spark to jump the gap.
In accordance with certain embodiments of the invention, the input circuitry may include a novel circuit which discontinues the operation of the triggered oscillator in the event that the system is left in an energized condition while the engine is not operated and a timing signal is continuously presented to the system. Also, the system may include an energy reservoir which provides temporary power to the system's output circuitry in the event that its primary input potential drops below a level to adequately maintain the high potential of the combustion initiating pulses.
The features of the present invention which are believed to be novel are set forth with particularity in the appended claims. The present invention, both as to its organization and manner of operation, together with further objects and advantages thereof, may best be understood by making reference to the following description taken in conjunction with the accompanying drawing in which like reference characters refer to like elements in the several views.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of an electronic ignition system according to the present invention;
FIG. 2 is a block diagram according to one embodiment of the present invention;
FIG. 3 is a block diagram of an electronic ignition system according to another embodiment of the present invention;
FIG. 4 is a schematic diagram of the ignition system of FIG. 3;
FIGS. 5a-5d are diagrammatic illustrations of voltages at specific points in the electronic ignition system of FIG. 4; and
FIG. 6 is a schematic illustration of a high spark energy circuit in accordance with still another embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings and more particularly to the block diagram of FIG. 1, there is shown an electronic ignition system 11 for use with an internal combustion engine (not shown). Either an ignition timing signal in the form of a voltage pulse of energy or the closing of a switch (points) usually located in the engine's distributor is coupled or connected to the input terminal 13 of a relatively high frequency oscillator 15.
The oscillator 15 is of the type which will produce an output only when triggered by the ignition timing signal, and for as long as the timing signal is present. Although the frequency of oscillation for best operation has been found to be about 5 kHz, the invention provides advantageous results in the range from about 4 kHz to 20 kHz. Preferably, the input switching timing signal has a relatively fast rise and fall time characteristic, generally <0.1 μs. In the case where the timing signal is provided by the opening and closing of ignition points in a distributor, the trigger pulse width will depend upon the cam angle as well as the RPM. Converted into time: ##EQU1##
The output pulses of relatively high frequency generated by the oscillator 15 are coupled to the input of a constant-current pulse circuit 17. This circuit senses and compensates for any changes in voltage supplied to the system so that the pulses coupled to an output coupling circuit 19 have a constant pulse current magnitude over the operating range of supply voltage for the system 11.
The output coupling circuit 19 may include a step up transformer, the output winding which provides, at its output terminal 21, the ignition timing signal-synchronized constant current pulses of high voltage, high frequency energy directly to an internal combustion engine's spark distribution system (not shown).
FIG. 2 illustrates another embodiment of the invention. Here, the system 31 is shown to include a fast rise time solid state switch circuit 33 having an input connected to a set of distributor points, for example, at 35. The switch circuit isolates the points from the input to the oscillator 15 and generally provides a better shaped trigger signal to the oscillator.
This system can further be expanded, as shown by system 41 in FIG. 3, to include a safety, time-on limit circuit 43 located between points 45 and the fast rise time switch 33. Also provided in the system 41 is a pulse driver circuit 47 and an output switching circuit 49 coupled between the output of the constant pulse current circuit 17 and a driver transformer 51. In this embodiment of the invention, the output of the driver transformer is coupled to a conventional ignition "coil" 53. In order to obviate any possible problem of providing a weakened "spark" to the spark plugs when the engine is being started by a starting motor due to its very heavy current drain, this preferred system further includes a boost circuit 55 which stores energy therein prior to the use of the starting motor, and which provides to the driving transformer circuit 51 a continuous high level of source energy through the aforementioned period of reduced potential level. A more complete description of this presently preferred embodiment is provided in connection with the schematic diagram shown in FIG. 4.
It can be seen in this figure that a source of primary power, usually in the form of a storage battery (not shown), is connected to a positive power input terminal 61, a negative terminal 63, and through an ignition switch (not shown) to a switched positive input power terminal 65. When positive potential is provided to terminal 65, it is applied to circuits 15, 17, 33, 43 and 47 through a conventional reverse-polarity protective diode 71, while a positive potential is always applied to terminal 61 and circuits 49, 53 and 55 (see FIG. 3).
Resistors 73 and 75 act as a voltage divider and filter network in conjunction with capacitor 77. In the time-on limit circuit of FIG. 4, conventional ignition points 79 are connected to the timing signal input terminals 81 and 83, the latter being connected to the common bus 85 or ground, while the former connects the junction 87 of resistor 75 and a timing capacitor 89. The other side of the capacitor 89 is connected to the junction 91 of resistor 93 and the cathode of diode 95. Timing pulses propagating through capacitor 89 and appearing between ground and the junction 91 are seen across the lower leg of a voltage divider circuit comprising the resistor 93 and a resistor 96 connected between a base terminal 97 of an NPN transistor 99 (such as a 2N2222, for example) and ground.
The emitter terminal 101 of transistor 99 is grounded and its collector terminal 103 is connected to a conventional FET switch circuit 105 in parallel with a load resistor 107 and a protective diode 109. Source potential is provided to the FET switch (terminal 105-2) and the collector of transistor 99 through a current limiting resistor 110. The FET switch circuit 105 is utilized because of its fast rise and fall time characteristic. However, other circuits having similar attributes may be utilized. Primary source potential is provided to terminal 105-3 of the FET switch 105 and to transistor 99 by the use of a series resistor 111 and a parallel peak voltage limiting filter combination of Zener diode 112 and capacitor 113. The diode voltage rating should be about a volt or two above the primary source potential.
The output of the switch circuit 105 is provided at terminal 105-4 thereof and is coupled directly to terminals 117-4 and 117-8, and through resistor 114 to terminal 117-7 and also through resistor 115 to terminal 117-6 of a conventional oscillator type integrated circuit (IC) 117, such as an NE 555, for example. Pin 117-1 of IC 117 is grounded while a decoupling capacitor 119 is provided between pin 117-5 and ground. Capacitor 121 is connected between pin 117-6 of IC 117 and ground and functions with resistor 115 to determine the frequency of operation of the oscillator circuit 15.
The output high frequency pulse energy from the oscillator circuit is coupled from terminal 117-3 to the base 123 of an NPN transistor 125 in the constant-current pulse circuit 17 through a current limiting resistor 127. The collector electrode 129 of the transistor 125 derives its operating potential through a resistor 131, and the emitter electrode 133 is connected to ground through a series resistor 135 and the collector 137-emitter 139 junction of an NPN transistor 141. The base 143 of this transistor is connected to a voltage divider arrangement comprising grounded resistor 145 and resistor 147 leading to Zener diode 149, the cathode of which is coupled to the primary source potential at bus 151 downstream of the resistor 111. The voltage rating of this Zener diode is chosen to be about 3 or 4 volts less than the source potential so that the diode 149, resistors 145, 147 and transistor 141 act as a voltage sensing circuit which limits the current output of the transistor 125 to compensate for changes of the primary source potential. For example, in a 12 volt system, the diode 149 may be rated at 9 volts, while resistors 145, 147 divide the voltage present at the anode of diode 149 in a 1-to-3 ratio.
The input 153 of the pulse driver circuit 47 is coupled to the output of the circuit 17 at the emitter terminal 133 of transistor 125. In this embodiment, the circuit 47 is a conventional Darlington pair incorporated in a unitary package and includes NPN transistors 155 and 157, and resistors 159 and 161 appropriately connected between associated base/emitter terminals. As is common in Darlington pair packaging, a protective diode 163 is connected across output terminals 165 and 167, the latter being connected to the base electrode 169 of a series-pass NPN transistor 171 and to a resistor 173 to ground, in the output switching circuit 49. The emitter 175 is connected to ground while the collector terminal 177 of transistor 171 is connected to terminal 165 of circuit 47 and to terminal 179 of the primary winding 181 of the driver transformer 183 in the driver transformer circuit 53. Another protective diode 185 is provided across the collector-emitter terminals of transistor 171, and an appropriately poled diode 187 provides primary source potential from the unswitched terminal 61 to the opposite end 189 of the primary winding 181.
The transformer 183 includes a secondary winding 191 providing, in this case, a 1:25 step up ratio between primary and secondary. A first end 193 of the winding 191 is connected to ground and the first end 193 and a second end 195 are connected through appropriate insulated cabling 197 to opposite ends 201 and 203 of a primary winding 205 of a conventional ignition coil (transformer) 53. An end 207 of the transformer's secondary winding 209 is grounded, and the high potential end 211 is appropriately connected to an ignition distributor (not shown).
In operation, when points 79 close, the primary potential source (usually 12 volts), is dropped across resistors 73 and 75 to ground through the points 79, and there is no timing signal input at junction 87. However, when the points 79 first open, the base of transistor 99 sees about 7 volts peak and it starts to conduct. The voltage at the base decreases at first gradually as capacitor 89 changes. Once changed this capacitor is charged, the voltage at the base electrode 97 drops off more rapidly, as seen in FIG. 5. Diode 95 allows capacitor 89 to discharge very quickly just as the points 79 close. This diode also prevents capacitor 89 from discharging through the base-to-emitter leakage path in transistor 99, and places zero voltage at junction 91. At this time, transistor 99 is turned off (ceases to conduct), as shown in FIG. 5b by the voltage curve at the collector electrode 103.
When transistor 99 is conducting, the collector approaches ground potential, and the primary 12 volt source potential appears across a voltage divider circuit comprising resistors 107 and 110. In the conducting state of this transistor, diode 109 is effectively a short across resistor 107, and resistor 110 and resistor 111 act to limit transistor current to a desired value. The function of diode 109 is to bypass pulse kickback when transistor 99 rapidly stops conducting. This protects the input circuit of the FET switch 105 from damage.
The FET switch 105 is "turned on" when the voltage at its input terminal 105-1 drops to near zero by the conduction of transistor 99. This action cause the output of the switch 105, seen at its terminal 105-4 to very rapidly go from zero to a predetermined high "on" potential (usually the regulated potential on bus 151). This voltage is applied to the input voltage terminals 117-4 and 117-8 of the oscillator IC 117, which causes it immediately to start oscillating at a predetermined frequency determined by resistor 115 and capacitor 121. The duty cycle of this oscillating state is determined by resistor 114, and is usually set at about 50 percent. For a frequency of 5 kHz and a 50% duty cycle, resistor R114 is 1.3 k ohms, while resistor R115 is 13 k ohms and capacitor 121 has a capacitance of 0.01 μfd.
The output signal from the oscillator 117 is provided at terminal 117-3 and is in the form of pulses of relatively high frequency (preferably approximately 5 kHz) having a repetition rate and duration determined by the timing signal, provided in this embodiment by points 79. The pulse oscillator energy is coupled through the current limiting resistor 127 to the base electrode 123 of transistor 125.
In order to provide a desired constant high pulse potential to the spark plugs even when the primary potential source varies in magnitude, as is often the case in practice, circuit 17 is provided to compensate for such potential (voltage) variations. As noted previously, circuit 17 includes a primary voltage sensing and current regulating arrangement made up of the Zener diode 149, and the voltage divider comprised of resistors 145 and 147 providing a bias potential to the base electrode 143 of the current controlling transistor 141. The change in bias potential brought on by potential changes sensed in the bus 151 limits the current output from the current regulated transistor 125 seen at its emitter electrode 133.
The pulse driver amplifier stage 47 now receives the constant current, high frequency pulse signal at its input terminal 153. As noted previously, this circuit is a conventional Darlington pair design comprising tandemly coupled transistors 155 and 157, and a diode 163 disposed across the amplifier's output terminals 165 and 176, for transient protection. This circuit provides to the base electrode 169 of the high power transistor 171 with the drive necessary for this power stage to produce, through the primary winding 181 of the transformer 183, a constant current, high potential, high frequency pulse signal at the secondary winding 191 that drives the external conventional "coil" 53. This produces the required very high potential pulses which are uniform in magnitude for distribution to the engine's spark plugs.
The driver transformer 183 should be designed for high frequency operation with low loss. For example, this transformer may use an E core design using 0.014 inch laminations of silicon oriented grain iron. Alternately, transformers 185 and 53 may be replaced by a single transformer having the desired high frequency-low loss characteristics with a higher step up ratio to provide the desired very high voltage pulses to the externally located spark plugs.
In order to prevent the possible harmful effects of negative-going transients produced in the primary winding 181 of transformer 183 (due to the inductive load) from reaching the sensitive transistor circuitry of the system, diode 71 is disposed in series with primary potential source from the key switch found at terminal 65. Both diodes 71 and 187 act as protection diodes if a reverse polarity potential is accidentally applied to the system.
It has been found in conventional systems that at the time when the primary potential source (storage battery) is used to activate the engine's starting motor, there is a great amount of current utilized (usually over 200 amps) and the voltage appearing at the ignition system drops due to the internal resistance of the source. This, of course, causes the voltage available at spark plugs to be lower than desirable for reliably starting the engine. In order to overcome this problem, the present system may include a storage capacitor 215 (approximately 2,500 μfd.) connected between ground and the unswitched positive input terminal 61. Prior to the time the starter motor is energized, the capacitor 215 is charged to its maximum capacity. Then, it can provide the desired constant potential level to the amplifier/transformer circuitry for the limited time period that the system's primary potential source is being heavily drained in starting the engine.
Yet another embodiment of the invention, which incidentally can be used with any electronic ignition system producing pulses of high frequency energy, is illustrated in FIG. 6. Here there is shown a spark energy intensifier circuit 215 which has input terminals 217 and 219 coupled to the output of a high frequency CW ignition system, such as terminals 207 and 211 of the ignition coil 53, for example.
The circuit 215 includes a diode rectifier 121 connected in series with a rectified energy storage capacitor 123 between the input terminals 117 and 119. Output terminals 125 and 127 are connected across the capacitor 123 and are coupled by appropriate wiring (and usually a distributor) to the terminals 129 and 131 of a conventional spark plug 133.
High frequency energy appearing across the input terminals 117, 119 is rectified by the rectifier 121 and appears across the capacitor 123. The capacitor thus begins its charge cycle. The voltage seen across the capacitor 123, and the output terminals 125 and 127 is also applied across the spark plug points 129 and 131, and when this potential reaches a sufficient magnitude, as determined largely by the gap distance at the plug, an arc will occur and the capacitor is immediately discharged.
In conventional ignition systems, about 6 to 15 thousand volts is applied across the points which are gapped to arc at this potential. On the other hand, in the present invention the gap may preferably be widened so that as the rectified potential reaches approximately 15 to 20 thousand volts, a spark will occur across the points 129, 131 to discharge the capacitor and start a new cycle.
In an application where an 8 cylinder engine is operating at 12,000 RPM and the distributor cam angle is 30°, the distributor rotor speed is 6,000 RPM or 100 revolutions per second and rotates through 36,000 degrees. When each plug is reached every 45° of rotor rotation (for eight plugs), 800 pulses per second will occur, and the period between each such pulse is 12.5 milliseconds. However, since the cam angle is set at 30°, the pulse width of each pulse may be calculated from ##EQU2## In this example, the pulse width will be 800 μsec. Where the spark plug gap is set so that a spark will occur when the potential across the points reach approximately 20 kv, the charge/discharge time is approximately 30 μsec. Thus it can be seen that the approximately 27 discharges per pulse (800/30) of rectified energy will occur for the parameters set by this example.
To be stressed in connection with this embodiment is the greatly increased energy released in the combustion chamber of the internal combustion engine. The discharge energy for the capacitor 123 may be calculated from the relationship of
E=CV.sup.2 /2 joules,
where C is the capacitance (usually between 500 and 1,000 pfd) of the capacitor and V is the voltage across the capacitor (and across the spark plug points) at the time it is discharged. It has been found that this circuit provides approximately 10,000 times more energy at the spark plugs than is available in a conventional ignition system.
Although the rectifier 121 is illustrated as a single unit, it may consist of several series-connected rectifiers having lower voltage ratings than that required for a single unit. Of course, the voltage rating of the capacitor 123 should be sufficient for reliable operation at the operating potential. Also, a current limiting resistor 135 may be incorporated in the series circuit, depending upon the characteristic of the diode or diodes 121.
Another advantage of this embodiment of the invention is that the cam angle ("on time") may be increased while decreasing the dwell angle ("off time"). However, where a cam angle over 30° is to be utilized in an engine speed range over 10,000 RPM, a light emitting diode (LED) or magnetic distributor timing arrangement should be used.
From the foregoing, it should be evident that there has herein been described a new and useful solid state ignition system providing a very desirable high frequency, constant current pulse energy output for the ignition system of an internal combustion engine, and which provides for greatly increased energy release in the combustion chamber for ignition.
Although the present invention has been shown and described with reference to particular embodiments, it should be understood that various changes and modifications which are obvious to persons skilled in the art to which the invention pertains are deemed to lie within the spirit, scope and contemplation of the invention.
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A solid state ignition system operating from a relatively low potential direct current input source for use with an internal combustion engine in which a combustible gaseous mixture is detonated by means of the introduction therein of a spark produced by a relatively high potential, high frequency, constant current pulse generator in response to ignition timing signals associated with the engine, the generator including a relatively high frequency pulse energy oscillator triggered by the ignition timing signals and providing such pulse energy to a circuit producing constant current pulses of such energy over a relatively wide input potential operating range, the high frequency continuous wave pulse energy then being power amplified to operate a solid state switch opening and closing the primary circuit of transformer circuitry coupled to the engine's spark plugs.
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BACKGROUND OF INVENTION
1. Field of the Invention
The present invention relates, generally, to pressure chambers. More particularly, the invention relates to Stirling engines with a dual shell pressure chamber.
2. Background Information
The maximum Stirling engine efficiency is related to the Carnot efficiency which is governed by the ratio of maximum working fluid temperature relative to the minimum fluid temperature. Improvements in technologies which increase the margin between the two temperature extremes is beneficial in terms of total cycle efficiency. The lower working fluid temperature is typically governed by the surrounding air or water temperature; which is used as a cooling source. The main area of improvements result from an increase in the maximum working temperature. The maximum temperature is governed by the materials which are used for typical Stirling engines. The materials, typically high strength Stainless Steel alloys, are exposed to both high temperature and high pressure. The high pressure is due to the Stirling engines requirement of obtaining useful power output for a given engine size. Stirling engines can operate between 50 to 200 atmospheres internal pressure for high performance engines.
Since Stirling engines are closed cycle engines, heat must travel through the container materials to get into the working fluid. These materials typically are made as thin as possible to maximize the heat transfer rates. The combination of high pressures and temperatures has limited Stirling engine maximum temperatures to around 800° C. Ceramic materials have been investigated as a technique to allow higher temperatures, however their brittleness and high cost have made them difficult to implement.
U.S. Pat. No. 5,611,201, to Houtman, shows an advanced Stirling engine based on Stainless Steel technology. This engine has the high temperature components exposed to the large pressure differential which limits the maximum temperature to the 800° C. range. U.S. Pat. No. 5,388,410, to Momose et al., shows a series of tubes, labeled part number 22 a through d, exposed to the high temperatures and pressures. The maximum temperature is limited by the combined effects of the temperature and pressure on the heating tubes. U.S. Pat. No. 5,383,334 to Kaminiishizono et al, again shows heater tubes, labeled part number 18, which are exposed to the large temperature and pressure differentials. U.S. Pat. No. 5,433,078, to Shin, also shows the heater tubes, labeled part number 1, exposed to the large temperature and pressure differentials. U.S. Pat. No. 5,555,729, to Momose et al., uses a flattened tube geometry for the heater tubes, labeled part number 15, but is still exposed to the large temperature and pressure differential. The flat sides of the tube add additional stresses to the tubing walls. U.S. Pat. No. 5,074,114, to Meijer et al., also shows the heater pipes exposed to high temperatures and pressures.
The Stirling engine disclosed in the inventor's U.S. Pat. No. 6,041,598 overcomes the limitations and shortcomings of the above prior art by providing a dual shell pressure chamber. An inner shell surrounds the heat transfer tubing and the regenerator. The portion surrounding the heat transfer tubing contains a thermally conductive liquid metal to facilitate heat transfer from a heat source to the heat transfer tubing and also to transmit external pressure to the heat transfer tubing. An outer shell that acts as a pressure vessel surrounds the inner shell and contains a thermally insulating liquid between the inner and outer shells. Pressure of the working fluid as it flows through the regenerator is transmitted through the inner shell to the insulating liquid and back across the inner shell to the liquid metal surrounding the heat transfer tubing. This system tends to balance the pressure across the heat transfer tubing and the inner shell, thereby allowing the engine to operate with the working fluid at a high pressure to generate significant power while keeping the wall of the heat transfer tubing thin to facilitate heat transfer.
The preferred material for the insulating liquid is a salt or glass such as Boron Anhydride or a mixture of Boron Anhydride and Bismuth Oxide. Those materials are fairly viscous when liquid, but still allow significant convection currents. A filler material such as ceramic fiber or similar material is placed in the liquid salt region to minimize convective currents. While this can work very well to transmit and balance the pressure across the inner shell and across the heat transfer tubing, combining the filler material and the liquid salt and installing it between the shells in a manner that does not produce voids can be difficult. Also, before the salt melts it does not transmit pressure. Therefore, significant preheating must be done to thoroughly melt the salt before the engine can be run with significant pressure in the working fluid.
The present invention improves on the dual shell pressure chamber and overcomes the difficulties in using the insulating liquid between the shells by using gas instead of a liquid.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal vertical cross sectional view showing the overall arrangement for a complete Stirling engine system;
FIG. 2 is a detailed view of the circled portion of FIG. 1 illustrating an aperture in the inner shell and an insulating gas backup medium between the shells;
FIG. 3 is a detail view similar to FIG. 2 showing an annular gas backup chamber;
FIG. 4 is a detailed view similar to FIG. 2 showing an annular gas backup chamber and an insulation protection wall; and
FIG. 5 is a partial longitudinal vertical cross sectional view of the upper portion of the Stirling engine showing the placement of a gas backup chamber within the inner shell above the heat transfer tubing.
DETAILED DESCRIPTION
U.S. Pat. No. 6,041,598 granted Mar. 28, 2000, and hereby incorporated by reference, discloses a dual shell pressure chamber as used with a Stirling engine. Referring to FIG. 1 , a cylinder 10 is provided with an expansive bellows 11 , a working fluid, such as Helium, is contained in cylinder 10 above power piston 12 and is shuttled through heat transfer tubing 14 , regenerator 16 , and cooling pipes 18 by the action of displacer piston 20 . Lower housing 22 has an inner area 24 which acts as a reservoir for the working fluid and is in fluid communication with the working fluid in cylinder 10 through throttle ports in cylinder 10 .
The inner shell 30 surrounds the heat transfer tubing 14 and regenerator 16 . The upper portion 32 of inner shell 30 contains a liquid metal region 34 filled with a thermally conductive liquid metal, such as silver, which surrounds the heat transfer tubing 14 . The regenerator 16 is preferably a coiled annulus of thin material disposed between cylinder 10 and inner shell 30 . Outer shell 40 surrounds inner shell 30 and acts as a pressure vessel. The inner shell 30 , outer shell 40 and flange 36 bound a pressure backup region 42 . The pressure backup region is filled with a material to provide pressure backup against inner shell 30 and consequently through liquid metal region 34 to heat transfer tubing 14 . It is also desirable that the pressure backup region 42 contain an insulating material 44 , as depicted in FIG. 2 , to minimize the heat transfer between the hot elements (heat transfer tubing 14 , upper portion 32 of the inner shell, and the upper portion of regenerator 16 ) and cold elements (lower portion of regenerator 16 , and flange 36 ) and to minimize the overall heat loss through the outer shell 40 .
As an alternative to using an insulating liquid in the pressure backup region 42 , as disclosed in U.S. Pat. No. 6,041,598, the present invention uses a gas, preferably the same gas as the working fluid, such as helium, in the pressure backup region 42 , preferably in conjunction with the insulating material 44 such as carbon fiber mat or cloth, or ceramic fiber mat or cloth. In the alternative a lower conductivity gas such as Argon could be used as long as the gas in the backup region is not allowed to mix with the working fluid in cylinder 10 . The insulating material 44 prevents significant convection current flow in the gas, thereby significantly reducing heat transfer through pressure backup region 42 as would occur with the use of gas alone. Since the gas is compressible, it does not transmit pressure like a liquid, so it will not transfer the transient pressure from the working fluid in the regenerator 16 to the liquid metal region 34 , and consequently to the heat transfer tubing 14 , like the liquid will when the engine is running. However, the gas does provide a fairly uniform backup pressure against the outside of the inner shell 30 which is transmitted to the liquid metal region 34 and consequently to the heat transfer tubing 14 .
During engine operation with a heat source of approximately 2000 degrees F., pressure fluctuates inside cylinder 10 over a range of approximately 1000 psi during each cycle of the power piston 12 . By pressurizing pressure backup region 42 to a desired amount, inner shell 30 and heat transfer tubing 14 can see only tensile, only compressive, or a combination tensile and compressive load. For example if the nominal pressure of the working fluid inside cylinder 10 is 1000 psi, during operation the pressure will range between 500 and 1500 psi. If the pressure in backup region 42 is set at 1500 psi, shell 30 and heat transfer tubing 14 see only a 0–1000 psi compressive load. This may be desirable to prevent any tensile cracking from occurring in those structures. In that case shell 30 may be compressed against regenerator 16 which may detrimentally effect the regenerator. Alternatively, the backup pressure may be set at 500 psi such that shell 30 and heat transfer tubing see only a 0–1000 psi tensile load, thus preventing any compression of shell 30 against the regenerator, but requiring shell 30 and heat transfer tubing 14 to have sufficient tensile strength. Setting the backup pressure at 1000 psi results in a ±500 psi tensile and compressive load across shell 30 and heat transfer tubing 14 . The inventor believes this is the best mode of operation because it subjects the structures to the lowest absolute load.
Using the gas pressure backup in this manner, the pressure of the working fluid can be raised to any desirable level to produce significant power in the engine while the loads on the heat transfer tubing 14 and the inner shell 30 are kept low. The upper bounds of the pressure is limited only by safety and manufacturing considerations for the outer shell 40 and the lower housing 22 , which function as a pressure vessel against the atmosphere. Lower housing 22 can be designed to enclose an electrical generator connected to the output shaft 43 of the dual shell Stirling engine, thereby eliminating the need for any external high-pressure seal against a rotating shaft extending through the lower housing.
Referring also to FIG. 2 , when it is desired to operate the engine such that the backup pressure region 42 provides an average tensile and compressive load across inner shell 30 , a small aperture 50 is provided through inner shell 30 , preferably near flange 36 . The advantage of placing the aperture in a low position is that it is in the cold section of the engine and thus the metal is stronger. Aperture 50 thereby allows fluid communication between backup pressure region 42 and the working fluid contained in cylinder 10 and the working fluid reservoir in inner area 24 of lower housing 22 . When the engine is not running, all the pressures in these regions equalize. The working fluid for the engine may be charged to a desired nominal pressure, 1000 psi for example, using a single port, such as through the lower housing 22 into its inner area 24 . Pressure in cylinder 10 and in backup pressure region 42 will also equalize at that pressure. When the engine starts to run, the pressure inside cylinder 10 will fluctuate plus or minus approximately 500 psi. Because the aperture 50 is very small, preferably approximately 0.02 to 0.06 and the engine is running typically over 1000 rpm, the movement of the gas through aperture 50 will be oscillatory and rather minimal. Thus the backup pressure in backup pressure region 42 is maintained at approximately a nominal level. The use of the small aperture 50 is preferred since it allows an averaging of pressures during each cycle. The advantage is that it tracks the average pressure ratio which may change during operation.
As pointed out above, the gas backup provides a fairly uniform backup pressure which is of advantage if the pressure in the region 42 were to track pressure in the regenerator region 16 . As also mentioned, the aperture 50 allows an averaging of pressures during each cycle of the engine. As the size of the hole 50 increases, the pressures start to match. This is a favorable condition for stresses in the material but is detrimental to engine power which drops as more and more flow goes in and out of the port 50 with each stroke. FIG. 3 illustrates one method of reducing the required gas flow through the port 50 which involves the use of a material in the region 44 a which may be either a solid or only a slightly porous material. This material acts as an insulation and may comprise a cast ceramic material which is both rigid and fairly low in thermal conductivity. Filling the region 42 which such a ceramic material reduces the volume of gas required, which is restricted to the annular space 45 maintained between the ceramic insulation and the wall of the inner shell 30 . This smaller volume would be much easier to pressurize in a time varying manner. As illustrated, the annular space 45 is connected to the working fluid, i.e. the helium gas in regenerator 16 as previously described.
FIG. 4 illustrates still another embodiment similar to the FIG. 3 embodiment wherein the ceramic insulation material 44 b is spaced from the wall of the inner shell 30 with a thin stainless steel wall 46 being located on the inner border of the material 44 b . The wall 46 is spaced a slight distance from the inner shell 30 , defining a narrow annulus 45 for gas containment as previously described. In this instance, the ceramic insulator may be slightly porous for the purpose of improving its heat transfer properties. The ceramic insulator would be constructed strong enough to hold the pressure field being applied on the inside of the thin wall. This structure provides the narrow annulus which is pressurized with the gas thereby allowing a reduced volume requirement for a time varying pressure match. Aperture 50 in this instance could be larger to more closely match the pressure i.e. approximately 0.2 to 0.5 inches in diameter. Several holes 50 could be placed around the wall to provide a more balanced time varying pressure.
FIG. 5 illustrates still another embodiment wherein the gas backup medium may be placed above the liquid metal region 34 . The region 42 would be provided with a ceramic insulation material 44 c as previously described, completely filling the region between the inner and outer shells. In the alternative, in this embodiment, the region 42 could be filled with an insulating liquid salt or glass as disclosed in applicant's previous patent. As shown in FIG. 5 , a feeder pipe 47 extends from the upper portion of the cylinder 10 containing the working fluid, traverses through the liquid metal region 34 and communicates with the backup gas region 48 above the liquid metal region. As described for previous embodiments, the backup gas area 48 thus is connected to the working fluid and allows an averaging of pressures during each cycle. Although backup gas region 48 may be directly interfaced with the liquid metal region 34 , it may be desirable to place solid ceramic or metal layer such as the layer 49 between the liquid metal and the backup gas to keep the liquid metal from splashing into the inside of the engine. The backup gas arrangement in this embodiment performs substantially in the same manner as previously described in the various embodiments in allowing an averaging of pressures during each cycle or a time varying pressure dependent on the size of pipe 47 .
Because the backup pressure region 42 or region 48 , the working fluid area inside cylinder 10 , and the working fluid reservoir in inner area 24 of lower housing are all in fluid communication, the overall average pressure in all these areas may be adjusted upward or downward, such as through a single port in the lower housing, while the engine is running.
The descriptions above and the accompanying drawings should be interpreted in the illustrative and not the limited sense. While the invention has been disclosed in connection with the preferred embodiment or embodiments thereof, it should be understood that there may be other embodiments which fall within the scope of the invention.
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A Stirling engine which utilizes an inner and outer dual shell pressure containment system surrounding the high pressure and temperature engine components. The space between the shells is filled with a pressure backup gas and an insulation material with the backup gas being in communications with the working fluid. The backup gas and insulation provide a time varying pressure field, driven by the pressure variations in the Stirling engine working fluid, which cancels the pressure differential on the heat transfer tubing and allows an averaging of pressures during each cycle of engine operation. In one embodiment the backup gas is placed inside the inner shell.
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BACKGROUND
[0001] 1. Field of the Invention
[0002] The present invention relates to the field of network publications through a feed service and, more particularly, to using a group list server as a syndication feed server.
[0003] 2. Description of the Related Art
[0004] Conventionally, list management servers and syndication feed servers are special purpose servers—each serving a different function, each using different protocols and conventions, each being implemented by separate server software, and each being used by separate client software. To elaborate, a list management server traditionally is used to create and manage network-based group definitions and associated lists of members for defined groups. The list management server can maintain access lists, permissions, and other service specific properties associated with groups and group members. Use of a list management server permits a user's contact list, such as an email list or a personal address book, to be specified and used in an application independent manner. This can allow a user's contact list to be used by an email program at work and at home, by a mobile telephony device of the user, and the like. List management servers also support group list nesting so that one list can be referenced within another. The list management server further permits multiple users to share lists, such as sharing contact lists among employees in a company. Numerous standards exist to ensure compatibility of server managed lists, such as the XML Configuration Access Protocol (XCAP) standard of the Internet Engineering Task Force (ETF).
[0005] In contrast, a syndication server permits users to subscribe to syndication feeds. A syndication feed, such as a Really Simple Syndication (RSS) or an Atom Syndication Format (ATOM) feed, are used to provide items containing short descriptions of Web content together with a link to a full version of the content and/or with a text version of the full content. Syndication feeds are used to publish frequently updated content, such as BLOG entries, news headlines, or podcasts. Feed content can be read using a feed reader or an aggregator. That is, users subscribe to a feed by entering the feed's link into the reader. The reader regularly checks subscribed feeds for new content and downloads any new content related to these feeds.
[0006] FIG. 1 (Prior Art) is included to pictorially illustrate conventional implementations of a feed server shown in arrangement 110 and a list server shown in arrangement 150 . In the prior art feed server arrangement 110 , a client 120 can subscribe to a feed server 130 that provides syndication feeds. The feed server 130 can gather content from one or more Web sources 140 . For instance, one or more Web servers 140 can provide Hyper Text Markup Language (HTML) pages to the feed server 130 responsive to server 130 issued requests. The feed server 130 can utilize a converter 132 to extract content from the HTML pages and to repackage it into an XML format. The repackaged content can differ from the original content in that it no longer includes presentation information, but only content. Users of interface 122 can trigger a poll event to one or more feed servers 130 which results in a streamed update. The update can contain any content corresponding to the subscription that the server 130 has received since a last poll. A single client 120 can include an aggregator 124 component that combines content from multiple feed servers 130 into a user configured view. Aggregation can also occur within a Web server (not shown) that provides feed content to client 120 .
[0007] In the group list server arrangement 150 , different communication nodes 160 can each connect to a list management server 172 via network 170 . Each node 160 can include a user 162 - 164 and a computing device 166 - 168 . The same user 162 - 164 can use the list management server 172 as a central repository for storing contact information used by multiple different devices 166 - 168 . Further, different users 162 - 164 can share a common set of server 172 maintained information, such as sharing updated business contact information among a set of business agents. The list management server 172 can maintain and use a set of list server tables 180 . These tables 180 can include a group table 182 , a participant table 186 , and a linkage table 184 , which links the group 182 and participant tables 186 . The group table 182 can maintain information concerning the groups that the list server 172 manages, such as a group id, a group name, a description and other attributes. The participant table 186 can maintain information concerning group members, such as a participant id, name, device address, and status. The linkage table 184 can associate group table 182 items to participant table 186 items in a many-to-many relationship.
SUMMARY OF THE INVENTION
[0008] The present invention discloses a solution for modifying a group list server to perform syndication feed operations in accordance with an embodiment of the inventive arrangements disclosed herein. More specifically, a syndication feed creation software component, a content gathering component, and a content extraction converting component can be added to a group list server. The modified group list server can continue to function as a traditional list server and can also function as a traditional feed server, able to interoperate with standard, client-side feed readers. In one embodiment, the modified list server can repurpose syndication groups to operate as syndication feed channels and can repurpose group members to operate as feed items. The disclosed solution permits security, management, scalability, reliability, and performance of a group list server to be directly applied to a syndication feed environment.
[0009] The present invention can be implemented in accordance with numerous aspects consistent with the material presented herein. For example, one aspect of the present invention can include a group list server that includes list management software and syndication feed software, both of which can be stored in a machine readable medium and which include a set of programmatic instructions that are executable by a machine. The list management software can manage network-based group definitions and lists of members for defined groups. The syndication feed software can serve syndication feeds to remotely located clients.
[0010] Another aspect of the present invention can include a system for providing syndication feeds that includes an acquisition engine and a syndication engine. The acquisition engine can extract content from network servers and can place extracted content in a syndication format, which is stored in at least one group list table. Each group list table can correspond to a syndication channel. The syndication engine can serve syndication feeds to remotely located clients. The served syndication feeds are obtained from the group list tables. The remotely located clients can be standard syndication feed clients. Communications to/from the syndication feed clients can conform to at least one of a Really Simple Syndication (RSS) based protocol and an Atom Syndication Format (ATOM) based protocol.
[0011] Still another aspect of the present invention can include a method for handling syndication feeds. The method can include a step of identifying at least one syndication feed item associated with a syndication channel. The syndication channel can be represented as a list management server group. At least one syndication feed item in a group table managed by the list management server group can be stored by a list management server. The server can serve the stored syndication feed item to at least one syndication feed client responsive to a syndication feed request.
[0012] It should be noted that various aspects of the invention can be implemented as a program for controlling computing equipment to implement the functions described herein, or as a program for enabling computing equipment to perform processes corresponding to the steps disclosed herein. This program may be provided by storing the program in a magnetic disk, an optical disk, a semiconductor memory, any other recording medium, or can also be provided as a digitally encoded signal conveyed via a carrier wave. The described program can be a single program or can be implemented as multiple subprograms, each of which interact within a single computing device or interact in a distributed fashion across a network space.
[0013] The method detailed herein can also be a method performed at least in part by a service agent and/or a machine manipulated by a service agent in response to a service request.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] There are shown in the drawings, embodiments which are presently preferred, it being understood, however, that the invention is not limited to the precise arrangements and instrumentalities shown.
[0015] FIG. 1 (Prior Art) pictorially illustrates conventional implementations of a feed server and a list server.
[0016] FIG. 2 is a schematic diagram of a system that includes a list management server having syndication feed server capabilities in accordance with an embodiment of the inventive arrangements disclosed herein.
[0017] FIG. 3 is a schematic diagram of a system in which a list management server provides syndication feed data to one or more clients in accordance with an embodiment of the inventive arrangements disclosed herein.
[0018] FIG. 4 is a flow chart of a method for utilizing a list server as a syndication feed server in accordance with an embodiment of the inventive arrangements disclosed herein.
DETAILED DESCRIPTION OF THE INVENTION
[0019] FIG. 2 is a schematic diagram of a system 200 that includes a list management server 210 having syndication feed server capabilities in accordance with an embodiment of the inventive arrangements disclosed herein. The list management server 210 can maintain list server functionality. A syndication channel ( 240 - 242 ) can correspond to a list server group 244 and syndication items can correspond to group list elements. One of more software routines, such as a syndication engine 214 and an acquisition engine 216 can exist within the list management server 210 . In one embodiment, these engines 214 - 216 can be plug-ins, such as JAVA servlets, that enhance a list management server 210 . Although the engines 214 and/or 216 can be contained within the server 210 , the engines 214 and/or 216 can also be located in one or more remote machines (not shown) that pre-/post-process information to/from the list management server 210 . In one embodiment, the list management server 210 can be a standard commercial off-the-shelf (COTS) server.
[0020] The acquisition engine 216 can obtain syndication content 232 from remote network servers, can convert the content 232 to a syndication feed format, and can store the converted content 232 in a syndication channel table 240 - 242 of data store 218 . Syndication formats of the stored syndication feed items can include a Really Simple Syndication (RSS) compliant format, an Atom Syndication Format (ATOM) compliant format, an Extensible Markup Language (XML) based syndication format, as well as other feed formats. Syndication of feeds refers to a publishing of frequently updated content such as blog entries, news headlines or podcasts. A syndication feed item or document is often referred to as a feed, a web feed, or a channel. One network location from which syndication content 232 can be extracted from can be a Web server, where the syndication content 232 is Web content. The invention is not to be construed as limited in this regard, however, and any content source can be used. Additionally, each syndication feed item can contain a summary of content from an associated Web site, the full text extracted from the Web site, and related data items.
[0021] For example, Syndication Channel AAA 240 can contain syndication feed items (e.g., AAAA, BBBB, CCCC, and DDDD) each having an associated update time, content, and source address. The Syndication Channel AAA 240 can be maintained in a repurposed group table, as is Syndication Channel BBB 242 . Storing syndication channels within group tables 240 - 242 can occur in a non-interfering manner that does not affect operation of standard list server group tables 244 .
[0022] The syndication engine 214 can accept feed requests 230 from remote clients. Each request 230 can be a request for all updates to a particular syndication channel that have occurred since a last update time. Recently updated feed items 234 can be provided in response to the requests 230 . A sample syndication feed item 236 is shown as an XML document in RSS format that includes two items, one for 2002/09/01 and another for 2002/09/02.
[0023] In one embodiment, the requests 230 can originate from feed readers and/or feed aggregators contained in requesting clients. That is, the requests 230 can be standard requests from RSS or ATOM clients, which the list management server 210 can handle in accordance with the applicable standards (e.g., RSS or ATOM standards). Although compatible with existing syndication standards, the engines 214 - 216 provide a highly flexible solution that is able to be adapted to non-standard feed requesting techniques. For example, new feed request techniques, such as a Session Initiation Protocol (SIP) technique, can be implemented to permit any SIP compatible device to request and receive syndication feed items. In other words, system 200 can be a multi-channel access system for obtaining the feed items 234 from the server 210 , where RSS (e.g., HTTP based access in general) is one “channel” or access technology for obtaining the feed items 234 , SIP can be an access technology for another “channel”, XML Configuration Access Protocol (XCAP) can be an access technology associated with yet another access channel (as illustrated in FIG. 3 ), and so forth.
[0024] As used herein, the list management server 210 can allow for the creation and management of network-based group definitions and associated lists for members of those groups. In one embodiment, the server 210 can be a generic XML document management server that is able to specify document lists used by member groups. The server 210 , when enhanced by engines 214 and 216 , can also handle syndication feeds. The list management server 210 can operate in accordance with numerous open standards, such as an XML Configuration Access Protocol (XCAP) based standard, an Open Mobile Alliance (OMA) XML Document Management Server (OMA XDMS) based standard, and the like. The list management server 210 can be implemented using numerous commercially available solutions, such as the GROUP LIST MANAGEMENT SERVER (GLM) for IBM IMS. The invention is not limited to being implemented in this fashion, however, and other solutions can be used including the NOKIA LIST MANAGEMENT SERVER, the HP OPENCALL XML DOCUMENT MANAGEMENT SERVER, and the like.
[0025] The data store 218 can be a physical or virtual storage space configured to store digital information. Data store 218 can be physically implemented within any type of hardware including, but not limited to, a magnetic disk, an optical disk, a semiconductor memory, a digitally encoded plastic memory, or any other recording medium. The data store 218 can be a stand-alone storage unit as well as a storage unit formed from a plurality of physical devices. Additionally, information can be stored within the data store 218 in a variety of manners. For example, information can be stored within a database structure or can be stored within one or more files of a file storage system, where each file may or may not be indexed for information searching purposes. Further, data store 218 can utilize one or more encryption mechanisms to protect stored information from unauthorized access.
[0026] The list management server 210 can be communicatively linked to one or more remotely located computing devices via a network (not shown) over which items 230 - 234 are digitally conveyed. The network can include any hardware/software/and firmware necessary to convey data encoded within carrier waves. Data can be contained within analog or digital signals and conveyed though data or voice channels. The network can include local components and data pathways necessary for communications to be exchanged among computing device components and between integrated device components and peripheral devices. The network can also include network equipment, such as routers, data lines, hubs, and intermediary servers which together form a data network, such as the Internet. The network can also include circuit-based communication components and mobile communication components, such as telephony switches, modems, cellular communication towers, and the like. Additionally, the network can include line based and/or wireless communication pathways.
[0027] FIG. 3 is a schematic diagram of a system 300 in which a list management server 330 provides syndication feed data to one or more clients 310 - 314 in accordance with an embodiment of the inventive arrangements disclosed herein. The list management server 330 can be implemented in accordance with the details described in system 200 : That is, system 300 represents one contemplated architecture for implementing a syndication feed solution. As shown in system 300 , the list management server 330 provides multi-channel access using different access protocols, such as HTTP, SIP, and XCAP.
[0028] Specifics of system 300 are shown as being implemented using JAVA ( 340 ), SIP, XML configuration access protocol (XCAP), Extensible style sheet language transformation (XSLT), and/or XML Path Language (XPath) based technologies, standards, and formats, which are used for illustrative purposes only and are not intended to be limitations imposed on the invention. In different contemplated embodiments, C++, .NET, or other code languages can be substituted for any JAVA specific references, and other protocols/standards can replace SIP, XCAP, XSLT, XPath, and the like yet still be considered within a scope of the disclosed invention.
[0029] In system 300 , the JAVA 340 component can read an XML file 375 that specifies the Uniform Resource Locators (URLs) of Hypertext Markup Language (HTML) pages that are to be converted to syndication channel content. Along with each URL, the XML file can indicate an XSLT 367 or XPath 377 document that is used to extract content from the HTML page. The content can be stored by the list management server 330 in a repurposed list group, which functions as a syndication channel. The URL for the HTML page can be saved as a group name and all URL links to the page can be saved as group members. The XSLT 376 or XPath 377 document can fetch from the page a title and description for each link. The documents 376 - 377 can also enrich the original HTML content by adding text of their own. The extracted title and description can be saved in the list management server 330 as attributes to the GLS member (URL) with which these elements correspond.
[0030] In one embodiment, the JAVA component 340 can subscribe 371 to the lists and can set a timer 332 so that the component 340 is notified 370 when a list should be refreshed. In addition to the timer 332 triggering a refresh event, the list can be refreshed whenever the JAVA component 340 or list management server 330 detects a change to the corresponding list. For instance, one of the clients 310 - 314 can update list content through the list management server 330 .
[0031] Information managed by the list management server 330 can be accessed by different clients 310 - 314 in different manners. One manner is to push 360 updated data from a list management server 330 to clients 310 , which subscribe to a related syndication feed. For example, SIP SUBSCRIBE/NOTIFY interfaces and conventions can be used, where a client 310 subscribes to a syndication channel (e.g., group name) and is automatically NOTIFIED by the list management server 330 whenever that channel's data changes.
[0032] Another technique to acquire data from the list management server 330 is for a client 312 to pull 362 data from the server 330 . For example, an RSS client can choose to use XCAP 374 to fetch a data channel. Unlike the SIP based technique ( 360 ), the client 312 must poll the server 330 for updates.
[0033] Still another technique for acquiring syndication data from server 330 is to utilize a convention syndication client 314 and access methodology. In other words, the client 314 can send an HTTP request to a Web server 320 for a syndication resource provided by server 330 that is associated with a syndication channel 322 . The Web server 320 can execute a servlet that sends an XCAP 374 message to the group list server 330 to fetch the syndication channel 322 information. In another implementation, the server 320 can use a SIP based interface to communicate with the server 330 . The Web server 320 can format the received data as an XML stream, which it conveys to the client 314 .
[0034] Appreciably, clients 310 - 312 are non-traditional clients of syndication data in that they receive data from a syndication channel, which each of the receiving clients 310 - 312 internally organizes in this respect, client 314 can be a “true RSS” client, while clients 310 - 312 are not.
[0035] In system 300 , each of the clients 310 - 314 can be any computing device capable of exchanging messages over a network. The clients 310 - 314 can include, but are not limited to, a computer, a small business server, a standard telephone, an SIP based telephone, a mobile telephone, a two-way radio, a personal data assistant, a media player, a video game entertainment system, a chat terminal, a wearable computing device, and the like. Various ones of the communication devices 310 - 314 can be capable of different communication modalities. For example, a computer (device 310 - 314 ) can be able to communicate using a Voice over Internet Protocol (VOIP) phone, a local application's Graphic User Interface (GUI), a Web interface, and the like. The syndication content from the list management server 330 can be obtained using any of these communication modalities.
[0036] FIG. 4 is a flow chart of a method 400 for utilizing a list server as a syndication feed server in accordance with an embodiment of the inventive arrangements disclosed herein. The method 400 includes a process 405 that shows a manner in which a list server interacts with syndication data sources. A different process 450 of method 400 shows a manner in which the list server interacts with syndication clients. The method 400 call be performed in the context of a system 200 or a system 300 .
[0037] Process 405 can begin with a step 410 , where a group list server (GLS) group can be treated or purposed as a syndication channel. In step 415 , a network server can be queried to receive a Web page or other content. In step 420 , content can be extracted. In step 425 , extracted content can be converted/re-formatted into a proper format for a syndication feed entry. In step 430 , the feed entry can be added as a group item for the GLS group. In step 435 , a set of re-query conditions can be compared against a set of current system conditions. When re-query conditions are not satisfied in step 435 , the method can wait for a delay period, at which point the re-query conditions of step 435 can be checked again. When the re-query conditions are satisfied, the process 405 can progress from step 435 to step 415 , where the network server can be queried for updated content.
[0038] Process 450 can begin in step 455 , where a request for syndication data can be received from a syndication feed client. In step 460 , a last update time for the client can be determined. In step 465 , the GLS group that has been purposed as a syndication channel can be searched to determine a set of syndication feed items that have been updated since the last request. In step 470 , a set of discovered feed items since the last update can be conveyed to the requesting client. The process 450 can repeat for each syndication client and for each syndication request.
[0039] The present invention may be realized in hardware, software, or a combination of hardware and software. The present invention may be realized in a centralized fashion in one computer system or in a distributed fashion where different elements are spread across several interconnected computer systems. Any kind of computer system or other apparatus adapted for carrying out the methods described herein is suited. A typical combination of hardware and software may be a general purpose computer system with a computer program that, when being loaded and executed, controls the computer system such that it carries out the methods described herein.
[0040] The present invention also may be embedded in a computer program product, which comprises all the features enabling the implementation of the methods described herein, and which when loaded in a computer system is able to carry out these methods. Computer program in the present context means any expression, in any language, code or notation, of a set of instructions intended to cause a system having an information processing capability to perform a particular function either directly or after either or both of the following: a) conversion to another language, code or notation; b) reproduction in a different material form.
[0041] This invention may be embodied in other forms without departing from the spirit or essential attributes thereof. Accordingly, reference should be made to the following claims, rather than to the foregoing specification, as indicating the scope of the invention.
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The present invention discloses a solution for modifying a group list server to perform syndication feed operations. A syndication feed creation software component, a content gathering component, and a content extraction converting component can be added to a group list server. The modified group list server can continue to function as a traditional list server and can also function as a traditional feed server that is able to interoperate with standard, client-side feed readers. In one embodiment, the modified list server can repurpose syndication groups as to operate as syndication feed channels and can repurpose group members to operate as feed items.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The application claims priority to U.S. Provisional Patent Application 62/120,457, entitled “Backward Compatible System and Method for Using 4P Audio Jack to Provide Power and Signal to Headset with Active Noise Cancellation,” filed Feb. 25, 2015, which application is hereby incorporated herein by reference in its entirety.
BACKGROUND
[0002] A. Technical Field
[0003] The present invention relates generally to accessory management and data communication via an audio port on an electronic device.
[0004] B. Background of the Invention
[0005] Audio sockets have been commonly used in various electronic devices, such as computers, laptops, media players, smart phones, etc. to communicate with audio accessories having audio jacks. The mostly common used jack plugs have 2.5 mm, 3.5 mm or 6.35 mm (¼ inch) configurations with 2, 3 or 4 conductors (2P, 3P or 4P) for mono, stereo or stereo plus microphone compatibility. Stereo 3.5 mm jacks may be used for line in/out, headset out, loudspeaker out, microphone in, etc. Three-conductor connectors are common on older electronic devices, while 4-conductor 3.5 mm connectors are more commonly used on modern electronic devices, including most smart phones.
[0006] A 2-conductor jack is called TS connector with a tip and a sleeve for mono audio communication. A 3-conductor jack is called TRS connector with a tip, a ring and a sleeve for stereo audio communications. A 4-conductor jack is usually called TRRS connector with a tip, two rings and a sleeve for stereo plus microphone line communications. In certain circumstances, it is desirable to use a TRRS jack to transmit additional audio and/or data signal to host electronic devices.
[0007] Beyond receiving audio signal input from electronic device, some audio accessory, such as headset with active noise control (ANC) also need power input to operate its noise control circuit. Traditionally, the ANC headset is powered by separate battery, which causes bulky size for the headset and limited operation time.
[0008] Efforts have been done to explore further potential applications using audio jack connection. 5-conductor jack has been proposed and developed recently. However, it is very difficult to make those 5-conductor jacks backward compatible to most modern electronic devices. Additional cost will be needed for customer connector and hardware for 5-conductor jacks. Given the variety in the audio accessories of different characteristics and preferred settings, it would be desirable to provide improved accessory management and signal communication via 4P audio port with backward compatibility for supporting interactions between electronic devices and accessories.
SUMMARY OF THE INVENTION
[0009] The invention relates to accessory management and data communication, and more particularly, to backward compatible systems and methods for using 4P audio jack in an electronic device to provide power and signal to headset with active noise cancellation (ANC) as well as accessories that require an external power.
[0010] The method involves automatically deciding at the electronic device accessory type after accessory insertion detected and choosing accessory communication mode based at least on the decided accessory type and accessory input signal. The accessory communication mode may be an accessory power mode or an accessory microphone mode. In the accessory power mode, the electronic device provides power to the accessory over a microphone line (MIC line) operated beyond traditional microphone bias voltage level. In the accessory microphone mode, the electronic device provides MIC bias and audio signals to the accessory.
[0011] In certain embodiments, communication starts after the jack insertion is detected. The accessory's ID and audio jack configuration are initially checked. The audio jack configuration check verifies the type of the audio jack (TS, TRS or TRRS jack) and also the type of the accessory. The accessory type detection method includes impedance detection of audio lines as well as MIC line.
[0012] If the accessory is detected to be a traditional 4P headset, the electronic device provides MIC bias and audio signals to the 4P headset. If the accessory is detected to be a 4P accessory requesting power support, the host electronic device provides power to the accessory over the microphone line (MIC line).
[0013] In certain embodiments, some accessories have one audio line (L-audio or R-audio) multiplexed with the MIC line. The electronic device detects and monitors microphone bias on at least one audio line, such as L-audio or R-audio line. If the microphone bias is detected and is higher than V ref1 for duration of time longer than t deb1 , then the audio line is being used as a microphone and the electronic device routes the audio line as a microphone input and turn on an audio bypass switch. If the microphone bias is lower than V ref1 for duration of time longer than t deb1 , the electronic device latches the audio line for audio signal output from an audio drive circuit within the electronic device.
[0014] In certain embodiments, when the electronic device provides power to the accessory over the microphone line (MIC line), the MIC line voltage is monitored. If the MIC line voltage is below the V ref2 for duration of time longer than t deb2 , the electronic device is not supporting the accessory power mode and the accessory operates in low power mode (legacy mode) and optional bypass mode.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Reference will be made to exemplary embodiments of the present invention that are illustrated in the accompanying figures. Those figures are intended to be illustrative, rather than limiting. Although the present invention is generally described in the context of those embodiments, it is not intended by so doing to limit the scope of the present invention to the particular features of the embodiments depicted and described.
[0016] FIG. 1 is a schematic diagram of an electronic device in communication with an accessory in a system via an audio jack in accordance with an embodiment of the present invention.
[0017] FIG. 2 is an exemplary schematic diagram of an accessory according to various embodiments of the invention.
[0018] FIG. 3 is an exemplary schematic diagram of the accessory control IC according to various embodiments of the invention.
[0019] FIG. 4 is an exemplary block diagram of the accessory in communication with an electronic device for host detection according to various embodiments of the invention.
[0020] FIG. 5 is an exemplary schematic diagram of an electronic device according to various embodiments of the invention.
[0021] FIG. 6 is an exemplary block diagram of the accessory in communication with an electronic device for accessory detection according to various embodiments of the invention.
[0022] FIG. 7 is another exemplary block diagram of the accessory in communication with an electronic device for accessory detection according to various embodiments of the invention.
[0023] One skilled in the art will recognize that various implementations and embodiments of the invention may be practiced in accordance with the specification. All of these implementations and embodiments are intended to be included within the scope of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] In the following description, for the purpose of explanation, specific details are set forth in order to provide an understanding of the present invention. The present invention may, however, be practiced without some or all of these details. The embodiments of the present invention described below may be incorporated into a number of different electrical components, circuits, devices, and systems. Structures and devices shown in block diagram are illustrative of exemplary embodiments of the present invention and are not to be used as a pretext by which to obscure broad teachings of the present invention. Connections between components within the figures are not intended to be limited to direct connections. Rather, connections between components may be modified, re-formatted, or otherwise changed by intermediary components.
[0025] When the specification makes reference to “one embodiment” or to “an embodiment”, it is intended to mean that a particular feature, structure, characteristic, or function described in connection with the embodiment being discussed is included in at least one contemplated embodiment of the present invention. Thus, the appearance of the phrase, “in one embodiment,” in different places in the specification does not constitute a plurality of references to a single embodiment of the present invention.
[0026] Various embodiments of the invention are used for accessory management and data communication via audio port in systems comprised of one or more integrated circuits (IC). An IC may be a memory, microcontroller, microprocessor, secure authenticator or any other devices within a system that communicates and/or receives information within the system. These systems, and the IC(s) therein, may be integrated on a single component or contain discrete components. Furthermore, embodiments of the invention are applicable to a diverse set of techniques and methods.
[0027] FIG. 1 shows a schematic diagram of a system 100 according to various embodiments of the invention. The system 100 comprises an electronic device 200 in communication with an accessory 300 . Communication between the device and the accessory begins after an audio jack 310 on the accessory 300 inserts into an audio socket 210 on the electronic device 200 . The electronic device may detect the type of the accessory and communicates to the accessory in different operation modes accordingly. On the other hand, the accessory may detect the capacity and operation mode of the electronic device and adjust accessory configurations based on the detected operation mode.
[0028] The electronic device 200 may be a computer device, a laptop, a portable media player, such as a MP3 player, a smart phone, etc. The accessory 300 may be an audio accessory such as a microphone, a headphone, loudspeakers, an audio amplifier, or be an electronic accessory having audio jack for voice and data communications. In an embodiment, the accessory 300 has a stereo or mono earphone and a microphone for audio input to the electronic device 200 .
[0029] The audio socket 210 is a 4P audio socket. The audio jack 310 may have 2.5 mm, 3.5 mm or 6.35 mm (¼ inch) configurations with 2, 3, 4 or even 5 conductors for mono, stereo, stereo plus microphone, and stereo plus microphone with power compatibility.
[0030] In one embodiment, the electronic device 200 has an audio socket 210 , an I2C interface 220 , a microprocessor 230 , a memory 240 , a power source 250 and an audio driver circuit 260 . The microprocessor 230 is configured to operatively connect to the I2C interface 220 , the memory 240 , the power source 250 and the audio driver circuit 260 . The I2C interface 220 is an Inter-Integrated Circuit used for attaching peripheral audio socket 210 to the microprocessor 230 . The memory 240 is configured to store a non-volatile computer readable logic or code for the implementation of desired function when the logic or code is executed by the microprocessor 230 .
[0031] In one embodiment, the accessory 300 comprises an accessory control IC 320 , an audio jack 310 and an earphone 340 . In another embodiment, the accessory 300 has a microphone 350 coupled to the accessory control IC 320 . In yet another embodiment, the accessory 300 also has a secure authenticator 330 and an audio sensor 360 for noise control purpose. In some embodiment, the accessory control IC 320 may be an active noise control (ANC) circuit or a stereo speaker balance circuit, etc. The accessory control IC 320 couples to the audio jack 310 , the earphone 340 , audio sensor 360 , and the microphone 350 . In some embodiments, the audio sensor 360 is a stereo audio sensor comprising an L-audio sensor 362 , R-audio sensor 364 .
[0032] FIG. 2 illustrates an exemplary schematic diagram of an accessory according to various embodiments of the invention. The accessory 300 has a TRRS audio jack 310 , a stereo earphone 340 (L-earphone 342 and R-earphone 344 ), a microphone 350 , an accessory control IC 320 and a secure authenticator 330 . The audio jack 310 comprises an L-audio conductor 311 , an R-audio conductor 312 , a ground conductor 313 and a microphone conductor 314 . The L-audio conductor 311 , R-audio conductor 312 and a microphone conductor 314 are connect to L-audio input port 321 , R-audio input port 322 and power input port (PWR) 323 of the accessory control IC 320 respectively.
[0033] The accessory control IC 320 also comprises an L-Mic port 328 , a R-Mic port 329 , a L-audio output port 326 , R-audio output port 327 operatively connected to the L-audio sensor 362 , R-audio sensor 364 , L-earphone 342 and R-earphone 344 , respectively. During the operation of the accessory 300 , audio jack 310 is inserted to the audio socket 210 of the electronic device 200 for audio/MIC signal communication. The accessory control IC 320 receives audio signal inputs from the audio jack 310 and the audio sensor 360 , processes those signals via internal signal processing circuit (not shown in FIG. 2 ) and generates outputs signals to the earphone 340 .
[0034] In another embodiment, the accessory control IC 320 comprises a MIC input port 324 and a MIC bias port 325 to receive/output signal to the microphone 350 . The accessory control IC 320 may be operated to receive signal input from the microphone 350 and send the signal to the electronic device 200 through the microphone conductor 314 . The accessory control IC 320 may be alternatively operated to receive bias input from the electronic device 200 via the microphone conductor 314 and output the bias signal to the microphone 350 through the MIC bias port 325 . The accessory control IC 320 may also be operated to receive digital communication such as 1-wire or ultra sound input from the electronic device 200 via the microphone conductor 314 and output the bias signal to the microphone 350 through the MIC bias port 325 .
[0035] FIG. 3 illustrates an exemplary schematic diagram of accessory control IC according to various embodiments of the invention. The accessory control IC 320 comprises a digital signal processing (DSP) circuit 371 , a R-audio/MIC selection switch 373 , a low dropout regulator (LDO) 378 , a LDO switch 379 , a MIC line voltage comparator 374 and a power line voltage comparator 377 . The DSP circuit 371 couples between signal input ports (L-audio input port 321 , R-audio input port 322 , L-Mic port 328 and R-Mic port 329 ) and audio output ports (L-audio output port 326 and R-audio output port 327 ). The DSP circuit 371 may be a DSP (digital signal processing) circuit for ANC or power accessory applications. In one embodiment, the accessory control IC 320 also comprises an optional button detection interface 372 to detect/receive button operations and send the detected operations to the DSP circuit 371 for further processing. In another embodiment, the LDO 378 comprises soft-start circuit to limit inrush current and control output voltage rising time during power-up.
[0036] The power line voltage comparator 377 has one input coupled to the power input port (PWR) 323 and compares the voltage at the power input port to a predetermined threshold voltage. The output of the power line voltage comparator 377 is coupled to the LDO switch 379 via a latch component 376 with a predetermined debounce time to switch ON/OFF the LDO switch 379 . In one embodiment, the predetermined threshold voltage is an input voltage required to operate the LDO 378 . In one embodiment, the predetermined threshold voltage is set at 2.8V. When the voltage at the power input port is larger or equal to the predetermined threshold voltage, the LDO switch 379 is switched ON to enable LDO 378 operation and thus provide power to the DSP circuit 371 .
[0037] In one embodiment, the accessory control IC 320 comprises a bypass switch 375 coupled between signal input ports (L-audio input port 321 , R-audio input port 322 ) and output ports (L-audio output port 326 and R-audio output port 327 ). In one embodiment, the bypass switch 375 is a double pole, single throw (DPST) switch. When the bypass switch 375 is closed, the L-audio input port 321 and R-audio input port 322 are connected to the L-audio output port 326 and R-audio output port 327 directly, thus bypassing the DSP circuit 371 .
[0038] In one embodiment, the R-audio/MIC selection switch 373 is a DPDT switch. When the R-audio/MIC selection switch 373 is switched ON (closed), the R-audio input port 322 connects to the MIC input port 324 directly and is used as a MIC communication port to transfer MIC input from the microphone 350 to the electronic device. At the same time, the L-audio input port 321 couples to both L-audio output port 326 and R-audio output port 327 for mono audio signal output. The earphone 340 (L-earphone 342 and R-earphone 344 ) thus operates in a mono mode.
[0039] In one embodiment, the R-audio/MIC selection switch 373 is controlled by the MIC line voltage comparator 374 , which compares the voltage at the R-audio input port 322 to at least one reference voltage. In one embodiment, the R-audio/MIC selection switch 373 is controlled by the MIC line voltage comparator 374 and/or the power line voltage comparator 377 .
[0040] One skilled in the art will recognize that the above-described accessory control IC is only one structure example. In one embodiment, the DSP circuit 371 , LDO 378 , stitches 373 and 375 , voltage comparators 374 and 377 may be integrated within one IC chip. In another embodiment, those components may be placed among a plurality of IC chips. The DSP circuit 371 may also comprise embedded memory storage module to store preloaded logic codes executable by the DSP circuit to implement desired active noise control processing.
[0041] FIG. 4 is an exemplary block diagram of the accessory in communication with an electronic device for host detection according to various embodiments of the invention.
[0042] Communication between the accessory 300 and the electronic device 200 starts after the audio jack 310 of the accessory 300 is inserted into the audio socket of an electronic device. At step 410 , the accessory control IC 320 checks whether the microphone conductor (MIC line) 314 has a power line voltage. If not, the accessory control IC 320 verifies that the electronic device 200 is a traditional host not providing power support to accessory via 4P audio socket at step 430 . If the microphone line (PWR) voltage is present (in step 420 ), the accessory control IC 320 is configured to draw no more than a minimum allowable current for a predetermined debounce time. Moreover, the DSP circuit 371 is in sleep mode. After the predetermined debounce time, the power line voltage at the microphone conductor (MIC line) 314 is compared to a predetermined voltage at step 440 . In one embodiment, the predetermined voltage is the working voltage for the LDO 378 . In another embodiment, the predetermined voltage is set as 94% of LDO working voltage based on I2C communication PIO level. For example, the predetermined voltage may be set at 2.5V. If the power line voltage is less than the predetermined voltage, the accessory control IC 320 verifies that the electronic device 200 does not provide power support over MIC line via 4P audio socket at step 450 . The electronic device may be a traditional host supporting stereo audio output and MIC signal input. If the power line voltage is larger than the predetermined voltage, the accessory control IC 320 verifies that the electronic device 200 supports power input over MIC line via 4P audio socket at step 460 . The power switch 379 is then switched to latch the LDO 378 to the power input port (PWR) 323 such that the DSP circuit 371 is powered up.
[0043] In some embodiments, the power line voltage is further verified to check whether the voltage is the same as a first reference voltage V Ref1 at step 470 . The first reference voltage V Ref1 is higher than the predetermined voltage. If yes, the accessory enters a mono mode (or a call mode for a phone electronic device, such as a smart phone) at step 472 and the accessory control IC 320 is configured to switch ON the R-audio/MIC selection switch 373 to connect the R-audio input port 322 to the MIC input port 324 directly. At the same time, the L-audio input port 321 couples to both L-audio output port 326 and R-audio output port 327 for mono audio signal output. In one embodiment, the first reference voltage V Ref1 is set as 3.15V.
[0044] In some embodiments, the power line voltage is also verified to check whether the voltage is the same as a second reference voltage V Ref2 at step 480 . The second reference voltage V Ref2 is higher than the predetermined voltage but lower than the first reference voltage V Ref1 . If yes, the accessory enters a stereo mode at step 482 , wherein the R-audio input port 322 is coupled to the R-audio output port 327 to provide a stereo audio output together with the L-audio output port 326 . In one embodiment, the second reference voltage V Ref2 is set as 2.8V.
[0045] FIG. 5 is an exemplary schematic diagram of an electronic device according to various embodiments of the invention. The electronic device 200 has an audio socket 210 to receive an audio jacket from an accessory, an I2C circuit 220 , a microprocessor 230 , and an audio driver circuit 260 . The electronic device also has other components (not shown in FIG. 5 ) including memory, power source and at least one I/O interface, such as touch screen, keyboard, pin pad, etc. The microprocessor 230 is configured to couple to the I2C circuit 220 and the audio driver circuit 260 (and also the memory, the power source and I/O interfaces).
[0046] The audio socket 210 comprises an L-audio socket conductor 211 , a R-audio socket conductor 212 , a socket ground conductor 213 and a socket microphone conductor 214 , which respectively contact the L-audio conductor 311 , R-audio conductor 312 , ground conductor 313 and a microphone conductor 314 after the insertion of the audio jack 310 . In one embodiment, the audio socket 210 comprises an audio insertion detection conductor 215 to contact the L-audio conductor 311 after the audio jack 310 insertion. The audio insertion detection conductor 215 couples to the I2C circuit 220 via pin 222 and is configured to detect audio jack insertion.
[0047] The L-audio socket conductor 211 couples to an L-A (left audio output) port 261 of the audio driver circuit 260 to receive audio signal. The R-audio socket conductor 212 couples to either an R-audio output port 262 or a MIC-bias port 263 of the audio driver circuit 260 via a controllable switch 270 . In one embodiment, the controllable switch 270 is a DPDT (double pole double through) switch such that when the R-audio socket conductor 212 is able to couple to both the MIC-bias port 263 and an MIC port 264 of the audio driver circuit 260 simultaneously. The controllable switch 270 is controlled by the microprocessor 230 or by a MIC Bias and Power LDO 221 within the I2C circuit 220 . The MIC Bias and Power LDO 221 sends an INT signal to the controllable switch 270 through pin 226 for switch control according to electronic device audio setup preferences.
[0048] The MIC Bias and Power LDO 221 may couple to the socket microphone conductor 214 via a MIC IN pin 224 to send power or to receive signal from the microphone conductor 314 . The MIC Bias and Power LDO 221 may also couple to the socket microphone conductor 214 via a RES (reset) pin 225 to send power to or to receive signal from the accessory 300 via the microphone conductor 314 . The voltage output from the MIC Bias and Power LDO 221 to the RES (reset) pin 225 is configurable to be different levels according to electronic device audio setup preferences.
[0049] FIG. 6 is an exemplary block diagram of the accessory in communication with an electronic device for accessory detection according to various embodiments of the invention. At step 610 , the electronic device detects the types of accessory after audio jack insertion detected. The accessory detection may be done by checking the impedance at the L-Audio line 311 and/or the MIC line 314 and/or the secure authenticator 330 . The secure authenticator 330 could be also a digital ID as well as a secure authenticator.
[0050] At step 620 , the electronic device configures the control setup for the controllable switch 270 based on preferred audio setting. In some embodiments, the electronic device is a smart phone and the controllable switch 270 may be configured as mono mode for phone calls and stereo mode for music playing. At mono mode, the R-audio socket conductor 212 is latched both the MIC-bias port 263 and an MIC port 264 of the audio driver circuit 260 . At stereo mode, the R-audio socket conductor 212 is latched to R-audio output port 262 of the audio driver circuit 260 . In some embodiments, the electronic device also configures the MIC bias and power LDO 221 based on preferred audio setting. For example, the LDO 221 may output a voltage of V Ref1 when the electronic device is in mono mode for phone calls and output a voltage of V Ref2 when the electronic device is in stereo mode for music playing. In some embodiments, the first reference voltage V Ref1 is higher than the second reference voltage V Ref2 . For example, the first reference voltage V Ref1 may be set as 3.15V and the second reference voltage V Ref2 may be set as 2.8V.
[0051] At step 630 , the accessory control IC 320 compares the power line voltage at the microphone conductor (MIC line) 314 to a predetermined voltage. If the power line voltage is larger than the predetermined voltage, the accessory control IC 320 verifies that the electronic device 200 supports power input over MIC line via 4P audio socket. The power switch 379 is then switched to latch the LDO 378 to the power input port (PWR) 323 such that the DSP circuit 371 is powered up. The power line voltage is further verified to check whether the voltage is equal to the first reference voltage V Ref1 at step 632 . If yes, the accessory enters a mono mode (or a call mode for a phone electronic device, such as a smart phone) at step 636 and the accessory control IC 320 is configured to switch ON the R-audio/MIC selection switch 373 to connect the R-audio input port 322 to the MIC input port 324 directly. At the same time, the L-audio input port 321 couples to both L-audio output port 326 and R-audio output port 327 for mono audio signal output. In one embodiment, the first reference voltage V Ref1 is set as 3.15V.
[0052] At step 634 , the power line voltage is further verified to check whether the voltage is equal to the second reference voltage V Ref2 . If yes, the accessory enters a stereo mode at step 638 , wherein the R-audio input port 322 is coupled to the R-audio output port 327 to provide a stereo audio output together with the L-audio output port 326 . Therefore, by controlling the MIC bias and power LDO 221 output voltage to the socket microphone conductor 214 , the electronic device may set the operation mode of the accessory according to its preferred audio setting.
[0053] At step 640 , the accessory control IC 320 checks whether the power line signal at the microphone conductor (MIC line) 314 is a MIC input signal, which is typically smaller than the predetermined voltage. If yes, then the accessory control IC 320 configures to latch the LDO power switch 379 to MIC input, latch the R-A/MIC switch 373 to R-audio signal and close the bypass switch 375 to bypass the DSP circuit 371 .
[0054] FIG. 7 is another exemplary block diagram of the accessory in communication with an electronic device for accessory detection according to various embodiments of the invention. Similar to FIG. 6 , at step 630 , the accessory control IC 320 compares the power line voltage at the microphone conductor (MIC line) 314 to a predetermined voltage. If the power line voltage is larger than the predetermined voltage, the accessory control IC 320 verifies that the electronic device 200 supports power input over MIC line via 4P audio socket. Then, the accessory control IC 320 checks the signal at the R-audio input port 322 . At step 710 , the accessory control IC 320 checks if the signal at the R-audio input port 322 has a MIC bias. If yes, the accessory enters a mono mode (or a call mode for a phone electronic device, such as a smart phone) at step 712 and the accessory control IC 320 is configured to switch the R-audio/MIC selection switch 373 to latch the R-audio input port 322 to the MIC input port 324 directly. At the same time, the L-audio input port 321 couples to both L-audio output port 326 and R-audio output port 327 for mono audio signal output.
[0055] At step 720 , the accessory control IC 320 checks if the signal at the R-audio input port 322 is a regular audio signal, which typically has a lower voltage than the MIC bias voltage. If yes, the accessory enters a stereo mode at step 722 , wherein the R-audio input port 322 is coupled to the R-audio output port 327 to provide a stereo audio output together with the L-audio output port 326 .
[0056] The foregoing description of the invention has been described for purposes of clarity and understanding. It is not intended to limit the invention to the precise form disclosed. Various modifications may be possible within the scope and equivalence of the application.
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A backward compatible system and method for using 4P audio jack in an electronic device to provide power and signal to headset with active noise cancellation (ANC) as well as accessories that require an external power are disclosed. The method involves automatically deciding at the electronic device accessory type after accessory insertion detected and choosing proper accessory communication mode based at least on the decided accessory type and accessory input signal. The accessory communication mode may be an accessory power mode or an accessory microphone mode.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to adjustable hinges and more particularly relates to adjustable hinges and self-closing adjustable hinges that are adjustable in multiple directions.
[0003] 2. Discussion of the Background
[0004] Furniture, such as cabinets or the like, generally must be individually adjusted to compensate for unavoidable manufacturing tolerances. Such adjustment is generally required in two or more dimensions, and if the door has two or more hinges as is usually the case, must be carried out on each hinge with respect to the other hinges. Hinges today generally suffer from various disadvantages including difficulty of installation, undesirable correlation between adjustments in different directions which require multiple readjustments in small increments, coordination of these adjustments collectively with respect to the other hinges, complex construction and correspondingly high manufacturing costs, and instability of the selected adjustments.
[0005] Adjustable hinges may but are not required to include self-closing mechanisms. Hinges having self-closing mechanisms are known in the art. For instance, U.S. Pat. Nos. 4,290,167; 4,376,324; 4,716,622; 5,027,474; and 5,617,612 each disclose hinges having a self-closing mechanism. These references are incorporated by reference herein.
[0006] Hinges are commonly manufactured with connecting parts of two lengths. The first connecting part length is approximately 65 millimeters and is commonly known as a “long arm.” The second connecting part length is approximately 36 millimeters and is commonly known as a “short arm.” Today, short arm hinges require a gap of at least 5 millimeters between connected pieces of furniture, such as between a door and a frame, in a closed position.
[0007] Thus, as noted above, there currently exists numerous deficiencies in the adjustable hinges that are known in the prior art.
SUMMARY OF THE INVENTION
[0008] Accordingly, one aspect of the present invention is to provide an adjustable hinge fixture that includes a base plate for adjustable fixation to an article of furniture, a connecting plate assembly including a generally U-shaped cross-section formed by a top portion and a pair of spaced apart side walls, and an adjustment screw operable to move the connecting plate assembly relative to the base plate about a curved region of the connecting plate assembly. The connecting plate assembly has a projection through a curved region to a lower portion of the projection positioned between the side walls and generally parallel to the top portion. The curved region is elastically deflectable to permit the lower and top portions to move relative to each other. The lower portion is adjustably connected to the base plate.
[0009] Another aspect of the present invention is to provide an adjustable hinge that includes an adjustable hinge fixture, a door-related part secured to a second article of furniture, and a linkage means for movably interconnecting the door-related part and the adjustable hinge fixture. The adjustable hinge fixture includes a base plate for adjustable fixation to an article of furniture, a connecting plate assembly including a generally U-shaped cross-section formed by a top portion and a pair of spaced apart side walls, and an adjustment screw operable to move the connecting plate assembly relative to the base plate about a curved region of the connecting plate assembly. The connecting plate assembly has a projection through a curved region to a lower portion of the projection positioned between the side walls and generally parallel to the top portion. The curved region is elastically deflectable to permit the lower and top portions to move relative to each other. The lower portion is adjustably connected to the base plate.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] A more complete appreciation of the present invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following detailed description when considered in conjunction with the accompanying drawings, wherein:
[0011] FIG. 1 is a perspective view of an adjustable hinge in an open position according to an embodiment of the present invention;
[0012] FIG. 2 is a top view of an adjustable hinge in an open position according to an embodiment of the present invention;
[0013] FIG. 3 is a side view of an adjustable hinge in an open position according to an embodiment of the present invention;
[0014] FIG. 4 is an exploded perspective view of an adjustable hinge according to an embodiment of the present invention;
[0015] FIG. 5A is a perspective view of a base plate of an adjustable hinge according to an embodiment of the present invention;
[0016] FIG. 5B is a top view of a base plate of an adjustable hinge according to an embodiment of the present invention;
[0017] FIG. 6A is a side view of adjustment screw of an adjustable hinge according to an embodiment of the present invention;
[0018] FIG. 6B is a side view of an eccentric of an adjustable hinge according to an embodiment of the present invention;
[0019] FIG. 7A is a perspective view of a connecting plate assembly of an adjustable hinge according to an embodiment of the present invention;
[0020] FIG. 7B is a side view, partially in section, of a connecting plate assembly of an adjustable hinge according to an embodiment of the present invention;
[0021] FIG. 7C is a top view of a connecting plate assembly of an adjustable hinge according to an embodiment of the present invention;
[0022] FIG. 7D is a rear view of a connecting plate assembly of an adjustable hinge according to an embodiment of the present invention;
[0023] FIG. 7E is a top view of a connecting plate assembly and base plate of an adjustable hinge according to an embodiment of the present invention;
[0024] FIG. 7F is a cross-sectional view through the connecting plate assembly and base plate of FIG. 7E according to an embodiment of the present invention;
[0025] FIG. 7G is a cross-sectional view through the connecting plate assembly and base plate of FIG. 7E illustrating an eccentric having a rivet according to an embodiment of the present invention; and
[0026] FIG. 8 is a perspective view of an adjustable hinge in a closed position according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0027] Referring now to the drawings, wherein like reference numerals designate identical or corresponding parts throughout the several views, preferred embodiments of the present invention are described.
[0028] Referring to FIGS. 1-4 and 8 , an adjustable hinge according to an embodiment of the present invention as indicated overall by 10 is shown. The adjustable hinge 10 serves for pivotally connecting a piece of furniture. For instance, in one embodiment, the adjustable hinge 10 may be used to pivotally connect a cabinet door to a door opening of which is confined by a frame. The adjustable hinge may also be a self-closing adjustable hinge. The adjustable hinge 10 includes a door-related part 12 , a connecting plate assembly 14 , a hinge arm 16 and a base plate 18 . In one embodiment, the adjustable hinge 10 is arranged such that the gap between the cabinet door and the door opening is reduced and/or substantially eliminated. The adjustable hinge 10 is also arranged such that its overall longitudinal length is reduced. In one embodiment, the connection plate assembly 14 has a length of approximately 36 millimeters. However, other lengths are possible within the scope of the invention. It is of course to be understood that the present invention is not limited to the above identified connecting components and that other connecting components may be used within the scope of the present invention. Each of the adjustable hinge 10 components may be made from any material. In one embodiment, the components of the adjustable hinge 10 are made from metal formed from pressure casting or stamping.
[0029] The door-related part 12 includes a top portion 70 having circular holes 72 and 74 , and a cup or disc portion 68 . The door-related part 12 is secured to a piece of furniture, such as a cabinet door, by screws, dowels or the like, which are projected through the holes 72 and 74 . The cup or disc portion 68 of the door-related part 12 is inserted into a recess of the piece of furniture (e.g., the cabinet door).
[0030] The hinge arm or linkage 16 pivotally interconnects, at opposite ends of the hinge arm 16 , the door-related part 12 and the connecting plate assembly. The hinge arm 16 is pivotally connected to the door-related part 12 by links 52 and 50 to form a four-bar linkage. Links 52 and 50 protrude through side walls of the cup or disc portion 68 of the door-related part 12 . The connecting plate assembly 14 is pivotally connected to the hinge arm 16 by a hinge pin 48 . It is of course to be understood that the present invention is not limited to the above-identified connections between the connecting components and that other connections may to used within the scope of the present invention.
[0031] Referring to FIGS. 7A-7G , the connecting plate assembly 14 of the adjustable hinge 10 according to an embodiment of the present invention is shown in various perspectives and views. The connecting plate assembly 14 generally has a U-shaped cross-section configuration defined by a pair of opposing side walls 44 a and 44 b , and a top portion 35 along a longitudinal center axis. The top portion includes a screw thread opening 36 and an access opening 38 . In one embodiment, the access opening 38 has a generally rectangular shape. An elongated portion 42 extends from the top portion 35 through a curved region 41 to an end portion 43 that is substantially parallel to the top portion 35 along the pair of opposing side walls 44 a and 44 b . The elongated portion 42 is provided with a cam hole 40 positioned below the access opening 38 . According to the present invention, the curved region 41 is configured to allow the top portion 35 to be angularly displaced in a vertical direction relative to the elongated portion 42 as described below.
[0032] Referring to FIGS. 5A and 5B , perspective and top views of the base plate 18 of the adjustable hinge 10 according to an embodiment of the present invention are respectively shown. The base plate 18 includes an elevated section or boss 56 and wing portions 54 a and 54 b that extend transversely of the center axis on opposite sides of the base plate 18 .
[0033] The elevated section 56 is generally configured such that it may be fitted between the side walls 44 a and 44 b of the connecting plate assembly 18 . Each connecting wing portion ( 54 a and 54 b ) includes an elongated slot ( 62 and 64 ) and a downward extending flap ( 66 a and 66 b ) which is configured to rest against the door frame at a side facing the door. The base plate 18 is adjustably secured to the frame such that the U-shaped elevated section 56 extends in a direction that is longitudinal of the center axis by screws or the like projected through the elongated slots 62 and 64 . The elongated slots 62 and 64 of the base plate 18 are arranged such that base plate 18 may be aligned or properly adjusted on the frame in a direction that is transverse of the center axis. The elevated section 56 includes an elongated open slot 60 , extending in a direction that is longitudinal of the center axis, and a cam hole 58 . The elongated open slot 60 is configured to hold an adjustment screw 26 in place when the elevated section 56 is positioned between the side walls 44 a and 44 b of the connecting plate assembly 18 .
[0034] As shown in FIGS. 4 and 6B , an eccentric 20 is provided with a screw head 22 and a protruding off-center cam 24 . The eccentric 20 movably connects the connecting plate assembly 18 to the base plate 18 with the cam 24 projected through the cam holes 40 and 58 of the connecting plate assembly 18 and the base plate 18 , respectively. The eccentric 20 is arranged such that the plate assembly 18 may be aligned or properly adjusted in a longitudinal direction of the center axis. In one embodiment, the elongated portion 42 of the connecting plate assembly 18 is adjustably secured to the base plate 18 between the screw head 22 and a rivet head, larger than the cam hole 58 , formed by the deformation of an end portion 23 of the cam 24 using an orbital riveter or the like, as shown in FIG. 7G . Optionally, the eccentric 20 may utilize a bolt or other securing mechanism instead of a rivet head. The components of the adjustable hinge 10 are arranged such that turning the screw head 22 of the eccentric 20 results in the displacement of the connecting plate assembly 18 on the base plate 18 in a direction that is longitudinal of the center axis.
[0035] As shown in FIGS. 4 and 6A , an adjustment screw 26 is provided with a screw head 28 and a shaft 32 . The adjustment screw 26 includes a threaded portion 30 and a circular holding disk 34 , each having larger diameters than the shaft 32 , at opposite ends of the shaft 32 . The adjustment screw 26 is arranged such that the plate assembly 18 may be aligned or properly adjusted in a vertical direction relative to the base plate 18 . In one embodiment, the threaded portion 30 operatively engages the screw thread opening 36 of the plate assembly 18 , and the shaft 32 is situated between the open slot 60 of base plate 18 and secured thereto in a vertical direction by the threaded portion 30 and the disk 34 . Turning the screw head 28 of the adjustment screw 26 results in the top portion 35 of the connecting plate assembly 18 and the base plate 18 being titled with respect to each other about the curved region 41 of the elongated portion 42 such that the top portion 35 of the connecting plate assembly 18 is angularly displaced in a vertical direction relative to the base plate 18 . Such angular displacement being centered at the curved region 41 of the elongated portion 42 .
[0036] Obviously, many other modifications and variations of the present invention are possible in light of the above teachings. The specific embodiments discussed herein are merely illustrative, and are not meant to limit the scope of the present invention in any manner. It is therefore to be understood that within the scope of the disclosed concept, the invention may be practiced otherwise then as specifically described.
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An adjustable hinge fixture that includes a base plate for adjustable fixation to an article of furniture, a connecting plate assembly including a generally U-shaped cross-section formed by a top portion and a pair of spaced apart side walls, and an adjustment screw operable to move the connecting plate assembly relative to the base plate about a curved region of the connecting plate assembly. The connecting plate assembly has a projection through a curved region to a lower portion of the projection positioned between the side walls and generally parallel to the top portion. The curved region is elastically deflectable to permit the lower and top portions to move relative to each other. The lower portion is adjustably connected to the base plate.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of application Ser. No. 920,886, filed June 30, 1978, now abandoned.
BACKGROUND OF THE INVENTION
Peroxydicarbonates of the formula R--OCO--OO--OCO--R, wherein R is an organic radical derived from monohydric alcohols of the type ROH, are widely used as initiators in the polymerization of unsaturated monomers as described, for example, in U.S. Pat. No. 2,464,062.
The peroxydicarbonates are typically prepared by the so-called "peroxide slurry method" wherein a chloroformate of the formula R--OCO--Cl (wherein R is as above defined) is reacted with a concentrated aqueous slurry of sodium peroxide as described, for example, in U.S. Pat. No. 2,370,588.
It has been found, however, that during the addition of the sodium peroxide slurry to the reaction mixture, the reaction product tends to hydrolyze to form the corresponding alcohol resulting in an impure product having a reduced peroxydicarbonate assay. In addition, hydrolysis of the reaction product reduces the net yield of peroxydicarbonate.
Since the lower molecular weight alcohols, for example, ethanol, isopropanol, n-propanol, t-butanol, sec-butanol, and the like are relatively water soluble, such lower molecular weight alcoholic impurities can be readily removed from the peroxydicarbonate by washing with water. However, since the water solubility of alcohols generally decreases with increasing molecular weight, the higher molecular weight alcoholic impurities such as, for example, 2-ethylhexanol, are not readily removed from the peroxydicarbonate by typical product purification means, e.g., water washing.
Regardless of the ease of removal of the alcoholic impurity formed by hydrolysis of the reaction product upon addition of the sodium peroxide slurry, the yield of peroxydicarbonate is reduced in proportion to the extent of hydrolysis.
Published German Patent application No. 1,443,840 discloses adding sodium hydroxide to a colloidal dispersion of hydrogen peroxide and chloroformate, which entails the use of costly, complex equipment. Moreover, the process described in said German application requires the addition of a perhalogenated solvent before, during or at the completion of the reaction, with the consequence that only dilute solvent solutions of peroxydicarbonate are obtained. Although the German application states that peroxydicarbonate can be recovered from the solvent solution by distillation, this requires an additional costly and time consuming processing step which is potentially hazardous.
SUMMARY OF THE INVENTION
High purity peroxydicarbonate is produced in high yield by reacting a mixture containing chloroformate and dilute aqueous hydrogen peroxide with a dilute aqueous alkali metal hydroxide solution. The process of the invention is conducted batchwise, and requires only simple agitation or stirring sufficient to adequately mix the reactants to bring them into intimate contact thus avoiding the necessity of having to form a colloidal dispersion of the hydrogen peroxide and chloroformate.
DESCRIPTION OF THE INVENTION
In accordance with this invention, a peroxydicarbonate of the formula R--OCO--OO--OCO--R is prepared by reacting a mixture containing dilute aqueous hydrogen peroxide and a chloroformate of the formula R--OCO--Cl, with a dilute aqueous alkali metal hydroxide solution.
The invention is particularly applicable to producing di-n-propyl peroxydicarbonate (NPP), diisopropyl peroxydicarbonate (IPP), di-sec-butyl peroxydicarbonate (SBP), and di-(2-ethylhexyl) peroxydicarbonate (EHP), although in its broadest aspects, the invention contemplates the production of other peroxydicarbonates in addition to the preferred NPP, IPP, SBP and EHP.
Thus, although in the above formulae R preferably represents n-propyl, isopropyl, sec-butyl, and 2-ethylehexyl, R may represent other linear or branched, substituted or unsubstituted alkyl or cycloalkyl radicals derived from a monohydric alcohol and containing up to about 18 carbon atoms. Other organic radicals of which R is representative include, for example, ethyl, butyl, n-butyl, isobutyl, t-butyl, hexyl, cyclohexyl, benzyl, 2-phenoxy ethyl, cetyl, allyl, tetradecyl, amyl, lauryl, and the like.
The chloroformate aqueous hydrogen peroxide mixture contains from about 10 percent to 35 percent by weight and preferably from about 14 percent to about 30 percent by weight hydrogen peroxide based on the weight of water, with sufficient hydrogen peroxide being present to provide at least about a 4 percent stoichiometric excess and preferably an 8 percent to 12 percent stoichiometric excess of hydrogen peroxide based on the quantity of chloroformate.
The chloroformate aqueous hydrogen peroxide mixture may also contain from about 5 percent to about 15 percent, preferably about 10 percent by weight, based on the weight of chloroformate, of a lower alcohol or mixture of lower alcohols, such as, for example, methanol, ethanol, isopropanol, n-propanol, or the like. The inclusion of a lower alcohol has been found to enable better reaction temperature control.
In order to produce high purity, i.e., 98 percent or higher, peroxydicarbonate, the chloroformate starting material, should, of course be as pure as possible. Chloroformate having an assay of at least 99 percent is preferred for use in accordance with the invention.
The aqueous alkali metal hydroxide solution contains from about 20 percent to 40 percent by weight, preferably from about 25 percent to 35 percent by weight alkali metal hydroxide, sufficient of said solution being used for reaction with the chloroformate/hydrogen peroxide mixture to provide at least about a 1 percent and preferably from about 2 to 10 percent stoichiometric excess of alkali metal hydroxide based on the quantity of chloroformate.
The alkali metal hydroxide may be sodium hydroxide or potassium hydroxide as each has been found to give substantially equivalent results.
The reaction between the hydrogen peroxide/chloroformate mixture and the alkali metal hydroxide solution is conducted with continuous stirring at a temperature of from about -10° C. to not more than about 30° C., preferably not more than about 15° C.
The alkali metal hydroxide solution is added, with continuous stirring, to the hydrogen peroxide/chloroformate mixture incrementally over a period of about 10 minutes to one hour, usually not more than 30 minutes. Following the addition of the alkali metal hydroxide solution, the mixture is usually stirred for an additional period typically not more than about 30 minutes and usually not more than about 10 to 15 minutes to assure substantially complete conversion of chloroformate to peroxydicarbonate.
At the completion of the reaction, liquid or solid peroxydicarbonate is recovered by any suitable, conventional means. In the case of liquid peroxydicarbonate, the reaction mixture readily phase separates and the organic or peroxydicarbonate phase is drawn-off, washed with cold water to remove water soluble impurities and dried by, for example, contact with an inert drying agent such as, magnesium sulfate or sodium sulfate. A solid peroxydicarbonate may be recovered by sedimentation or centrifugation followed by washing with cold water and drying.
Peroxydicarbonate assaying in excess of 98 percent with substantially quantitative conversion of chloroformate can routinely be obtained by the practice of this invention.
Although the invention has been described with particular reference to a preferred embodiment, it is evident that variations may be made therein without departing from the spirit and scope thereof. For example, it has been found that satisfactory results are obtained by simultaneously adding a dilute aqueous hydrogen peroxide solution along with a dilute aqueous alkali metal hydroxide solution to the chloroformate. The respective strengths of said solutions and the stoichiometric excesses of hydrogen peroxide and alkali metal hydroxide are the same as described hereinabove with respect to the preferred manner of practicing the invention, i.e., by adding the alkali metal hydroxide solution to the hydrogen peroxide/chloroformate mixture.
The process of this invention enables the production of higher yields of higher purity peroxydicarbonate in a shorter reaction time with better reaction temperature control than the heretofore used peroxide slurry method. The process of this invention also avoids the disadvantages attendant on forming and handling colloidal dispersions or emulsions of hydrogen peroxide and chloroformate.
The invention is further illustrated by the following examples.
EXAMPLE 1
The reactor used consisted of a 500 milliliter capacity round bottom, three-neck flask. The flask was fitted with a pH electrode, a type "J" thermocouple, and a stirring rod having a TEFLON® paddle powered by a variable speed mixer. The temperature of the reactor was controlled by pumping ice water through a spray ring positioned around the reactor.
96.3 grams (0.5 mole) 2-ethylhexyl chloroformate, 65.1 grams of 14.1 weight percent aqueous hydrogen peroxide solution (0.27 mole H 2 O 2 ), and 9.63 grams of isopropanol were added to the reactor. 81 grams of 25.7 weight percent aqueous sodium hydroxide solution (0.52 mole NaOH) were added to the reactor over a 25 minute period. After completion of the sodium hydroxide addition, the mixture was permitted to react for an additional 30 minutes. Throughout the sodium hydroxide solution addition period and reaction period, the reactor contents were continuously stirred and maintained at a temperature of 15° C.
At the completion of the reaction, stirring was discontinued and the reaction mixture was permitted to phase separate. The organic phase was withdrawn, washed with cold water, dried with sodium sulphate, and submitted for analysis. Di(2-ethylhexyl) peroxydicarbonate product assaying at 99.3 percent was obtained.
EXAMPLE 2
136.5 grams (1 mole) of sec-butyl chloroformate, 62 grams of 30.5 weight percent aqueous hydrogen peroxide solution (0.56 mole H 2 O 2 ), and 13.65 grams isopropanol were added to the reactor described in Example 1. 109 grams of 40.4 weight percent aqueous sodium hydroxide solution (1.1 mole NaOH) were added to the reactor over a 30 minute period and the reaction mixture was permitted to react an additional 30 minutes. The reactor contents were continuously stirred and maintained at a temperature of 15° C. throughout the addition of the sodium hydroxide solution and the reaction period.
At the completion of the reaction, stirring was discontinued, the reaction mixture was permitted to phase separate, the organic phase was withdrawn, washed with cold water, dried with sodium sulphate, and submitted for analysis. Di-sec-butyl peroxydicarbonate assaying at 99.2 percent was obtained.
EXAMPLE 3
122.5 grams (1 mole) of isopropyl chloroformate and 91.3 grams of 20.5 weight percent aqueous hydrogen peroxide solution (0.55 moles H 2 O 2 ) were added to the reactor described in Example 1. 130 grams of 32.3 weight percent aqueous sodium hydroxide solution (1.05 moles NaOH) were added to the reactor over a 34 minute period and the reaction mixture was permitted to react an additional 30 minutes. The contents of the reactor was continuously stirred and maintained at a temperature of 15° C. throughout the addition of the sodium hydroxide solution and the reaction period.
At the completion of the reaction, stirring was discontinued, the reaction product was phase separated, the organic phase was withdrawn, washed with cold water, dried with sodium sulphate, and submitted for analysis. Diisopropyl peroxydicarbonate assaying at 99.0 percent was obtained.
EXAMPLE 4
The procedure of Example 3 was followed except that n-propyl chloroformate was used in place of isopropyl chloroformate. Di-n-propyl peroxydicarbonate assaying at 99.4 percent was obtained.
EXAMPLE 5
96.3 grams of 2-ethylhexyl chloroformate, 9.63 grams of isopropanol, and 25 grams of water were added to the reactor described in Example 1. 40.94 grams of 50.8 percent aqueous sodium hydroxide solution was diluted with 25 grams of water. 18.18 grams of 50.5 percent aqueous hydrogen peroxide solution was diluted with 40 grams of water. Each solution had a volume of 53 milliliters. Each solution was added separately but simultaneously to the reactor via a dual-head Master Flex pump over a period of about 33 minutes. After completion of addition of the sodium hydroxide and hydrogen perioxide solutions, the mixture was permitted to react for an additional 30 minutes. Throughout the solution addition period and reaction period, the reactor contents were continuously stirred and maintained at a temperature of 15° C.
At the completion of the reaction, stirring was discontinued, the reaction mixture was permitted to phase separate, the organic phase was withdrawn, washed with cold water, dried with sodium sulphate, and submitted for analysis. Di(2-ethylhexyl) peroxydicarbonate assaying at 99.1 percent was obtained.
Although the invention has been described with specific references and specific details of embodiments thereof, it is to be understood that it is not intended to be so limited since changes and alterations therein may be made by those skilled in the art which are within the full intended scope of this invention as defined by the appended claims.
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A process for preparing peroxydicarbonate is disclosed wherein a mixture of chloroformate and dilute aqueous hydrogen peroxide is reacted with a dilute aqueous alkali metal hydroxide solution.
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CROSS REFERENCE TO RELATED APPLICATIONS
N/A
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
N/A
BACKGROUND OF THE INVENTION
The present invention generally relates to methods and compositions for treating the natural cane reed used in woodwind instruments, employing a polymer or polymerizing solution, preferably a waterborne polymer or waterborne polymerizing solution, to impregnate and protect the reed from saliva-related microbial and enzymatic degradation, without rendering the reed waterproof.
The wooden reed used in woodwind instruments is usually cut from natural cane (e.g., the species Arundo donax ). Being highly porous, the reed is susceptible over time, to infiltration and degradation by contact with saliva during playing. As a musician blows air over a cane reed, which is typically clamped at its distal end or “heel” in the instrument's mouthpiece, the reed is caused to vibrate, thereby inducing vibrations in the moving column of air within the instrument to produce musical tones. During a single playing session, the physical and musical properties of a reed may change for the better or worse. This is not surprising, because even after several minutes pre-soaking, i.e., “conditioning,” of the mouth end of the reed in water, the subsequent contact with warm saliva during a playing session tends to further soften the reed. Some softening may be beneficial during the initial breaking-in period when a reed is new and somewhat unresponsive. However, after an initial period during which the reed may become optimally playable (over a few days or even after a week or more), any further softening may be undesirable. That is, as the cane structure becomes degraded and the reed becomes too flexible, the reed must be discarded.
There is considerable variability in the sound quality and longevity of individual cane reeds, even within a group of presumably equivalent reeds from any particular manufacturer. In fact, a musician may find that no more than one or two out of every ten reeds possess ideal tone and playing characteristics. Due to difficulties and frustrations with the lack of uniformity and short lifetime of natural cane reeds, a number of synthetic reeds, composite reeds and structurally reinforced natural reeds have been developed. A number of exemplary patents detailing such structurally modified reeds follows. Fiber-reinforced plastic reeds are described in Brilhart, U.S. Pat. No. 2,919,617. Reeds containing glass fiber-reinforced synthetic resin are described in Burns, U.S. Pat. No. 3,165,963. Synthetic reeds are described in Gamble, U.S. Pat. Nos. 3,905,268 and 4,014,241. Shaffer, U.S. Pat. No. 4,355,560, describes a synthetic composite reed structure producing an acoustic impedance similar to the cane reed. Backus, U.S. Pat. No. 4,337,683 describes a graphite-reinforced epoxy resin synthetic woodwind reed having proper elasticity and density. Cusack et al., U.S. Pat. No. 5,227,572 describes a titanium reed for woodwind instruments. Hartmann et al., U.S. Pat. No. 5,542,331 describes a fiber-reinforced plastic reed in which different fiber materials are combined for the purpose of damping vibrations.
Extending the lifetime of natural cane reeds has been the goal of a number of previous inventors. These inventors have appreciated that in addition to mechanical fatigue, degradative enzymes, bacteria and other constituents of human saliva infiltrate the porous structure of the cane reed during use, and contribute to a shortened lifetime. Reed failure may occur suddenly, as when the tip of the reed splits, or may occur gradually as the reed softens and loses tone quality. Rinsing the reed is only partially effective in removing enzymes, bacteria and saliva residues. Vogt, U.S. Pat. No. 5,379,673, describes a hydrogen peroxide and humectant-containing composition for soaking, disinfecting and conditioning natural cane reeds after use, to prolong their life.
To inhibit the process of reed degradation by saliva, inventors have developed a number of protective coating treatments for the natural cane reed. As early as 1930, Newton et al., U.S. Pat. No. 1,776,566, describes reeds for musical instruments whose pores have been adequately filled with cellulose or nitrocellulose in an organic solvent, to render the reed waterproof and resistant to the destructive action of the juices of the human mouth. Ogilvie, U.S. Pat. No. 1,790,167, describes a thin, flexible coating of celluloid material, applied in a quick-drying organic solvent to the surface of the cane reed in such a manner that the reed surface becomes waterproof while the pores inside of the reed remain open, i.e., empty. Petzke, U.S. Pat. No. 3,340,759, describes a natural cane reed whose pores have been impregnated with a cured vinyl plastisol. The plastisol is described as a synthetic resin which is essentially 100% solids, and free of solvents or diluents which would evaporate and cause undesirable shrinkage. The pores of the reed are substantially sealed to prevent moisture absorption, thereby rendering the reed waterproof. Similarly, Knotik et al., U.S. Pat. No. 3,705,820, describes wind instrument reeds which have been soaked in partially polymerized methylmethacrylate which is then polymerized in the reed by ionizing radiation. This treatment fills the pores, effectively waterproofing the reed, and controlling moisture-induced swelling and loss of elasticity.
Other sealing coatings which are applied externally to the natural cane reed have been described. Killian, U.S. Pat. No. 4,145,949, describes a natural cane reed having a thin protective coating of fine particulate matter, e.g., metallic powder, deposited on the tip and edges of the reed but not on the heart or main vibratory section of the reed. A plastic-coated cane reed is also described by Rico International (Sun Valley, Calif.) for musicians who have a limited amount of control over their playing environment or need instant playability without having to re-wet their reeds. These plastic coated reeds have improved durability compared to uncoated reeds, but have playing characteristics which differ markedly from the uncoated natural cane reed.
BRIEF SUMMARY OF THE INVENTION
This invention features methods and compositions for treating the natural cane reed used to produce musical tones in woodwind instruments. The treatment utilizes a polymer or polymerizing solution, preferably a waterborne polymer or waterborne polymerizing solution, to impregnate the reed, but not render the reed waterproof. The absorbed polymer protects the reed from microbial and enzymatic degradation, thereby extending the lifetime of the reed. Surprisingly, this protection can be achieved while allowing the reed to absorb essentially normal levels of moisture from the mouth. The normal playing characteristics of the original reed are thereby either sustained or enhanced over the lifetime of the reed by the treatment.
Preferably a non-toxic waterborne polymer (or other suitable solvent-borne polymer), polymer suspension, polymer emulsion, or an aqueous-based (or other suitable solvent-based) polymerizing solution (collectively termed “waterborne or aqueous polymer treatment liquid,” “polymer treatment liquid,” or simply “polymer liquid”) is used to impregnate the reed material. “Polymer liquid” and similar terms shall refer to both aqueous and non-aqueous liquids unless indicated to the contrary, e.g., a non-aqueous polymer liquid, an aqueous polymer liquid, or an alcoholic polymer liquid. This impregnation can be accomplished by submersion of the entire reed, or at least submersion of the proximal portion, i.e., the mouth-end portion, of the reed, in the polymer liquid under conditions that provide sufficient polymer uptake to provide degradation-resistance, e.g., a liquid contact period of at least 0.5 hr at room temperature and one atmosphere. Impregnation may be accelerated (and the treatment period reduced) by methods well known in the art, including reducing the external pressure over the reed prior to impregnating the reed, and then increasing the external pressure to accelerate the entry of polymer into the pores of the reed. While the use of waterborne polymer treatment liquids are preferred, other liquids can also be used, e.g., alcohols such as ethanol and isopropanol. Preferably, the liquid is non-toxic, at least at residual levels. While the aspects of the present invention are described in connection with exemplary aqueous solutions or emulsions, other embodiments involve other liquids as just indicated. Therefore, the descriptions herein apply to both aqueous and non-aqueous liquids, though aqueous liquids are preferred.
Following contact with the polymer liquid during impregnation, free liquid residing on the surface of the reed is wiped away or otherwise substantially removed. This removal step is useful because the excess polymer material would otherwise dry on the reed surface and might undesirably seal the surface and pores of the reed, rendering it waterproof. The fact that the reed remains water-permeable after the polymer inside the reed has been allowed to dry or cure, has been demonstrated by gravimetric measurement of the rates of water absorption over a 30-60 minute period, comparing the untreated reed with the polymer-treated reed. At a minimum, the initial rate of liquid absorption under specified conditions for the treated reeds (e.g., total weight of water absorbed during the first 30-60 minutes of water immersion, divided by the time of immersion, measured at 22° C. and one atmosphere) remains equal to, or greater than 25% of the rate of liquid absorption for the untreated reed. Preferably, the rate of liquid (e.g., water) absorption for the treated reed remains equal to, or greater than 30%, 40%, 50%, 60% or even more, compared to the rate of absorption for the untreated reed. In many instances, though not necessaily, both the rate and the total amount of liquid (e.g., water) absorption after 10, 30 and 60 minutes of submersion in liquid (e.g., water) for the treated and untreated reeds are very similar (see Examples 1 and 2 below).
Thus, in the present invention, the polymer coating which protects the reed against degradation by saliva, microbial flora, and the like, is formed not as an outer waterproof barrier on the reed surface, but as a coating within the microscopic channels of the porous reed matrix, i.e., within the pores, channels and interstices of the reed. This “internally” protective polymer coating, that allows entry of water into the reed, differs markedly from both the space-filling pore-sealants and the waterproof exterior coatings formed on reeds described in other patents. Most importantly, the playing characteristics and musical sound quality of the untreated reed, are substantially preserved, i.e., sustained in the treated reed. Applicant believes that sustaining a substantial degree of water-permeability in the treated reed may be an important element in preserving many of the original sound characteristics of the untreated reed.
Typical preferred examples of useful aqueous polymer treatment liquids, include water-based emulsions (largely free of organic solvents) from the polyurethane polymer family, water-based emulsions from the polyacrylate polymer family, and combinations thereof. The proportion of polymer solids in the aqueous polymer treatment liquid is between 10% and 60% by weight, preferably 25%-40% by weight. In contrast to Petzke, U.S. Pat. No. 3,340,759, which utilized a resin containing 100% solids, the presence of a substantial proportion of water or other appropriate solvent in the present polymer treatment liquid is advantageous. This is because after the water component in the treatment liquid has evaporated, and normal curing and/or shrinkage of the polymer has occurred, the pores and channels within the reed will remain open because they have been coated rather than filled with polymer.
The polymers in the aqueous (or other) treatment liquid may possess at least a partially hydrophilic polymer component or co-polymer component. Therefore, when the water, i.e., solvent, portion of the coating evaporates, and the polymer, i.e., resin, component has coalesced, dried, polymerized, and/or otherwise fully cured, this partially hydrophilic property of the resin allows water not only to wet the reed's external surface, but also to penetrate the reed's internal channels and pores. Remarkably, this aqueous polymer treatment of the natural cane reed has a negligible effect on the mouthfeel and natural water absorbency of the reed, while the durability and the lifetime of the reed are greatly increased. As an additional benefit, the initial break-in period required for new reeds (the time required for a new reed to develop good playing characteristics) is typically shortened by the aqueous (or other) polymer treatment (see below).
In summary, protective coatings formed in reeds according to the present invention, differ from other reed treatments, as the presently described treatment does not block permeation by water, i.e., the reeds are not rendered waterproof.
The term “waterproof,” means that which is “covered or treated with a material to prevent permeation by water” (Websters Third New International Dictionary, G. & C. Mirriam Company, Springfield, Mass.). While it has been recognized by some inventors that the surface of coated reeds should be wettable by water and saliva, it has not been appreciated that treated reeds should also allow water permeation, i.e., water absorption to occur. In fact, the prior treatments lead away from water-permeability, instead teaching that the reed and its pores should be sealed by any one of several different coating treatments to render the reed waterproof.
In contrast, the present invention suggests that water absorption by the cane reed is an important aspect for preserving the natural vibration and tone properties which characterize the untreated reed. Thus, the present invention involves a process of impregnating the porous cane reed to generate a dried/cured, non-toxic protective polymer coating within and about the water-conductive channels, pores, fibers and woody cells constituting the porous structure of the reed, in which the reed structure remains water-permeable.
On a macroscopic scale, the actual rates of water uptake by untreated, and aqueous polymer-treated reeds were measured gravimetrically by submerging reeds in ambient distilled water for defined periods of time, then removing the reeds and wiping away unabsorbed surface water, and finally measuring the precise weight of the reeds to determine the amounts of water absorbed versus the time submerged (see Examples below).
In one aspect, the present invention features a method for treating the natural cane reed used in woodwind musical instruments. The method includes contacting at least the proximal portion of the reed with a polymer treatment liquid (preferably an aqueous liquid), in which this contacting process delivers at least 1% by weight of polymer into the reed based upon the percentage increase in dry weight of that portion of the reed contacted by the liquid. The reed remains substantially water-permeable, yet is rendered resistant to degradation by saliva.
In a related aspect, preferably following the above polymer liquid contacting, the liquid is removed from the surface of the treated reed, allowing the polymer components within the reed to dry or cure and become water-insoluble. For example, the liquid can be wiped away. The surface can further (or alternatively) be cleaned to remove polymer from the surface with an appropriate solvent.
In preferred embodiments, the polymer treatment liquid is water-based and non-toxic.
In preferred embodiments, the polymer treatment liquid is selected from the group consisting of aqueous polyurethanes, aqueous polyacrylates and combinations thereof.
In yet another preferred embodiment, the polymer treatment liquid contains between 10% and 60% (inclusive) by weight polymer solids. More preferably, the polymer treatment liquid contains between 20% and 50% by weight polymer solids. In particular embodiments, the polymer treatment liquid contains 10 to 40%, 30 to 60%, 20 to 40%, or 30 to 50%.
In another aspect, the present invention features a method for treating the natural cane reed used in woodwind musical instruments. The method includes contacting the reed with a polymer treatment liquid (preferably aqueous). The reed absorbs at least one-third of the amount of polymer absorbed by an equivalent untreated reed contacted with the same liquid for 10 hr at 22° C. and 1 atmosphere pressure, where determination of the amount of polymer absorbed is based upon the percentage increase in dry weight of the reed. The reed remains substantially water-permeable, yet is rendered resistant to degradation by saliva. Preferably the reed absorbs at least 40%, 50%, 60%, 70%, 80% 90%, 100% or even more of the amount of polymer absorbed under the above specified conditions.
Preferably following the above liquid contacting, the liquid is removed from the surface of the treated reed, allowing the polymer components within the reed to dry or cure and become water-insoluble. Alternatively, polymer is removed from the surface after at least partially drying or curing, e.g., with an appropriate solvent, or by abrasion or scraping.
In preferred embodiments, the polymer treatment liquid is water-based and non-toxic.
In preferred embodiments, the polymer treatment liquid is selected from the group consisting of aqueous polyurethanes, aqueous polyacrylates and combinations thereof.
In preferred embodiments, the polymer treatment liquid contains between 10% and 60% (inclusive) by weight polymer solids. More preferably, the polymer treatment liquid contains between 20% and 50% by weight polymer solids. In other embodiments, the polymer treatment liquid contains 10 to 40%, 30 to 60%, 20 to 40% or 30 to 50%.
In another aspect, this invention features a method for treating the natural cane reed used in woodwind musical instruments. The method includes the steps of providing a non-toxic (preferably waterborne) polymer treatment liquid, and contacting at least the proximal portion of the reed with the liquid. At least 1% by weight of polymer is delivered into the reed, based upon the percentage increase in dry weight of that portion of the reed contacted by the liquid. Subsequently, contact between the reed and the liquid is ceased, and the liquid is removed from the surface of the reed. Finally, the polymer components within the reed are allowed to dry or cure and become water-insoluble. The reed remains substantially water-permeable, yet is rendered resistant to degradation by saliva.
In another aspect, the present invention provides a natural cane reed for a musical instrument, in which the reed has been impregnated with a polymer treatment liquid (preferably aqueous). At least the proximal portion of the reed has been impregnated by a liquid which contains a non-toxic polymeric material that is water-insoluble upon drying or curing within the reed. The impregnated portion of the reed is at least 25% as permeable to water as an identical portion of an equivalent untreated reed, yet is resistant to degradation by saliva.
In another aspect, a natural cane reed for a musical instrument is provided, in which at least the proximal portion of the reed has been impregnated by a polymer treatment liquid that contains a non-toxic polymeric material that is water-insoluble upon drying or curing within the reed. The impregnated portion of the reed contains at least 1% by weight of the polymer material, based upon the percentage increase in dry weight of the impregnated portion. The impregnated portion of the reed remains substantially water-permeable, yet is resistant to degradation by saliva.
In a preferred embodiment, the non-toxic polymeric material is selected from the group consisting of polyurethanes, polyacrylates and combinations thereof.
In another embodiment, the polymeric material is removed from the surface of the impregnated portion of the reed before the polymeric material has dried or cured, thereby enhancing the water-permeability of the impregnated portion of said reed.
In another preferred embodiment, the reed has been treated with a waterborne polymer treatment liquid selected from the group consisting of aqueous polyurethanes, aqueous polyacrylates and combinations thereof.
In still another preferred embodiment, the reed has been treated with a waterborne polymer treatment liquid comprising between 10% and 60% by weight polymer solids. More preferably, the reed has been treated with a waterborne polymer treatment liquid comprising between 20% and 50% by weight polymer solids.
As used herein, the term “woodwind musical instruments” refers to, and includes all musical instruments that utilize a removably attached reed as described herein, including clarinets, oboes, bassoons, and saxophones. “Natural cane reeds” used in woodwind musical instruments are widely available from commercial sources, and are described herein in considerable detail.
The reed is tapered in thickness, and its proximal end is thinnest (typically 0.003-0.006 inches thick at the tip), making it especially susceptible to degradation by saliva. The “proximal portion of the reed” is that portion which is placed in the mouth and subjected to wear and tear by vibration and contact with saliva. At a minimum, the first one-quarter inch, and preferably the first one-half inch of the proximal end portion (i.e., the portion of the reed's length measured from the proximal end) should be treated with polymer treatment liquid. For example, at a distance of 0.5 inches from the proximal end of a typical tenor saxophone reed, the reed is still quite thin, ranging from approximately 0.015 to 0.025 inches in thickness, depending upon the distance inward from the side edge of the reed (and varying somewhat among different reed manufacturers). More preferably, at least 0.75, 1.0, and 1.5 inches of the proximal end of the reed are treated with polymer treatment liquid. One inch inward from the proximal end of the tenor reed, the reed's thickness has approximately doubled (compared to its thickness at the 0.5 inch position). The other end of the reed, i.e., the distal or heel portion, is robust and is removably attached to the instrument (e.g., to the mouthpiece). The heel portion is not significantly contacted or degradated by saliva.
“Polymer treatment liquids” as used herein for impregnating reeds are described above in considerable detail. These liquids may be solvent-borne or water-borne polymer solutions, emulsions and the like. Non-toxic water-based polymer treatment liquids are preferred. For example, polyrethanes, polyacrylates and combinations thereof are available in either solvent or non-toxic waterborne coating systems.
The term “non-toxic” is meant to indicate that the dried coating contains no substantial amount of toxic heavy metals or other toxic materials which could be released into the musician's mouth while playing the treated reeds.
The term “contacting” refers to physical contact between the cane reed and the polymer treatment liquid, e.g., submersion of the reed in the polymer liquid. One convenient means of submerging a reed in a polymer liquid is to nearly fill a cylindrical vial (e.g., a plastic or glass “shell vial” measuring ¾-⅞ inch in diameter×3.5 inches tall) with polymer liquid, then place the reed(s) with their thin edge downward into the liquid, and finally cap the vial. A duration of liquid contact between the reed and the polymer treatment liquid of between two and four hours (by submersion in polymer treatment liquid) is typically sufficient for the desired extent of polymer penetration of the reed. Polymer penetration may or may not reach saturation, i.e., that amount of polymer in the reed at which, little or no additional polymer solids will enter the reed with continued polymer liquid contact. At completion of the polymer contacting treatment of the reed, excess or free polymer liquid is removed from the surface of the treated reed. This “removing” may be accomplished, for example, by wiping the wet reed with an absorbent sheet such as a low lint paper towel. Solvent, e.g., water evaporation allows the polymer components in the liquid within the reed to dry or cure and become water-insoluble. After reeds have been fully immersed in polymer treatment liquid for approximately 10 hours at room temperature (22∞ C.) under ambient conditions (1 atmosphere pressure), little if any additional polymer enters the reeds, i.e., the reed's “polymer saturation level” has been reached. After fully drying a polymer-soaked reed, it is typical to measure a 3-4% weight increase in the reed. For the purpose of the present invention, a satisfactory polymer treatment must result in an incorporation of at least 1% by weight of polymer into the cane reed (based upon dry weight of that portion of the reed that has been treated). Preferably, the polymer incorporation is 2% by weight, and more preferably 3% to 4% by weight. Alternatively, at least one-fourth (25%) of the reed's polymer saturation level must be absorbed by the reed (based upon the reed's maximum dry weight increase from polymer solids, e.g., measured after approximately 10 hours soaking). Preferably, polymer absorption in the treated reed reaches 50%, 60%, or 70%. Most preferably, polymer absorption reaches 80%, 90% or even 100% of the reed's polymer absorption capacity at saturation.
The term “substantially water-permeable” when used to describe the treated reeds, means that the treated reeds absorb water at a rate (milligrams of water per minute) that is at least 25% as great as the untreated reeds. Preferably, the water absorption rate is 50% as great, and more preferably 75% or more as great as for an equivalent untreated reed.
The term “resistant to degradation by saliva” means that the treated reed resists softening by contact with saliva over a period of days or weeks of playing the instrument using the reed. More specifically, the lifetime of the treated reed is extended at least 100%, i.e., the reed is playable for at least twice as many hours as an equivalent untreated reed. The lifetime of a reed is determined by the number of hours the reed can be played before it reaches the point that a musician finds the reed too soft, unpredictable, unresponsive or lacking in tone response to continue playing. Aqueous polyurethanes, aqueous polyacrylates and combinations thereof (typically constituting the waterborne polymer treatment liquid used to treat reeds herein) are well known in the art, and commercial examples thereof are provided herein. It is preferred that so-called “interior finish” polyurethanes and polyacrylates are used, rather than exterior finishes since the latter typically contain additives including fungicides, mildewcides, UV protectants and other chemicals that are not suitable for contact with the lips and mouth. In fact, the preferred interior finishes contain no persistent additives, i.e., non-volatile additives, that are toxic or that could be irritating or sensitizing to the lips or the mouth. The 10%-60% or 20%-50% or other range of polymer solids in the polymer treatment liquids is chosen so that the polymer liquid will coat rather than fill the channels and pores in the reed, so as to allow entry of water, i.e., capillary flow of water, after the polymer has dried and/or cured in these channels and pores.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
FIGS. 1 and 2 are graphical representations of relative porosities of polymer-treated reeds as evidenced by the amount (weight) of water absorbed by individual treated and untreated natural cane reeds, as a function of the time immersed in water (see Examples 1 and 2 below, respectively). Polymer treatments were as follows:
FIG. 1 (i) gloss finish aqueous polyurethane; (ii) satin finish aqueous polyurethane; (iii) satin finish alkyd polyurethane; (iv) untreated reed.
FIG. 2 (i and ii duplicate reeds) satin finish aqueous polyurethane; (iii) alcohol-based shellac, 1 coating, (iv) alcohol-based shellac, 2 coatings; and (v) untreated reed.
FIG. 3 is a graphical representation of the uptake of polyurethane polymer treatment liquid and actual polymer solids by natural cane reeds, as evidenced by: (i) the amount (weight) of treatment liquid absorbed by individual reeds as a function of time immersed in the treatment liquid; and (ii) the net increase in dry weight of these same reeds due to absorbed polymer solids (two reeds weighed “wet” and then dried at each time interval, see Example 3 below).
DETAILED DESCRIPTION OF THE INVENTION
Methods and compositions are described for treating natural cane reeds used in woodwind instruments. The object of this treatment is to protect the reed from microbial and enzymatic degradation caused by contact with saliva. The lifetime of the natural reed is extended, without compromising the playing characteristics of the reed. The treatment utilizes a polymer or polymer solution, preferably a waterborne polymer or waterborne polymerizing solution, to impregnate the reed. Surprisingly, this protection is achieved without the reed being rendered waterproof. The original musical playing characteristics of the reed are reported to be either sustained or enhanced over the extended lifetime of the reed by the treatment.
Method of Treating Reeds
A convenient means for impregnating cane reeds with aqueous polymers described herein is to immerse the entire reed, or at least its proximal portion (i.e., the thinned portion of the reed which is placed in the mouth and therefore susceptible to degradation by saliva) in an aqueous liquid emulsion, suspension, or solution containing the polymer. Alternatively the reed may be immersed in a monomer-containing liquid, wherein the monomer can be polymerized in situ (within the reed), by use of a catalyst, by irradiation, by increased temperature, or the like, to form such a polymer. In the case of aqueous polyurethane polymer impregnation of cane reeds, the reeds may be immersed in commercially available emulsion products. Two polyurethane-containing emulsions which were utilized, were Aqua Zar brand “Water-Based Polyurethane-Interior Gloss” product #32412 LR1194, and Aqua Zar brand “Water-Based Polyurethane-Interior Satin” product #20325925 L891 containing between 30% and 40% by weight solids [United Gilsonite Laboratories (UGL, Inc.), Scranton, Pa.]. The material safety data sheet provided by UGL, Inc. states that in addition to the polyurethane resin component (15% by weight), these Aqua Zar products contain approximately an equal amount of acrylic copolymer resin (15-20% by weight). It is well known in the art that such a mixture of resins provides a combination of properties, i.e., the acrylic resin contributes greater hardness while the polyurethane resin contributes greater elasticity to the dried coating. Reeds were immersed for between 0.5 hr and 12 hr, and preferably between 1 hr and 6 hr. In the case of aqueous polyacrylate polymer treatments, reeds can be similarly immersed in these emulsions (e.g., Clear wood sealer/topcoat #SCX-1970 gloss polyacrylate resin from S.C. Johnson Polymer, Inc. Sturtevant, Wis.). This particular polyacrylate emulsion contained approximately 38% by weight resin solids, to which 3.4% by weight dipropylene glycol methyl ether and 2.3% dipropylene glycol n-butyl ether were added as coalescing solvent. For the purpose of comparing the performance of the above aqueous polymers, with non-aqueous-based coating materials, an alkyd polyurethane varnish (Zar brand “Interior Polyurethane, Clear Wood Finish, satin” product #20106 LR1294, manufactured by UGL, Inc.), and a shellac containing 31% by weight solid shellac in an alcohol-based solvent (Bulls Eye brand manufactured by William Zinsser and Company, Inc., Somerset, N.J.) were obtained and used to treat reeds. Upon removal of all reeds from the polymer emulsions, excess polymer liquid was drained from the reeds, the reeds were briefly wiped with a low lint paper towel, and finally allowed to air-dry at room temperature until the polymer was fully dry and cured (approximately 24 hrs). To accelerate the polymer impregnation process, the reeds and polymer solution may be subjected to a reduced air pressure ( e.g., 1 p.s.i. rather than the normal atmospheric pressure of 14.7 p.s.i.) in order to remove air from within the porous structure of the reed. When the air pressure is then returned to normal (or even increased above atmospheric pressure), the polymer liquid flows easily into the reed channels and pores.
Water Flow into Polymer-Treated Reeds
While the presently described dried and/or cured aqueous polymer coatings (e.g., polyurethane and polyacrylate coatings) may be partially hydrophobic, these coatings must also be sufficiently hydrophilic to allow substantially unimpeded water absorption into the pores of the reed. Normal absorption and capillary movement of water into untreated and polymer-treated reeds has been visualized by light microscopy (through the tips of cane reeds having a thickness of approximately 0.004 inch). Phase contrast light microscopy (150×magnification) of cane reeds whose tips were immersed in distilled water on a glass microscope slide (tenor saxophone reeds manufactured by Rico International Company) was utilized for visualization of capillary water flow. The observation of microscopic air bubbles moving through capillary channels in the reed, as well as air bubbles escaping through the tip end and through surface pores in the reed, and the increasing size of water droplets within intracellular spaces provided direct visual evidence of normal water migration and infiltration into both aqueous polymer-treated and untreated reeds.
Musical Properties of Treated Reeds
A professional musician playing a tenor saxophone (Selmer Inc., Super 80 model) compared the playing properties of the above-described aqueous polyurethane-treated reeds, with both untreated “control” reeds and the above-described alkyd varnish and shellac-treated reeds of the same manufacture (Rico Royal #3) described in Examples 1 and 2. The shellac and alkyd polyurethane-treated reeds were reported to be more difficult to play than untreated reeds and produced a harsh “edgy” and “buzzy” tone. However, the aqueous polyurethane-treated reeds were easily playable, and were described as producing a “natural-sounding” tone equal to or superior to that of the untreated reeds. The dynamic responsiveness of the latter reeds was reported to be excellent over the full tonal range of the instrument. Surprisingly, it was reported by two independent saxophone playing musicians, that while untreated cane reeds always require a break-in period before the reeds exhibit good playability and responsiveness, the aqueous polyurethane-treated reeds required little if any conditioning or break-in period. Typically, the polyurethane-treated reeds could be played immediately with a smoothness and consistency which was superior to untreated cane reeds. Therefore, in addition to extending the lifetime of the natural cane reed, the aqueous polymer treatment facilitates use of new reeds by reducing or eliminating the break-in period.
Extended Lifetime of Treated Reeds
A professional musician (tenor saxophone), who had been accustomed over a period of years to using Rico Royal #3 reeds, switched to playing his instrument using the same reeds which had been treated with the aqueous polyurethane polymer (Zar brand, satin interior finish) according to Example 1. Over a period of three months the musician reported his observations. In addition to eliminating the need for any break-in period (before which the reed is difficult or uncomfortable to play), the musician reported that the polymer-treated reeds remained playable for over a month. The comparable untreated reeds were reported to be playable for only 1-2 weeks (for a comparable average number of hours per day played). The principal difference reported for the treated reeds was a remarkable resistance to the gradual softening process which limits the lifetime of the reed. This resistance is significant because out of a group of ten or more new cane reeds, a professional musician may find only one or two reeds which would be deemed “good to excellent” for their professional playing needs. Extending the lifetime of such selected reeds two or three-fold has a substantial practical as well as a commercial value. Selected used reeds that already have been played for some time (e.g., several days or a week), may also be polymer-treated to extend their lifetime. In the case of such used reeds, it is recommended that the reeds be washed with a mild detergent and dried before treatment. Washing may also include a disinfection treatment, e.g., soaking 2-10 minutes in 3% hydrogen peroxide solution.
EXAMPLES
Example 1
Reeds were impregnated by submerging them in either aqueous polyurethane resin (see above) for 4 hr or in alkyd polyurethane resin for 2.5 hr. Reeds were drained and wiped free of surface liquid polyurethane, and dried overnight. The amounts of absorbed water were then gravimetrically measured as a function of the time for which the reeds were immersed in distilled water (at room temperature) as described above. Reeds treatments were as follows for single reeds: (i) gloss finish aqueous polyurethane-treated; (ii) satin finish aqueous polyurethane-treated; (iii) satin finish alkyd, i.e., oil-based polyurethane-treated; and (iv) untreated cane reed “control”. All reeds were Rico Royal tenor saxophone #3 reeds, Rico International, Inc., Sun Valley, Calif.).
The results of this experiment (see FIG. 1) show that treatment of natural cane reeds with either of two aqueous polyurethane polymer formulations (gloss or satin finish), caused very little change in the rate of water absorption compared to an untreated reed. The presence of fumed silica (dulling agent in the satin finish product) did not appear to influence water permeability. By contrast, the alkyd polyurethane treatment significantly diminished permeability to water (by approximately 50%-60% during the first 15 minutes of water exposure). This decrease occurred despite the fact that free, i.e., unabsorbed resin liquid had been wiped from the reed following treatment (same as for the aqueous polyurethane treated reeds), and immersion time in the alkyd polyurethane was shorter than in the aqueous treatment.
Example 2
Reeds were impregnated with polymer coating materials, surface-wiped upon removal from the polymer treatment liquids, dried overnight, and tested for water absorption, i.e., relative permeability to water, as in Example 1, except that the reed treatments were as follows: (i) and (ii) duplicate reeds immersed for 8 hr in satin finish aqueous polyurethane (36% solids); (iii) single reed immersed for 8 hr in shellac (Bulls Eye brand, 33% by weight solids), (iv) single reed immersed for 8 hr in shellac, wiped, dried, briefly re-immersed in shellac for 10 min, re-wiped, and re-dried (two shellac treatments); and (v) single untreated cane reed “control”.
The results of this experiment (see FIG. 2) confirm those results of Example 1. Again, even with prolonged immersion in aqueous polyurethane, water absorption in the treated reeds is similar to that of untreated reeds. It should be emphasized that the step in which excess surface liquid (polyurethane polymer) is wiped or otherwise removed from the reed (following the polymer immersion treatment, and prior to drying and curing) is crucial for maintaining water permeability in the reed. If this step is not followed, and a continuous polyurethane polymer coating (either aqueous or alkyd-based) is allowed to form over the reed's surface, the reed subsequently exhibits very little water permeability (data not shown). Regarding the shellac treatment of reeds, the single treatment decreased water permeability by approximately 60% during the first 15 minutes of water exposure, while two shellac treatments (with a drying step in between) decreased water permeability by approximately 80% during the same time period.
Example 3
To determine the immersion time required for saturating untreated reeds with aqueous polyurethane polymer, five pairs of untreated natural cane reeds (Rico Royal tenor saxophone #3 reeds) were treated for increasing periods of time by submerging them in Aqua Zar brand “Water-Based Polyurethane-Interior Gloss” (see above). Accordingly, after 0.5 hr, 1 hr, 2 hr, 3 hr and 4 hr of polymer treatment, pairs of reeds which had been accurately weighed before treatment were removed from the polyurethane, drained and wiped free of surface liquid, and weighed again to determine the amount of liquid absorbed. For experimental reproducibility, prior to weighing, the reeds were incubated overnight in a warming oven (45° C.) to assure a constant level of relative humidity in the reeds both before and after polyurethane treatment. In this manner an accurate measurement of the increase in dry weight of the reeds, i.e., the actual amount of polymer absorbed by the reeds, could be determined. The results of this experiment (see FIG. 3) indicate that for the first two hours, the cane reeds rapidly absorbed liquid after which time absorption slowed markedly. Measurement of the increase in dry weight of the reeds shows similar kinetics for polymer uptake (saturation within approximately 3 hrs). Therefore, a treatment duration, i.e., liquid immersion of 2-4 hours, is typically sufficient for achieving saturation.
Interestingly, the actual proportion of polymer solids being absorbed by the reeds compared to absorbed liquid was approximately 10% (e.g., 30-40 mg solids absorbed versus 350-400 mg liquid), while the polyurethane treatment liquid contained 36% by weight solids. The more rapid entry of water compared to absorbed polymer indicates that the pores of the reed partially restrict entry of polymer material. This is not surprising given that the particle size reported by the manufacturer for this waterborne polyurethane coating is approximately 0.5-1.0 microns.
Example 4
Waterborne acrylates constitute another major polymeric coating group that Applicant has used to treat natural cane reeds, to protect them from degradation, and extend their playable lifetime. To determine the immersion time required for saturating untreated reeds with an aqueous polyacrylate polymer, five pairs of untreated natural cane reeds (Rico Royal tenor saxophone #3.5 reeds) were treated for increasing periods of time by submerging them in a styrene-acrylic coating solution. This solution, containing 29% by weight solids, and known in the art as a “one pack self-crosslinking polymer” contained (by weight percentages): 76% styrene acrylic emulsion #SCX-1970 (8% by weight solids) manufactured by S.C. Johnson Polymer, Inc. Sturtevant, Wis., 17.3% water, and as coalescing solvents, 4% dipropylene glycol methyl ether (DPM) and 2.7% dipropylene glycol n-butyl ether (DPnB). The manufacturer of SCX-1970 reports that the styrene acrylic particle size is approximately 0.1 microns. After 0.5 hr, 1 hr, 2 hr, 3 hr and 7 hr of submersing the pairs of reeds in closed vials containing the waterborne polyacrylate solution, pairs of reeds which had been accurately weighed before treatment, were removed from the solution, wiped free of surface liquid, and briefly weighed to determine the amount of liquid absorbed. As in Example 3, prior to determining final dry weights (to determine amount of incorporated polymer in the reeds), the reeds were incubated overnight in a warming oven (45° C.) to assure a constant level of relative humidity in the reeds both before and after acrylate treatment. The results of this experiment (not shown) differed only slightly from those in Example 3. As in Example 3, the actual proportion of polymer solids absorbed by the reeds at saturation, compared to absorbed liquid, was approximately 7%-10% (e.g., 30 mg solids absorbed versus 300 mg liquid) while the styrene acrylic treatment solution contained 29% by weight solids. Again, as in Example 3, the more rapid entry of water compared to absorbed polymer indicates that the pores of the reed partially restrict entry of polymer material.
All patents and publications mentioned in the specification are indicative of the levels of skill of those skilled in the art to which the invention pertains. All references cited in this disclosure are incorporated by reference to the same extent as if each reference had been incorporated by reference in its entirety individually.
One skilled in the art would readily appreciate that the present invention is well adapted to carry out the objects and obtain the ends and advantages mentioned, as well as those inherent therein. The specific methods and compositions described herein as presently representative of preferred embodiments are exemplary and are not intended as limitations on the scope of the invention. Changes therein and other uses will occur to those skilled in the art which are encompassed within the spirit of the invention are defined by the scope of the claims.
It will be readily apparent to one skilled in the art that varying substitutions and modifications may be made to the invention disclosed herein without departing from the scope and spirit of the invention. For example, those skilled in the art will recognize that the invention may suitably be practiced using any of a variety of sources of said polymer treatment liquids.
The invention illustratively described herein suitably may be practiced in the absence of any element or elements, limitation or limitations which is not specifically disclosed herein. Thus, for example, in each instance herein any of the terms “comprising,” “consisting essentially of” and “consisting of” may be replaced with either of the other two terms. The terms and expressions which have been employed are used as terms of description and not of limitation, and there is not intention that in the use of such terms and expressions of excluding any equivalents of the features shown and described or portions thereof, but it is recognized that various modifications are possible within the scope of the invention claimed. Thus, it should be understood that although the present invention has been specifically disclosed by preferred embodiments and optional features, modification and variation of the concepts herein disclosed may be resorted to by those skilled in the art, and that such modifications and variations are considered to be within the scope of this invention as defined by the appended claims.
In addition, where features or aspects of the invention are described in terms of Markush groups or other grouping of alternatives, those skilled in the art will recognize that the invention is also thereby described in terms of any individual member or subgroup of members of the Markush group or other group. For example, if there are alternatives A, B, and C, all of the following possibilities are included: A separately, B separately, C separately, A and B, A and C, B and C, and A and B and C. Thus, the embodiments expressly include any subset or subgroup of those alternatives, for example, any subset of the types of polymer treatment liquids. While each such subset or subgroup could be listed separately, for the sake of brevity, such a listing is replaced by the present description.
While certain embodiments and examples have been used to describe the present invention, many variations are possible and are within the spirit and scope of the invention. Such variations will be apparent to those skilled in the art upon inspection of the specification, drawings and claims herein.
Other embodiments are within the following claims.
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A method for treating the natural cane reed used in woodwind musical instruments. The method includes contacting at least the proximal portion of said reed with a polymer treatment liquid, in which the liquid delivers at least 1% by weight of polymer into the reed, based upon the percentage increase in dry weight of that portion of said reed contacted by the liquid. The reed remains substantially water-permeable, yet is rendered resistant to degradation by saliva. An impregnated reed is also described, in which at least the proximal portion of the reed has been impregnated by a liquid that includes a non-toxic polymeric material that is water-insoluble upon drying or curing within the reed. The impregnated portion of the reed is at least 25% as permeable to water as an identical portion of an equivalent untreated reed, yet is resistant to degradation by saliva.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims priority to pending U.S. Provisional Patent Application No. 61/697,171 filed Sep. 5, 2012 which is incorporated herein by reference.
BACKGROUND
[0002] The present invention is related to an improved hermetically sealed polymer capacitor and method of making an improved hermetically sealed polymer capacitor.
[0003] Hermetically sealed capacitors comprising polymeric cathodes have been utilized in the art for some time. One systemic problem with hermetically sealed capacitors comprising polymeric cathodes is a gradual increase in equivalent series resistance (ESR) and direct current leakage (DCL) at elevated temperatures. These systemic problems have always been considered a function of cathode breakdown and have therefore been accepted as an inherent function of the capacitor type.
[0004] Through diligent research the present inventors have discovered a mechanism of degradation which was previously unrealized and not predicted. By eliminating the unexpected mechanism of degradation hermetically sealed capacitors comprising polymeric cathodes can be manufactured with significant improvement in ESR and DCL thereby providing capacitors with a thermal stability previously considered unavailable.
[0005] The present invention provides a method of manufacturing a hermetically sealed capacitor comprising a polymeric cathode wherein the capacitor has improved thermal stability as indicated by improved ESR and DCL after exposure to elevated temperatures.
SUMMARY
[0006] It is an object of the invention to provide an improved hermetically sealed capacitor and method of making the hermetically sealed capacitor.
[0007] A particular feature of the invention is a hermetically sealed capacitor, comprising a polymeric cathode, wherein the capacitor has improved ESR and DCL performance after exposure to elevated temperatures.
[0008] These and other advantages, as will be realized, are provided in a process for forming a capacitor. The process includes the steps of: providing a case;
[0000] applying a solder and a flux to an interior surface of the case;
flowing the solder onto the interior surface;
washing to remove flux thereby forming a flux depleted solder;
providing a capacitive element comprising:
an anode of a valve metal; an anode lead in electrical contact with the anode; a dielectric on the anode; and a cathode layer on the dielectric wherein the cathode comprises a doped conductive polymeric cathode and a solderable layer; inserting the capacitive element into the casing; reflowing the flux depleted solder thereby forming a solder joint between the case and the solderable layer; and sealing the case.
BRIEF DESCRIPTION OF DRAWINGS
[0009] FIG. 1 is a cross-sectional schematic view of an embodiment of the invention.
[0010] FIG. 2 is a flow chart representation of an embodiment of the invention.
[0011] FIG. 3 is a graphical representation of the CAP of an inventive example.
[0012] FIG. 4 is a graphical representation of the DF of an inventive example.
[0013] FIG. 5 is a graphical representation of the ESR of an inventive example.
[0014] FIG. 6 is a graphical representation of the LKG of an inventive example.
[0015] FIG. 7 is a graphical representation of the CAP of a comparative example.
[0016] FIG. 8 is a graphical representation of the DF of a comparative example.
[0017] FIG. 9 is a graphical representation of the ESR of a comparative example.
[0018] FIG. 10 is a graphical representation of the LKG of a comparative example.
DESCRIPTION
[0019] The present invention is directed to an improved hermetically sealed polymeric cathode capacitor and a method for making same.
[0020] The invention will be described with reference to the figures forming an integral, non-limiting, component of the disclosure. The figures are intended to facilitate an understanding of the invention and are not intended to limit the invention in any way. Throughout the figures various elements will be numbered accordingly.
[0021] An embodiment of a hermetically sealed solid electrolytic capacitor of the present invention will be described with reference to FIG. 1 . In FIG. 1 , a hermetically sealed capacitor is represented in schematic cross-sectional view at 101 . The capacitor, comprises an anode, 110 , which may be a monolithic anode body or multiple anodes comprising a valve metal. An anode wire, 112 , extends from the anode body and can be attached to the anode body for example by welding, or the anode wire can be embedded in the anode body by compression. A dielectric, 114 , is on the surface of the anode body and preferably at least partially encases the anode body. A conductive layer, 116 , which functions as the cathode, is on the surface of the dielectric of the anode body and preferably at least partially encases the dielectric layer. As would be realized, the anode and cathode separated by a dielectric form the capacitive element. Additional conductive layers, 117 , are preferably employed to provide an adequate interface for subsequent connection to the casing and the optional cathode lead wire, 124 . The casing itself can function as the cathodic termination to a circuit trace. The additional conductive layers preferably include layers comprising carbon, silver, copper, nickel or other conductive materials, either in a binder or as a layer of deposited metal, and may include multiple layers. The deposited metal layers can be provided by vapor deposition, electroplating or electroless plating.
[0022] The capacitive element is hermetically sealed in a casing, 132 , which in a preferred embodiment is a conductive casing. Flux depleted solder, 126 , connects the conductive layers, 117 , to the casing, 132 , or to the cathode lead wire, 124 . The optional cathode lead wire, 124 , is attached to the casing or it may extend into the flux depleted solder, 126 . An external anode lead, 118 , is connected, preferably by welding, to the anode wire, 112 . The external anode lead extends out of the casing. A positive seal, 128 , contains at least a portion of the external anode lead and/or the anode wire. An edge seal, 131 , hermetically seals the casing with the cap material, 130 . While not limited thereto, the external anode lead and cathode lead are preferably nickel. Although many metallic and glass to metal seal materials can be used to provide hermetic sealing of the casing, the positive seal material and the edge sealing material are preferably solder.
[0023] The method of manufacturing the hermetically sealed solid electrolytic capacitor will be described with reference to FIG. 2 .
[0024] In FIG. 2 , an anode is formed at 200 . In a preferred embodiment the anode is formed from a powder which is compressed and sintered to form a monolithic body. In another embodiment the anode is a foil which is optionally, and preferably, etched to increase surface area. The shape and dimension of the anode is not particularly limited herein. In the case of a compressed powder anode an anode wire can be attached to the anode after compression, such as by welding, or the anode wire can be inserted into the powder and the powder compressed around the anode wire thereby forming an anode with an anode wire embedded in the anode and extending therefrom.
[0025] A dielectric is formed on the anode at 202 . While not limited thereto, a preferred dielectric is an oxide of the anode material. This is preferred primarily for manufacturing convenience. Preferably, the dielectric is an oxide of Al, W, Ta, Nb, Ti, Zr and Hf with Al 2 O 3 , Ta 2 O 5 and Nb 2 O 5 being most preferred. The method of forming the dielectric is not limited herein. Anodization of a valve metal to form a dielectric is well understood in the art and described in detail in U.S. Pat. Nos. 7,678,259; 7,248,462; 6,755,959; 6,652,729; 6,480,371; 6,436,268; 6,346,185; 6,267,861; 6,235,181; 5,716,511; 5,185,075 and 4,812,951. One method for anodization employs anodizing solutions having a water content below approximately 30% in combination with alkanol amine, phosphoric acid and an organic solvent. Monoethanol amine, diethanol amine, triethanol amine, ethyl diethanolamine, diethyl ethanolamine, dimethyl ethanolamine and dimethyl ethoxy ethanolamine (dimethyl amino ethoxy ethanol) are mentioned as alkanol amines. Ethylene glycol, diethylene glycol, polyethylene glycol 300 and tetraethylene glycol dimethyl ether, are mentioned as solvents. It is generally desirable to conduct the anodizing at temperatures below about 50° C., preferably within a pH range of 4-9 which can be adjusted with phosphoric acid if desired.
[0026] A cathode is formed on the dielectric at 204 . The cathode is a conductor preferably comprising an intrinsically conductive polymeric material as known in the art. The cathode may include multiple layers wherein adhesion layers are employed to improve adhesion between the conductor and the termination. Particularly preferred adhesion layers include carbon, silver, copper, or another conductive material in a binder or a metalized layer such as nickel or silver. Conductive polymeric materials are employed as a cathode material. Particularly preferred intrinsically conductive polymers include polypyrrole, polyaniline, polythiophene and their derivatives. A particularly preferred conductive polymer is poly 3,4-ethylenedioxythiophene (PEDT). PEDT can be made by in situ polymerization of 3,4-ethylenedioxythiophene (EDT) monomer such as Clevius M V2, which is commercially available from Hereaus Clevious, with an oxidizer such as ferric tosylate solution available as Clevios®C from Hereaus Clevios. The application and polymerization of heterocyclic conductive polymers such as polypyrrole, polyaniline, polythiophene and their derivatives is widely described and well known to those of skill in the art. Additional conductive layers preferably include layers comprising carbon, silver, copper, nickel or other conductive materials, either in a binder or as a layer of deposited metal, and may include multiple layers which are preferably deposited on the polymeric cathode layer to improve subsequent adhesion. The conductive polymer typically includes at least one dopant which can be incorporated into the polymer during the polymerization process. Dopants can be derived from various acids or salts, including aromatic sulfonic acids, aromatic polysulfonic acids, organic sulfonic acids with hydroxy group, organic sulfonic acids with carboxylhydroxyl group, alicyclic sulfonic acids and benzoquinone sulfonic acids, benzene disulfonic acid, sulfosalicylic acid, sulfoisophthalic acid, camphorsulfonic acid, benzoquinone sulfonic acid, dodecylbenzenesulfonic acid, toluenesulfonic acid. Other suitable dopants include sulfoquinone, anthracenemonosulfonic acid, substituted naphthalenemonosulfonic acid, substituted benzenesulfonic acid or heterocyclic sulfonic acids as exemplified in U.S. Pat. No. 6,381,121 which is included herein by reference thereto. Polystyrene sulfonate is a particularly preferred dopant. Through diligent research it has now been realized that the degradation upon exposure to elevated temperature is due to the unexpected reaction of the flux, present in the solder, and the dopant, present in the conductive polymer. The flux was previously not considered as a culprit since the flux was previously considered to be active during reflow after which the flux was considered to be no more than an included inert impurity, as an oxide or slag, in the solder matrix. At elevated temperatures the flux, most likely as a vapor, has been determined to react with the conductive polymer cathode causing ESR and DCL increases.
[0027] Solder is applied to the inside of the can and the can is washed at 206 . The solder includes a flux which leaches the native oxide from the surface of the interior of the can. The solder is converted to a flux depleted solder by washing with an organic solvent which removes most of the residual flux. The preferred organic solvents include alcohol, glycol, ketone, ether, ester, dimethyl-formamide (DMF), dimethyl sulfoxide (DMSO), methylene chloride, N-methyl-2-pyrrolidinone (NMP), with isopropyl alcohol and acetone being most preferred. In one embodiment the solvent is reclaimed and analyzed for impurities, such as by chromatography and particularly gas chromatography, for impurities consistent with the flux. A flux depleted solder is achieved when a lack of significant impurities is achieved. Preferably, the impurities in the solvent are at a level of less than 1 wt % and more preferably less than 0.1 wt %.
[0028] The capacitive element, which comprises an anode and cathode with a dielectric there between, is inserted into a casing at 208 . The flux depleted solder is reflowed thereby forming a solder bond between the cathode of the capacitive element and the casing. The casing preferably has a cavity within which the capacitive element resides. The anode wire is electrically connected to an external anode connection and the cathode may be electrically connected to an external cathode connection.
[0029] The can is sealed at 210 either in ambient air, inert atmosphere, moist air or some combination thereof as exemplified in U.S. Pat. No. 8,379,311 which is incorporated herein by reference.
[0030] It is preferred that the capacitors be tested at 212 . One preferred portion of the testing is a burn-in wherein the capacitor is subjected to 1.0 to 1.5 times of the rated voltage at a temperature of 50° C. to 150° C. More preferably, the capacitor is aged at 1.2 to 1.4 times of the rated voltage at a temperature of 75° C. to 125° C.
[0031] The anode is a conductor preferably selected from a metal or a conductive metal oxide. More preferably the anode comprises a mixture, alloy or conductive oxide of a valve metal preferably selected from Al, W, Ta, Nb, Ti, Zr and Hf. Most preferably, the anode comprises at least one material selected from the group consisting of Al, Ta, Nb and NbO with tantalum being most preferred.
[0032] The anode wire is most preferably constructed of the same material as the anode. The anode wire can be welded onto the anode surface under protective atmosphere or inserted into a powder prior to compression of the powder to form a porous anode body.
[0033] The dielectric is a non-conductive layer which is not particularly limited herein. The dielectric may be a metal oxide or a ceramic material. A particularly preferred dielectric is an oxide of an anode metal due to the simplicity of formation and ease of use.
[0034] The casing can be a metal or a ceramic. The casing may include a single layer or multiple layers with aluminum nitride, aluminum oxide, silicon oxide, magnesium oxide and calcium oxide being mentioned as exemplary materials. Conductive materials, such as a metal, are mentioned as exemplary for demonstration of the invention. The metal casing may include a surface coating on the interior and/or exterior thereof to increase conductivity or to improve solderability. A conductive casing may be constructed of brass with a solder coating, such as a Sn/Pb plating, on the inside and outside of the casing. The width, length and depth of the casing are selected for the application and are not otherwise limited herein. It would be readily apparent that a minimal size consistent with the application is preferred. In general, a length of 1 to about 25 millimeters with a width, or diameter in the case of a cylindrical case, of 0.5 to 10 millimeters is mentioned as being suitable for demonstration of the invention.
[0035] The internal conductive traces or conductive pads may be electrically connected to external conductive traces or pads thereby allowing the hermetically sealed capacitor to be mounted on a surface. The internal conductive traces or conductive pads and external conductive traces or conductive pads are electrically connected by any method known in the art. The conductive material may extend through the casing or may be in the form of pins, pads, sheets, etc. The external conductive traces or conductive pads are preferably as thin as possible to minimize total size of the hermetically sealed capacitor with the proviso that adequate conductivity is achieved. The solder is preferably a Pb/Sn based solder with 30-50 wt % Pb and the balance selected from Sn and other minor components such as silver. A solder with 30-50 wt % Pb, 45-69 wt % Sn and 1-5 wt % Ag is particularly preferred. A Pb/Sn/Ag solder with a 36/62/2 wt % ratio is particularly suitable.
[0036] The flux is preferably an organic acid capable of leaching the oxide from the surface of a material to be soldered. The flux increases the quality of the joint since oxides are detrimental to a solder joint. It was previously thought that the flux formed inert slag and any unreacted flux would either be an inert included impurity in the solder or minor portions would float to the surface of the solder. It was surprisingly found that a sufficient amount of flux remains on the surface of the solder as to be visible and the flux is detrimental to the capacitor performance especially under high temperature. Particularly preferred fluxes include organic acids selected from carboxylic acids. More preferred fluxes are based on natural or purified rosin such as those with RMA (Rosin Mildly Activated) in the MIL QQS Classification or L0 and L1 types in the ANSI classification. In a particularly preferred embodiment the flux is included with the solder in a core-shell arrangement wherein the solder has internal voids with flux contained therein. A particularly useful solder is referred to as a flux core solder wherein the solder is in the form of a hollow tube with flux contained therein. This is particularly advantageous since the flux/solder ratio is constant during the application of the solder. The flux depleted solder preferably has no visible flux residue on the surface of the solder. Without washing flux is visible. A cleanliness check can be performed by analyzing the solvent used to wash out the flux residuals, for example by using gas chromatography. A lack of significant impurities in the solvent from the last cycle of washing indicates an acceptable flux residual depletion. More preferably the solvent has less than 1 wt % impurities and even more preferably less than 0.1 wt % impurities.
[0037] A series of identical capacitive elements were prepared with a cylindrical tantalum anode with a diameter of 4.7 mm and a length of 10.2 mm comprising a tantalum wire lead. A tantalum pentaoxide dielectric was prepared as taught in accordance with U.S. Pat. No. 5,716,511. A cathode layer was formed using prepolymerized PEDT dispersion with polystyrene sulfonate dopant, Clevios K, available from Hereaus Clevios as taught in U.S. Pat. No. 7,563,290. Carbon containing and silver containing layers were coated on the PEDT layers. The samples were then separated into two groups for different treatments. For one set of samples (referred as control samples), each capacitive couple was placed in a solder coated brass casing with an outside diameter of 7.1 mm, a height of 16.5 mm and a wall thickness of 0.30 mm. Using a Sn/Pb/Ag/62/36/2 RMA flux core solder an electrically conductive bond was formed between the cathode and the casing. For the other set of samples (inventive samples) the same Sn/Pb/Ag/62/36/2 RMA flux core solder was placed inside the solder coated brass can and reflowed to obtain an electrically conductive bond between the solder and the can. The flux was then washed with acetone and isopropanol alcohol to obtain flux depleted solder. The capacitive element was then placed in the flux depleted soldered can. They were heated to melt the solder and an electrically conductive bond between the capacitive element and the casing was obtained. The entire population of sealed capacitors was heated to a temperature of 125° C. for up to 2000 hours. The capacitance in microfarads (CAP), dissipation factor in percent (DF), equivalent series resistance in ohms (ESR) and DC leakage current in microamperes (LKG) were measured and recorded. CAP and DF were measured with an AC signal at 120 Hz while ESR was measured at 100 KHz, as well known in the industry. The DC leakage was measured at rated voltage of 60V and a charging time of at least 90 seconds. FIGS. 3-6 illustrate the CAP, DF, ESR and LKG, respectively, of the inventive samples. FIGS. 7-10 illustrate the CAP, DF, ESR and LKG, respectively, of the control samples. As can be seen from the data the CAP and LKG are relatively unchanged whereas there is a marked improvement in the ESR and DF for the inventive samples relative to the controls.
[0038] One of skill in the art would realize additional embodiments and improvements which are not specifically enumerated but which are within the scope of the invention as specifically set forth in the claims appended hereto.
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A process for providing an improved hermetically sealed capacitor which includes the steps of applying a solder and a flux to an interior surface of a case; flowing the solder onto the interior surface; remove flux thereby forming a flux depleted solder; inserting the capacitive element into the casing; reflowing the flux depleted solder thereby forming a solder joint between the case and the solderable layer; and sealing the case.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to fishing, and more particularly, to an improved fishing line holder.
[0003] 2. Description of the Related Art
[0004] Several designs for fishing line holders have been designed in the past. None of them, however, include a fishing line organizer that floats, prevents line kinks, works with modern terminal tackle and works with any length of line.
[0005] Applicant believes that the closest reference corresponds to U.S. Pat. No. 2,879,619 issued to Victor N. Peterson. However, it differs from the present device because, inter alia, the present device includes slots to catch a swivel (or other terminal tackle) and can float thereby reducing the possibility of losing the device in the water.
[0006] Other patents describing the closest subject matter provide for a number of more or less complicated features that fail to solve the problem in an efficient and economical way. None of these patents suggest the novel features of the present invention.
SUMMARY OF THE INVENTION
[0007] The present device is essentially a fishing line holder comprising a frame taking the form of a substantially rectangular plate with a first edge, a second edge, a third edge, a fourth edge, a first face and a second face. Said frame being buoyant and having a series of ridges on said first edge with a corresponding number of ridges on said third edge. Said second and said fourth edges being flat. Between each adjacent ridge is a slot dimensioned to permit the passage of fishing line into the slot but not the passage of terminal tackle.
[0008] The frame may be constructed from natural cork, synthetic cork, a core of rigid plastic fixed between two layers of cork, a core of rigid material fixed between two layers of material penetrable by a fishing hook, other material penetrable by a fishing hook.
[0009] The fishing line holder may also have channels in said first face and said second face of said frame that are parallel to said second edge and extend from each slot on said first edge to the corresponding slot on said third edge.
[0010] The fishing line holder may also have a rounded edge inside each slot on said first and third edge sufficient to reduce bends, kinks or creases in a fishing line wrapped around said frame and into said slots.
[0011] It is one of the main objects of the present invention to provide a device that floats.
[0012] It is another object of this invention to provide a device that reduces any creases or kinks in fishing line.
[0013] It is still another object of the present invention to provide a device that neatly stores fishing lines of widely varying lengths and with a wide variety of terminal tackle
[0014] It is yet another object of this invention to provide such a device that is inexpensive to manufacture and maintain while retaining its effectiveness.
[0015] Further objects of the invention will be brought out in the following part of the specification, wherein detailed description is for the purpose of fully disclosing the invention without placing limitations thereon.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] With the above and other related objects in view, the invention consists in the details of construction and combination of parts as will be more fully understood from the following description, when read in conjunction with the accompanying drawings in which:
[0017] FIG. 1 represents a perspective view of the device holding a section of fishing line.
[0018] FIG. 2 shows a perspective view of a cross-section of the device showing in detail the characteristics of the slot.
[0019] FIG. 3 illustrates several examples of terminal tackle commonly in use today.
[0020] FIG. 4 shows a perspective view of an embodiment of the device.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] Referring now to the drawings, where the device is generally referred to in FIG. 1 with numeral 10 , it can be observed that it basically includes a frame 12 , ridges 14 and slots 16 . Said frame 12 may take the form of a substantially rectangular plate having four edges, a first face and a second. Two of said edges of the frame 12 opposite each other have a series of ridges 14 separated by a series of slots 16 . One slot 16 is positioned between each of said ridges 14 and transverses the thickness of the frame 12 .
[0022] A usefulness of said ridges 14 is to prevent a fishing line from sliding along an edge of the frame and becoming entangled with other lines wrapped around the frame 12 . Said ridges 14 may have a triangular profile as demonstrated in FIG. 1 or may alternatively have a rounded profile. The dimensions of the ridges 14 are such that when a fishing line is wrapped multiple times around the frame 12 and between two adjacent ridges 14 the fishing line does spill over between another pair of ridges 14 .
[0023] Said slots 16 are positioned between each of said ridges 14 . The slots 16 are dimensioned to permit fishing line to pass to the base of the slot 16 but narrow enough to prevent terminal tackle, such as a swivel, clip, crimped loop or other typical fishing line connector, from being able to pass through the slot 16 . Multiple slots 16 are provided on each of two opposing edges. Each of the slots 16 is paired with a slot 16 on the opposing edge that work in cooperation to secure one or more fishing lines.
[0024] FIG. 1 shows an example of how the device could be used to secure a swivel 18 , a line 20 and a hook 22 . Generally, the line 20 near the swivel 18 is placed into said slot 16 and the line 20 is pulled so that the swivel 18 presses against the side of the slot 18 either against said first face or second face of the frame 12 . The line 20 is wrapped around the frame 12 and then through the corresponding slot 18 on the opposing edge of the frame 12 . The line 20 is repeatedly wrapped around the frame 12 and through the same two slots 16 until the length of the line 20 is exhausted and the hook 22 is then pierced into the side of the frame 12 under enough tension to prevent the line 20 from unwinding.
[0025] In a variation of the device said frame 12 is formed of a semi-rigid unitary piece of natural or artificial cork, foam, plastic or other material capable of maintaining the form of the device as described and pierce-able by the sharp point of a fishing hook and resistant to damage from repeated insertion and removal of fishing hooks. The material or materials the device is constructed from provides buoyancy sufficient to prevent the device from sinking even when wound with multiple fishing lines, hooks and other terminal tackle.
[0026] In another variation of the device the frame 12 is formed from a series of laminate layers. For example, a rigid layer sandwiched by pieces of natural or artificial cork, foam, plastic or other material pierce-able by the sharp point of a fishing hook and resistant to damage from repeated insertion and removal of fishing hooks.
[0027] FIG. 2 shows a cross-section of a variation of the device comprising, inter alia, a frame 12 , ridges 14 , a slot 16 , a slot 17 , an edge 24 and an edge 25 . The interior of slot 16 is shown in include an edge 24 with a rounded profile. A slot 17 is opposite slot 16 and corresponds to slot 16 and also has an edge 25 with a rounded profile. In typical use of the device fishing line is repeatedly wound around the frame 12 and in slot 16 and slot 17 . The rounded profiles of the edge 24 and edge 25 aid in preventing a crease, kink or bend in a fishing line wrapped around the device. In one embodiment of the device all of the several slots have rounded edges similar to the edge 24 and edge 25 .
[0028] FIG. 3 shows an example of several types of terminal tackle that are in common use today. Any of these and many other types of terminal tackle would be effective when used with the device. Commonly used and compatible with this device include, inter alia, a swivel 30 , a clip 34 , a swivel clip 32 and/or a crimped loop 36 . A segment of fishing line 38 is connected to any of the shown terminal tackle. Said fishing line 38 is wound around the device in typical use of the device.
[0029] FIG. 4 shows an alternate embodiment of the device comprising, inter alia, a frame 46 , ridges 40 , slots 42 and channels 44 . The device functions similar to any of the devices described herein and is further characterized in particular by said channel 44 . Said channel 44 provides a recess that fishing line lays in when wound around said frame 46 . When multiple fishing lines are wound around the frame 46 and each into adjacent slots 42 the channels 44 act to separate the fishing lines held in adjacent slots and channels and thereby aids in preventing tangling of the fishing lines.
[0030] The foregoing description conveys the best understanding of the objectives and advantages of the present invention. Different embodiments may be made of the inventive concept of this invention. It is to be understood that all matter disclosed herein is to be interpreted merely as illustrative, and not in a limiting sense.
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The disclosed device is an improved fishing line organizer that, among other features, provides a frame to wrap multiple and varying fishing lines and terminal tackle around for storage reducing tangling, preventing line kinks and maintaining each fishing line available for use. An embodiment of the device provides for construction of the device from a material (or materials) sufficiently buoyant to float when holding multiple fishing lines and terminal tackle.
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BACKGROUND
The present invention relates to a method and apparatus for economically ensuring the precise and reproducible automation of laboratory instrumentation. Particularly, the present invention relates to precision movement of laboratory instrumentation such as pipette tips in a manner that overcomes hysteresis inherent in gear-driven positioning mechanisms.
Automated laboratory handling systems require precise, repeatable movements to be made in a predictable manner, as the machinery used must meter out very small amounts of liquid and move within extremely small microplate wells with precision and accuracy. Laboratory pipetting systems, in particular, must be precisely controlled to move in the X, Y, and Z planes in order to position a bank of micropipette tips into the bottom of corresponding microplate wells. If a pipette tip is not inserted deeply enough into a well, a sufficient amount of the liquid may not be removed, potentially compromising the test or reaction. Further, if the pipette tip is inserted too deeply, damage could result to the pipette tip or delivery apparatus. Creating machinery with this type of predictability of movement is difficult due to the fact that numerous components comprising any mechanical system have a certain amount of imprecision in their fit with one another. When aggregated into a final assembly, an unpredictable amount of “play” in the final movement of the machinery occurs, often referred to as hysteresis. The presence of hysteresis indicates the inability to predict the exact location of a given component, which could result in broken instrumentation, reduced ability to uptake or adequately measure a given chemical in a chemical well, or contamination of a sample.
Reduction of hysteresis is often accomplished by utilizing highly precise components such as precision ground gears and precision servo motors, or by utilizing expensive position sensing systems. These methods leave much to be desired, as the components add substantial sums to the final cost of a system, and precision gears must be routinely replaced to account for the reduction in precision as friction takes its toll on the components. Further, although precision components are subject to a very small maximum value of error, the amount of error is not consistently the same. Therefore, these conventional methods of reducing hysteresis in mechanical devices result in high costs that do not necessarily guarantee precision or predictability.
Therefore, an efficient, reliable and low-cost hysteresis compensation device operable to reduce slop, play, or backlash associated with positioning laboratory equipment is desired.
SUMMARY
The present invention relates to economically ensuring the precise and reproducible automation of laboratory instrumentation. According to one embodiment of the present invention, an apparatus for reducing hysteresis in an automated laboratory device includes a liquid handling system that comprises a gear rack, a chassis assembly having at least one drive gear operable to engage the gear rack, and at least one hysteresis brake that engages the gear rack and resists rotation, thereby maintaining positive engagement of the drive train. This embodiment could further comprise a pipette assembly. Additionally, the embodiment could be arranged such that the hysteresis brake is positioned on the chassis assembly. Finally, the hysteresis brake in this embodiment could be a magnetic brake or an electromagnetic brake.
According to a second embodiment of the present invention, an apparatus for providing precision linear positioning of at least one laboratory pipette comprises a rack, a drive mechanism having a drive component operable to engage a linear rack, a magnetic brake engaging the rack operable to provide a force opposing movement of the drive mechanism. The second embodiment could further comprise a carriage assembly holding the drive mechanism and the magnetic brake. Further, the second embodiment could additionally comprise a pipette connected to the gear rack or the carriage assembly.
A third embodiment of the present invention could comprise an apparatus for increasing precision in liquid handling systems comprising a drive motor connected to a first gear, a rack in contact with the first gear, and a second gear equipped with a magnetic brake operable to provide a force opposing movement of the first gear. Additionally, this apparatus could further comprise software which can control the drive motor. Further, the software controlling the drive motor could adjust the work output of the motor so that the error margin of the apparatus is compensated when reversing direction of the drive motor.
A fourth embodiment of the present invention is a method for compensating hysteresis in laboratory liquid handling systems comprising the steps of providing a carriage with a drive gear that engages a linear gear rack; providing a motor in connection with the drive gear via a drive train; providing a hysteresis brake engaging the gear rack; adjusting the hysteresis brake so that resistance is provided to movement of the gear rack, causing the drive gear to remain in positive engagement with the gear rack; and engaging the motor so that the drive train is positively engaged, causing the drive gear to move the gear rack in a first direction. Additionally, this method could include the step of reversing the motor so that the drive gear moves the gear rack in a second direction. Further, after reversing the motor, the method could include the step of calculating an error margin caused by play in the drive train components involved in reversing direction of the gear rack. Finally, the method could include the step of compensating for the error margin that occurs by rotating the motor a calculated distance directly related to the error margin. The calculation of the error margin and compensation for the error margin could be accomplished by using a software program.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a perspective view of one embodiment of a pipette drive assembly with a hysteresis compensation mechanism.
FIG. 2 . shows an expanded perspective view of the pipette drive assembly of FIG. 1 .
FIG. 3 shows a perspective view of the magnetic hysteresis brake shown in FIG. 1 .
FIG. 4 shows an expanded view of the magnetic hysteresis brake of FIG. 3 .
FIG. 5 shows cross-sectional view of the interaction of the gear teeth of the gear rack and the drive gear of the pipette drive assembly of FIG. 1 .
FIG. 6 shows a block diagram of a method for compensating for hysteresis in a liquid handling system.
FIG. 7 shows a perspective view of a pipette drive system having multiple pipettes.
FIG. 8 shows a diagram of the basic force/velocity vectors involved when the pipette drive system with hysteresis compensation mechanism is in motion.
DESCRIPTION
The present invention relates to laboratory precision automation of instrumentation. More specifically, the invention relates to a laboratory pipetting system designed to operate in a manner such that positioning the automated pipette can be done predictably and reliably in an exact manner.
Turning now to FIG. 1 , a pipette drive assembly 10 according to one embodiment of the present invention comprises a gear rack 20 and a carriage assembly 30 engaging gear rack 20 such that carriage assembly 30 is operable to move relative to gear rack 20 . Gear rack 20 comprises a linear member having gear teeth 21 along one side and a ridge 22 on either side of the gear teeth. Carriage assembly 30 comprises chassis 35 , drive gear 40 , pass-thru holes 43 , and hysteresis brake 50 . Further, drive gear 40 engageably contacts gear rack 20 , and hysteresis brake 50 likewise engages gear rack 20 .
FIG. 2 shows an expanded view of pipette drive assembly 10 according to one embodiment of the present invention. As shown herein, the relationship between the gear teeth of drive gear assembly 40 and hysteresis brake 50 is more readily discernable. Drive gear 41 comprises multiple gear teeth which engageably mesh with the gear teeth 21 of gear rack 20 when carriage assembly 30 is engageably mounted to gear rack 20 . Carriage assembly 30 includes channels 33 that slidably engage the ridges 22 of gear rack 20 in a manner that properly orients the carriage assembly 30 with respect to the gear rack 20 and ensures that gear teeth 21 of gear rack 20 are a proper distance from the drive gear 41 to engage the teeth of the drive gear. Drive gear 41 includes a rectangular bore through its central axis designed to receive a drive shaft from a drive motor that provides torque to turn the drive gear 41 . Hysteresis gear 51 of hysteresis brake assembly 50 also has teeth which engageably mesh with the teeth 21 of gear rack 20 when carriage assembly 30 is engageably mounted to gear rack 20 . Therefore, drive gear assembly 40 , if rotatably attached to a motor or some other turning force is operable to move gear rack 20 in a linear fashion relative to carriage assembly 30 .
In one embodiment such as that shown in FIG. 7 , a drive train connects an electric motor to drive gear assembly 40 . The drive train comprise a motor, a drive shaft in the form of a square shaft extending through the center rectangular bore of drive gear assembly 40 . In operation, the motor is signaled to rotate in a particular direction, causing adjoining square drive shaft to likewise turn and rotate drive gear assembly 40 . By the means described above, the rotation of drive gear assembly 40 causes gear rack 20 to move relative to carriage assembly 30 . Any number of additional drive components could also be used to provide translation of a force from the electric motor to the carriage assembly or rack, causing movement. Each permutation of a drive train or drive mechanism would transfer a force into movement of the carriage assembly or rack. However, each connection point or component within the drive train offers an addition of mechanical play where hysteresis is introduced.
FIG. 3 shows a perspective view of hysteresis brake assembly 50 , a component of pipette drive assembly 10 shown in FIGS. 1 and 2 . FIG. 4 shows an expanded view of the magnetic hysteresis brake assembly 50 of FIG. 3 . As shown in FIGS. 3 and 4 , hysteresis brake assembly 50 comprises hysteresis gear 51 sandwiched between two mounting plates 52 . Each mounting plate includes an inner face 52 a directed toward the hysteresis gear 51 and an outer face 52 b directed away from the hysteresis gear 51 . A plurality of magnets 53 are positioned around the inner face 52 a of the mounting plates 52 . The hysteresis gear 51 includes a circular toothed gear portion 51 a positioned between two circular metal side plates 51 b . An attached axle 54 extends from the center of both sides of the circular toothed gear portion, such that rotation of the toothed gear portion 51 a results in rotation of the axle 54 . Each mounting plate 52 includes a bushing 52 c designed to support axle 54 and allow rotation of the axle relative to the mounting plates 52 . The mounting plates 52 are fixed to the carriage allow hysteresis brake assembly 50 to be rotatably mounted to carriage assembly 30 . In operation of the hysteresis brake, the magnets 52 on the mounting plates 52 are attracted to the metal side plates 51 b . This magnetic attraction acts to provide a force that resists rotation of the metal side plates 51 b and attached hysteresis gear 51 relative to the mounting plates 52 . Hysteresis brake assembly 50 is representative of several commercially available assemblies, of which Magnetic Technologies Ltd. of Oxford, Mass. is one manufacturer. Functionally, hysteresis brake assembly 50 operates to resist rotation of hysteresis gear 51 because rotation thereof causes internal magnets 53 to rotate through lines of magnetic force.
In operation, hysteresis gear 51 engages gear rack 20 and rotates axle 54 as gear rack 20 is moved relative to carriage assembly 30 . According to the orientation of FIG. 1 , as gear rack 20 is driven downward by counter-clockwise rotation of drive gear 40 , carriage assembly 30 remains static. During this action, hysteresis gear 51 of hysteresis brake assembly 50 rotates with axle 54 in a counter-clockwise fashion. Likewise, as gear rack 20 is driven upward, carriage assembly 30 remains static, and hysteresis gear 51 rotates clockwise with axle 54 . Because the magnets of the hysteresis brake assembly 51 resist rotation of the hysteresis gear, hysteresis gear assembly provides a braking force that resists movement of the gear rack 20 relative to the carriage assembly 30 . FIG. 8 provides a graphical display of the this braking force. In particular, FIG. 8 shows the gear rack 20 moving downward with respect to the chassis 35 at a given velocity (v) and with a driving force (F 1 ) applied by drive gear assembly 40 . As the gear rack 20 moves downward, the hysteresis brake 50 resists movement of the gear rack 20 relative to the chassis 35 , which results in an upward force (F 2 ) applied to the gear rack. When the drive gear stops rotating, the downward driving force (F 1 ) is removed from the gear rack. However, the upward force from the hysteresis brake remains. Accordingly, all components of the drive train remain completely engaged. If the upward force from the hysteresis brake 50 were absent, stopped movement of the gear rack would result in introduction of hysteresis back into the drive system, and that hysteresis would have to be compensated before the gear rack would start to move following the stop.
Because hysteresis brake 50 is operable to resist linear movement of gear rack 20 relative to carriage assembly 30 , a force greater than the resistance of hysteresis brake 50 must be applied to drive gear 41 in order to move gear rack 20 . Further, because the resistance of hysteresis brake 50 remains relatively constant, and because the resistance of hysteresis brake 50 is greater than external forces which might otherwise disengage the drive components of the drive train (e.g., gravity, momentum), the drive train remains in “positive engagement” even when the drive train comes to a stop. The term “positive engagement” as used herein refers to the state of the drive train where each of the drive train components remain sufficiently engaged such that incremental rotation of the motor will result of equivalent movement of the driven device with little or no mechanical play or hysteresis between the components. Therefore, when the drive train is in “positive engagement”, the teeth of drive gear 41 remain fully engaged and in positive contact with the teeth 21 of the gear rack 20 such that incremental rotation of the drive gear 41 results in equivalent movement of the gear rack 20 with no play between the teeth. Furthermore, when the drive train is once again powered after coming to a stop, the teeth of drive gear 41 remain in positive contact with the teeth of gear rack 20 , provided the rotation of drive gear 41 remains in the same direction as the direction of travel prior to coming to a stop. Additionally, the constant resistance of hysteresis brake 50 during a stop likewise ensures positive contact of all components of the drive train, not just the teeth of the drive gear and gear rack. Thus, because hysteresis is not introduced into the drive train during a stop, the play between drive train components is removed and the distance carriage assembly 30 is moved for every rotation of drive gear 41 remains constant (again, provided that the new direction of drive train travel is the same as the previous direction of drive train travel). Thus, rotation of drive gear 41 results in movement of gear rack 20 in a predictable and precise manner.
As set forth in the preceding paragraph, the resistance caused by hysteresis brake 50 retains positive engagement of the teeth of drive gear 41 with the gear teeth of gear rack 20 . Positive engagement remains while drive gear 41 turns in one direction and remains provided that the drive gear 41 stops and continues in the same direction as its previous direction. As discussed previously, this positive engagement remains because of the resistive force provided by the hysteresis brake. However, if the direction of the drive train is ever reversed, the hysteresis inherent in the drive train will be introduced into the system once again. An example of such hysteresis can be seen with respect to FIG. 5 . As shown in FIG. 5 , if the rotation of drive gear 41 is reversed from clockwise rotation to counter-clockwise rotation, the tooth 60 of drive gear 41 must rotate an additional distance 200 before the first tooth 70 of the gear rack 20 is disengaged and the second tooth 71 of gear rack 20 is fully engaged. Once drive gear tooth 60 moves the additional distance 200 and engages second gear rack tooth 71 positive engagement of drive train is again achieved. This additional distance 200 provides an example of the hysteresis that may be found between drive train components. Of course, similar hysteresis may be found between other drive train components, which results in an aggregated error margin or total hysteresis of the drive system. Fortunately, the total hysteresis of the drive system when the drive train switches direction can be calculated with reasonable accuracy. Because play between gear teeth is isolated to a predictable distance that occurs only upon a change in direction of the drive gear 41 , movement of carriage assembly can be precisely calculated and repeated, and hysteresis is eliminated or greatly reduced.
As set forth above, hysteresis brake 50 ensures positive engagement of each mechanical junction of any drive train components as long as the motor is turned in the same direction.
Further, positive engagement in one direction ensures that when motor direction is reversed, the distance motor turns before positive engagement returns is repeatable. This repeatable, predictable distance, referred to herein as the “error margin,” can be calculated through calibration of the machinery to determine the distance the motor must rotate before positive engagement is reinstated. Further, the error margin can be calibrated and compensated through a software program or other means. Since the error margin is predictable after it has been calculated, the computer program can instruct the motor driver to rotate the motor the distance related to the error margin when the direction of the drive train is reversed. This additional distance compensate for play between the drive train components when the direction of the drive train is reversed and positively engages the drive train in the reversed direction. Having compensated for the error margin, the motor may be rotated a distance sufficient to drive driven component a requested distance of travel when the drive train components are in positive engagement.
FIG. 6 is a flow chart delineating one embodiment of a method for compensating for the predictable error margin in moving gear rack 20 in relation to carriage assembly 30 . As can be seen from FIG. 6 , before the system is put in use, the error margin (or total hysteresis) is first calibrated, either manually or through the use of software, as noted by reference numeral 100 . This error margin reflects the amount of hysteresis between positive engagement of the drive train in one direction and positive engagement of the drive train in the opposite direction. With this error margin, the software calculates the amount of motor rotation required in order to switch from a condition of positive engagement of the drive train in one direction and positive engagement of the drive train in the opposite direction (i.e., the amount of motor rotation required before the gear rack 20 is moved when the drive train switches directions). Once the error margin is calculated, the system is ready for normal operation and is operable to allow for compensation of the error margin upon reversal of direction.
In normal operation, as indicated by reference numeral 102 in FIG. 6 , the software receives some input from the user of the system for the drive train to move a driven component (e.g., the gear rack and associated pipette) a requested direction of travel and distance of travel. As indicated by reference numeral 104 , the system then determines if the requested direction is the same as the previous direction of travel of the drive train. If the requested direction is the same direction as the previous direction, each turn of the motor results in the movement of gear rack 20 a given distance in relation to carriage assembly 30 , as noted by reference numeral 108 . As discussed above, precise determination of the number of rotations required for the drive motor to move the gear rack a desired distance is possible because the hysteresis brake maintains positive engagement of the drive train elements while the drive train is stopped. Therefore, when the requested direction is the same direction as the previous direction, any incremental rotation of the drive motor results in a related movement of the gear rack. On the other hand, as indicated by reference numeral 106 , if the requested direction is different from the previous direction of drive train movement, the calculated error margin is added to the rotations that would otherwise be required to move the gear rack the desired distance. Therefore, by recognizing whether the direction requested is the same or opposite from the previous direction requested, the software can determine whether the error margin must be calculated in the number of turns the motor is to make. If the direction requested is the same as the previous direction the motor was moving, no error margin should be included in the calculation of the number of turns the motor is to make. However, if the direction requested is not the same as the previous direction the motor was moving, the software will compensate for the error margin by turning the motor in the new direction the calibrated number of turns necessary for positive engagement in the new direction. Additionally, the program will calculate and execute the number of turns the motor must make in the new direction to move gear rack 20 the distance requested in relation to carriage assembly 30 . Thereafter, as indicated by reference numeral 110 the software resets the previous direction indicator to equal the most recently requested direction of travel. Finally, as indicated by reference numeral 112 , the program stops the motor and awaits further instruction on a desired direction of travel and distance of travel.
Turning now to FIG. 7 , one embodiment of a pipette system with a hysteresis compensation mechanism includes eight pipette drive assemblies 10 ganged together in a vertical position. Each pipette drive assembly includes a carriage assembly 30 fixed in position vertically and operably joined to a gear rack 20 such that the gear racks 20 may be moved vertically with respect to the carriage assemblies 30 . The gear racks 20 and associated carriage assemblies 30 are arranged in two separate rows, with the gear racks on the first row rotated 180° from the gear racks on the second row. A horizontal rack assembly 100 is operable to move the ganged pipette drive assemblies 10 in the horizontal plane. Attached to the bottom of each gear rack assembly 20 is a pipette connector 110 , designed for attachment to pipette tips and operable to pipette liquids. Each carriage assembly has an associated drive motor positioned upon the horizontal rack assembly. An elongated drive shaft 120 extends from each drive motor. Each elongated drive shaft 120 engages the drive gear assembly 40 on one of the carriages and extends through the pass-thru holes 43 of the other carriages in the row. In this embodiment, rotation of the drive gears 41 results in linear movement of gear racks 20 either upward or downward. Also, because each gear rack 20 and associated carriage assembly 30 is connected to a different motor and drive shaft 120 , each gear rack 20 and the pipette connected thereto may be moved independent of the other gear racks and pipettes.
Although the present invention has been described in considerable detail with reference to certain preferred versions thereof, other versions are possible. For example, a hysteresis brake as described above could be used in conjunction with a drive gear engaging another circular gear to prevent play and backlash. Further, gear rack 20 could be held stationary while carriage assembly 30 moves along gear rack 20 . Other embodiments of drive mechanisms engaging a rack are further possible. For example, rubber wheels could be used in place of gears. Additionally, means for resisting movement could comprise springs, elastic bands or rubber bands to resist movement of components and ensure positive engagement. As another example, any number of different pipette systems may be used with the Hysteresis Compensation System. For example, the system shown in FIG. 7 could include gear racks that are 180° opposed to the gear racks shown. As another example, any number of gear racks and associated pipettes could be used in any one system. Furthermore, the present invention is not limited to liquid handling systems, but may be used for any number of other automated laboratory devices where a motor and a drive train is used to automatically advance a driven component. Therefore, the spirit and scope of the appended claims should not be limited to the description of the preferred versions contained herein.
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A system and method for compensating for hysteresis in laboratory liquid handling apparatus. The system comprises a carriage holding a drive gear that meshes with and drives a gear rack. A hysteresis brake is also provided on the carriage and opposes the movement of the drive gear to provide continued positive engagement of the drive gear with the gear rack even when the system is static. When the direction of travel of the gear rack is reversed, the drive gear rotates an additional distance that compensates for the aggregate hysteresis found in the drive train.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
A combined indicator and barrier structure designed to be selectivity positioned between an upstanding vehicle blocking position and a collapsed orientation wherein the respective positions are intended to either block or allow entry of a vehicle into a given parking space.
2. Description of the Prior Art
Typically in almost all industrial, commercial and even residential areas, a number of specified spaces used for the parking of automobiles, trucks, etc. are reserved and designated for specific vehicles. Due to general overcrowding in highly populated areas, any indication of reserved parking is frequently ignored. This is true whether informative indicia, signs, or the like are placed on the surface of the parking area itself over which the vehicle is parked or in front of the space adjacent to or on a curb structure. This problem exists primarily because while signs, exhibits, etc. are generally clear and informative to the extent of indicating a reserved parking space, they do not perform the function of physically restraining or blocking the vehicle from entering the space. Accordingly, in overcrowded situations or relative emergencies, unauthorized vehicles will enter the space and operators of these vehicles will ignore any indication, exhibit or sign that the space is in fact reserved.
In order to overcome problems of this type, people have resorted to the use of portable barriers, frequently or commonly referred to as "saw horses." These barriers are temporarily positioned within the parking space until the authorized vehicle arrives. The operaor must then remove the barrier from the space and place it in some other designated location or within the vehicle itself. It is frequently inconvenient to find an additional location for storage of the portable barrier. In addition, such portable barriers do not serve their intended purpose since operators of unauthorized vehicles merely move the portable barrier themselves and park in the reserved space after repositioning, discarding or even stealing the portable barrier.
There is a need for a combination barrier and indicator assembly which is capable of informing unauthorized vehicles that a given parking space is in fact reserved while at the same time having a structure designed to prevent entry of the vehicle into the designated space. Such a preferred structure should be capable of being permanently affixed to the parking space so as to prevent theft or unauthorized removal of the barrier. Finally, the overall structure should be such that once permanently installed, the barrier is capable of being disposed in a stored attitude or orientation to allow entry of an authorized vehicle onto a designated space.
SUMMARY OF THE INVENTION
The present invention is directed towards a combined indicator and blocking assembly of the type designed to be substantially permanently affixed on the surface of a parking space within and distanced from the peripheral borders thereof. The assembly comprises a base means having a substantially elongated configuration and a substantially hollow interior portion extending along a majority of the length thereof. A head portion is movably mounted within the interior portion and is interconnected and supported on the base means by support means movably secured to both the head portion and the base means and structured to be collapsible. This collapsible structure serves to allow selective positioning of the head portion in an outwardly extended position substantially defined by disposition of the head portion in spaced relation above the base means. The head portion is further disposable into a collapsed position which is substantially defined by the head portion disposed on the interior of the base means within the hollow interior portion.
Further structural features of the invention include the provision of a lid means pivotally attached to the head portion and being disposable in an exposed position wherein indicia and like informative messages can be placed on the interior surface of the lid means. When the structure is disposed in the collapsed position, the lid means serves to effectively cover or close the hollow interior portion. When in the collapsed position, the overall structure of the assembly is such as to have a height and overall configuration sufficient to allow passage of a vehicle over the assembly so as to allow it to be parked in the space in which the indicator assembly is mounted.
Based on the above, it is obvious that when the head portion is disposed in its outwardly extended position, it serves as a barrier in that it is raised above the base means to a sufficient height to block the entrance of any vehicle into the parking space in which the assembly is mounted. In that the base is substantially fixedly or permanently secured within the space, theft or unauthorized removal of the indicator assembly is prevented. Further, locking means may be mounted in association with the head portion so as to prevent the positioning of the head portion into its collapsed position or alternately from providing access to the interior of the base portion and repositioning the head portion therein when it is desired to maintain the overall assembly into its collapsed position.
An important structural feature of the present invention comprises the existence of the support means designed to include a collapsible structure which includes a first and a second leg component. Correspondingly positioned ends of each leg component are slidably mounted within a track assembly of the head portion and also a track assembly within the base portion. Therefore, the correspondingly positioned opposite ends of each leg component slidably travel along a predetermined length of the head portion and base portion respectively while the head portion is being moved between the two outwardly extended position and collapsed position as set forth above. Further, the two leg components are cooperatively structured so as to be brought in a substantially mating or nesting relation with one another. Therefore in its compact or collapsible position, the entire assembly is of a limited dimension and configuration sufficient to allow passage of an automobile thereover and further to allow adequate room for the vehicle to park in the designated space.
BRIEF DESCRIPTION OF THE DRAWINGS
For a fuller understanding of the nature of the present invention, reference is made to the following detailed description taken in connection with the following drawings, in which:
FIG. 1 is an isometric view of the subject assembly in its outwardly extended position.
FIG. 2 is an isometric view of the structure of FIG. 1 in its collapsed position.
FIG. 3 is a sectional view taken along line 3--3 of FIG. 2 showing the interior structural details and components of the subject assembly.
FIG. 4 is a sectional view along line 4--4 of FIG. 1 wherein a closed position of the lid structure is represented in broken lines.
FIG. 5 is an isometric view in partial cutaway showing details of the track assembly and means of movably sliding leg components thereon.
FIG. 6 is an isometric view in partial cutaway showing structural details of another leg component of the present invention.
FIG. 7 is a sectional view along line 7--7 of FIG. 4.
FIG. 8 is a sectional view along line 8--8 of FIG. 1 showhing the end structure and anchoring structure of the subject assembly.
FIG. 9 is a bottom view in partial section along line 9--9 of FIG. 7 showing structural details of the movable attachment of one end of one leg component of the present invention.
FIG. 10 is a bottom view in partial section along line 10--10 of FIG. 7 showing structural details of the interconnection of the leg component to the track assembly and a stop structure mounted therein.
Like reference characters refer to like parts throughout the several views of the drawings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to FIGS. 1 and 2, the present invention is directed towards an indicator and barrier assembly generally indicated as 15 and structured to include a head portion generally indicated as 20, movably interconnected to a base means generally indicated as 70 by a support means generally indicated as 50. More specifically, the base means 70 includes an outer casing 72 which, in the preferred embodiment (FIG. 8), has a reinforcing fill structure 74 which may be fiberglass or like material disposed in supporting relation on the interior of the outer casing 72. The base means 70 includes a substantially hollow interior 71 extending along at least the majority of the length thereof and terminating in an upper opening 69 through which the entire head portion 20 may pass. As will be explained in greater detail hereinafter, the hollow interior portion 71 is specifically configured and dimensioned to house the support means 50, defined in part by a collapsible structure, as well as the head portion 20.
Further, the head portion 20 includes a lid structure 21 pivotally secured (FIG. 4), by an elongated tongue 34 rotatably mounted in curved channel 24, to the barrier platform 30. The lid portion 21 is further dimensioned and configured to serve as a cover when the entire assembly is disposed in its collapsed position on the interior 71 of the base means 70. This cover substantially corresponds to the interior dimensions of the opening 69 and substantially fits therein to close the inteior 71, as best shown in FIG. 2. Again with reference to FIG. 1, an inner surface 22 of the lid element 21 may have indicia or informative material 24 thereon which serves to indicate that the space in which the assembly is mounted is reserved.
With regard to the base means 70, end portions 73 serve to close off opposite ends of the hollow interior portion 71 and each further incorporates a tongue structure 100 (FIG. 8) being apertured to allow passage therethrough of a connector bolt 104. The bolt may be fit within an expandable socket or receiving channel 106 so as to securely anchor or affix the assembly, and in particular the base means 70, to the ground or surface 110 on which it rests.
With reference to FIG. 3, the base means includes elongated side portions 73' which also have the reinforcing filler 74 made of fiberglass or like material on the interior of casing wall 72. An important structural feature of the present invention is that the wall of the casing 72 may be made of a plastic and/or aluminum or like material which may be extruded into a single piece such that the casing 72, as seen in section in FIG. 3, includes a one-piece construction which extends into the interior of and defines at least in part the boundaries of the hollow interior portion 71. Again with reference to FIG. 3, the casing 72 also includes the platform 76 of the base means forming the lowermost channel or trough thereof. The support runners 79 are also integrally formed as part of the platform 76 so as to have an inwardly angular orientation as will be explained in greater detail hereinafter.
With reference to FIGS. 1, 2, 3 and 5 through 6, the assembly generally indicated at 15 is disposable between an outwardly extended position as represented in FIG. 1 and a collapsed position as shown in FIG. 2. It is obvious that in the outwardly extended position of FIG. 1, the head portion 20 serves as a barrier, along with the support means 50 so as to prevent vehicles from entering into a space in which the assembly 15 is mounted. However, when the assembly is disposed in its collapsed position (FIG. 2), the collective height of the assembly in such position is such as to allow passage of a vehicle thereover so as to not interrupt or serve as a barrier when an authorized vehicle is parked in the designated parking space. Referring to the support means 50, a collapsible structure at least partially defining the supporting means includes a first leg component 54 pivotally interconnected as at 56 to a second leg component 53 wherein the second leg component includes leg portions 52 and 52' disposed in spaced apart relation to one another in substantially parallel orientation on opposite sides of the first leg component 54. The pivot pin 56 serves to provide pivotal movement of the first and second leg components 54 and 53 respectively relative to one another and such relative movement causes positioning of the head portion between its outwardly extended position (FIG. 1) and its collaped position (FIG. 2) on the interior hollow portion 71 of base means 70.
With specific reference to FIGS. 5, 6, 7, 9 and 10, correspondingly positioned lower ends 54' and 53' of first and second leg components 54 and 53 respectively, are each movably mounted within the base means 70. This is accomplished through the provision of track means including a base track assembly 75 formed within the hollow interior portion 71 of the base means 70. As best shown in FIGS. 5 and 6, correspondingly positioned ends 54' and 53' are each interconnected to a slide plate 80 and 90 respectively which incudes a pivot pin 88 extended or connected at opposite ends to upstanding ears 84 wherein the pin 88 is secured by a conventional connector element 86. The ears 84 are disposed in spaced apart, substantially parallel relation to one another and fixed at their bottom to the respective slide plates 80 and 90. Slide plates 80 and 90 are disposed and structured to fit within runner channels 78 formed within opposite longitudinal sides of the length of hollow interior portion 71. Therefore, channels 78 effectively overlap the peripheral edges 89 of slide plates 80 and 90 as shown. Further, each of the slide plates 80 and 90 ride above or in spaced relation from the surface of the platform 76 and rest on and travel along runner elements 78' extending along the length and on the interior of the runner channel 78. The runner elements 78' are formed from a Teflon, Nylon or like relatively smooth and friction resistant material so as to allow for easy reciprocal movement of the slide plates thereon. It should be noted that runner elements 78' and runner channels 78 are angularly oriented to substantially slant downwardly and inwardly. This angular orientation allows displacement of dirt and debris when the respective slide plates travel therealong.
The track means further includes a head track assembly as shown in FIGS. 7 and 9. Slide plates 38 and 47 are fixedly attached to upstanding ears 56 and 56' respectively which in turn are pivotally connected to end 53" and 54" of the second and first leg components respectively (see FIGS. 9 and 10) wherein slide plate 38 has upstanding ear portions 56' secured thereto. End 53" and 54" of respective leg component 54 and 53 are pivotally secured (FIGS. 7 9 and 10) to the respective slide plates 38 and 47 which are slidably movable in a reciprocal fashion between stop members 64 and 42 and stop members 48 and 64' at the opposite ends of the head track assembly. A retaining spring 60 is interconnected between spring bracket 41 mounted on plate portion 40 by connectors 39 and wherein the opposite end of the spring 60 is connected to spring bracket 58. This spring 60 is disposed and structured to bias the leg ends 53" and 54" of the first leg component 54 and the second leg component 53 respectively towards one another. This in turn tends to bias the overall assembly into its outwardly extended position wherein the head portion 20 is raised above the base means 70. However, when a downward force is exerted on the head portion 20, both the leg component ends 53" and 54" move in opposite directions against the biasing force of spring 60 as indicated by directional arrows 61. While this extends the biasing spring 60, it also forces the head portion down into the interior of the hollow interior 71 of the base means 70.
Further with regard to the stop means described above with reference to FIGS. 5 and 6, slide plates 80 and 90 associated with ends 54' and 53' of the respective leg components are meant to travel a limited distance within the base track assembly 75. This distance is defined by intermediate stop members 82 and 92 disposed in interruptive relation to the path of travel of slide plates 80 and 90 respectively. Similarly, at the opposite ends of the base track assembly 75, tongue portions 100 are disposed at the extreme opposite ends of the base track assembly 75 and also are disposed in interruptive relation to the path of travel of slide plates 80 and 90. Therefore, as the head portion moves between its outwardly extended position and is collapsed position on the interior of the base means 70, the respective slide plates 80 and 90 move between opposite end stop members 100, also serving as the tongue portions for mounting of anchor connector 104, and the intermediate stop members 82 and 92 respectively.
Other structural features of the present invention include bearing pads 66 and 66' located at opposite ends of the track assembly on the undersurface of the barrier portion 30 of the head portion 20. These serve to pass beneath the slide plates 38 and 47 and to absorb a certain amount of the force or weight exerted thereon when the head portion is maintained on the hollow interior portion 71 of the base means 70. Similarly, bearing pads 101 are located at opposite ends of the base means on the interior thereof and substantially adjacent to the end portion 73' of the base means and beneath the mounting tongue 100 associated with the anchor connector element 104. These bearing pads pass beneath slide plates 80 and 90 associated with the base track assembly and serve to bear the weight of certain of the components when the assembly is in its collapsed position.
Further structural features include the specific structure of the first and second leg components 54 and 53 respectively wherein the first leg component 54 is formed from a single one-piece construction having spaced apart but integrally secured leg portions 93 and 91 interconnected by span 92. However, the second leg component (see FIGS. 3 and 6) includes spaced apart leg portions 96 and 97 disposed substantially parallel to one another but not having an interconnectng span similar to span 92 of the first leg component 54. Support flanges 98 extend outwardly from the outer longitudinal surfaces of the leg portions 96 and 97 of the second leg component 53. As best shown in FIG. 3, the spaced apart orientation of the leg components 96 and 97 and their spaced apart distance allows the leg portions 93 and 91 of the first leg component 54 to fit therebetween and thereby establish a nesting relation between the first and second leg components on the interior of the base means within the hollow interior portion 71. This nesting alignment allows for compact disposition of the structural components of the subject assembly and further allows for an overall, collective height being such to allow a vehicle to pass thereover when the overall assembly (FIG. 2) is disposed in its collapsed position.
It is to be understood therefore that the following claims are intended to cover all of the generic features of the invention herein described, and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.
Now that the invention has been described,
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A combined indicator and blocking assembly structured for mounting on the ground or surface within a designated parking space wherein the assembly includes a head portion selectively positionable upwardly from a base mounted on the surface of the parking space to the extent that the head portion and attendant supporting structure serves as a barrier in preventing unauthorized vehicles to enter the parking space. A sign or other indicator structure may be mounted on the interior surface of a lid element which is attached to the head portion and provided with proper informative indicia. The base is structured to house the head portion therein in a compact assembly when not in use, wherein the assembly has a height sufficient to pass underneath authorized vehicles parking in the space.
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FIELD OF THE INVENTION
The present invention relates to the production of catalysts such as can be used, for example, in the manufacture of isoprene from isobutylene and formaldehyde, and more particularly to a method of preparing a calcium phosphate catalyst for use in decomposing 1,3-dioxanes and, in particular, 4,4-dimethyl-1,3-dioxane (hereinafter referred to as DMD) into isoprene, as well as in alcohol dehydration reactions.
BACKGROUND OF THE INVENTION
It has been known in the prior art to prepare phosphates of metals of Group II of the Periodic Table, usable as catalysts for selective cleavage of C--O--bonds in organic compounds, and, specifically, for converting 4,4-dimethyl-1,3-dioxane into isoprene, as well as for dehydration of alcohols, by precipitating normal phosphates of Group II metals from aqueous solutions of their salts taken in conjunction with water-soluble salts of phosphoric acid, followed by separating the precipitate, washing the paste obtained, and shaping it into catalyst granules (cf. U.S. Pat. No. 3,872,216).
Catalysts prepared by the above technique, however, are characterized by low selectivity (78-82 mole %), low activity resulting in low DMD space velocity (0.7 h -1 ), and high operating temperatures (ca. 375° C.).
Selectivity is defined as the ratio of the amount in moles of isoprene formed to the amount in moles of DMD converted.
Selectivity is quantitatively dependent upon catalyst composition and structure, as well as upon the process conditions under which the catalyst operates.
Increased selectivity will lead to reduced stockfeed (DMD) consumption rates per unit of finished product, thus per ton of isoprene. The relatively low selectivity of the catalyst obtainable by the aforesaid prior technique would result in high feedstock consumption rates in isoprene production, varying between ca. 2.10 and 2.25 kg DMD per kg of isoprene.
The activity of calcium phosphate catalysts is dependent upon their acidity which is determined by the number and efficiency of the active centres and can be characterized by the DMD conversion degree.
DMD conversion is defined as the ratio of the amount of DMD converted to that of DMD used, expressed in percent.
There is also known in the art to produce calcium phosphate catalysts by reacting a calcium salt with a phosphoric acid salt in aqueous ammonia; followed by washing and drying the resulting precipitate and heat treatment with the use of super-heated steam or a mixture of steam and air at high temperatures (cf. U.S. Pat. No. 3,846,338).
The catalysts obtainable by this prior art technique are relatively low in activity.
Furthermore, calcium phosphate catalysts prepared by the aforesaid technique have a low efficiency (0.3 to 0.4 ton/h of isoprene per cubic meter of catalyst).
The efficiency of a catalyst depends on its activity and selectivity, as well as on the feedstock space velocity.
In the prior technique, heat treatment is carried out at high temperatures, which involves overheating of the heat carrier to temperatures as high as 650° to 800° C. and high process power inputs, as well as special heat-resistant materials for reactors adapted to produce the catalyst.
One further disadvantage associated with the catalyst obtainable by the aforesaid technique is a relatively short service life (250 hours).
The catalyst life depends on many factors including catalyst composition and structure, catalyst activity, operating temperatures, and coke deposition. Coke deposition is understood to denote coke deposits on the catalyst in the process of DMD decomposition. It is determinable as the ratio of the amount in moles of coke deposited to the amount in moles of DMD converted, expressed in percent.
In spite of the advantages inherent in the prior art technique for preparation of calcium phosphate catalysts, no commercial process based on said technique has been developed so far, since there is no catalyst as yet, with selectivity and stability such as to justify a commercial process.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a method for preparing a high-activity calcium phosphate catalyst.
Another object of this invention is to provide a method for preparing a high-efficiency calcium phosphate catalyst.
A further object of the present invention is to provide a method of preparing a high-selectivity calcium phosphate catalyst.
A still further object of the present invention is to provide a method of preparing a calcium phosphate catalyst, such as would enable the obtaining of catalysts with a long service life and low coke deposition during the service thereof.
With these and other objects in view, there is provided a method of preparing a calcium phosphate catalyst, which comprises reacting calcium salts with phosphoric acid salts in aqueous ammonia, separating the resulting precipitate from the reaction mixture, suitably shaping said precipitate, drying it, and subjecting it to heat treatment at high temperatures in the presence of steam, wherein, according to the invention, heat treatment is performed within a temperature range of 450° to 600° C. in the presence of steam mixed with phosphoric acid or an aldehyde, or an oxygen-containing heterocyclic compound, or an alcohol, or a diene hydrocarbon, or steam mixed with an inert gas or air and phosphoric acid, or steam mixed with an inert gas and an aldehyde, or an oxygen-containing heterocyclic compound, or an alcohol, or a diene hydrocarbon.
Formaldehyde and acetaldehyde are preferable to be used as said aldehyde.
It is advisable that as said oxygen-containing heterocyclic compound use is made of methyl dihydropyrane or methylene tetrahydropyrane.
The suitable alcohols are trimethyl carbinol and isopropenyl ethyl carbinol.
The suitable diene hydrocarbons are isoprene or piperylene.
It is also advisable that the reaction of calcium salts with phosphoric acid salts in an aqueous ammonia be carried out with the starting reactants taken in the molar ratio of 1.5:1.
The preferred embodiment is for the reaction of calcium salts with phosphoric acid salts in aqueous ammonia to be effected with the starting reactants taken in a molar ratio within 1.5:1 to 5.0:1 and for the reaction mixture obtained to be treated with a phosphoric acid solution to a pH of from 5.0 to 7.0.
It is desirable to treat the reaction mixture with a phosphoric acid solution to a pH of from 5.5 to 6.0.
According to the herein-proposed method, a catalyst can be obtained featuring high selectivity (86.0 to 87.5 mole %), high activity (96.0-97.0%), and low coke deposition (below 1 mole %).
The aforesaid and other objects and features of the present invention are set forth in the appended claims, and the present invention will be more fully apparent from the detailed description of its embodiments presented hereinunder.
DETAILED DESCRIPTION OF THE EMBODIMENTS
The proposed method of preparing a calcium phosphate catalyst can be realized as follows.
The starting reactants to be used are solutions of calcium salts, e.g. calcium chloride, and phosphoric acid salts, e.g. diammonium phosphate, disodium phosphate, etc. A suitable amount of agua ammonia is added to the phosphoric acid salt solution prior to reacting it with the calcium salt solution for pH control of the medium.
The calcium salt and phosphoric acid salt solutions are gradually introduced into a vessel fitted with a stirrer, while continuously stirring the slurry being formed. The reaction is carried out with the calcium salt and phosphoric acid salt taken in the molar ratio of 1.5:1. However, the reaction is realizable with the starting reactants having a molar ratio anywhere within the range of 1.5:1 to 5.0:1, preferably 2.5:1. In cases such as these, the reaction mixture is to be treated with a phosphoric acid solution to a pH of from 5.0 to 7.0, preferably 5.5 to 6.0.
The above ranges of molar ratios of calcium salts to phosphoric acid salts and pH values of the reaction medium are consistent with obtaining a calcium phosphate catalyst of desired structure and composition.
The resulting precipitate is separated by filtration or any other known method, washed with distilled water to remove calcium salt anions, shaped into granules by a conventional technique, and dried at a temperature between 110° and 140° C., thus obtaining a raw calcium phosphate which is then loaded for further treatment into a reactor.
The reactor is a quartz tube measuring 20 to 26 mm in diameter. The reactor is placed into an electrically heated oven for the catalyst enclosed in the reactor to be subjected to heat treatment at a temperature within 450° to 600° C., using steam with an addition of phosphoric acid or an organic compound.
The organic compounds that may be used as additions to steam include formaldehyde, acetaldehyde, methyl dihydropyrane (MDHP), methylene tetrahydropyrane (MTHP), trimethyl carbinol (TMC), isopropenyl ethyl carbinol (IPEA), isoprene, and piperylene.
Where a calcium phosphate catalyst is obtained without pretreatment of the reaction mixture with phosphoric acid solution, heat treatment is preferably performed at 450° C.
However, where the method of calcium phosphate catalyst preparation comprises the step of treating the slurry with phosphoric acid to control the pH values of the reaction mixture to within 5.0 to 7.0, the heat treatment temperature should preferably be 500° C.
Heat treatment can also be carried out using steam mixed with an inert gas such as nitrogen, argon, etc., and with air (when phosphoric acid is added to the steam).
Steam is fed in at a space velocity of 1.0 to 2.0 h -1 .
The feed rate of phosphoric acid used for catalyst heat treatment is 0.05 to 0.25 g/h per kg of catalyst.
Heat treatment times are within 2 to 50 hours, preferably between 20 and 30 hours. Space velocity for the organic compounds used is 0.7 to 1.5 h -1 , preferably 1.0 h -1 .
After the catalyst has been treated wih steam mixed with any one of the above-listed organic compounds or with steam mixed with an inert gas and any one of the above compounds in order to burn out the coke deposited on the catalyst surface, the catalyst is now subjected to regeneration by a mixture of steam and air at temperatures between 450° and 600° C., preferably between 500° and 550° C. Space velocity for air ranges from 500 to 700 h -1 , and for steam, from 1.0 to 2.0 h -1 .
The calcium phosphate catalyst thus obtained has the following characteristics: DMD conversion at the level of 96 to 97%, selectivity 86.0 to 87.5 mole %, coke deposition below 1%.
The following typical examples will further illustrate certain aspects of the present invention, deliniating more clearly the features and advantages specific to it.
EXAMPLE 1
The starting reactants used for catalyst preparation are 1.78 l of a calcium chloride solution containing 101.892 g of salt per 1 l of the solution and 1.608 l of a diammonium phosphate solution containing 51.02 g of salt per 1 l of the solution. An ammonia solution with a concentration of 152.15 g/l is added to the diammonium phosphate solution on the basis of having 2.33 moles of ammonia per 1 mole of diammonium phosphate immediately prior to the reaction.
The calcium chloride and diammonium phosphate solutions are gradually poured into a vessel fitted with a stirrer. The pouring procedure continues for 2 hours, the resulting slurry being continuously stirred all the while. Reaction is carried out with the solutions introduced kept practically in a constant ratio to ensure a calcium salt to phosphoric acid salt molar ratio of 2.5:1 and the slurry having a pH value within 9.0±0.05. The resultant slurry is treated with 150 ml of phosphoric acid concentrated to 281.26 g/l in order to reduce the pH value to 5.75. The resulting precipitate is separated from the reaction medium by filtration, washed with distilled water to remove chlorine ions, shaped into granules, and dried at ca. 120° C. The raw calcium phosphate thus obtained is loaded, in an amount of 24 cm 3 , into a reactor which has the form of a quartz tube measuring 20 to 26 mm in diameter. The reactor is placed into an electrically heated oven. Steam mixed with phosphoric acid added on the basis of 0.2 g/h acid per 1 kg of catalyst is passed through the catalyst at 400° C. for 30 hours.
The resulting catalyst is test run in a DMD decomposition reaction in an atmosphere of steam. The DMD decomposition process is carried out at atmospheric pressure and a mean temperature of 320° C. for the duration of 2 hours.
DMD is fed in at the rate of 24 cm 3 /h, and water at 48 cm 3 /h, which gives a DMD space velocity of 1.0 h -1 and a DMD to steam dilution ratio of 1:2.
The contact cycle is followed up by a regeneration cycle which comprises burning out the coke deposited on the catalyst and is to be repeated after every two hours of catalyst operation.
The regeneration cycle is carried out at 425° C., using 48 cm 3 /h of water and 16,800 cm 3 /h of air. The catalyst is analyzed using gas-liquid chromatography techniques. The quantity of coke deposited is determined by a conventional method.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 2
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is performed as described in Example 1, at 500° C.
The resulting catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 3
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1. Heat treatment of the raw calcium phosphate is performed as described in Example 1, at 600° C.
The resulting catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 4
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1. Heat treatment of the raw calcium phosphate is carried out at 500° C., using steam mixed with phosphoric acid added on the basis of 0.2 g/h of phosphoric acid per 1 kg catalyst and with nitrogen taken in an amount of 4800 cm 3 per hour, a gas space velocity being 200 h -1 .
The resulting catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 5
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1. Heat treatment of the raw calcium phosphate is carried out at 500° C., using steam mixed with phosphoric acid added on the basis of 0.2 g/h phosphoric acid per 1 kg catalyst and with air taken in an amount of 4800 cm 3 /h, the space velocity of air being 200 h -1 .
The resulting catalyst is test run as descrined in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 6
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1. Heat treatment of the raw calcium phosphate is carried out at 450° C., using steam with an addition of 7% by weight of aqueous solution of formaldehyde for the duration of 4 hours.
Steam space velocity (accounting for the 7% addition of the aqueous solution of formaldehyde) is 2.0 h -1 .
The resultant catalyst is subjected, prior to the test run, to a procedure for burning out the coke deposited on its surface, said procedure being carried out at 500° C., using 48 cm 3 /h of water and 16,800 cm 3 /h of air.
The catalyst thus prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 7
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is performed as described in Example 6, at 500° C.
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 8
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is performed as described in Example 6, at 600° C.
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 9
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C., using steam with an addition of 5% by weight of acetaldehyde.
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 10
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 400° C., using steam mixed with 7% by weight of aqueous solution of formaldehyde and with nitrogen in an amount of 4800 cm 3 /h, the total corresponding to a gas space velocity 200 h -1 and the heat treatment procedure continuing for 4 hours.
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 11
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C., using steam with an addition of 31.4% by weight of MDHP, for the duration of 2 hours. MDHP space velocity is 1.0 h -1 , steam space velocity, 2.0 h -1 .
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 12
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C., using steam with an addition of 31.6% by weight of MTHP, for the duration of 2 hours. MTHP space velocity us 1.0 h -1 , steam space velocity, 2.0 h -1 . The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 13
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described in Example 11, at 400° C.
The resultant catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 14
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described in Example 11, at 600° C.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 15
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. for 2 hours, using steam mixed with 31.4% by weight of MDHP and with nitrogen in an amount of 4800 cm 3 per hour, the total corresponding to a gas space velocity of 200 h -1 .
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 16
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. for the duration of 2 hours, using steam mixed with 28.3% by weight of trimethyl carbinol (TMC). TMC space velocity is 1.0 h -1 , that of steam, 2.0 h -1 (on the liquid basis).
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 17
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. for the duration of 2 hours, using steam mixed with 30.9% by weight of isopropenyl ethyl carbinol (IPEC). IPEC space velocity is 1.0 h -1 , that of steam, 2.0 h -1 (on the liquid basis).
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 18
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described above in Example 16, at 400° C.
The resultant catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 19
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described above in Example 16, at 600° C.
The resultant catalyst is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 20
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. for the duration of 6 hours, using steam mixed with 28.3% by weight TMC and that of nitrogen in an amount of 4800 cm 3 per hour, the total corresponding to a gas space velocity of 200 h -1 .
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 21
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 450° C. during 9 hours, using steam with an addition of 25.4% by weight of isoprene. Isoprene space velocity is 1.0 h -1 , that of steam, 2.0 h -1 (on the liquid basis).
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 22
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described above in Example 21, at 500° C.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 23
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate and the coke deposit burning-out procedure that follows are carried out as described above in Example 21, at 600° C.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 24
The procedure used to prepare the calcium phsophate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. during 9 hours, using steam mixed with 25.4% by weight of isoprene and with nitrogen taken in an amount of 4800 cm 3 per hour, the total corresponding to gas space velocity of 200 h -1 .
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 25
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 1.
Heat treatment of the raw calcium phosphate is carried out at 500° C. for the duration of 9 hours, using steam mixed with 25.3% by weight of piperylene. Piperylene space velocity is 1.0 h -1 , that of steam, 2.0 h -1 .
The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 1.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 26
The starting reactants used for catalyst preparation are 1.18 l of a calcium chloride solution containing 99.8 g of calcium chloride in 1 l of solution and 2.0 l of a disodium phosphate solution containing 50.21 g of salt in 1 l of solution. An ammonia solution with a concentration of 130 g/l is added to the disodium phosphate solution on the basis of having 1.3 moles of ammonia per 1 mole of disodium phosphate immediately prior to the reaction.
The calcium chloride and disodium phosphate solutions are gradually poured into a vessel fitted with a stirrer. The pouring procedure continues for 2 hours, the resulting slurry being continuously stirred all the while. Reaction is carried out with the solutions introduced kept in a constant volume ratio to ensure a calcium chloride to disodium phosphate molar ratio of 1.5:1 and the slurry having a pH value of 9.0±0.05. The resulting precipitate is separated by filtration, washed with distilled water to remove chlorine ions, shaped into granules, and dried at a temperature of 120° C. Heat treatment of the raw calcium phosphate is performed as described in EXample 1, using a temperature of 500° C.
The catalyst so prepared is test run as described in Example 1, using a contact temperature of 375° C.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 27
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 26.
Heat treatment of the raw calcium phosphate is carried out as described in Example 1, using a temperature of 400° C.
The catalyst so prepared is test run as described in Example 26.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 28
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 26.
Heat treatment of the raw calcium phosphate is performed as described in Example 6. The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 26.
The catalyst test results are presented hereinunder in Table 1.
EXAMPLE 29
The procedure used to prepare the calcium phosphate catalyst is the same as described in Example 26.
Heat treatment of the raw calcium phosphate is carried out as described in Example 13. The resultant catalyst is subjected, prior to the test run, to the procedure for burning out the coke deposited on its surface as described above in Example 6.
The catalyst so prepared is test run as described in Example 26.
The catalyst test results are presented hereinunder in Table 1.
In describing the above examples of embodiments of the present invention, a limited terminology has been employed for greater clarity. it will be understood, however, that the present invention is by no means limited by the terminology adopted herein and that each of the terms used covers all equivalent elements such as may serve the same function and be used to solve the same problems.
Although the present invention has been described herein with reference to the preferred typical embodiments thereof, it will be apparent to those skilled in the art that there may be minor modifications made in the procedures comprised in the inventive method of calcium phosphate catalyst preparation without departing from the spirit of the invention.
All such modifications and variations are contemplated to be embraced in the spirit and scope of the invention, as defined in the appended claims.
TABLE 1______________________________________RESULTS OF CATALYST TESTINGIN DMD DECOMPOSITION RUNSOperating temperature: 320° C.DMD volume flow rate: 1 h.sup.-1DMD: H.sub.2 O dilution ratio: 1:2Catalysts Characteristic valuesas per DMD conversion, Selectivity, Coke formation,Example Nos. % mole % mole %1 2 3 4______________________________________ 1 97.5 86.9 1.53 2 97.2 87.2 0.84 3 96.0 87.5 0.56 4 97.4 86.9 1.04 5 97.3 86.8 1.09 6 97.5 87.0 1.50 7 97.3 87.5 0.54 8 96.0 87.3 0.47 9 97.4 87.3 0.6110 97.4 86.9 1.5811 97.2 87.3 0.6512 97.2 87.2 0.6913 97.4 86.9 1.6014 95.9 87.5 0.4815 97.3 87.2 0.8016 97.1 87.0 0.7017 97.0 87.2 0.6818 97.5 86.8 1.7019 95.8 87.4 0.4620 97.1 86.9 0.7421 97.4 86.9 1.6122 96.8 87.1 0.6323 95.9 87.5 0.5624 97.0 87.0 0.7225 96.9 87.3 0.6626 94.7 87.2 0.5927 95.2 86.4 1.7828 95.0 86.6 0.5229 94.8 87.0 0.5030 94.7 86.8 0.5231 94.9 86.6 0.58______________________________________
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Disclosed is a method of preparing a calcium phosphate catalyst, which comprises reacting a calcium salt with a phosphoric acid salt in aqueous ammonia, separating the precipitate resulting from the reaction mixture thus obtained, suitably shaping said precipitate, drying it, and subjecting it to heat treatment within a temperature range of 450° to 600° C. in the presence of steam mixed with at least one of the components selected from the group consisting of an inert gas, air, phosphoric an acid, aldehyde, an oxygen-containing heterocyclic compound, an alcohol, and a diene hydrocarbon.
The reaction of calcium salts with phosphoric acid salts in aqueous ammonia is effected with the starting reactants taken in the molar ratio of 1.5:1 if no phosphoric acid treatment is used, or with the starting reactants in a molar ratio within the range of 1.5:1 to 5.0:1 if the reaction mixture is treated with a phosphoric acid solution to a pH of from 5.0 to 7.0.
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CROSS-REFERENCE TO RELATED APPLICATION
This is a continuation-in-part of U.S. patent application Ser. No. 12/379,392 filed on Feb. 20, 2009 now abandoned.
BACKGROUND OF THE INVENTION AND RELATED ART STATEMENT
The present invention relates to an electric power converter that generates a DC output from a DC power supply or from an AC power supply. Specifically, the present invention relates to the soft switching function of an electric power converter capable of conducting two-way operations.
The circuit of a conventional electric power converter capable of conducting two-way operations is disclosed in the following Patent Document 1: Japanese Unexamined Patent Application Publication No. 2004-147475. The conventional circuit disclosed in the Patent Document 1 is shown in FIG. 3A .
The conventional circuit shown in FIG. 3A is described in connection with a single-phase AC power supply. The conventional circuit consists of a rectifier circuit including a diode bridge circuit having diodes 2 through 5 , and a chopper circuit including reactor 21 , diode 6 , and switching device 15 .
As switching device 15 is turned on, AC power supply 1 is short-circuited via the diode bridge circuit and reactor 21 , energy is stored in reactor 21 , and an AC input current increases.
Then, as switching device 15 is turned off, the energy stored in reactor 21 is fed via diode 6 to capacitor 33 and load 34 , which constitute a DC output.
By controlling the ON and OFF of switching device 15 , a rectified AC voltage (DC voltage) is converted to an arbitrary DC voltage. A soft switching circuit for the chopper circuit is configured by capacitor 31 , diodes 7 , 9 , 10 , voltage clamping element 30 , transformer 22 and switching device 17 .
FIG. 3B is a wave chart describing the operations of the circuit shown in FIG. 3A .
As switching device 17 is turned on, the current that circulates, during a period t 1 , from reactor 21 to reactor 21 via diode 6 , capacitor 33 , diode bridge circuit 40 , and AC power supply 1 gradually changes the current path so as to circulate, due to the influence of the leakage inductance of transformer 22 , from reactor 21 to reactor 21 via diode 7 , primary winding 22 a of transformer 22 , switching device 17 , diode bridge circuit 40 , and AC power supply 1 . Since the current that flows through switching device 17 increases gradually from zero during the commutation described above, switching device 17 performs soft switching at the turn-ON thereof.
Then, a period t 2 starts. During the period t 2 , the current flowing through switching device 17 becomes equal to the current flowing through reactor 21 and diode 6 becomes OFF. Since the current flowing through diode 6 decreases gradually to zero, the surge voltage and the reverse recovery losses caused by the reverse recovery are reduced. At the same time, the electric charge stored in capacitor 31 (or in the parasitic capacitance of switching device 15 ) is discharged via a path connecting capacitor 31 , diode 7 , primary winding 22 a of transformer 22 , switching device 17 , and capacitor 31 . The electric charge stored in capacitor 31 is regenerated to the output side via secondary winding 22 b of transformer 22 and diode 10 .
By turning on switching device 15 after the voltage thereof lowers to zero in a period t 3 , a difference current, which is the difference between the current flowing through primary winding 22 a of transformer 22 and the current flowing through reactor 21 , flows through switching device 15 . Since the difference current that flows through switching device 15 initially flows through parasitic diode 12 , the current that flows through switching device 15 increases gradually from a negative value. Therefore, switching device 15 performs soft switching at the state of the turn-ON thereof.
Then, the current that has been circulating from reactor 21 to reactor 21 via diode 7 , primary winding 22 a of transformer 22 , switching device 17 , diode bridge circuit 40 , and AC power supply 1 gradually changes so as to circulate from reactor 21 to reactor 21 via switching device 15 , diode bridge circuit 40 , and AC power supply 1 . At the same time, the energy stored in the leakage inductance of transformer 22 is fed to the output side via secondary winding 22 b of transformer 22 and diode 10 . The current that flows through switching device 17 decreases gradually to zero. Since switching device 17 is brought into the OFF-state thereof after the current that flows through switching device 17 reaches zero, switching device 17 performs soft switching at the state of the turn-OFF thereof.
When switching device 15 is turned off, the voltage of switching device 15 rises gradually due to the current flowing through capacitor 31 . Therefore, the turn-OFF losses are reduced. Thus, switching devices 15 and 17 perform soft switching.
In a period t 4 , a reset voltage equal to the voltage clamped by voltage clamping element 30 is caused across primary winding 22 a of transformer 22 . A voltage, which is as high as the product of the reset voltage and the winding ratio of transformer 22 , is generated across secondary winding 22 b of transformer 22 . The sum of the DC output voltage and the voltage across secondary winding 22 b of transformer 22 is applied to diode 10 . By setting the clamping voltage of voltage clamping element 30 to be low, the voltage applied to diode 10 is reduced.
FIG. 4A is a circuit diagram of another conventional electric power converter disclosed in the Patent Document 1.
In FIG. 4A , a rectifier circuit is configured by reactor 21 , diodes 2 through 5 , and switching devices 15 and 16 . Switching device 15 and capacitor 31 are connected in parallel to diode 3 . Switching device 16 and capacitor 32 are connected in parallel to diode 5 . AC power supply 1 is connected between the series connection point of diodes 2 and 3 and the series connection point of diodes 4 and 5 via reactor 21 . Capacitor 33 and load 34 are connected between the DC terminals of the diode bridge circuit.
The parasitic diode of switching device 15 may be used in substitution for diode 3 . The parasitic diode of switching device 16 may be used in substitution for diode 5 . The soft switching circuit for the rectifier circuit is configured by diodes 7 through 10 , switching device 17 , transformer 20 , and voltage clamping element 30 .
FIG. 4B is a wave chart describing the operations of the circuit shown in FIG. 4A .
As switching device 15 is turned on when the AC power supply voltage is positive, the AC input current, circulating from AC power supply 1 to AC power supply 1 via reactor 21 , switching device 15 , and diode 5 , increases while storing energy in reactor 21 . Then, as switching device 15 is turned off, the energy stored in reactor 21 is fed to the DC output side via a path connecting reactor 21 , diode 2 , capacitor 33 , diode 5 , AC power supply 1 and reactor 21 . Therefore, it is possible to convert an AC power supply voltage to an arbitrary DC voltage by controlling the ON and OFF of switching device 15 when the AC power supply voltage is positive. In the same manner, it is possible to convert an AC power supply voltage to an arbitrary DC voltage by controlling the ON and OFF of switching device 16 when the AC power supply voltage is negative.
In FIG. 4A , diodes 7 and 8 are disposed in substitution for diode 7 in FIG. 3A . In FIG. 4A , diode 8 works for diode 7 in FIG. 3A , when the AC power supply voltage is positive. Diode 7 works for diode 7 in FIG. 3A , when the AC power supply voltage is negative. Since switching device 15 is turned on and off when the AC power supply voltage is positive, the electric charge stored in capacitor 31 is regenerated to the DC output side through the operations similar to the operations conducted in the circuit shown in FIG. 3A . Since a current always flows through diode 5 when the AC power supply voltage is positive, capacitor 32 stores no electric charge.
When the AC power supply voltage is negative, the electric charge stored in capacitor 32 is regenerated to the load side through the operations similar to the operations conducted in the circuit shown in FIG. 3A . Therefore, the circuit shown in FIG. 4A conducts operations similar to the operations conducted by the circuit shown in FIG. 3A . Switching devices 15 , 16 , and 17 and diodes 2 and 4 conduct soft switching. Since the sum of the DC output voltage and the secondary winding voltage of transformer 22 is applied to diode 10 in the circuit shown in FIG. 4A in the same manner as in FIG. 3A , the voltage applied to diode 10 is reduced by setting the clamping voltage of voltage clamping element 30 to be low.
For performing two-way electric power conversion, Patent Document 2: Japanese Unexamined Patent Application Publication No. Sho 64 (1989)-064557 discloses a combination of a buck chopper and a boost chopper. For the boost chopper, a boost chopper including an auxiliary chopper and disclosed in Patent Document 3: Japanese Unexamined Patent Application Publication No. Hei 05 (1993)-328714 may be used. However, the boost chopper including an auxiliary chopper and disclosed in the Patent Document 3 includes many circuit component parts. Moreover, the boost chopper including an auxiliary chopper and disclosed in the Patent Document 3 is large in size and expensive.
For realizing two-way electric power conversion in the conventional circuit shown in FIG. 3A , it is necessary to replace diode 6 by a switching device. For realizing two-way electric power conversion in the conventional circuit shown in FIG. 4A , it is necessary to replace diodes 2 and 4 by switching devices. The replacing switching device or the replacing switching devices can not perform soft switching.
In view of the foregoing, it would be desirable to obviate the problems described above, and to provide a two-way electric power converter that facilitates conducting soft switching operations inexpensively with low conversion losses.
Further objects and advantages of the invention will be apparent from the following description of the invention.
SUMMARY OF THE INVENTION
According to the subject matter of a first aspect of the invention, there is provided an electric power converter including:
a first series circuit including a reactor and a first switching device, the first series circuit being connected between DC input terminals;
a second series circuit including a second switching device and an output capacitor including a terminal working for a DC output terminal, the second series circuit being connected in parallel to the first switching device;
a load connected in parallel to the output capacitor;
a third series circuit including a first capacitor, a first diode, a primary winding of a transformer, and a third switching device, the third series circuit being connected in parallel to the first switching device;
a fourth series circuit including a second capacitor, a fourth switching device, the primary winding of the transformer, and a second diode, the fourth series circuit being connected in parallel to the second switching device;
a fifth series circuit including a third diode and the secondary winding of the transformer, the fifth series circuit being connected between the DC output terminals; and
a voltage clamping means connected in parallel to the primary winding of the transformer.
According to the subject matter of a second aspect of the invention, there is provided an electric power converter including:
an AC power supply;
a first series circuit including a first switching device and a second switching device connected in series to each other via an internal connection point, N pieces of the first series circuits being connected in parallel to each other, said N being a nonnegative integer equal to or more than 2;
a reactor connected between the AC power supply and the internal connection point in the first one of the first series circuits;
an output capacitor including a DC output terminal, the DC output terminals being connected between the parallel connection points of the N pieces of the first series circuits;
a load connected between the DC output terminals of the output capacitor;
the first series circuit including a first capacitor and a second capacitor connected in parallel to the first switching device and the second switching device, respectively;
a first diode including an anode terminal connected to the internal connection point of the first series circuit and a cathode terminal, the cathode terminals of the first diodes being connected collectively;
a second series circuit including the primary winding of a transformer and a third switching device; the second series circuit being connected between the cathode terminals of the first diodes and the DC output terminal;
a second diode including a cathode terminal connected to the internal connection point of the first series circuit and an anode terminal, the anode terminals of the second diodes being connected collectively;
a third series circuit including the primary winding of the transformer and a fourth switching device, the third series circuit being connected between the anode terminals of the second diodes and the DC output terminal;
a fourth series circuit including a third diode and the secondary winding of the transformer, the fourth series circuit being connected between the DC output terminals; and
a voltage clamping means connected in parallel to the primary winding of the transformer.
The electric power converter according to the invention that conducts two-way electric power conversion facilitates performing soft switching with a minimal circuit added thereto and reducing the losses caused thereby.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a circuit diagram showing the circuit configuration of an electric power converter according to a first embodiment of the invention.
FIG. 1B is a wave chart describing the operations of the circuit shown in FIG. 1A .
FIG. 2A is a circuit diagram showing the circuit configuration of an electric power converter according to a second embodiment of the invention.
FIG. 2B is a wave chart describing the operations of the circuit shown in FIG. 2A .
FIG. 2C is a circuit diagram showing the circuit configuration of an electric power converter according to a third embodiment of the invention.
FIG. 2D is a circuit diagram showing the circuit configuration of an electric power converter according to a fourth embodiment of the invention.
FIG. 3A is a circuit diagram of a conventional electric power converter.
FIG. 3B is a wave chart describing the operations of the circuit shown in FIG. 3A .
FIG. 4A is a circuit diagram of another conventional electric power converter.
FIG. 4B is a wave chart describing the operations of the circuit shown in FIG. 4A .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Now, the invention will be described in detail hereinafter with reference to the accompanied drawings which illustrate the preferred embodiments of the invention.
FIG. 1A is a circuit diagram showing the circuit configuration of an electric power converter according to a first embodiment of the invention.
In the circuit shown in FIG. 1A , DC power supply 51 is employed in substitution for AC power supply 1 and rectifier circuit 40 . Switching device 18 is connected in parallel to diode 6 . DC power supply 51 , reactor 21 , diodes 6 and 12 , and switching devices 15 and 18 constitute a chopper circuit.
By turning on and off switching device 15 in the chopper circuit described above, electric power is fed from the DC power supply side to the load side. By turning on and off switching device 18 in the chopper circuit described above, electric power is regenerated from the load side to the DC power supply side. A soft switching circuit is configured by diodes 7 , 9 , 10 , 41 , and 42 ; switching devices 17 and 20 ; transformer 22 ; and voltage clamping element 30 .
For feeding electric power from the DC power supply side to the load side, switching devices 15 and 17 and diode 6 are made to conduct soft switching in the same manner as in the circuit shown in FIG. 3A . The electric power converter according to the first embodiment is different from the conventional electric power converters in that the electric power converter according to the first embodiment makes it possible to conduct soft switching in regenerating electric power from the load side to the DC power supply side by adding a few circuit component parts. Now the regeneration operation conducted by the electric power converter according to the first embodiment will be described in detail below.
By turning on switching device 18 in FIG. 1A , the energy stored in capacitor 33 is transferred to reactor 21 via switching device 18 and regenerated to DC power supply 51 . Then, as switching device 18 is turned off, the energy transferred to reactor 21 is regenerated to DC power supply 51 through a path connecting reactor 21 , DC power supply 51 , and diode 12 . Thus, the energy stored in the capacitor on the load side is regenerated to the DC power supply side by controlling the ON and OFF of switching device 18 .
Capacitor 71 ; diodes 9 , 10 , 41 , and 42 ; voltage clamping element 30 , transformer 22 ; and switching device 20 form a soft switching circuit for the regeneration operation mode that regenerates electric power from the load side to the DC power supply side. In the same manner as in FIG. 3A , diodes 9 and 10 ; voltage clamping element 30 ; and transformer 22 are employed also for configuring a soft switching circuit for the operation mode that feeds electric power from the DC power supply side to the load side.
FIG. 1B is a wave chart describing the operations of the circuit shown in FIG. 1A .
As switching device 20 is turned on, the electric charge stored in capacitor 71 (or in the parasitic capacitance of switching device 18 ) is discharged in a period t 1 through a path connecting capacitor 71 , switching device 20 , the primary winding of transformer 22 , and diode 42 . At the same time, the electric charge stored in capacitor 71 is regenerated to the output side via the secondary winding of transformer 22 and diode 10 . Since the current flowing through switching device 20 gradually increases due to the leakage inductance of transformer 22 , switching device 20 performs soft switching during the state of the turn-ON thereof.
As soon as the current value flowing through switching device 20 becomes equal to the current value flowing through reactor 21 , a period t 2 starts and diode 12 becomes OFF. Since the current flowing through diode 12 decreases gradually to zero, the surge voltage caused by the reverse recovery and the reverse recovery losses are reduced. As switching device 18 is turned on in a period t 3 after the voltage of switching device 18 becomes zero, a difference current, equal to the difference between the current flowing through the primary winding of transformer 22 and the current flowing through reactor 21 , flows through switching device 18 . Since the difference current that flows through switching device 18 initially flows through diode 6 , the current that flows through switching device 18 gradually increases from a negative value. Therefore, switching device 18 performs soft switching during the state of the turn-ON thereof.
When switching device 15 is turned off, the voltage of switching device 15 rises gradually due to the current flowing through capacitor 31 . Therefore, the turn-OFF losses are reduced. Thus, switching devices 15 and 18 perform soft switching at the turn-OFF thereof. In a period t 4 , a reset voltage equal to the voltage clamped by voltage clamping element 30 is caused across the primary winding of transformer 22 . A voltage, which is as high as the product of the reset voltage and the winding ratio of transformer 22 , is generated across the secondary winding of transformer 22 . The sum of the DC output voltage and the voltage across the secondary winding of transformer 22 is applied to diode 10 . By setting the clamping voltage of voltage clamping element 30 to be low, the voltage applied to diode 10 is reduced.
FIG. 2A is a circuit diagram showing the circuit configuration of an electric power converter according to a second embodiment of the invention.
As shown in FIG. 2A , a rectifier circuit is configured by reactor 21 , diodes 2 through 5 , and switching devices 15 , 16 , 18 and 19 . Switching device 18 and capacitor 71 are connected in parallel to diode 2 in a diode bridge circuit configured by diodes 2 through 5 . Switching device 15 and capacitor 31 are connected in parallel to diode 3 in the diode bridge circuit. Switching device 19 and capacitor 72 are connected in parallel to diode 4 in the diode bridge circuit. Switching device 16 and capacitor 32 are connected in parallel to diode 5 in the diode bridge circuit. AC power supply 1 is connected between the series connection point of diodes 2 and 3 and the series connection point of diodes 4 and 5 via reactor 21 . Diodes 2 through 5 may be replaced by the parasitic diodes of switching devices 15 , 16 , 18 , and 19 , respectively.
Diodes 7 through 10 , 13 , 41 through 43 ; switching devices 17 and 20 ; transformer 22 ; and voltage clamping element 30 form a soft switching circuit. In detail, the soft switching circuit is configured in the following manner. The anode of diode 8 is connected to the series connection point of diodes 2 and 3 . The anode of diode 7 is connected to the series connection point of diodes 4 and 5 . The cathode of diode 42 is connected to the series connection point of diodes 2 and 3 . The cathode of diode 43 is connected to the series connection point of diodes 4 and 5 . The cathodes of diodes 7 and 8 and the source terminal of switching device 20 , to which diode 41 is connected in parallel, are connected to the first terminal of the primary winding in transformer 22 . The anodes of diodes 42 and 43 and the drain terminal of switching device 17 , to which diode 13 is connected in parallel, are connected to the second terminal of the primary winding in transformer 22 . The drain terminal of switching device 20 is connected to the positive terminal of the DC output. The source terminal of switching device 17 is connected to the negative terminal of the DC output. A series circuit of diode 9 and voltage clamping element 30 is connected in parallel to the primary winding of transformer 22 . A series circuit of diode 10 and the secondary winding of transformer 22 is connected in parallel to capacitor 33 , that is the DC output. The parasitic diodes of switching devices 17 and 20 may be employed in substitution for diodes 13 and 41 with no problem.
In feeding electric power from the AC power supply side to the load side in the circuit shown in FIG. 2A , soft switching is performed by switching devices 15 through 17 and diodes 2 and 4 in the same manner as in the conventional circuit shown in FIG. 4A . The circuit shown in FIG. 2A is different from the conventional circuit shown in FIG. 4A in that the circuit shown in FIG. 2A facilitates performing soft switching even in regenerating electric power from the load side to the AC power supply side with a few circuit component parts added thereto.
As switching devices 16 and 18 are turned on when the AC power supply voltage is positive in the circuit configuration shown in FIG. 2A , the energy stored in capacitor 33 is transferred to reactor 21 through a path connecting capacitor 33 , switching device 18 , reactor 21 , AC power supply 1 , and switching device 16 and regenerated to AC power supply 1 . Then, by turning off switching device 18 , the energy transferred to reactor 21 is regenerated to AC power supply 1 through a path connecting reactor 21 , AC power supply 1 , switching device 16 and diode 3 .
As switching devices 19 and 15 are turned on when the AC power supply voltage is negative in the circuit configuration shown in FIG. 2A , the energy stored in capacitor 33 is transferred to reactor 21 through a path connecting capacitor 33 , switching device 19 , AC power supply 1 , reactor 21 , and switching device 15 and regenerated to AC power supply 1 . Then, by turning off switching device 19 , the energy transferred to reactor 21 is regenerated to AC power supply 1 through a path connecting reactor 21 , AC power supply 1 , switching device 15 and diode 5 . Thus, by controlling the ON and OFF of switching device 18 or 19 , the energy stored on the load side is regenerated to the AC power supply side.
Capacitors 71 and 72 , diodes 9 , 10 , 41 through 43 , voltage clamping element 30 , transformer 22 , and switching device 20 form a soft switching circuit for the regeneration operation mode that regenerates electric power from the load side to the AC power supply side. In the same manner as described with reference to FIG. 4A , diodes 9 and 10 , voltage clamping element 30 , and transformer 22 are employed also for configuring a soft switching circuit for the operation mode that feeds electric power from the AC power supply side to the load side.
FIG. 2C is a circuit diagram showing the circuit configuration of an electric power converter according to a third embodiment of the invention.
As shown in FIG. 2C , reactors 211 through 213 are connected to each phase of a three-phase AC power supplies. A rectifier circuit is configured by diodes 111 through 116 and switching devices 101 through 106 , and a rectifier diode bridge circuit configured by diodes 111 through 116 . Switching device 101 and capacitor 121 are connected in parallel to diode 111 . Switching devices 102 through 106 and capacitors 122 through 126 are connected in parallel to diodes 112 through 116 , respectively. AC power supplies are connected between the series connection point of diodes 111 and 112 via reactor 211 . AC power supplies are connected between the series connection point of diodes 113 and 114 and the series connection point of diodes 115 and 116 via reactors 212 and 213 , respectively. Diodes 111 through 116 may be replaced by the parasitic diodes of switching devices 101 through 106 , respectively.
Diodes 9 , 10 , 131 through 133 , 173 , 174 , and 141 through 143 , switching devices 171 and 172 , transformer 22 , and voltage clamping element 30 form a soft switching circuit.
In detail, the soft switching circuit is configured in the following manner. The anode of diode 131 is connected to the series connection point of diodes 111 and 112 . The anode of diode 132 is connected to the series connection point of diodes 113 and 114 . The anode of diode 133 is connected to the series connection point of diodes 115 and 116 . The cathode of diode 141 is connected to the series connection point of diodes 111 and 112 . The cathode of diode 142 is connected to the series connection point of diodes 113 and 114 . The cathode of diode 143 is connected to the series connection point of diodes 115 and 116 . The cathodes of diodes 131 through 133 and the source terminal of switching device 171 , to which diode 173 is connected in parallel, are connected to the first terminal of the primary winding in transformer 22 . The anodes of diodes 141 through 143 and the drain terminal of switching device 172 , to which diode 174 is connected in parallel, are connected to the second terminal of the primary winding in transformer 22 . The drain terminal of switching device 171 is connected to the positive terminal of the DC output. The source terminal of switching device 172 is connected to the negative terminal of the DC output. A series circuit of diode 9 and voltage clamping element 30 is connected in parallel to the primary winding of transformer 22 . A series circuit of diode 10 and the secondary winding of transformer 22 is connected in parallel to capacitor 33 , that is the DC output. The parasitic diodes of switching devices 171 and 172 may be employed in substitution for diodes 173 and 174 with no problem.
In feeding electric power from the AC power supply side to the load side or from the load side to the AC power supply side shown in FIG. 2C , soft switching is performed by switching devices 101 through 106 , 171 , and 172 , and diodes 111 through 116 . The operation is described as follows.
As switching devices 101 and 104 are turned on when the U-phase of AC power supply voltage is positive in the circuit configuration shown in FIG. 2C , the energy stored in capacitor 33 is transferred to reactors 211 and 212 through a path connecting capacitor 33 , switching device 101 , reactor 211 , AC power supply, reactor 212 , and switching device 104 and regenerated to AC power supply. Then, by turning off switching device 101 , the energy transferred to reactor 211 is regenerated to AC power supply through a path connecting reactor 211 , AC power supply, reactor 212 , switching device 104 , and diode 112 .
As switching devices 113 and 112 are turned on when the U-phase of AC power supply voltage is negative in the circuit configuration shown in FIG. 2C , the energy stored in capacitor 33 is transferred to reactors 211 and 212 through a path connecting capacitor 33 , switching device 113 , reactor 212 , AC power supply, reactor 211 , and switching device 102 and regenerated to AC power supply. Then, by turning off switching device 113 , the energy transferred to reactors 211 and 212 are regenerated to AC power supply through a path connecting reactor 212 , AC power supply, reactor 211 , switching device 112 , and diode 113 . Thus, by controlling the ON and OFF of switching devices 101 through 106 , the energy stored on the load side is regenerated to the AC power supply side.
Capacitors 121 through 124 , diodes 9 , 10 , 173 , 174 , 131 , 132 , 141 , and 142 , voltage clamping element 30 , transformer 22 , and switching devices 171 and 172 form a soft switching circuit for the regeneration operation mode that regenerates electric power from the load side to the AC power supply side. In the same manner as described with reference to FIG. 4A , diodes 9 and 10 , voltage clamping element 30 , and transformer 22 are employed also for configuring a soft switching circuit for the operation mode that feeds electric power from the AC power supply side to the load side.
FIG. 2D is a circuit diagram showing the circuit configuration of an electric power converter according to a fourth embodiment of the invention.
As shown in FIG. 2D , reactors 211 through 214 are connected to each phase of a four-phase AC power supplies. A rectifier circuit is configured by diodes 111 through 118 and switching devices 101 through 108 , and a rectifier diode bridge circuit configured by diodes 111 through 118 . Switching device 101 and capacitor 121 are connected in parallel to diode 111 . Switching devices 102 through 108 and capacitors 122 through 128 are connected in parallel to diodes 112 through 118 , respectively. AC power supplies are connected between the series connection point of diodes 111 and 112 via reactor 211 . AC power supplies are connected between the series connection point of diodes 113 and 114 , the series connection point of diodes 115 and 116 , and the series connection point of diodes 117 and 118 via reactors 212 , 213 , and 214 , respectively. Diodes 111 through 118 may be replaced by the parasitic diodes of switching devices 101 through 108 , respectively.
Diodes 9 , 10 , 131 through 134 , 173 , 174 , and 141 through 144 , switching devices 171 and 172 , transformer 22 , and voltage clamping element 30 form a soft switching circuit.
In detail, the soft switching circuit is configured in the following manner. The anode of diode 131 is connected to the series connection point of diodes 111 and 112 . The anode of diode 132 is connected to the series connection point of diodes 113 and 114 . The anode of diode 133 is connected to the series connection point of diodes 115 and 116 . The anode of diode 134 is connected to the series connection point of diodes 117 and 118 . The cathode of diode 141 is connected to the series connection point of diodes 111 and 112 . The cathode of diode 142 is connected to the series connection point of diodes 113 and 114 . The cathode of diode 143 is connected to the series connection point of diodes 115 and 116 . The cathode of diode 144 is connected to the series connection point of diodes 117 and 118 . The cathodes of diodes 131 through 134 and the source terminal of switching device 171 , to which diode 173 is connected in parallel, are connected to the first terminal of the primary winding in transformer 22 . The anodes of diodes 141 through 144 and the drain terminal of switching device 172 , to which diode 174 is connected in parallel, are connected to the second terminal of the primary winding in transformer 22 . The drain terminal of switching device 171 is connected to the positive terminal of the DC output. The source terminal of switching device 172 is connected to the negative terminal of the DC output. A series circuit of diode 9 and voltage clamping element 30 is connected in parallel to the primary winding of transformer 22 . A series circuit of diode 10 and the secondary winding of transformer 22 are connected in parallel to capacitor 33 , that is the DC output. The parasitic diodes of switching devices 171 and 172 may be employed in substitution for diodes 173 and 174 with no problem.
In feeding electric power from the AC power supply side to the load side or from the load side to the AC power supply side shown in FIG. 2D , soft switching is performed by switching devices 101 through 108 , 171 , and 172 , and diodes 111 through 118 . The operation is described as follows.
In FIG. 2D , in the same manner as described in FIG. 2C , as switching devices are turned on based on the voltage of each phase of the AC power supplies, the energy stored in capacitor 33 is transferred to reactors 211 through 214 through a path connecting capacitor 33 , switching device (such as 101 ), reactor (such as 211 ), AC power supply, reactor (such as 212 ), and switching device ( 104 ) and regenerated to AC power supply. Then, by turning off switching device (such as 101 ), the energy transferred to reactor is regenerated to AC power supply through a path connecting reactor ( 211 ), AC power supply, reactor ( 212 ), switching device ( 104 ), and diode ( 112 ).
Thus, by controlling the ON and OFF of switching devices 101 through 108 , the energy stored on the load side is regenerated to the AC power supply side.
Capacitors 121 through 124 , diodes 9 , 10 , 173 , 174 , 131 , 132 , 141 , and 142 , voltage clamping element 30 , transformer 22 , and switching devices 171 and 172 form a soft switching circuit for the regeneration operation mode that regenerates electric power from the load side to the AC power supply side. In the same manner as described with reference to FIG. 4A , diodes 9 and 10 , voltage clamping element 30 , and transformer 22 are employed also for configuring a soft switching circuit for the operation mode that feeds electric power from the AC power supply side to the load side.
FIG. 2B is a wave chart describing the operations of the circuit shown in FIG. 2A .
By turning on switching device 20 when the AC power supply voltage is positive, the electric charge stored in capacitor 71 (or in the parasitic capacitance of switching device 18 ) is discharged in a period t 1 through a path connecting capacitor 71 , switching device 20 , the primary winding of transformer 22 , and diode 42 . At the same time, the electric charge stored in capacitor 71 is regenerated to the output side via the secondary winding of transformer 22 and diode 10 . Since the current flowing through switching device 20 increases gradually from zero due to the leakage inductance of transformer 22 , switching device 20 performs soft switching at the turn-ON thereof.
As soon as the current value flowing through switching device 20 becomes equal to the current value flowing through reactor 21 , a period t 2 starts and diode 3 becomes OFF. Since the current flowing through diode 3 decreases gradually to zero, the surge voltage caused by the reverse recovery and the reverse recovery losses are reduced. As switching device 18 is turned on in a period t 3 after the voltage of switching device 18 becomes zero, a difference current, equal to the difference between the current flowing through the primary winding of transformer 22 and the current flowing through reactor 21 , flows through switching device 18 . Since the difference current that flows through switching device 18 initially flows through diode 2 , the current flowing through switching device 18 increases gradually from a negative value. Therefore, switching device 18 performs soft switching at the turn-ON thereof.
When switching device 18 is turned off, the voltage of switching device 18 rises gradually due to the current flowing through capacitor 71 . Therefore, the turn-OFF losses are reduced. Thus, switching devices 18 and 20 perform soft switching.
In a period t 4 , a reset voltage equal to the voltage clamped by voltage clamping element 30 is caused across the primary winding of transformer 22 . A voltage, which is as high as the product of the reset voltage and the winding ratio of transformer 22 , is generated across the secondary winding of transformer 22 . The sum of the DC output voltage and the voltage across the secondary winding of transformer 22 is applied to diode 10 . By setting the clamping voltage of voltage clamping element 30 to be low, the voltage applied to diode 10 is reduced.
When the AC power supply voltage is negative, the electric charges stored in capacitor 72 are regenerated to the load side in the same manner as described above. Therefore, the rectifier circuit in FIG. 2A works in the same manner as the rectifier circuit in FIG. 1A . Switching devices 15 through 20 and diodes 2 through 5 perform soft switching.
The Disclosure of Japanese Patent Application No. 2008-047706 filed on Feb. 28, 2008 is incorporated in the application.
While the invention has been explained with reference to the specific embodiments of the invention, the explanation is illustrative and the invention is limited only by the appended claims.
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An electric power converter facilitates performing soft switching in the two-way electric-power-conversion operation thereof, and reducing the manufacturing costs thereof and the losses caused therein, The electric power converter includes a first switching device; a second switching device; a first series circuit including capacitor, a diode, the primary winding of transformer, and a third switching device; a second series circuit including a capacitor, a fourth switching device, the primary winding of transformer, and a diode; a third series circuit including a diode and the secondary winding of transformer; and a voltage clamping element connected in parallel to the primary winding of transformer. The first series circuit is connected in parallel to the first switching device, and the second series circuit is connected in parallel to second switching device. The third series circuit is connected between the DC output terminals.
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TECHNICAL FIELD
[0001] The present invention relates to antennas. More specifically, the present invention relates to dipole antennas with a ring useful for beamforming and increasing gain.
BACKGROUND OF THE INVENTION
[0002] The telecommunications revolution of the late 20 th century has given rise to a plethora of new communications devices and methods. With this rise in communications capability comes a need for better means for disseminating radio based signals.
[0003] Previously, omnidirectional antennas were used for most radio based applications. Nowadays, more focussed antennas with a narrower beamwidth are use. These antennas can be placed in arrays to provide greater telecommunications coverage for densely packed areas such as sporting arenas, shopping malls, and the like.
[0004] To arrive at a narrower beamwidth, such as, for example, a 65 degree beamwidth, previous attempts have been made. However, none of these attempts have been satisfactory.
[0005] Previous attempts include using two elements in parallel in the azimuth plane with a proper feed network. Using this approach, the number of elements should be twice of a 65 degree element. Another approach involves staggering the elements to make two columns. Again, the number of elements required is higher than for an antenna with elements which have a beamwidth of 65 degrees. Another approach is that of controlling the height of the dipole antenna and the reflector size or side fences. However, none of these approaches can offer a stable beamwidth over 1710-2690 MHz. Another approach is that of using several parasitic elements in parallel to the reflector which increases the antenna depth.
[0006] In addition to the above issues, these approaches also have additional issues. Using two elements by staggering elements or in quad format increases the number of elements used. This increases the cost of the antenna. In addition, a beamwidth of 65 degrees is not guaranteed as beamwidth variation over 1710-2690 MHz is more than 5 degrees. If one reduces the height of the dipole antenna and uses a large reflector, this increases the size of the overall antenna. Again, this approach has a beamwidth variation of more than 5 degrees. If multiple resonators are used in parallel with a reflector, this increases the depth of the antenna.
[0007] Based on the above, this is therefore a need for systems, methods, and devices which avoid the shortcomings of the prior art.
SUMMARY OF INVENTION
[0008] The present invention provides systems, methods, and devices relating to antennas. A crossed dipole antenna element has a ring encircling the antenna. The ring, constructed of a conductive material, is not touching the arms of the dipole antenna and the distance between the ring and the arms of the antenna can be optimized. The antenna element assembly can be used in one or two dimensional antenna arrays.
[0009] In a first aspect, the present invention provides an antenna comprising:
a dipole antenna having two arms; at least one beamforming structure encircling said dipole antenna, the or each of said at least one beamforming structure being spaced apart from said two arms;
wherein the or each of said at least one beamforming structure is constructed from a conductive material.
[0012] In a second aspect, the present invention provides an antenna array having at least two antenna elements, each antenna element comprising:
a crossed dipole antenna; at least one beamforming structure encircling said crossed-dipole antenna;
wherein said at least one beamforming structure is constructed from a conductive material; and
wherein said at least one beamforming structure is spaced apart from arms of said crossed dipole antenna.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The embodiments of the present invention will now be described by reference to the following figures, in which identical reference numerals in different figures indicate identical elements and in which:
[0016] FIG. 1 is a diagram illustrating an antenna according to one aspect of the invention;
[0017] FIG. 2 is a plot showing the return loss and cross-pole isolation for the antenna illustrated in FIG. 1 ;
[0018] FIG. 3 is a diagram illustrating a variant of the antenna in FIG. 1 ;
[0019] FIG. 4 is a diagram illustrating another variant of the antenna in FIG. 1 ;
[0020] FIG. 5 is a two-dimensional array of antenna elements using a variant of the antenna in FIG. 1 ;
[0021] FIG. 6 is a plot which compares antenna directivity for a dipole antenna without a beamforming structure and for antennas which use different variants of the beamforming structure;
[0022] FIG. 7 illustrates the azimuth pattern for a dipole antenna not equipped with a beamforming structure for different frequencies;
[0023] FIG. 8 illustrates the azimuth pattern for a dipole antenna equipped with a beamforming structures for frequencies similar to those used for FIG. 7 ;
[0024] FIG. 9 shows a one dimensional array of antenna elements using a variant of the antenna in FIG. 1 ; and
[0025] FIG. 10 shows a three-sector antenna using antenna elements which are a variant of the antenna in FIG. 1 .
DETAILED DESCRIPTION
[0026] Referring to FIG. 1 , an antenna 10 according to one aspect of the invention is illustrated. The antenna 10 has two dipole antennas 20 , 30 which, together, form a crossed dipole antenna. A beamforming structure 40 encircles the crossed dipole antenna.
[0027] In FIG. 1 , two dipole antennas 20 , 30 are used. However, a single dipole antenna may also be used. As well, the beamforming structure 40 in FIG. 1 is in the form of a ring. Other loop shapes, such as square loops, rectangular loops, cross loops, and other quadrilateral loops, may also be used. Depending on the beamforming shape, dipoles may be designed and tuned accordingly. The center of the beamforming structure is, preferably, collinear or coincident with the center axis of the dipole or crossed dipole antennas. As such, the center of the beamforming structure would be collinear with the axis where one dipole antenna meets another. For a crossed dipole antenna, the axis where all four single pole antennas meet is coincident with the center of the beamforming structure. Other variants of the beamforming structure will be explained below.
[0028] The use of the beamforming structure, especially in the form of a ring or an annulus, stabilizes the azimuth beam width, increases the antenna gain, and reduces grating lobe, cross-pole isolation, and beam squint. In addition, since rings do not have contact with a reflector, they do not generate passive intermodulation.
[0029] The beamforming structure is developed primarily for 1710-2690 MHz band. However, the concept has been applied to other frequency bands including but not limited to other cellular bands such as 1710-2360 MHz, 698-896 MHz, 698-960 MHz, and 596-960 Mhz. In either case using a ring with dipole configuration may increase the antenna gain, may stabilize the beamwidth, and may reduce grating lobe and cross-pol isolation.
[0030] With the use of a ring beamforming structure, it is possible to adjust the azimuth and elevation beamwidth without modifying the dipole antenna. This allows for the reconfiguration of the element pattern when the antenna is used in different antenna arrays. The beamforming structure can have its radius, height, or spacing from the dipole antenna adjusted depending on the desired operation band and dipole height.
[0031] The configuration illustrated in FIG. 1 is for an antenna with 65 degree azimuth beam width over 1710-2690 MHz. It may be modified to add additional rings with similar or different shapes. Addition of such rings modifies the impedance of the antenna as well. However, the dipole antenna can be re-tuned to work with either single or multiple rings. In practise, the crossed dipole antenna and the ring shaped beamforming structure is optimized for impedance matching by taking into account the ring in the system design.
[0032] The antenna in FIG. 1 is a dual polarization dipole antenna surrounded by a suspended ring and is for dual slant +/−45 degree polarization. Each dipole has a parasitic element with the same width but longer in length to offer 45% bandwidth which covers 1710-2690 MHz.
[0033] Referring to FIG. 2 , the plot shows the return loss and cross-pole isolation for the antenna element. The plot shows that the antenna element has a better than 14 dB Return Loss and has a better than 30 dB cross-polarity isolation at 1710-2690 MHz.
[0034] Referring to FIGS. 3 and 4 , variants of the present invention are illustrated. The embodiment illustrated in FIG. 1 has a beamforming structure that is tube-shaped. The shallow tube which encircles the dipole antenna is spaced apart from and is not in contact with the arms of the dipole antenna. In FIG. 3 , the beamforming structure is a thin circle while in FIG. 4 , the beamforming structure is annular in shape. Other shapes, as noted above, are also possible.
[0035] The beamforming structure may be placed below the arms of the dipole antenna as in FIGS. 3 and 4 . Similarly, the beamforming structure may be located at the edge of the arms of the dipole antenna as in FIG. 1 . The beamforming structure may be raised above the ground plane by suitable non-conductive supports. Alternatively, the beamforming structure may be suspended above the ground plane by suitable clips which attach the beamforming structure to the circuit boards on which the traces define the dipole antenna.
[0036] Regarding the design parameters for the beamforming structure, if a circular or annular shape is used, the diameter of the beamforming structure is preferably less than one wavelength based on the highest operating frequency. In one implementation, the height of the rings is around 10 mm for best performance. However, the height can be varied from 1-2 mm to 20 mm. In this implementation, the spacing between the reflector and ring shaped beamforming structure is close to the dipole height. Preferably, there is no metallic contact between the beamforming structure and the reflector base plate. This lack of contact between the base plate and the beamforming structure is good for passive inter-modulation.
[0037] Spacing between the beamforming structure and the reflector can be less than the dipole height and this determines the operating band of the antenna. The diameter of the ring-shaped beamforming structure is preferably about the length of dipole but can be smaller depending on the structure's height, frequency band, and application. Smaller diameter structures can be used for planar arrays where antenna elements need to be compact. Depending on the application, multiple beamforming structures with similar or different radii may also be used.
[0038] Regarding signal feed to the dipole antenna, FIGS. 1, 3, and 4 show dipole antennas which are fed from below. However, the dipole antenna can also be configured to be fed from above.
[0039] It should be noted that the data presented in this document for different sized beamforming structures is based on a fixed dipole antenna height. By modifying the dipole height and adding more beamforming structures, azimuth beamwidth can be modified.
[0040] The use of the ring shaped beamforming structure provides a number of advantages. Specifically, a 65 degree antenna azimuth pattern can be achieved over 1710-2690 MHz by adjusting the beamforming structure height. Another feature of the ring shaped beamforming structure is that azimuth and elevation beamwidth can be controlled by modifying the structure height for a fixed dipole. Using this feature allows one to design antennas with a reconfigurable pattern. As well, other antenna parameters such as antenna gain (by as much as 1 dB), cross-polarity isolation, cross-polarity discrimination, grating lobe, and beam squint are improved when a suitably designed beamforming structure is used. As another advantage, the deployment of a ring-shaped beamforming structure reduces the dipole size by around 10%.
[0041] Regarding construction, the beamforming structure may be constructed from any suitable conductive material. The dipole antenna may be constructed using conventional and well-known construction methods and materials.
[0042] Referring to FIG. 6 , a plot is provided that compares the antenna directivity for a dipole antenna without a ring-shaped beamforming structure, a dipole antenna with a large ring-shaped beamforming structure, and a dipole antenna with a small ring-shaped beamforming structure. As can be seen, antenna directivity at 2.7 GHz is increased by 2 dB by adding the large beamforming structure and is increased by 0.7 dB when a small beamforming structure is used.
[0043] Referring to FIG. 7 , the figure shows the azimuth pattern for a dipole antenna not equipped with a beamforming structure on a 155 mm square reflector for 1.71 GHz, 2.2 GHz and 2.69 GHz. It can be seen that azimuth beamwidth varies from 67 degree at 1.71 GHz to 81 degree at 2.69 GHz. FIG. 8 shows the azimuth pattern for a dipole antenna which uses a large ring-shaped beamforming structure for 1.71 GHz, 2.2 GHz and 2.69 GHz. It can be seen from FIG. 8 that azimuth beamwidth is 65 degree for the three frequencies when a beamforming structure is used. When a dipole antenna is used, azimuth beamwidth variation is within +/−3 degree variation.
[0044] As noted above, antennas using the beamforming structure may be used in arrays. FIG. 9 illustrates a 2-port, one-dimensional array using a suitably designed crossed dipole antenna elements which use a beamforming structure. FIG. 5 shows a 4-port, two dimensional array with crossed dipole antenna elements with beamforming structures. Both antenna arrays in FIGS. 5 and 9 use the beamforming structure to obtain 65 degree azimuth beamwidth that has a frequency range of 1710-2690 MHz. Finally, FIG. 10 illustrates a six port tri-sector antenna in which each sector is covered with a panel with 65 degree azimuth beamwidth. The antenna elements used in the antenna of FIG. 10 also used crossed dipole antennas with a beamforming structure. Other configurations for antenna arrays are, of course, possible.
[0045] A person understanding this invention may now conceive of alternative structures and embodiments or variations of the above all of which are intended to fall within the scope of the invention as defined in the claims that follow.
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Systems, methods, and devices relating to antennas. A crossed dipole antenna element has a ring encircling the antenna. The ring, constructed of a conductive material, is not touching the arms of the dipole antenna and the distance between the ring and the arms of the antenna can be optimized. The antenna element assembly can be used in one or two dimensional antenna arrays.
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FIELD OF THE INVENTION
[0001] The present invention relates to a disposable, absorbent sheet of paper or other suitable material for adhesive installation in front of urinals and toilets in public restrooms, at the bottom of small animal or bird cages, on the floors of kitchen or foodservice areas in restaurants, and other suitable locations. The invention especially relates to pads or rolls of such sheets, each pad or roll containing a plurality of sheets affixed to one another by a strip of light to moderately tacky adhesive at a location on the underside of each sheet in a manner analogous to the POST-IT pads of adhesive notes commonly used to annotate office documents.
DISCUSSION OF PRIOR ART
[0002] Attempts are known in the art to maintain sanitary conditions in restrooms near toilets and wall-mounted urinals using trays, mats, or sheets, particularly in public restrooms for men where unwanted moisture, odor and bacteria on the floors commonly present both sanitary and aesthetic problems. For example, U.S. Pat. No. 4,125,656 to Creamer shows a pleated absorbent sheet for use around the base of a pedestal toilet to absorb moisture. Unfortunately, the pleated Creamer sheet is small and only suitable to absorb condensation dripping down the sides of the pedestal of a toilet. As such, it is not at all suitable for use at a wall-mounted urinal. Further, even at the base of a toilet it is not suitable for a user to stand upon or directly over and, therefore, does not aid in collecting drips or spills attributable to the user himself. The time-consuming and complicated pleating, folding, and adjustment features of the Creamer sheet further reduce the utility of this invention as it is expensive to manufacture and difficult to install.
[0003] Other absorbent sheets in the prior art are designed to be held within bulky, rigid and non-disposable trays. These trays themselves are subject to odor, moisture, and unsanitary bacteria. They are also expensive to manufacture and often unattractive. Thus, they potentially do not save in cleaning time, nor do they necessarily provide the desired improved sanitary environment.
[0004] Of concern is the risk of an absorbent sheet slipping out of position while in use. Again, unsatisfactory attempts to prevent this problem exist in the prior art. Some embodiments secure a sheet or a collection of sheets through use of strings, tape, or staples. These additional materials make the sheets both more difficult to manufacture and more time-consuming to install and remove. For example, U.S. Pat No. 2,057,162 to Richey utilizes strings to tie absorbent sheets to toilet pedestals. Not only would the Richey sheet be difficult to install, but it would be unsanitary as well since the attendant would have to reach behind the toilet to install the device.
[0005] In short, there is a desire and need in the art for an absorbent sheet of paper or other suitable material for use in restrooms and elsewhere that combines the benefits of being sanitary, capable of absorbing moisture and odor, inexpensive, secure, easy to install, easy to remove, easy to manufacture, capable of containing advertising or other messages to the user, capable of incorporating scented or antibacterial properties, easy to store in the form of self-contained pads or rolls of such sheets, and also providing an aesthetically pleasing appearance.
SUMMARY OF INVENTION
[0006] The present invention provides for a disposable, absorbent sheet suited for use around the base of a toilet, under a urinal, at the bottom of bird or animal cages, or on the floors of kitchen or foodservice areas in restaurants, and that may be simply and effectively secured to and removed from a floor or other surface in an efficient manner by means of a light to moderately tacky adhesive element.
[0007] In one embodiment of the present invention, a sheet for absorbing fluids and soils adjacent to the base of a urinal may include an adhesive strip on the underside of the sheet's edge lying furthest from the restroom wall. The adhesive strip releasably secures the sheet to a floor surface and is configured to enable a user to stand upon part of the sheet without inadvertently detaching it from the floor.
[0008] In another embodiment of the present invention, a sheet for absorbing fluids and soils adjacent to the base of a toilet also includes a semi-circular, rectangular, or other suitably shaped “cut-out” that permits the sheet to be installed around the toilet's pedestal. This sheet is also configured to enable a user standing in front of or over the toilet to stand upon part of the sheet without inadvertently detaching it from the floor.
[0009] In another embodiment of the present invention, a sheet for absorbing fluids and soils includes an adhesive element on a bottom surface to releasably secure the sheet to the bottom of a bird cage or animal cage.
[0010] In another embodiment of the present invention, a large roll of absorbent material has light to moderately tacky adhesive strips along both edges running the length of the sheet making it suitable for the floors of kitchens or foodservice areas in restaurants where moisture and food spills make those areas both unsanitary and dangerous.
[0011] In yet another embodiment of the present invention, a method of using a plurality of sheets in the form of a pad of such sheets includes the steps of: removing a first sheet from a pad including a plurality of absorbent sheets; adhesively securing the first sheet to a surface; discarding the first sheet as it becomes soiled; removing a second sheet from the pad; and adhesively securing the second sheet to a surface.
[0012] In yet another embodiment of the present invention, a method of using a plurality of sheets in the form of a continuous roll includes the steps of: pulling and then tearing a desired length of absorbent material from a continuous roll; adhesively securing the first sheet to a surface; discarding the first sheet as it becomes soiled; pulling and then tearing a second desired length of absorbent material from the continuous roll; and adhesively securing the second sheet to a surface.
[0013] In all embodiments of the present invention, a plurality of disposable sheets of absorbent material may be manufactured and conveniently stored in the form of pads or rolls of such sheets. The adhesive element both connects the plurality of sheets to one another and also permits them to be removed from the pad or roll and then adhesively secured to a floor or other surface. Such pads or rolls may be stacked and stored horizontally or vertically and, in the case of pads of such sheets, may also be hung vertically from a prefabricated hole near the edge of the pad.
[0014] Other features of the present invention will become more apparent to persons having ordinary skill in the art to which the present invention pertains from the following description and claims taken in conjunction with the accompanying companying figures.
BRIEF DESCRIPTION OF DRAWINGS
[0015] The foregoing features, as well as other features, will become apparent with reference to the description and figures below in which like numerals represent like elements and in which:
[0016] FIG. 1 is a perspective view of a sheet of the present invention positioned adjacent to a toilet base;
[0017] FIG. 2 is a perspective view of sheets of the present invention positioned beneath a pair of urinals;
[0018] FIG. 3 is a plan view of an embodiment of a pad of the present invention;
[0019] FIG. 4 is a perspective view of a sheet of the present invention positioned at the bottom of a small animal cage;
[0020] FIG. 5 is a perspective view of a sheet of the present invention positioned at the bottom of a bird cage;
[0021] FIG. 6 is a sectional view taken along line 6 - 6 in FIG. 3 ; and
[0022] FIGS. 7 a and 7 b are perspective views of an embodiment of the present invention in the configuration of a continuous roll of sheets.
DETAILED DESCRIPTION
[0023] The present invention is a disposable, absorbent sheet suitable for adhesive installation in front of urinals and toilets, at the bottom of bird or animal cages, on the floors of kitchen or foodservice areas in restaurants, and other suitable locations. The invention provides a remedy for unsightly and unsanitary moisture, odor, and bacteria that commonly forms at the base of urinals and toilets and typically remains until the next scheduled mopping. In addition to soiling and creating an offensive odor in public restrooms, these conditions are inevitably tracked back into the more public areas they serve such as restaurants, bars, gas stations, hotel lobbies, airline terminals, offices, schoolrooms, retail spaces, nursing homes and the like. The present invention provides a low cost-per-unit solution that is securable, capable of absorbing moisture and odor, easy to install, easy to manufacture, capable of incorporating scented or antibacterial properties, and easy to store, while also providing an aesthetically pleasing appearance. The invention's low per-unit cost, ease of installation, and ease of removal allow it to be replaced on a daily or, in some cases, on an even more frequent basis as needed.
[0024] Described in more detail below are specific embodiments of the present invention, one for use under a urinal, another for under a pedestal toilet, a third for use at the bottom of a small animal cage or bird cage, and a fourth in the configuration of a continuous roll. Under a wall-mounted urinal, the present invention may be a simple, rectangular sheet of absorbent paper large enough to catch drips and spills, large enough to permit a printed message or advertising, and simple enough in shape (i.e., no tapering or cut-outs) to make it easy and inexpensive to manufacture. The sheet may be single- or multi-ply paper and with or without a non-absorbent (waxy) backing. It should be highly-absorbent and, further, may be scented, may be infused with an antibacterial material, and may be textured and/or printed so as to conceal stains or drips. A single adhesive strip on the underside of each sheet may run the width of the sheet and be positioned on the edge of the sheet farthest away from the restroom wall. Other embodiments of the invention could have the adhesive strip at both ends (or even at all four sides) of the absorbent sheet. It is anticipated, however, that a single strip positioned away from the restroom wall and under the feet of the user would be less expensive to manufacture, easier to install, and easier to remove from restroom floors, while providing sufficient adhesion to a restroom floor.
[0025] An alternate embodiment for use at the base of a pedestal toilet would further include a cut-out to allow the sheet to extend around the pedestal and thus further underneath the bowl of the toilet.
[0026] An alternate embodiment for use at the bottom of a small animal or bird cage could also include additional adhesive elements as friction may be applied anywhere on the sheet rather than primarily along one edge.
[0027] An alternate embodiment for use on the floors of kitchen or foodservice areas in restaurants would include adhesive elements on both sides of a large, continuous roll of paper or other absorbent material.
[0028] Referring specifically to the figures, two embodiments of the present invention are illustrated in use under a pedestal toilet ( FIG. 1 ) and a wall mounted urinal ( FIG. 2 ). In each case, a sheet 22 may be positioned adjacent to a toilet or urinal. The sheet 22 may be made of a variety of different materials including various grades of absorbent and resilient paper or other material and be similar to a thick and slightly stiffened “paper towel” or “shop towel.” Single- or multi-ply absorbent papers, with or without a non-absorbent (waxy) backing, and with or without a thin or infused layer of specialized odor-absorbing materials such as carbon may be utilized. Further, the thickness and degree of absorbency of the material used may vary depending on the needs and desire of the user.
[0029] As shown, sheet 22 may be configured in a variety of different shapes and sizes to accommodate the use in front of different toilet and urinal configurations. For example, FIG. 1 shows a rectangle having a cut-out 24 . In FIG. 2 , two embodiments of sheet 22 are shown, a rectangular shaped embodiment indicated at A and an embodiment with external cut-outs 18 indicated at B. In the embodiment of FIG. 2B , the user is not intended to have his feet contact sheet 22 . Therefore, dirt and soils transferred from users will accumulate at a reduced rate and may increase the usable life of sheet 22 .
[0030] In all embodiments of the present invention, sheet 22 includes an adhesive element 26 on a bottom surface such as an adhesive strip along an edge of sheet 22 as shown in the figures. Adhesive element 26 may be any material having a light to moderate tackiness capable of both holding each sheet securely to a floor surface 28 and to an adjacent sheet in a pad as described below, while also allowing easy installation and removal. In a preferred embodiment, adhesive element 26 runs the entire length of one edge as shown in FIG. 1 . The adhesive element 26 may be approximately 5.1 cm to 12.7 cm (2 inch to 5 inches) in width. Alternatively, the adhesive element 26 may be located under any of the peripheral edges, around the entire periphery of the sheet, or even under the entire underside of sheet 22 . Further, the adhesive element 26 may be continuous or (to save on manufacturing or material costs) spotted or segmented. Alternatively, adhesive element 26 may include any of a variety of different shapes and sizes and be positioned at a variety of locations on the bottom surface of sheet 22 .
[0031] Adhesive element 26 enables sheet 22 to be secured to the floor surface 28 to reduce the chance of a sheet 22 slipping out of position while in use and thereby preventing a littered and unsightly appearance. Using adhesive element 26 , sheets 22 are easily installed, easily removed and easily suited for use on a variety of surfaces including metal or glass (in the case of animal cages), tile, concrete, wood, or even carpeted floors. Further, the adhesive element 26 is compatible with an endless variety of either single- or multi-ply absorbent sheet papers, with or without non-absorbent (waxy) backings.
[0032] Adhesive element 26 also enables a plurality of sheets 22 to be adhesively and releasably connected vertically on top of one another to form pad 20 as shown in FIGS. 3 and 6 . Again, this would be a similar configuration to the sheets of paper in a POST-IT note pad. Each sheet 22 is individually peeled off pad 20 as needed. As shown in FIG. 6 , a base sheet 16 may be included and adhesively affixed to the bottommost sheet 22 in pad 20 . Base sheet 16 may be constructed of the same material as sheets 22 or other suitable materials such as a wax paper to cover and protect the adhesive element 26 on the bottommost sheet 22 of pad 20 .
[0033] Sheet 22 and a resultant pad 20 may also include a hole 32 as shown in the figures. Hole 32 permits pad 20 to be stored vertically on a hook or peg. Multiple pads 20 may be stacked vertically or horizontally in a storage area, or alternatively may be hung on a peg or hook in a storage room or other location convenient for use near a toilet or urinal. This improved storageability over separate and loose sheets prevents possible damage from wrinkling, tearing, or fluid spills caused by contact with other objects or by individual sheets falling off a shelf within a storage area or facility.
[0034] Sheet 22 may also include decorative graphics or text to provide a more aesthetically pleasing appearance. For example, printed colors or geometric or swirling patterns that help hide drips and stains may improve the overall appearance of sheets 22 before, during, and after use. As shown in FIG. 3 , a message 34 , such as the name of the product itself or the establishment utilizing the product (e.g., the name of a hotel or restaurant chain) may also be printed on a top surface of sheets 22 . Sheet 22 may also include other desirable features such as infused fragrance or antibacterial chemicals (not shown).
[0035] In use, as shown in FIGS. 1 and 2 , sheet 22 may be peeled from pad 20 and positioned adjacent to a urinal or toilet to provide a means to absorb fluids that may drip or splash from the toilet, urinal or user. As the sheet 22 that is in use becomes soiled, it may be easily removed from the floor surface 28 and disposed. A clean sheet 22 may then be peeled from pad 20 and positioned on floor surface 28 . This process may continue until all of the plurality of sheets 22 in pad 20 have been depleted.
[0036] As sheets 22 are removed from the position next to a toilet or urinal to be discarded, they may also serve as a large, resilient and absorbent paper towel for a bathroom attendant to further clean other moist areas within a restroom. This additional utility would be dependent on the stiffness of the paper used, whether it utilizes a non-absorbent backing, and how soiled it may be after a toilet or urinal has been visited many times. In this regard, sheet 22 is superior to prior art in that it requires no strings, pleats, staples, or tape to attach it to floor surface 28 and that might hinder its usefulness as a paper towel. Even if a restroom floor is wet from an overnight mopping, for instance, sheet 22 could be adhesively affixed (“posted”) to the wall next to each urinal or toilet with adhesive element 26 as a means of making sheet 22 easily accessible for later installation.
[0037] In another embodiment of the present invention, sheet 22 may be configured from a continuous roll of absorbent material 38 as shown in FIGS. 7 a and 7 b . In this embodiment one or both edges of the roll of absorbent material 38 may include adhesive element 26 in the form of an adhesive strip. The roll of absorbent material 38 may be placed on a spool dispenser 40 or one similar to a dispenser of paper towels. Spool dispenser 40 may be mounted on a wall ( FIG. 7 b ) or alternatively placed or attached on a surface such as a table top ( FIG. 7 a ). Spool dispenser 40 may also include a cutting edge 42 and a pair of springs 44 . A user may pull on the exposed end of the roll 38 until a desired section 46 of absorbent material is obtained, and then cut section 46 with cutting edge 42 . Springs 44 impress cutting edge 42 upon the roll of absorbent material 38 . Therefore as sections 46 are removed, cutting edge 42 applies consistent pressure upon the increasingly smaller roll of absorbent material 38 .
[0038] Additional embodiments of the invention need not be limited to restroom use. Other applications may include the use of sheets 22 for small animal cages (as illustrated in FIG. 4 ), bird cages (as illustrated in FIG. 5 ), shop table tops, temporary automobile mats (for use at detail shops, car washes, oil change businesses, etc.), photocopy repair (where photocopy toner could soil the floor of an establishment where a photocopier is being repaired), kitchen floors and foodservice areas of restaurants, and any other place where a user would benefit from the quick installation and removal afforded by a strip (or strips) of light to moderately tacky adhesive element 26 on an absorbent sheet 22 of paper or other material.
[0039] While the invention has been described in conjunction with specific embodiments, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, the present invention attempts to embrace all such alternatives, modifications and variations that fall within the spirit and scope of the appended claims.
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A disposable sheet of absorbent material including at least one adhesive element on a bottom surface to releasably secure the sheet to a floor or other surface. The sheet may be included in a pad or roll containing a plurality of such sheets adhesively and releasably connected together. A pad of such sheets may include a hole through the sheets to enable the pad to be stored on a hook. The sheets may be configured in a variety of different shapes to conform to different sized toilets and urinals and may include decorative graphics, writings, and various colors or textures to provide a means of advertising, concealing drips and stains, and improving the appearance of a restroom. The sheets may also be configured to be used at the bottom of bird cages, small animal cages, the floors of kitchens and foodservice areas of restaurants.
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BACKGROUND OF INVENTION
This invention relates to production of coal in situ wherein vertical wells are drilled into an underground coal seam, the walls are linked together through the coal to form reaction zones and the coal is produced as gases and liquids. The invention more particularly is directed to methods of accomplishing the linkage channels through the coal.
It is well known in the art how to produce coal in situ, the most common method being to set the coal afire underground, with the fire sustained by continuous injection of an oxidizer. By proper control of the oxidizer, a reducing environment is established in the reaction zone in the coal with the resultant generation of combustible gases. If air is used as the oxidizer, produced combustible gases generally range from about 80 to 200 BTU per standard cubic foot.
In the early experiments with burning coal in situ, shafts were excavated from the surface of the earth to the bottom of the underground coal seam. Channels were then dug through the coal to provide communication with at least two shafts. Workmen ignited the coal face and then evacuated to the surface. The fire was propagated by injecting an oxidizer such as air into one shaft and removing the products of reaction from the second shaft. In this manner a low BTU gas was generated with a heat content in the order of 150 BTU per standard cubic foot. As the burning proceeded and the linkage channel became larger, the heat content of the generated gases would become lower and lower due to oxygen bypass of the burning face. A part of the injected oxidizer would be consumed in the fire and a part would proceed to the exit shaft where the hot low BTU gas would be further burned. In severe cases the resulting flue gases would have a heat content too low for combustion and were therefore useless as a fuel gas.
One of the prime objectives of early experiments in producing coal in situ was to minimize the time workmen were required underground. After many years of experimentation it became apparent that underground workmen would not be required if wells were drilled into the coal seam. This raised the problem of how to link the wells together with a communication passage through the seam. Through the years various linkage schemes were tried including hydraulic fracturing, directional drilling, explosive fracturing, electro-linking using electrical current, various methods of burning the channel and the like.
More experimental work on linkage has been performed in Russia than the combined experimental work done in the other countries of the world. The Russian technicians have perfected a reliable method of linkage using a reverse burn between two or more vertical wells. A detailed description of the successful linking procedure may be found in U.S. Pat. No. 4,036,298 of Kreinin et al. In its elementory form the Russian procedure provides for two wells drilled to the bottom of the coal seam. High pressure air is injected into a first well and hot ignition material is placed into a second well. The air injected into the first well will migrate radially outward and a portion of the air will reach the second well, causing ignition of the coal seam and propagation of the underground fire through the coal seam towards the on coming oxygen supply. The air passing through the coal seam proceeds through paths of least resistance, a path that is unknown to the operator except in the most general sort of way. Thus the channel burned as the fire proceeds from the ignition well to the injector well is always something other than a straight line, and often is a path quite circuitous in nature. As long as the burned channel remains near the bottom of a flat coal seam, straightness of the path is not a critical consideration. Should the burned channel have significant deviations in a vertical direction, difficult operating problems will arise later in the production cycle due to flame override.
Linked vertical wells using the Russian procedures work exceptionally well when there is a thin parting in the coal near the bottom of the seam. In this case the oxidizer release point is established in the coal below the parting and the burned channel is thus restrained from migrating upward. Once the reaction zone is well established from the burned channel, the parting is broken by generated heat and roof fall, and the seam is consumed from the bottom up.
In the Russian procedure the linkage burn proceeds as a reverse burn, that is, the burn moves in an opposite direction from the direction of flow of the oxidizer. Once the channel burns through to the oxidizer injection well, permeability to the flow of gases is greatly increased, injection pressure drops significantly and the burn reverses itself and proceeds as a forward burn away from the injection well. In this manner a reaction zone is established in the coal with an oxidizer injected into one well and the products of reaction withdrawn from a second well.
In and around the reaction zone three significant environments are established. At the fire face the environment is highly oxidizing, down stream away from the fire a shortage of oxygen establishes a reducing environment, and the coal adjacent to the fire is subjected to a pyrolyzing environment. In the oxidizing environment coal is consumed and converted into carbon dioxide, sulfur dioxide and water vapor, gases that have little use except for their sensible heat. At these gases proceed down stream into the reducing environment the carbon dioxide is converted to carbon monoxide and the sulfur dioxide is converted into hydrogen sulfide, with further enrichment by the gases of pyrolysis.
There are obvious limits of effectiveness in the Russian system of linkage. A practical limit is established in maximum well spacing due to the requirement of initially injecting the oxidizer in all directions from the injection well. A distant second well might never receive enough oxygen for ignition. Should the path of least resistance between the wells happen to be a path near the top of the seam, flame override and all of its attendant problems are sure to occur. Also in wet coal seams the path of least resistance to air flow normally will be above the water, a situation that sets the stage for flame override.
When a coal seam is an aquifer of significance, it is necessary to lower the water table in the coal. Percolation of water through the coal is quite slow and lowering the water table in a uniform manner is virtually impossible when using pumps to withdraw the water. By placing pumps in sumps below the coal seam the water table can be lowered to the bottom of the seam in the immediate vicinity of the well bore. Water will remain at an angle of repose away from the well bore, and at a point some distance from the well bore, the localized water table can be several feet above the bottom of the coal seam.
In this case of residual water residing in an uneven water table, the path of least resistance to air flow normally is a path that overrides the water. In attempting linkage between two wells using the reverse burn procedure, the resultant linkage channel will stray considerably from the bottom of the seam.
It is possible to substantially remove the free water in a coal seam using procedures as described in U.S. Pat. No. 2,973,811 of Rogers. The methods of Rogers provide for injecting gas such as air into the aquifer under such pressure as necessary to drive the water out of the area of influence. Such pressures are considerable higher than those used in the Russian procedures of linkage, although a certain amount of water displacement occurs in the Russian procedure.
A reasonable amount of free water remaining in a coal seam is beneficial to the reactions of coal gasification, therefore driving all of the free water out of the coal to be gasified is not desirable. Water reacts with hot coal to form carbon monoxide and hydrogen, two desirable gases with heat contents exceeding 300 BTU per standard cubic feet. Water driven out of a coal seam can be made to return by slacking off on pressure. The rate of return, however, is generally too slow to be of commercial interest. Thus it is preferable to leave most of the water in the seam provided linkage can be accomplished at or near the bottom of the seam.
Another method of linkage that is independent of the water content of coal is described in U.S. Pat. No. 4,062,404 of Pasini et al. A well is drilled some distance away from the intended reaction zone and the well is deviated until the bore encounters the underground coal in a direction substantially parallel to the seam. Directional drilling continues along the bottom of the seam for the desired distance planned for the reaction zone. The circuit is completed by drilling a vertical well to intercept the bottom of the deviated hole. Such an arrangement provides a channel at or near the bottom of the seam, but has the disadvantage of difficult and costly drilling procedures.
Still another method of linkage is described in U.K. Pat. No. 756,852 of Montagnon which provides for establishing a permeable channel with a flow of electric current between two points in the coal seam. The flow of electric current is somewhat analogous to the flow of air, in that the current will flow through the path of least electrical resistance. Coal, being a non-homogeneous rock, has unpredictable paths of electrical circuits. Over long distances between electrodes the likelihood increases for the path to stray substantially above the bottom of the coal, resulting in a path that promotes flame override.
Flame override can be a serious detriment to successful production of coal in situ. The natural tendency of a fire is to burn upward as long as there is a source of fuel in that direction. The worst case in the reverse burn procedure for linkage occurs when the injected air migrates to the top of the seam and persists in that location until it nears the location of the lower pressure in the ignition well. The burned channel, for the most part, will lie at the top of the seam. Upon burn through and the establishment of a reaction zone, the two wells will appear initially to be performing satisfactorily, with produced gases containing approximately 170 BTU per standard cubic foot. The first sign of trouble is signalled by a steady drop in the BTU content of produced gas. The reaction zone, with no fuel above it, is gradually becoming engulfed in its own ashes. A partial remedy can be applied by significantly increasing the velocity of the gases through the reaction zone, thus picking up the ashes into the flue gas for removal above ground. Such a procedure defeats one of the purposes of in situ gasification of coal; that is, to leave the ash content of the coal underground. Increased velocities of the oxidizer also aggrevates the oxygen by pass problem where combustible gases are subjected to unplanned burning underground with the resultant destruction of combustible gases. Also, attempting to burn an underground fire downward is something other than a rewarding task.
From the foregoing it is apparent that successful gasification of coal in situ requires reaction zones that begin at the bottom of the coal seam. In this mode the fire has the preponderence of the fuel supply above it and the ashes fall out of the path of the fire as it seeks new fuel. Also from the foregoing it is apparent that a lengthy reaction zone is desirable because the reducing environment portion of the underground channel provides the setting for generation and recovery of combustible gases. In the Russian procedures for linkage and establishment of reaction zones, well spacing is generally limited to short distances in the order of 70 feet. Greater distances between wells is desirable from an economic point of view as well as the desirability of having a longer distance for a reducing environment in the underground channel. Well spacings greater than that of the Russian procedures would provide more favorable economics and provide a setting for improved performance of the in situ reactions. Such lengthened spacing requires a correspondingly effective linkage procedure.
In U.S. Pat. No. 4,010,801 of the present inventor, methods are taught wherein a blind hole burn in coal creates underground channels and reaction zones for the production of coal in situ. The procedures of the present invention extend the teachings of U.S. Pat. No. 4,010,801 to include methods of linking two or more wells by burning channels along the bottom of the coal seam.
SUMMARY OF THE INVENTION
Two wells are drilled from the surface of the earth into and through a coal seam. The wells are hermetically sealed and an oxidizer injection tubing is lowered into each well together with a whipstock. The whipstock is capable of making a 90° bend in the oxidizer injection tubing. The whipstock is set in each case so that the oxidizer injection tubing emerging from the whipstock is aligned toward the opposite well. The coal is set afire and the fire is propagated by an oxidizer injected through the oxidizer injection tubing. The oxidizer is tempered with water vapor to control maximum temperatures of the fire and to provide cooling to the oxidizer injection tubing. Additional oxidizer tubing is inserted in each well as the channel is lengthened through the coal. Linkage between the two wells is thus attained.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a diagrammatical vertical section showing the arrangement of apparatus for the methods of the invention.
FIG. 2 is a diagrammatic plan view of a well pattern and the underground linkage channels.
FIG. 3 is a diagrammatical vertical section showing a well equipped for the methods of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, two wells 10 and 12 are drilled from the surface of the earth 11 through overburden 14, through coal seam 16 and forming sumps 27 and 29 in the underburden. The wells are hermetically sealed, for example by setting a casing to the top of the coal seam 16. A suitable closure 15 is affixed to the well casing. Into well 10 an oxidizer injection tubing 18 is inserted with whipstock 26 emplanted in sump 27 so that the oxidizer injection tubing 18 is bent at an appropriate angle, for example 90°, and the portion of oxidizer injection tubing 18 emerging from whipstock 26 is pointing toward well 12. Initially oxidizer injection tubing will emerge from whipstock 26 only a short distance, for example 2 inches, while the illustration of FIG. 1 shows the oxidizer injection tubing near the final stages of the linkage procedure. Oxidizer injection tubing 18 contains valve 19 for regulation of flow of the oxidizer. Well 10 has fluid withdrawal pipe 22 with valve 23, which permits the products of reactions to be withdrawn from the underground reaction zone and provides a means of applying back pressure control.
Likewise well 12 contains oxidizer injection tubing 20 containing valve 21 with whipstock 28 emplaced in sump 29. Whipstock 28 is set so that tubing 20 is pointed toward well 10 as it emerges from the whipstock. Well 12 has fluid withdrawal pipe 24 which contains valve 25.
Prior to initiating the linkage procedure it is preferred that water withdrawal pumps (not shown) be temporarily installed in sumps 27 and 29 and that the water table be lowered to the bottom of the coal seam in the vicinity of the production wells 10 and 12. When the water table is thus lowered the boundary of the water table 17 is distorted from its normal position. Coal 16A is substantially dry of free water and Coal 16B retains a considerable amount of free water within its void spaces. Such free water in Coal 16B provides a reasonably effective barrier to the migration of gases through the coal. Should linkage between wells 10 and 12 be attempted using the reverse burn technique, the linkage channel tends to occur in Coal 16A above the water table boundary 17. Such a linkage channel deviating a considerable distance above the bottom of the seam considerably reduces the overall efficiency of the underground burn.
After the water table has been lowered in the vicinity of wells 10 and 12 and the oxidizer injection tubings 18 and 20 have been positioned into whipstocks 26 and 28 as previously described, the linkage procedure of the present invention can be initiated. The procedure begins in well 10 by placing suitable ignition material in the lower portion of well 10, for example by opening closure 15 and dropping incandescent charcoal briquettes into the hole. Closure 15 is then returned to its sealed position and oxidizer injection is begun through oxidizer injection tubing 18. While any convenient ignition procedure may be used in the practice of the present invention, by way of example hot charcoal briquettes are used in sufficient quantity to contact the coal seam adjacent to the lower end of tubing 18. By continuing the injection of oxidizer, for example air, through tubing 18, coal 16 will reach its ignition temperature at a location in the path of the oxidizer blast in a relatively short time, for example approximately two to five minutes. Once the coal seam is ignited in a localized area, a channel through the coal is initiated. The channel 30 away from well 10 is lengthened by continuing injection of oxidizer through tubing 18, and by periodically inserting more length to tubing 18 so that the bottom end of tubing 18 remains in reasonable proximity to the burning end 40 of channel 30. In this manner channel 30 may be lengthened from the well bore of well 10 along the bottom of coal 16 for considerable distance, for example as much as several hundred feet. In some cases it may be practical to terminate channel 30 at or near the well bore of well 12, and thus preclude the necessity of initiating a second channel from well 12. Preferably, however, channel 30 is propagated to a point near the midpoint between wells 10 and 12.
In a like manner channel 32 is propagated toward well 10 from well 12 by igniting the coal at the well bore of well 12 and injecting oxidizer through tubing 20. Tubing 20 is lengthened into well 12 as channel 32 is burned toward well 10 and the lower end of tubing 20 is kept in reasonable proximity of burning end 42 of channel 32. Preferably channel 32 is propagated to a point near the midpoint between wells 12 and 10.
It is desirable that channel 30 and channel 32 be propagated until they merge, however it is not necessary that their paths be aligned so precisely. As illustrated in FIG. 2, channels 30 and 32 were imperfectly aligned. As a practical matter the channels may be aligned so that they do not intersect, yet the channels may be joined by an alternate procedure. For example, during the burning of channel 30, oxidizer is injected into tubing 18 and the products of reaction are withdrawn through withdrawal pipe 22. Likewise during the burning of channel 32, oxidizer is injected through tubing 20 and the products of reaction are withdrawn through withdrawal pipe 24. The coal around channels 30 and 32 is at pyrolysis temperature as a result of the underground fires and such coal is giving off the gases of pyrolysis. In a shrinking coal, the permeability of the coal adjacent to channels 30 and 32 is significantly increased. Thus when channels 30 and 32 are burned to points near each other, an alternate procedure can be employed to complete the linkage between burning ends 40 and 42. With the increased permeability in the coal between burning ends 40 and 42 due to pyrolysis, linkage can be completed, for example, by closing valves 19 and 25 and continuing oxidizer injection through tubing 20. Preferably the oxidizer injection pressure is increased, for example an increase in the range of 20% to 200%, in order to provide excess oxidizer. With this arrangement the burn in channel 32 will continue as a forward burn toward channel 30 and the burn in channel 30 will propagate as a reverse burn toward channel 32 until the two channels burn together, thus completing the linkage between wells 10 and 12.
It is preferred that the temperatures in the reaction zones of channels 30 and 32 be controlled to avoid severe damage to the metal parts installed in wells 10 and 12. Generally the temperatures should be in the range of above the ignition temperature of the coal, for example approximately 800° F., to a maximum range of about 1200° F. The maximum temperature of incandescent coal is generally about 2000° F. without flames. This temperature can be lowered to the preferred maximum range of about 1200° F. by injecting appropriate quantities of water into the reaction zone. Such injection of water preferably is done as a mixture of water and oxidizer injected through tubing 18 and 20. Such injection of a mixture of water and oxidizer will keep tubing 18 and 20 sufficiently cool to avoid significant damage to the tubing. Preferably tubing 18 and 20 is of relatively small diameter, for example less than 2", so that they may be properly bent in whipstocks 26 and 28.
Preferably oxidizer injection pressures are kept at relatively low levels, for example in the order of two atmospheres, although the pressures required will vary from site to site. For example in deep seams the hydraulic pressure of the water in Coal 16B may be sufficiently high that water encroachment into burning channels 30 and 32 becomes a problem. The reaction zones in channels 30 and 32 can be destroyed by quenching if encroachment water is permitted to enter the channels in sufficient volumes to reduce the temperature below that required for reaction of fluids with the coal. Thus control is required to limit encroachment of water into the reaction zones. Such control can be applied by increasing oxidizer injection pressures in tubing 18 and 20 while holding back pressure with the proper adjustment of values 23 and 25. By maintaining the pressure in channels 30 and 32 above that of the hydraulic head pressure, water can be excluded from the channels. By maintaining the pressure in the channels slightly below hydrostatic head pressure, free water in Coal 16B can be permitted to enter the channels and thus provide a measure of temperature control in the reaction zones. Such controlled water encroachment can serve as an alternate to injecting water with the oxidizer through tubing 18 and 20.
The emplacement of whipstocks 26 and 28 can be done in several ways. In one method tubing 18 is inserted into whipstock 26 prior to lowering into well 10, with a small length of tubing 18 emerging from the whipstock, for example 2" of tubing protruding outside of the whipstock. A stopper is inserted in the protruded end of tubing 18, such stopper serving as a temporary barrier to fluids entering tubing 18. The assembled unit of whipstock 26 and tubing 18 is lowered in well 10 until the whipstock reaches the bottom of sump 27. The assembled unit then is aligned so that the protruding tubing is pointed toward well 12. A suitable sealant, for example portland cement, is poured into sump 27 and allowed to set. Once the whipstock is thus emplaced, oxidizer is injected into tubing 18 with sufficient pressure to dislodge the stopper, thus permitting ignition and initiation of channel 30. In this method whipstock 26 becomes a permanent installation in well 10, and upon completion of the linkage procedure remains in well 10 as an expendable item.
It is important that tubing 18 and 20 be sufficiently rigid to withstand the compressive forces required to insert additional lengths of tubing into wells 10 and 12 through whipstocks 26 and 28. It is also important that tubing 18 and 20 be sufficiently flexible to be capable of bending through whipstocks 26 and 28 without causing failure to the tubing.
Looking now to well 10 as an example, once the burning of channel 30 is initiated, the hot gases from the reaction zone of channel 30 will significantly raise the temperature of whipstock 26 and tubing 18 located near the bottom of well 10. Such increase in temperature will facilitate the bending of tubing 18 through whipstock 26. Such increase in temperature also lessens the rigidity of tubing 18 between the whipstock and the well head. When the increase in temperature expected to be encountered within well 10 is sufficient to alter the regidity of tubing 18 to the point that the tubing tends to buckle, an alternate procedure should be used in emplacing whipstock 26.
In the alternate emplacing procedure (FIG. 3) a protective pipe 50 is affixed to whipstock 26, such pipe being of larger diameter then tubing 18 so that an annulus 51 is formed between tubing 18 and the protective pipe 50. While it is preferable that all of the tubing to be used as tubing 18 be in one piece, the protective pipe can be in several joints. The first joint of the protective pipe is affixed to whipstock 26 and preferably the protective pipe contains perforations 52 located immediately above whipstock 26. Thus the assembly to be lowered into well 10 contains the whipstock affixed to the protective pipe, tubing 18 inserted into whipstock 26 with a portion of tubing 18 protruding through the whipstock. The assembly is lowered into the well with extra joints of the protective pipe being added as the assembly is lowered. Once the whipstock reaches the bottom of sump 27, the assembly is aligned so that protruding tubing 18 is pointed toward well 12. The protective pipe is equipped with a water injection pipe 53 containing valve 54 and is hermetically sealed at the well head. Once channel 30 is initiated and the temperature of the protective pipe increases substantially, for example up to 250° F., water is injected into the annulus between tubing 18 and the protective pipe with the water flowing out of the perforations in the lower end of the protective pipe. Water flow into the annulus preferably is controlled so that upon exit through the perforation it is in the vapor phase. In this manner the rigidity of tubing 18 can be preserved between the whipstock and the well head.
Maintaining rigidity of tubing 18 between whipstock 26 and its lower end near burning face 40 is not a critical consideration, although some measure of rigidity should be maintained to assure that tubing 18 is capable of being lengthened as burning face 40 recedes into the coal. The cooling effect of the injected oxidizer, particularly when water is mixed with the oxidizer, is generally sufficient to maintain the required measure of rigidity for additional lengths of tubing 18 to be inserted into lengthening channel 30. A measure of flexibility of tubing 18 located in channel 30 is desirable in that by gravity tubing 18 will tend to remain close to the interface between the coal and the underburden. Thus by maintaining the oxygen release point at the bottom of the coal, channel 30 will lengthen at the preferred location. By emplacing the whipstock using a protective pipe affixed to the whipstock, upon completion of the linkage procedure, the whipstock can be removed from the wall.
Using the methods of the present procedure, two wells several hundred feet apart can be linked through the coal, with the linkage channel substantially following the bottom of the coal seam. As a practical matter, however, lengths of the linkage channel should be limited. While it is desirable to have linkage channels sufficiently long to provide an adequate length for a reducing environment, excessive lengths result in the ultimate lowering of the temperature of produced fluids to a point where condensible liquids accumulate in the channel. Excessive accumulations of condensed heavy liquids such as tars can severely restrict the flow of fluids through the underground channels, and in extreme cases the channels can become plugged. Generally the distance between wells should be limited to a maximum distance in the order of 300 feet.
Thus it may be seen that positive control may be applied in the linkage of two production wells with the channel through the coal being formed substantially at the bottom of the coal seam, that such linkage may be accomplished by removing only a part of the free water contained in the coal, and that the problem of flame override can be substantially eliminated by accomplishing such linkage.
While the present invention has been described with a certain degree of particularly, it is understood that the present disclosure has been made by way of example and that changes in detail of structure may be made without departing from the spirit thereof.
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In preparation for producing coal in situ two or more production wells are linked together through the coal seam by burned channels created by one or more blind hole burns.
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FIELD OF THE INVENTION
This invention relates to electrophotographic marking machines. More particularly, it relates to aerially correcting the process direction spot position using an electronically addressable liquid crystal plate.
BACKGROUND OF THE INVENTION
Electrophotographic marking is a well known and commonly used method of copying or printing documents. Electrophotographic marking is performed by exposing a substantially uniformly charged photoreceptor with a light image representation of a desired document. In response to that light image the photoreceptor discharges so as to create an electrostatic latent image of the desired document on the photoreceptor's surface. Toner particles are then deposited onto that latent image to form a toner image. That toner image is then transferred from the photoreceptor onto a copy substrate, such as a sheet of paper. The transferred toner image is then fused to the copy substrate, usually using heat and/or pressure. The surface of the photoreceptor is then cleaned of residual developing material and recharged in preparation for the production of another image.
The foregoing broadly describes a black and white electrophotographic marking machine. Electrophotographic marking can also produce color images by repeating the above process once for each color of toner that is used to make the composite color image. For example, in one color process, called the REaD IOI process (Recharge, Expose, and Develop, Image On Image), a charged photoreceptive surface is exposed to a light image which represents a first color, say black. The resulting electrostatic latent image is then developed with black toner to produce a black toner image. The recharge, expose, and develop process is repeated for a second color, say yellow, then for a third color, say magenta, and finally for a fourth color, say cyan. The various latent images and consequently the color toners are placed in a superimposed registration such that a desired composite color image results. That composite color image is then transferred and fused onto a substrate.
The foregoing color printing process can be performed in a various ways. For example, in a single pass printer wherein a composite image is produced in a single pass of the photoreceptor through the machine. This requires a charging, an exposing, and a developing station for each color of toner. Single pass printers are advantageous in that they are relatively fast since a composite color image can be produced in one cycle of the photoreceptor.
One method of exposing the photoreceptor is to use a Raster Output Scanner (ROS). A ROS is typically comprised of a laser light source (or sources), a rotating polygon having a plurality of mirrored facets, and pre-polygon and post-polygon optical systems. The light source radiates a laser beam into the pre-polygon optical system. The optical system collimates the laser beam and directs the collimated beam onto the rotating polygon facets. Those facets reflect the incoming beam into a sweeping beam that is directed into the post-polygon optical system. The post-polygon optical system corrects for various defects (such as wobble correction and scan line non-linearities) and focuses the sweeping beam onto a photoreceptor, thereby producing a light spot. As the polygon rotates the spot traces lines, referred to as scan lines, on the photoreceptor. By moving the photoreceptor in a process direction (also referred to as the slow scan direction) as the spot traces scan lines in the fast scan direction, the surface of the photoreceptor is raster scanned by the spot. During scanning, the laser beam is modulated by image data synchronized with the movement of the spot across the photoreceptor. Thus, individual picture elements (“pixels”) of the image are sequentially created on the photoreceptor.
While raster output scanners are beneficial, they have problems. One set of problems relates to scan line position errors in the slow scan direction. Scan line position errors of greater than 10% of the nominal line spacing can be noticeable in a half tone or continuous tone image. Because of the sensitivity of the human eye to color variations, color images are even more susceptible to scan line position errors.
Scan line position errors arise from many sources, such as polygon and/or photoreceptor motion flaws, facet and/or photoreceptor surface defects, photoreceptor stretching, and phasing errors between photoreceptor motion and facet position. Phasing errors arise because when the photoreceptor is in the proper position to receive an image a facet may not be in position to produce a scan line. As the printer delays writing a scan line until a facet is properly positioned the photoreceptor continues advancing. When a facet is properly positioned the photoreceptor has advanced, producing a scan line error. While phasing errors are generally small, in high quality systems, particularly color, the errors can be noticeable.
Scan line position errors can be corrected using closely spaced light valves (such as liquid crystal modulators, reflecting Fabry-Perot modulators, total internal reflective modulators, or a waveguide modulator/amplifier) that selectively block portions of a light beam from reaching the photoreceptor. Reference U.S. Pat. No. 5,049,897 issued on Sep. 17, 1991 to Ng entitled “Method and Apparatus for Beam Displacement in a Light Beam Scanner,” and U.S. Pat. No. 5,764,273, issued on Jun. 9, 1998 to Paoli entitled, “Spot Position Control Using a Linear Array of Light Valves.”
The use of closely spaced light valves to selectively block portions of a light beam is a useful technique since the position of a scan line on a photoreceptor is directly controlled by selecting which light valve(s) should pass light. That technique is particularly beneficial for correcting for phasing errors. Unfortunately, prior art techniques of selecting which light value(s) to turn on require the determination of the existence and the extent of scan line position errors. Only then can the proper light valve(s) be selected. U.S. Pat. No. 5,764,273 teaches using a feedback control system comprised of marks on the photoreceptor, a synchronization strobe and sensor, a signal processing circuit, a control apparatus, and a switching circuit that selects the proper light valves. Alternatively, U.S. Pat. No. 5,764,273 teaches using stored data and a switching circuit. U.S. Pat. No. 5,049,897 teaches using an encoder that monitors the web (photoreceptor) speed, phase-locking the raster output polygon motor to the web (photoreceptor), logic circuitry that compares the web (photoreceptor) speed with a predetermined constant, a logic and control unit (LCU) that calculates a potential scan line spacing error and that generates a control signal, and a driver that uses the control signal to select the proper light valve(s) to pass light.
While the prior art techniques of selecting the proper light valve(s) to correct for slow scan spot position errors are beneficial, they are rather complex, costly and/or difficult to implement. This is particularly true when correcting for phasing errors. Thus, a need exists for an improved method of determining which light valve(s) should be selected so as to correct for slow-scan direction spot position errors. Even more beneficial would be a simple, easily implemented method of selecting the proper light valve(s) to pass light when correcting for phasing errors.
SUMMARY OF INVENTION
The principles of the present invention provide for raster output scanner based printers that correct for polygon phasing errors. A printer in accordance with the principles of the present invention includes a laser-based raster output scanner, a moving photoreceptor, a page sensor for sensing the position of an image area on the photoreceptor, a start-of-scan sensor for sensing the start of scan, a light valve array having a plurality of electrically controlled light valves that selectively pass light, and a system controller that selects which light valve(s) that passes light. The system controller initially selects one of the light valves to pass light. When the page sensor senses the beginning of a page the system controller starts selecting sequential light valves, beneficially at a rate that depends upon the motion of the photoreceptor. When the start-of-scan sensor detects a start-of-scan, the system control stops sequencing the light valves. When the sequencing stops the light valve that passed light when the start-of-scan occurred continues to pass light. Beneficially, the system controller continues to monitor the photoreceptor motion. If the photoreceptor motion changes the system controller then selects a light valve such that the scan line moves toward the proper position.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features of the present invention will become apparent as the following description proceeds and upon reference to the drawings, in which:
FIG. 1 is a schematic illustration of a printing apparatus according to the principles of the present invention;
FIG. 2 is a schematic illustration of selected printer elements producing a scan line; and
FIG. 3 is schematically illustrates a system controller selecting a light valve that
DETAILED DESCRIPTION OF THE INVENTION
While the present invention will be described in connection with a preferred embodiment, it should be understood that the present invention is not limited to that embodiment. On the contrary, the scope of the present invention covers all alternatives, modifications, and equivalents as may be included within the spirit and scope of the appended claims.
FIG. 1 illustrates an electrophotographic printing machine 8 that is suitable for use with the principles of the present invention. The printing machine 8 is a single pass, Recharge-Expose-and-Develop, Image-on-Image (Read IOI) printer. However, it is to be understood that the present invention is applicable to many other types of systems. Therefore, it is to be understood that the following description of the printing machine 8 is only to assist the understanding of the principles of the present invention.
The printing machine 8 includes an Active Matrix (AMAT) photoreceptor belt 10 which travels in the direction indicated by the arrow 12 . Belt travel is brought about by mounting the photoreceptor belt about a driven roller 14 and about tension rollers 16 and 18 , and then driving the driven roller 14 with a motor 20 .
As the photoreceptor belt travels each part of it passes through each of the subsequently described process stations. For convenience, a single section of the photoreceptor belt, referred to as the image area, is identified. The image area is that part of the photoreceptor belt which is to receive the various actions and toner layers that produce the final composite color image. While the photoreceptor belt may have numerous image areas, since each image area is processed in the same way a description of the processing of one image area suffices to explain the operation of the printing machine 8 .
The imaging process begins with the image area passing a “precharge” erase lamp 21 that illuminates the image area so as to cause any residual charge which might exist on the image area to be discharged. Such erase lamps are common in high quality systems and their use for initial erasure is well known.
As the photoreceptor belt continues its travel the image area passes a charging station comprised of a DC corotron 22 . The DC corotron charges the image area in preparation for exposure to create a latent image for black toner. For example, the DC corotron might charge the image area to a substantially uniform potential of about −500 volts. It should be understood that the actual charge placed on the photoreceptor will depend upon many variables, such as the black toner mass that is to be developed and the settings of the black development station (see below).
After passing the charging station the image area advances to an exposure station 24 A. At the exposure station the charged image area is exposed to a modulated laser beam 26 A from a raster output scanner 27 A that raster scans the image area such that an electrostatic latent representation of a black image is produced. Significantly, the position of the laser beam 26 A on the photoreceptor is determined for each facet of a rotating, multi-faceted polygon that is within the exposure station. Using the determined position the scan line position is corrected and the laser beam modulation is controlled such that the black latent image is imaged at a known position on the photoreceptor. A more detailed description of the raster output scanner 27 A (as well as the raster output scanners 27 B- 27 D that are discussed below) and the determining and control of the laser beam's position is given subsequently.
Still referring to FIG. 1, after passing the exposure station 24 A the exposed image area with the black latent image passes a black development station 32 that advances black toner 34 onto the image area so as to develop a black toner image. Biasing is such as to effect discharged area development (DAD) of the lower (less negative) of the two voltage levels on the image area. The charged black toner 34 adheres to the exposed areas of the image area, thereby causing the voltage of the illuminated parts of the image area to be about −200 volts. The non-illuminated parts of the image area remain at about −500 volts.
After passing the black development station 32 the image area advances to a recharging station 36 comprised of a DC corotron 38 and an AC scorotron 40 . The recharging station 36 recharges the image area and its black toner layer using a technique known as split recharging. Split recharging is described in U.S. Pat. No. 5,600,430, which issued on Feb. 4, 1997, and which is entitled, “Split Recharge Method and Apparatus for Color Image Formation.” Briefly, the DC corotron 38 overcharges the image area to a voltage level greater than that desired when the image area is recharged, while the AC scorotron 40 reduces that voltage level to that which is desired. Split recharging serves to substantially eliminate voltage differences between toned areas and untoned areas and to reduce the level of residual charge remaining on the previously toned areas. This benefits subsequent development by different toners.
The recharged image area with its black toner layer then advances to an exposure station 24 B. There, a laser beam 26 B from a raster output scanner 27 B exposes the image area to produce an electrostatic latent representation of a yellow image. In a manner similar to that of the laser beam 26 A, the position of the laser beam 26 B on the photoreceptor is determined and controlled, and the laser beam modulated is controlled such that the yellow latent image is in superimposed registration with the black latent image. Again, a more detailed description of the raster output scanners ( 27 A- 27 D) and the determining and control of the laser beam's position are given subsequently.
The now re-exposed image area then advances to a yellow development station 46 that deposits yellow toner 48 onto the image area. After passing the yellow development station the image area advances to a recharging station 50 where a DC scorotron 52 and an AC scorotron 54 split recharge the image area.
An exposure station 24 C then exposes the recharged image area. A modulated laser beam 26 C from a raster output scanner 27 C then exposes the image area to produce an electrostatic latent representation of a magenta image. In a manner similar to that of the laser beams 26 A and 26 B, the position of the laser beam 26 C on the photoreceptor is determined and controlled, and the laser beam 26 C is modulated such that the magenta latent image is in superimposed registration with the black and yellow latent images. Again, a more detailed description of the raster output scanners ( 27 A- 27 D) and the determining and control of the laser beam's position are given subsequently.
After passing the magenta exposure station the now re-exposed image area advances to a magenta development station 56 that deposits magenta toner 58 onto the image area. After passing the magenta development station the image area advances another recharging station 60 where a DC corotron 62 and an AC scorotron 64 split recharge the image area.
The recharged image area with its toner layers then advances to an exposure station 24 D. There, a laser beam 26 D from a raster output scanner 27 D exposes the image area to produce an electrostatic latent representation of a cyan image. A more detailed description of the raster output scanners ( 27 A- 27 D) and the determining and control of the laser beam's position are given subsequently.
After passing the exposure station 24 D the re-exposed image area advances past a cyan development station 66 that deposits cyan toner 68 onto the image area. At this time four colors of toner are on the image area, resulting in a composite color image. However, the composite color toner image is comprised of individual toner particles that have charge potentials that vary widely. Directly transferring such a composite toner image onto a substrate would result in a degraded final image. Therefore it is beneficial to prepare the composite color toner image for transfer.
To prepare the composite toner image for transfer a pretransfer erase lamp 72 discharges the image area to produce a relatively low charge level on the image area. The image area then passes a pretransfer DC scorotron 80 that performs a pre-transfer charging function. The image area continues to advance in the direction 12 past the driven roller 14 . A substrate 82 is then placed over the image area using a sheet feeder (which is not shown). As the image area and substrate continue their travel they pass a transfer corotron 84 that applies positive ions onto the back of the substrate 82 . Those ions attract the negatively charged toner particles onto the substrate.
As the substrate continues its travel is passes a detack corotron 86 . That corotron neutralizes some of the charge on the substrate to assist separation of the substrate from the photoreceptor 10 . As the lip of the substrate 82 moves around the tension roller 18 the lip separates from the photoreceptor. The substrate is then directed into a fuser 90 where a heated fuser roller 92 and a pressure roller 94 create a nip through which the substrate 82 passes. The combination of pressure and heat at the nip causes the composite color toner image to fuse into the substrate. After fusing, a chute, not shown, guides the substrate to a catch tray, also not shown, for removal by an operator.
After the substrate 82 is separated from the photoreceptor belt 10 the image area continues its travel and passes a preclean erase lamp 98 . That lamp neutralizes most of the charge remaining on the photoreceptor belt. After passing the preclean erase lamp the residual toner and/or debris on the photoreceptor is removed at a cleaning station 99 . The image area then passes once again to the precharge erase lamp 21 and the start of another printing cycle.
The printer 8 also includes a system controller 101 that controls the overall operation of the printer. The system controller preferably comprises one or more programmable microprocessors that operate in accordance with a software program stored in a suitable memory. Of importance to understanding the principles of the present invention is that the system controller synchronizes the overall operation of the printer 8 and provides video information to the laser beams 26 A- 26 D.
The system controller also drives the motor 20 such that the photoreceptor 10 advances at a nominal rate. However, because of various factors discussed in the “Background of the Invention,” the absolute position of the image area is not accurately known. In particular, since the polygon rotation is not synchronized with the photoreceptor motion a facet is not necessarily in position to write a scan line when the image area is in position (hence phasing errors). The printer 8 addresses phasing error problems using printer elements shown in FIG. 2 .
As shown in FIG. 2, a generic raster output scanner 27 includes a laser diode 206 that produces a laser beam 26 . As emitted the laser beam 26 is diverging. A spherical lens 214 collimates the divergent beam and while a polarizing filter 215 polarizes the collimated beam. The polarized and collimated laser beam illuminates a liquid crystal array 216 that is comprised of a plurality of closely space, individually selectable, liquid crystal elements. The liquid crystal array includes a common (shared) back electrode and a plurality of front electrodes, one for each liquid crystal element. In a manner that is subsequently explained, the system controller 101 selects one (other systems may select more than one) liquid crystal element to pass the laser beam. The system controller then applies an excitation voltage to the selected liquid crystal element. That excitation voltage causes the liquid crystals of the selected liquid crystal element to align themselves orthogonal to the electrode. The result in that the portion of the polarized laser beam 26 that illuminates the selected liquid crystal element passes through the selected element without rotation. However, the potions of the polarized laser beam 26 that illuminates the unselected liquid crystal elements are rotated 90°. For example, FIG. 2 shows an upper laser beam 26 A and a lower laser beam 26 B. If the system controller applies an excitation voltage to an “upper” front electrode the laser beam 26 A passes through the selected upper element without a polarization shift. Alternatively, if a “lower” liquid crystal element is selected the laser beam 26 B passes through the selected lower liquid crystal element without a polarization shift.
After passing through the liquid crystal array 216 the laser beam illuminates a polarizer plate 218 . The polarizer plate is aligned such that it passes the portion of the polarized laser beam that passed through the selected liquid crystal element. The other portions of the laser beam 26 are blocked by the polarizer plate. Thus, by selecting various liquid crystal elements the system controller 101 controls where the laser beam emerges from the polarizer plate 218 . FIG. 2 shows the laser beam 26 A emerging.
Light passed by the polarizer plate 218 passes through a cylindrical lens 220 that focuses the beam in the slow scan (process) direction onto a polygon 222 having a plurality of mirrored facets 224 . The polygon 222 rotates in the direction 226 . This rotation causes the laser beam 26 to sweep in a scan plane. The sweeping laser beam passes through a post-scan optics system 228 that reconfigures the beam into a circular (or elliptical) cross-section and that refocuses that laser beam 26 onto the surface of the photoreceptor 10 . The post-scan optics also corrects for various problems such as scan non-linearity (f-theta correction) and wobble (scanner motion or facet errors). The laser beam produces a light spot that sweeps across the photoreceptor in the direction 103 , thereby tracing a scan line 230 .
The liquid crystal element selected by the system controller 101 influences the slow scan (process) direction position of the scan line 230 . For example, if the system controller selected a different liquid crystal element the relative position of the scan line 230 on the photoreceptor would change to that of scan line 230 ′. That change would depend upon the separation of the individual liquid crystal elements and on the system's magnification. For example, in one embodiment, if the system controller switches between liquid crystal elements that are separated by 100 microns, the scan line moves 60 microns on the photoreceptor.
The principles of the present invention relate to selecting the individual liquid crystal element or elements that pass the laser beam without a polarization rotation. For example, the printing machine 8 corrects for phasing errors by selecting among the individual liquid crystal elements. Phasing error correction corrects for the spatial difference caused by photoreceptor motion (in the direction 12 ) during the time between when the image area is in position and when a facet is in position. The mechanics of that correction is described below.
To sense when an image area is in position the printer 8 includes a page sensor 304 . The page sensor senses light 306 , from a light source 308 that passes through a slot 310 in the photoreceptor. When light is sensed the page sensor signals the system controller 101 . The system controller uses page sensor signals to know when to expose and image. The image area is exposed to produce a black image after one page sensor signal, then the image area is exposed to produce a yellow image at the next page sensor signal, and so on. Thus, the page sensor signals are used to register the individual exposures.
The printer 8 also includes a start-of-scan sensor 312 . The start-of-scan sensor signals the system controller 101 when the laser beam 26 begins to sweep across the sensor. From the start-of-scan signals the system controller 101 knows the exact position of the polygon at an instant in time.
Still referring to FIG. 2, the printer 8 further includes a motion sensor 432 that senses a plurality of evenly spaced marks 430 on the photoreceptor. The motion sensor outputs motion signals at a rate that depends upon the motion of the photoreceptor. If the photoreceptor motion increases, so does the rate of the motion signals.
Turning now to FIG. 3, the system controller 101 uses the page sensor signals, the start-of-scan sensor signals, and the motion signals to select which of the individual liquid crystal element(s) pass light. The system controller 101 includes N liquid crystal element control lines, the lines 402 A through 402 N. When an excitation voltage is applied to a particular control line an associated liquid crystal element passes light.
In operation, a Liquid Crystal Element Select network 422 within the system controller 101 initially “parks” the laser beam 26 at a predetermined position on the photoreceptor 10 by applying an excitation voltage to a control line 402 A. The system controller then determines how many motion signals occur between start-of-scan signals. That number is then divided by N (the number of liquid crystal elements), resulting in a number W. when a page signal is received a clock 420 begins counting the motion signals. After W motion signals the clock applies a step signal to the Liquid Crystal Element Select network 422 . The Liquid Crystal Element Select network 422 then moves the excitation voltage from control line 402 A to control line 402 B. After W more motion signals, the excitation voltage moves to 402 C. This process continues until a start-of-scan signal occurs. The Liquid Crystal Element Select network then holds the excitation voltage on the control line that was excited when a start-of-scan signal occurred. After the image is fully exposed the Liquid Crystal Element Select network once again parks the laser beam at a predetermined position until another page sensor signal occurs.
Tracking photoreceptor motion using motion signals and “locking” the excitation on a particular control line when a start-of-scan signal occurs is beneficial for correcting for phasing errors. However, the printer 8 also corrects for motion errors after the phasing errors are corrected. The system controller accomplishes this by tracking the motion signals. If the motion signals occur at a constant rate the system controller 101 knows that the photoreceptor motion is constant. However, if the motion signal rate changes the system controller knows that the motion of the photoreceptor has changed. In that case, the Liquid Crystal Element Select network steps the excitation voltage onto the control line that would bring the scan line back toward the proper position. That is, the position that would be proper if the photoreceptor motion was constant.
While the principles of the present invention have been described in conjunction with a specific embodiment, many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, the present invention is intended to embrace all alternatives, modifications and variations that fall within the spirit and scope of the claims.
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Printers that correct for polygon phasing errors. Such printers include a raster output scanner, a moving photoreceptor, a page sensor for sensing the position of an image area, a start-of-scan sensor for sensing the start of scan, a light valve array having a plurality of electrically controlled light valves for selectively passing light, and a system controller that controls the light valve(s). The system controller initially selects one of the light valves. When the page sensor senses the beginning of a page the system controller starts selecting sequential light valves at a controlled rate. After a start-of-scan occurs the system controller stops sequencing the light valves. The light valve that passed light when the start-of-scan occurred continues to pass light. Beneficially, the system controller monitors the photoreceptor motion. If the photoreceptor motion changes the system controller then selects a light valve that moves the scan line toward the proper position.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from the United States provisional patent application entitled DISCONNECT CABINET AND RECOMBINER BOX WITH WIRELESS MONITORING CAPABILITY, which was filed on May 3, 2013, and assigned the Ser. No. 61/818,940.
[0002] This application is being filed concurrently with a United States utility patent application entitled DISCONNECT CABINET WITH WIRELESS MONITORING CAPABILITY, which also claims priority from the provisional patent application entitled DISCONNECT CABINET AND RECOMBINER BOX WITH WIRELESS MONITORING CAPABILITY, which was filed on May 3, 2013, and assigned the Ser. No. 61/818,940. This co-pending application has a serial number of ______, and is hereby incorporated by reference in its entirety.
BACKGROUND
[0003] 1. Field
[0004] The present invention relates generally to components used in solar fields, and more particularly, to a master recombiner box that combines DC power from downstream combiner boxes, monitors the power coming from those combiner boxes, and wirelessly transmits data related to that monitoring.
[0005] 2. Related Art
[0006] A utility grade solar installation typically includes a plurality of solar collectors electrically grouped in an array. Direct Current (DC) power from each solar collector in the array is combined in a combiner box. A plurality of combiner boxes are electronically coupled to a recombiner box, which further combines the DC power. A plurality of recombiner boxes feed into an inverter, which converts the DC power into Alternating Current (AC) power, which is subsequently transmitted via power lines.
[0007] A variety of problems may decrease the power production of a given solar field. For example, individual solar collectors may be damaged, shaded, or have faulty connections such that power is not produced, is inadequately produced, or the generated power never makes it to the collector. Fortunately, technology for monitoring individual collectors, or small groups of collectors, is known. This technology is disclosed in U.S. patent application Ser. No. 12/871,234, having a filing date of Aug. 30, 2010, which is hereby incorporated by reference in its entirety.
[0008] Unfortunately however, this known technology is unable to handle high current, defined here as 100-600 amps. As a result, a solar field operator is effectively “flying blind” with respect to their combiner boxes in the field. Combiner box level disruptions are significant, and negatively affect the overall production and efficiency of the solar field.
[0009] Thus, there remains a need for a system that can monitor combiner box-level power. It is desirable that this system is capable of handling current in the 100-600 amp range. It is desirable that this system is integrated into a recombiner box. It is desirable that this system is capable of wirelessly transmitting data to a user. It is also desirable that this system optionally includes an integrated disconnect system.
SUMMARY OF THE INVENTIONS
[0010] The present invention combines and optionally monitors the current and voltage output of combiner and/or recombiner boxes in the solar field. This is accomplished using an assembly having multiple bus bars and sensors, as well as a control circuit board and antenna. The power from the solar field is combined in the present invention, then transferred to the inverter where it is changed from DC to AC. The invention optionally includes a disconnect switch for disconnecting the power from the output.
[0011] This invention is configured to monitor up to 20 different inputs from associated recombiner boxes. This allows a user to monitor the power output, so they know where there is a reduction in production and where maintenance is required. This invention can employ disconnect switches or circuit breakers to open the power supply circuit. The power is monitored by individual current transducers (CTs) and the monitoring control circuit board which are mounted inside a cabinet. The data from the CTs are encoded and transmitted by a radio frequency (RF) transmitter to the local computer on site. This data can then be evaluated from any computer on the internet with the correct security codes.
[0012] The ability to monitor up to 20 input circuits is accomplished by having fuses positioned on opposing sides of two bus bar. The monitoring is preferably performed on inputs having circuit protection fuses. This can be one or both inputs into the cabinet for a floating ground system. The monitoring system is powered by an external power supply.
[0013] One side of the power circuit is preferably routed through a disconnect device, and the other is attached to the bus bars at the bottom of the cabinet. A ground wire for each combiner box circuit can be landed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is the front view of a recombiner box system having monitoring capability with the cabinet open;
[0015] FIG. 2 is the front view of a recombiner box system without monitoring capability with the cabinet open;
[0016] FIG. 3 is a control circuit board with associated structures;
[0017] FIG. 4 is a schematic of a control circuit board,
[0018] FIG. 5 is a power supply for the monitoring component of the system;
[0019] FIG. 6 is right side view of recombiner box without monitoring;
[0020] FIG. 7 is left side view of recombiner box without monitoring; and
[0021] FIG. 8 is a front view of a recombiner box system with safety shields in place.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0022] In the following description, like reference characters designate like or corresponding parts throughout the several views.
[0023] The following terms will apply:
10 —Recombiner box system; 20 —Cabinet; 22 —Door; 24 —Hinge; 25 —Safety shield; 26 —Housing; 27 —Conduit; 28 —Conduit clamp; 29 —Backpanel 30 —Input bus bar; 35 —Fuse; 40 —Recombining bus bar; 45 —Disconnect switch; 50 —Output bus bar; 51 —Unfused combining bus bar 52 —Earth Ground bus bar 55 —Surge protector; 60 —Control circuit board; 62 —Power supply; 63 —Power input; 64 —Current transducer input; 65 —Current transducer (“CT”); 68 —Output to antenna; 70 —Antenna; 72 —Receiver; and 73 —Processor.
[0050] As shown in FIG. 1 , recombiner box system 10 is generally contained within cabinet 20 having housing 26 connected at hinge 24 to door 22 . Housing 26 is preferably mounted to a substantially horizontal and stationary surface, such as a floor. Door 22 is configured to mate with housing 26 in order to provide a substantially enclosed space there within, such that internal structures are protected from ambient environment and people.
[0051] The majority of components and structures of the system are positioned within housing 26 , with the exception of control circuit board 60 , which is preferably mounted on door 22 .
[0052] DC power from individual combiner boxes (not shown) enters system 10 at input bus bars 30 . One combiner box is coupled with one input bus bar 30 . A given system can be configured to have up to 20 input bus bars, corresponding with 20 combiner boxes. Each input to the bus bar is routed through an individual current transducer (CT) 65 . In this manner, each power output of each upstream combiner box is monitored. Power travels from input bus bar 30 , through fuse 35 , to recombiner bus bar 40 , where power is combined with power coming from other input bus bars of the system.
[0053] A suitable input bus bar is copper bus bar sized to carry the required current plated to prevent corrosion. A suitable fuse is SPFJ Series, Littlefuse, Chicago, Illinois. A suitable recombiner bus bar is copper bus bar sized to carry the required current plated to prevent corrosion.
[0054] Power from recombiner bus bar 40 goes to output bus bar 50 , then to an inverter (not shown) for conversion to AC power. Disconnect switch 65 is preferably positioned in pathway between recombiner bus bar 40 and output bus bar 50 . It is preferable to use a linkage assembly with disconnect switch, such as that disclosed in concurrently filed US application , previously noted as incorporated herein.
[0055] As shown in FIG. 1 , system 10 preferably also includes power supply 62 for powering control circuit board 60 , and surge protector 55 . A suitable power supply is CP-E series by ABB, Wichita Falls, Tex. A suitable surge protector is DS50PVS series by Citel, Miramar, Fla. Conduit clamp 28 provides a pathway for conduit 27 between door and housing, best shown in FIG. 1 . The ground wire is noted in FIG. 8 .
[0056] As shown in FIG. 2 , an embodiment of the present invention is a recombiner box without monitoring capability. More specifically this embodiment is substantially the same as the embodiment depicted in FIG. 1 , but lacks power associated structures such as disconnect switch 45 , control circuit board 60 , CTs 65 , and power supply 62 . Labels (not numbered) are preferably positioned to the left of hinge.
[0057] In the monitoring embodiment of FIG. 1 , the current and voltage of each combiner box that is coupled to the system is measured by an associated CT 65 . Block diagram of FIG. 4 shows how voltage is measured. As shown in FIG. 3 , control circuit board 60 receives CT input 64 , and this information is ultimately transmitted through output to antenna 68 . Antenna 70 is best shown in FIG. 1 . In the manner conventional for RF transmissions, RF waves (not shown) are transmitted via antenna 70 , and received by receiver 72 (not shown). Processor 73 (not shown) is communicatively coupled with receiver 72 , and displays information such as decreases in current of a specific combiner box. Access to this information may be facilitated by web-based software, so a user can access data through the internet. Access may be password protected, so only authorized users can access the software or information. Different users may be granted different levels of access, depending on their need-to-know. Users may be alerted to certain events, such as significant decreases in power production, by text messages, email messages, instant messaging, or other means.
[0058] A schematic of control circuit board 60 is set forth in FIG. 4 .
[0059] FIG. 5 is power supply 62 for running control circuit board 60 . Power is supplied form an external source and stepped down to the level required for the circuit board.
[0060] FIG. 6 depicts the right side of the cabinet with the side wall removed, and in particular, the earth ground bus bar and the unfused bus bar.
[0061] FIG. 7 depicts the left side of the cabinet with the side wall removed.
[0062] FIG. 8 depicts cabinet 20 with safety shields 25 attached. Safety shields 25 introduce a barrier between the high-powered system, and those who may accidentally come in contact with it. Once all the requisite connections are made, for example combiner boxes are electrically coupled to input bus bars, safety shields 25 are fitted in the inside areas of the housing and door, and the door is closed.
[0063] In use, a plurality of solar panels is connected to a combiner box. A plurality of combiner boxes is connected to a recombiner box of the present invention. The present invention receives power from each individual combiner box via the input bus bars. The input bus bars include current transducers that monitor the power of the corresponding combiner box. The power to the input bus bars is combined at the recombiner bus bar. The recombiner bus bar power is transmitted to the ouput bus bar, and subsequently goes to an inverter. The current transducers are connected to a control circuit board, which is coupled to an antenna for transmitting data via an RF signal. This RF signal is received at a location away from the recombiner box, processed, and alerts can be sent if appropriate. An example of an alert would be a user receiving a text message that there is a 98% reduction in power generated at combiner box ABC123.
[0064] Certain modifications and improvements will occur to those skilled in the art upon a reading of the foregoing description. By way of example, while this system is specifically designed for high amperage (100-600 amps) applications, it could be used with lower amperage applications. With modifications it could be used with even higher amperage (>600 amps) applications. Also, as used herein, “combiner boxes” and “recombiner boxes” may be interchangeable, depending on the configuration of a specific solar field. Also, the software and algorithms that analyze and display information can vary and have very simple, or very elaborate features. Also, recombiner box could provide arc fault detection. The system is able to deploy in positively grounded, negatively grounded, floating grounded, and bi-polar systems with minor internal modifications.
[0065] It should be understood that many modifications and improvements have been deleted herein for the sake of conciseness and readability but are properly within the scope of the following claims. It should also be understood that the illustrations are for the purpose of describing a preferred embodiment of the inventions and are not intended to limit the inventions thereto. It should also be understood that approximations allow variances of +/−10%, unless otherwise noted. As used herein, “substantially” and the like shall mean that the statement is generally true, notwithstanding minor variances due to materials, unusual properties or situations, irregularities, human limitations, expected human behavior, and so forth. By way of example, “substantially permanently attached” would mean an attachment would sustain regular usage, but could be separated through unusual effort. It should also be understood that all ranges set forth inherently include the endpoints themselves, as well as all increments, therebetween.
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A master recombiner box system includes a plurality of input bus bars that receive power from a corresponding combiner box in a solar field. Each input bus bar is coupled with a current transducer, thereby measuring the current of the associated combiner box. Power feeding into the plurality of input bus bars is combined at a recombiner bus bar, which leads to an output bus bar, and ultimately to an external inverter. The current transducers are linked to a control circuit board which utilizes an antenna to send RF signals to a receiver. In this manner individual combiner boxes in a solar field can be monitored wirelessly.
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RELATED APPLICATIONS
[0001] This application is a continuation in part and claims priority to U.S. Provisional Application No. 60/763,018 filed on Jan. 27, 2006 entitled “Shock Wave Treatment and Method of Use” and also claims priority to U.S. 60/688,927 filed on Jun. 9, 2005 entitled “Pressure Pulse/Shock Wave Therapy Methods for Organs” and to U.S. Ser. No. 11/238,731 filed on Sep. 29, 2005 entitled “Pressure Pulse/Shock Wave Therapy Methods for Organs”.
FIELD OF THE INVENTION
[0002] The present invention relates to a method and a device for generating shock waves generally, more specifically to a method and device for treating internal organs or tissue.
BACKGROUND OF THE INVENTION
[0003] The use of shock waves to treat various conditions affecting the bone or soft tissues of a mammal, usually a human is known.
[0004] Shock waves produce a high energy pulse that when focused can pulverize hard calcium deposits such as kidney stones. This technology is commonly and very successfully employed in lithotripsy.
[0005] More recently, the use of shock waves has been employed in the art of healing non union bone fractures and in treating soft tissues and organs extracorporeally in a non-invasive manner.
[0006] The pressure pulse or wave form when applied was thought to require a high energy to achieve a deep penetration to an affected organ, as a result focused beams were transmitted that had a focal point or region set at a distance deep enough to penetrate the underlying organ or tissue. It was believed that the skeletal system of hard bone mass greatly dampened the wave pattern making it difficult to treat such organs as the heart.
[0007] In U.S. Pat. No. 6,755,821 B1 entitled “A System and Method for Stimulation and/or Enhancement of Myocardial Angiogenesis” a proposed solution to treating the heart using shock waves was proposed. Shock-waves were applied using a combination lithotripsy probe/balloon system, comprising a needle and cannular balloon which can be inserted through the skin at a point between the ribs into the cavity beneath the chest wall and overlying the heart. Alternatively, the shock-wave can be administered extracorporeally or via a catheter. A fluid injector was connected to the balloon, allowing it to be inflated with saline or other appropriate fluid to fill the space (for transmission of shock waves and/or to displace tissue—such as lung) and contact the surface of the heart. A shock-wave (acoustic) generator was used to generate shock-waves through the lithotripsy probe, through the fluid and into the myocardial tissue. The fluid provides a uniform medium for transmission of the acoustic energy, allowing precise focus and direction of the shock-wave to induce repeatable cavitation events, producing small fissures which are created by the cavitation bubbles. In this case, channels would not be ‘drilled’ into the heart muscle, minimizing trauma to the tissue while still creating conditions that will stimulate increased expression of angiogenic growth factors.
[0008] The concept in U.S. Pat. No. 6,755,821 provides an alternative to procedures in place today that rely on lasers. As stated in the above referenced patent.
[0009] “Transmyocardial revascularization (TMR) using a laser (sometimes referred to as TMLR, LTMR, PMR, PTMR, or DMR) has been developed over the past decade, initially by a company called PLC Systems, Inc., of Franklin, Mass. PLC's system utilizes a high power (800-1000 W) carbon dioxide (CO.sub.2) laser which drills small channels in the outside (epicardial) surface of the myocardium in a surgical procedure. The holes communicate with the left ventricle, which delivers blood directly to the heart muscle, mimicking the reptilian heart. Many other companies are developing laser TMR systems, most introducing the laser light via optical fibers through a flexible catheter, making the procedure less-invasive. These companies include Eclipse Surgical Technologies, Inc., of Sunnyvale, Calif., and Helionetics, Inc., of Van Nuys, Calif. The Eclipse TMR system uses a Ho:YAG laser with a catheter-delivered fiber optic probe for contact delivery to the myocardium. The Helionetics system is based on an excimer laser. In addition to the holmium:YAG and excimer lasers, and other types of lasers have been proposed for TMR.
[0000] While the channels created during TMR are known to close within 2-4 weeks, most patients tend to improve clinically over a period of 2-6 months.
[0010] Such clinical improvement may be demonstrated by reduction in chest pain (“angina”), and a dramatic increase in exercise tolerance (“ETT”, or treadmill test). The mechanism of laser TMR is not fully understood, but it is postulated that the laser causes near-term relief of angina through denervation or patent channels, with subsequent long-term clinical improvement due to angiogenesis, i.e., growth of new blood vessels, mainly capillaries, which perfuse the heart muscle. These new “collateral” vessels enable blood to reach downstream (“distal”) ischemic tissues, despite blockages in the coronary arteries. Some of the possible mechanisms by which the laser induces angiogenesis could include activation of growth factors by light, thermal, mechanical, cavitational or shockwave means. In fact, all lasers which have been successfully used for TMR are pulsed systems, and are known to create shock waves in tissue, and resulting cavitation effects.”
[0011] The problem of delivery of a shock wave to an internal organ is more complex than simply avoiding bone tissue. In the case of treating the heart special care must be taken to avoid damaging the thin membrane of the nearby lung. Shock waves inadvertently transmitted to this area can cause bleeding and other damage.
[0012] Another problem for the use of shock waves is internal organs are three dimensional masses that in the case of the heart need the waves to be directed from two sides front and back, more preferably from at least three directions.
[0013] Accordingly the devices such as the laser or the shock wave system of U.S. Pat. No. 6,755,821 are limited to one surface of the heart or would require multiple points of entry.
[0014] The team of inventors of the present invention has developed both a device and a methodology for treating an internal organ which addresses these limitations and provides a multiple direction system for delivering shock waves.
SUMMARY OF THE INVENTION
[0015] The system for treating an internal organ has a generator source for producing a shock wave connected to a handheld or otherwise small shock wave applicator device, wherein the shock wave applicator device has a side-firing shock wave head having a variable angle adjustment relative to a release and lock connected handle or holder means for holding said device. The inclination of the shock wave head can be set to a fixed inclination to reach the organ at various locations or surfaces or can be pivotally inclined continuous to vary the treatment surface area.
[0016] The pulse or wave propagation being emitted from the head on a sideways direction relative to the holder means enables the surgeon to rotate the head about a longitudinal axis of the holder or tilt the head relative to the length of the holder providing an infinite number of angular choices for emitting the wave pattern. The device may employ acoustic shock waves from electromagnetic or piezo electric, ballistic or electro hydraulic sources or generators.
[0017] In a preferred embodiment the head portion or end includes two electrodes or two tips in one assembly of an electrode as is described in U.S. Pat. No. 6,217,531 and is commercially available under the trade name Smarttrode to create a shock wave generating spark, and the head portion further includes a reflector for redirecting and shaping the wave pattern. The head is preferably round or oval of a small geometric size sufficient to be positioned under or around the soft tissue of an organ to permit access around the periphery of the organ being treated. Alternatively the reflector and head of the applicator can be an oval of more ellipsoidal shape with the major axis lying along the longitudinal axis of the device. In such a case the minor diameter transverse to the longitudinal axis can be made 3 cm or preferably 2 cm or less. The device can further include an integral shielding means which would insure the only emitted shockwave energy was directed outward from the front cover or membrane of the shock wave head. The shielding means preferably would be an air cushion covering at least the back and preferably the sides of the applicator head to dissipate any transmitted energy. This is particularly useful to prevent damage to the thin lung membrane during an open heart procedure. Alternatively the shielding means can be made a part of a sterile sleeve or even a separate sterile layer positioned between the treated heart and the underlying lung. In one embodiment the device is disposable intended for one time use.
[0018] The applicator device may be used by placing it inside a disposable sterile sleeve or cover. In such a case the applicator can be simply cleaned with a disinfecting agent prior to use as it is not directly exposed to the tissue. Alternatively the applicator without a sleeve or cover can be used wherein the applicator should be sterilized prior to use. In either use the sleeve or cover or the applicator without a cover should be coupled acoustically to the treated tissue or organ by a sterile coupling fluid or viscous gel like ultrasound gels or even NaCl solution to avoid transmission loss.
[0019] The method of employing the shock wave applicator device comprises the steps of providing an at least partially exposed or direct access portal to an organ, activating an acoustic shock wave generator or source to emit acoustic shock waves from a shock wave applicator head of a shock wave applicator; and subjecting the organ to the acoustic shock waves stimulating said organ wherein the organ is positioned within an unobstructed path of the emitted shock waves, positioning the shock wave head adjacent to and on an inclination relative to the organ, firing the electrodes and emitting a shock wave pattern in a generally transverse direction relative to the applicator. The method further comprises repositioning the shock wave head at a second position or inclination and firing the electrode. The step of positioning the applicator may further include setting a holding means at an angle between 0° and about 360° more typically between 0° and 180° relative to the applicator prior the firing the electrodes, the holder means being a pivotable handle. In one embodiment the emitted shock waves are divergent or near planar. In another embodiment the emitted shock waves are convergent having a geometric focal volume or focal point at a distance of at least X from the source, the method further comprising positioning the organ at a distance at or less than the distance X from the source. The organ is a tissue having cells. The tissue can be an organ of a mammal. The mammal may be a human or an animal. The organ may be a heart, a brain, a liver or a kidney or any other organ with associated other types of tissue. The tissue may be a part of the vascular system, a part of the nervous system, a part of the urinary or reproductive system.
[0020] The method of stimulating an organ can further include a result wherein the step of subjecting the organ to acoustic shock waves stimulates at least some of said cells within said organ to release or produce one or more of nitric oxygen (NO), vessel endothelial growth factor (VEGF), bone morphogenetic protein (BMP) or other growth factors.
[0021] The organ can be a tissue having a pathological condition, a tissue having been subjected to a prior trauma, a tissue having been subjected to an operative procedure, or a tissue in a degenerative condition. The organ is at least partially surgically exposed if not removed from the patient during the exposure to an unobstructed shock wave treatment.
[0022] The method may further include the steps as activating the applicator device to transmit the shock wave pulses in response to a repetitive body or organ function. In particular the method may include triggering the shock wave pulse during the R phase of the QRS and T curve or the contraction of a heart wherein the R phase is that portion of the heartbeat depicted by and including the peak amplitude on an ECG monitored display. This controlled pulse triggering avoids irregular heartbeat patterns from being stimulated by the transmission of the shockwave pulses.
[0000] Definitions
[0023] “cirrhosis” liver disease characterized pathologically by loss of the normal microscopic lobular architecture, with fibrosis and nodular regeneration. The term is sometimes used to refer to chronic interstitial inflammation of any organ.
[0024] A “curved emitter” is an emitter having a curved reflecting (or focusing) or emitting surface and includes, but is not limited to, emitters having ellipsoidal, parabolic, quasi parabolic (general paraboloid) or spherical reflector/reflecting or emitting elements. Curved emitters having a curved reflecting or focusing element generally produce waves having focused wave fronts, while curved emitters having a curved emitting surfaces generally produce wave having divergent wave fronts.
[0025] “Divergent waves” in the context of the present invention are all waves which are not focused and are not plane or nearly plane. Divergent waves also include waves which only seem to have a focus or source from which the waves are transmitted. The wave fronts of divergent waves have divergent characteristics. Divergent waves can be created in many different ways, for example: A focused wave will become divergent once it has passed through the focal point. Spherical waves are also included in this definition of divergent waves and have wave fronts with divergent characteristics.
[0026] “extracorporeal” occurring or generated outside the living body.
[0027] A “generalized paraboloid” according to the present invention is also a three-dimensional bowl. In two dimensions (in Cartesian coordinates, x and y) the formula y n =2px [with n being ≠2, but being greater than about 1.2 and smaller than 2, or greater than 2 but smaller than about 2.8]. In a generalized paraboloid, the characteristics of the wave fronts created by electrodes located within the generalized paraboloid may be corrected by the selection of (p(−z,+z)), with z being a measure for the burn down of an electrode, and n, so that phenomena including, but not limited to, burn down of the tip of an electrode (−z,+z) and/or disturbances caused by diffraction at the aperture of the paraboloid are compensated for.
[0028] “myocardial infarction” infarction of the myocardium that results typically from coronary occlusion, that may be marked by sudden chest pain, shortness of breath, nausea and loss of consciousness, and that sometimes results in death.
[0029] “open heart” of, relating to, or performed on a heart which could be temporarily relieved of circulatory function and surgically opened for inspection and treatment.
[0030] A “paraboloid” according to the present invention is a three-dimensional reflecting bowl. In two dimensions (in Cartesian coordinates, x and y) the formula y 2 =2px, wherein p/2 is the distance of the focal point of the paraboloid from its apex, defines the paraboloid. Rotation of the two-dimensional figure defined by this formula around its longitudinal axis generates a de facto paraboloid.
[0031] “Plane waves” are sometimes also called flat or even waves. Their wave fronts have plane characteristics (also called even or parallel characteristics). The amplitude in a wave front is constant and the “curvature” is flat (that is why these waves are sometimes called flat waves). Plane waves do not have a focus to which their fronts move (focused) or from which the fronts are emitted (divergent). “Nearly plane waves” also do not have a focus to which their fronts move (focused) or from which the fronts are emitted (divergent). The amplitude of their wave fronts (having “nearly plane” characteristics) is approximating the constancy of plain waves. “Nearly plane” waves can be emitted by generators having pressure pulse/shock wave generating elements with flat emitters or curved emitters. Curved emitters may comprise a generalized paraboloid that allows waves having nearly plane characteristics to be emitted.
[0032] A “pressure pulse” according to the present invention is an acoustic pulse which includes several cycles of positive and negative pressure. The amplitude of the positive part of such a cycle should be above about 0.1 MPa and its time duration is from below a microsecond to about a second. Rise times of the positive part of the first pressure cycle may be in the range of nano-seconds (ns) up to some milli-seconds (ms). Very fast pressure pulses are called shock waves. Shock waves used in medical applications do have amplitudes above 0.1 MPa and rise times of the amplitude are below 100 ns. The duration of a shock wave is typically below 1-3 micro-seconds (μs) for the positive part of a cycle and typically above some micro-seconds for the negative part of a cycle.
[0033] Waves/wave fronts described as being “focused” or “having focusing characteristics” means in the context of the present invention that the respective waves or wave fronts are traveling and increase their amplitude in direction of the focal point. Per definition the energy of the wave will be at a maximum in the focal point or, if there is a focal shift in this point, the energy is at a maximum near the geometrical focal point. Both the maximum energy and the maximal pressure amplitude may be used to define the focal point.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] The invention will be described by way of example and with reference to the accompanying drawings in which:
[0035] FIG. 1 is a perspective view of the shock wave applicator according to the present invention.
[0036] FIG. 2 is a second perspective view showing the pivotable handle rotated 180° toward the shock wave head end of the device.
[0037] FIG. 3 is a third perspective view with a portion of the housing and handle removed exposing the internal components.
[0038] FIG. 4 is a plan view of the shock wave applicator internal components with the external housing and handle removed.
[0039] FIG. 5 is an exploded view of a portion of the handle and the pivot pin according to one embodiment of the invention.
[0040] FIG. 6 is a perspective view of a sterile prophylactic sleeve for use with the applicator.
[0041] FIG. 7 is a perspective view of a frontal region of a heart being shock wave treated by a shock wave head according to the method of the present invention.
[0042] FIG. 8 is a perspective view of the posterior region of a heart being shock wave treated according to the present inventive method.
[0043] FIG. 9 is a perspective view of a brain being shock wave treated according to the method of the present invention.
[0044] FIG. 10 is a perspective view of a liver being shock wave treated according to the method of the present invention.
[0045] FIG. 11 is a perspective view of a pair of kidneys, one of said kidneys being shown treated by shock wave from shock wave head according to the method of the present invention.
[0046] FIG. 12 is a schematic view of a shock wave system according to the present invention.
[0047] FIGS. 13-17 are illustrations of various shock wave patterns.
[0048] FIG. 18 is a cross sectional view of an applicator with an integral shielding means.
[0049] FIG. 19 is a view of the shielded applicator of FIG. 18 .
[0050] FIG. 20 is a separate shielding means for use with the device of FIG. 1 .
[0051] FIG. 21 is an alternative embodiment employing an ellipsoidal applicator head.
[0052] FIG. 22 is a view of a sterile applicator sleeve or cover with an integral shielding means.
DETAILED DESCRIPTION OF THE INVENTION
[0053] With reference to FIGS. 1 and 2 a small portable hand-held shock wave applicator device 2 is illustrated. The shock wave applicator 2 has a cable 1 extending from an end of an applicator housing 16 . The cable 1 is connected to a shock wave generator (schematically illustrated in FIG. 12 ) and as illustrated in FIGS. 1 and 2 fastened to the applicator housing 16 via a pair of threaded connectors 32 , 33 .
[0054] At the opposite end of the applicator 2 is an applicator head portion 40 as shown the applicator head portion 40 has a rounded contour with a diameter of approximately 5 cm, preferably smaller which enables the device to be easily positioned around or under the organ to be treated. It is in this portion 40 that the shock wave patterns are produced, reflected and emitted to the organ or tissue 100 being treated. The head portion 40 includes an outer membrane 3 which is sealed and retained by the annular fixation ring 4 which secures and holds the membrane 3 .
[0055] Attached to the applicator housing 16 is an external pivotable handle 5 which can be swiveled about a lock and release pin 6 . Preferably the handle 5 can be moved and fixed in position at various inclinations. In the illustrated embodiment the handle 5 is shown being movable in a range of 0° to 180° or more as much as 360° as can be seen in FIG. 1 compared to FIG. 2 . In use the handle can be fixed at any inclination so desired preferably between 0° and 180° as shown. In use the surgeon can grasp the handle 5 squeezing it to release the locking mechanism and pre-orient it relative to the applicator head portion 40 and then simply position the head portion 40 relative to the organ by manipulating the handle 5 . This feature is very useful when positioning the device under the heart or any other organ being treated that is partially exposed in the patient as a result of a surgical procedure.
[0056] With reference to FIG. 5 the pivotable handle 5 is shown attached to the pin 6 which has splines 60 providing an angular lock and release feature. The pivot hole 45 on the handle 5 has matching splines 62 and as the surgeon squeezes the handle the spline 60 disengages and the handle 5 can be rotated freely. By releasing pressure the splines 60 , 62 re-engage due to the spring like “u” shaped handle 5 pushing against the pin 6 . This feature provides a simple yet secure means for setting and releasing the handle 5 at a variety of inclinations.
[0057] With reference to FIG. 3 a cross sectional view of the shock wave applicator device 2 is shown exposing the internal components. Passing through the cable 1 is a high voltage cable or rod 8 surrounded by an elastomeric insulation bellows 7 . Encircling the rod 8 is a magnet 9 and a coil 10 for moving the magnet 9 . At a distal end of the coil 10 is an insulator inner probe housing 12 for centering and holding an inner probe tip or electrode 11 . At an opposite side of the applicator head portion 40 is an outer tip or electrode 13 embedded in an outer insulator housing 24 . As shown in FIG. 4 the tips 11 , 13 are aligned and gapped at a distance S to facilitate a spark gap which creates the shock wave when energized. Referring back to FIG. 3 , partially surrounding the tips 11 , 13 is a metal reflector 15 . The reflector 15 opens to the membrane 3 and the internal surface provides the shape of the emitted wave patterns as a function of its geometric shape. The reflector 15 can be made of a numerous variety of shapes to achieve a desired wave pattern as will be discussed later in detail.
[0058] A cavity 30 is formed between the membrane 3 and the reflector 15 is filled with a fluid medium preferably filled with water. The water helps create a cavitation bubble when the spark is generated from which a shock wave 200 is propagated outward to the tissue or organ 100 to be treated.
[0059] It is possible to reduce the size of the applicator head 40 from about 5 cm maximum to much smaller almost half that size by reducing the volume in the cavity 30 and the size of the reflector 15 . This can be accomplished by applying over pressure to the volume around the tips of the electrode to control the size of the emitted shock wave bubble. The size of the bubble will increase with the energy and this over pressure put on the tips of the electrode enable the wave propagation to be effectively the same as in the larger sized reflector head.
[0060] With reference to FIG. 4 the shock wave applicator 2 is shown with the housing 16 and handle 5 removed. As shown there are two water hoses illustrated, one water hose 17 is an inlet or supply hose 17 which is attached to the reflector 15 of the applicator head by a connector 19 . Water from the inlet hose 17 can be pumped into the reflector cavity 30 through inlet holes or passageways 21 . Water from the reflector cavity 30 can be removed via outlet holes or passageways 22 and sent back through the cable 1 by way of the outlet hose 18 which is connected to the reflector 15 by the connector 20 . As shown the two hoses 17 , 18 can be snugly secured on each side of the insulator bellows 7 by a strap 50 .
[0061] As further shown the activation of the shock wave head 40 can be triggered by the surgeon by depressing the switch button 42 which closes the switch 46 allowing the high voltage current to pass along the cable or rod 8 . Preferably this switch 46 including the switch button 42 is sealed within the housing 16 and the housing 16 can be squeezed to depress the switch button 42 . This minimizes the protruding portions on the device 2 which is important to avoid damaging vessels or nerves on insertion of the device 2 into the access portal provided by the surgical procedure. The switch 46 could also be replaced with a foot switch or a switch attached to the power and control unit 41 .
[0062] When treating an organ such as the heart the transmission of the shock waves can be triggered such that the shockwave pulse is emitted at a time when the heart is contracting. As is well known and observed in electro cardio graphs, ECG's, the heart transmits a repetitive beat or wave form often described as the QRS and T wave. The R portion of the curves includes the peak of the curve and it occurs during a heart contraction and during the contraction the heart is in a vironlevel phase such that the heart beat pattern cannot be altered during a triggering of the shockwave pulse. Accordingly it is preferred in sensitive patients that the shockwaves are transmitted during the R phase of QRS and T curves. To stimulate at other times during the heartbeat can create an alteration of the repetitive pattern of the heartbeat and could trigger an irregular and uncontrolled heart spasm which can easily be avoided by timing the shockwave pulse transmission to occur during the R curve portion of the heartbeat wave pattern. This method of controlling the transmission of the shockwave pulse can be tied to any number of repetitive body functions including, but not limited to pulse rate, pulmonary rate, breathing, brain wave activity or the like. The use of equipment monitoring devices to measure such body function can therefore be computer controlled to provide the necessary feedback to permit precise control of the triggering of the generator or shock wave source to insure a fully automated system wherein the temporal firing of the device is controlled without the need of the surgeon or physician intervention. A similar type technique of using the cardiac rhythm or pulse rate frequency of the patient was taught in U.S. Pat. No. 5,313,954 to control the shockwave frequency of generation and the subject matter of that patent is being incorporated by reference herein in its entirety. The advantage of such a technique is that it enables the determination of the frequency of extrasystoles such that the pulse generator can be deactivated for a given period of time to permit the patients circulation to regenerate itself during this interval. To do otherwise could induce irregular heart rates which in patients with weakened or damaged hearts is more problematic and potentially could be life threatening during the procedure of treatment. Accordingly in the case of treating the heart, in particular, such as the use of ECG gating to control the transmission or triggering of the shockwave pulse and the frequency of the pulse and the frequency of the pulse interval and dwell time between pulses is considered particularly important.
[0063] As shown the electrode tips 11 , 13 spacing can be controlled by using the magnet 9 and the coil 10 which can move the inner tip 11 to control the gap spacing (S). Alternatively the tips 11 , 13 can be replaced with adjustable electrodes using other means such as piezo ceramics, magnets, motors with gear boxes, pneumatic or hydraulic to change the tip distance.
[0064] A low cost alternative is to provide two fixed electrodes 11 , 13 which are pre-set at fixed gaps and are not adjustable. In this way the entire device can be disposable adapted for a one procedure use which would provide the surgeon with a shock wave applicator device 2 capable to treat a single patient after which the device 2 can be simply discarded. This is possible due to the very low cost such a non-adjustable device 2 would require to manufacture. It is believed such a simple device may be usable for up to 4 or more treatments prior to being rendered inefficient due to the burning of the electrode tips. Alternatively any of the devices 2 can be easily refurbished by replacing worn components generally by replacing the firing mechanisms such as the electrode or tips.
[0065] In practice the use of the device 2 can be enhanced by the addition of a light and or miniature camera system (not shown) integrally attached at the head portion 40 or housing 16 of the applicator 2 . The camera or light can be internal of the housing 16 and the housing can be or have a clear window portion for transmission. Preferably the light source is one or more LED's adapted for high light and low heat generation. The light and or viewing system combination can be connected to a remote optical monitor to enable the physician to focus on the rear of the organ being treated or any portion obstructed from view. Alternatively the surgeon may employ a flexible endoscope device to get light and a camera for viewing the treatment location and positioning the device 2 .
[0066] Additionally the device 2 as shown in FIGS. 18 and 19 can be used with a shielding system 74 to prevent damage to the lung membranes. Such a shielding system 74 can be thin flexible wave dampening plate adapted to dampen the wave propagation to the lungs. Alternatively, air filled or high damping, reflecting materials including cellular polyurethane foam with a thin film skin or covering might be used.
[0067] The shock wave device preferably can be packaged in a sterile wrap or package and opened and connected in the operating room by the technical staff.
[0068] Alternatively as shown in FIG. 6 the device can be covered by a sterile prophylactic covering 70 of synthetic material similar to a latex or plastic glove. Some of these are already in use for other type of equipment which is used in the operating procedure of the open surgery. Preferably the covering has a long tube like portion 72 with a closed end and an open end into which the applicator 2 and a portion of the cabling 1 can be slid into. This sterile covering 70 being thin and flexible would not interfere with the wave transmission or the pivotable use of the handle 5 . Shock wave transmission between the membrane and the sleeve as well between the sleeve and the tissue has to be achieved by sterile fluid medium like NACL solution or sterile ultrasound gel or other substances with coupling properties.
[0069] As shown in FIG. 22 the sleeve 70 may include an integral shield 75 formed by an air filled double layer membrane or other wave dampening material such that the area above the reflector 15 or transmission zone directly under the outer membrane 3 is a single layer 76 not shielded, but other areas such as the back and sides of the device are shielded. Alternatively a simple shield 80 may be used that is a wave damping sterile pad or layer positioned between a sterile device 2 and the underlying lungs (not shown) above the heart.
[0070] With reference to FIGS. 3 and 4 the reflector 15 it has the internal cavity 30 shown as a generalized paraboloid with a very divergent wave to stimulate the infarct tissue of a heart directly at the applicator exit or membrane 3 while only having a low pressure amplitude when being transmitted through the heart tissue which potentially might enter into the lung tissue. Alternatively, as shown in FIG. 21 the applicator device 2 can be made with an elliptical head portion 40 , the reflector cavity 30 might be an ellipsoid with its focal point about 1-2 cm after the aperture. This will make possible that the heart wall will be behind the focal point (F2 geometrical) and the divergent beam of the shock wave is treating the tissue. The lung on the other side of the heart will be in the already low pressure because of the divergent shock wave amplitude (pressure). This is the case when the distance to the focal point is very big. In an unfocused spherical wave the pressure is lowered according to 1/distance2 and such a wave form can be emitted using the applicator device 2 .
[0071] These and other aspects of the reflector characteristics and the use of the shock wave head have been described in co-pending application U.S. Ser. No. 11/238,731 portions of which are restated for a clear understanding of the method and use of the inventive device described above.
[0072] In the shock wave method of treating an organ of a mammal be it human or an animal with an at least partially exposed target site on the organ, the organ is positioned in a convenient orientation to permit the source of the emitted waves to most directly send the waves unobstructed to the target site to initiate shock wave stimulation of the target area with minimal, preferably no interfering tissue or bone features in the path of the emitting source or lens or membrane 3 . Assuming the target area is within a projected area of the wave transmission, a single transmission dosage of wave energy may be used. The transmission dosage can be from a few seconds to 20 minutes or more dependent on the condition. The number of shock waves could be from 10 to a few hundred or a few thousand within one treatment. The repletion frequency of shock waves per second could be from 0.5-20 per second. Preferably the waves are generated from an unfocused or focused source. Preferably the shock waves should be emitted at maximum energy densities of about 0.3 mJ/mm 2 or less. The unfocused waves can be divergent or near planar and having a low pressure amplitude and density in the range of 0.00001 mJ/mm 2 to 0.3 mJ/mm 2 or less, most typically below 0.2 mJ/mm 2 . The focused source preferably can use a diffusing lens or have a far-sight focus to minimize if not eliminate having the localized focus point within the tissue. Preferably the focused shock waves are used at a similarly effective low energy transmission or alternatively can be at higher energy but wherein the tissue target site is disposed pre-convergence inward of the geometric focal point of the emitted wave transmission.
[0073] These shock wave energy transmissions are effective in stimulating a cellular response and can be accomplished without creating the cavitation bubbles in the tissue of the target site. This effectively insures the organ does not have to experience the sensation of hemorrhaging so common in the higher energy focused wave forms having a focal point at or within the targeted treatment site.
[0074] If the target site is an organ subjected to a surgical procedure exposing at least some if not all of the organ within the body cavity the target site may be such that the patient or the portable shock wave applicator device 2 must be reoriented relative to the site and a second, third or more treatment dosage can be administered. The fact that the dosage is at a low energy the common problem of localized hemorrhaging is reduced making it more practical to administer multiple dosages of waves from various orientations to further optimize the treatment and cellular stimulation of the target site. Heretofore focused high energy multiple treatments induced pain and discomfort to the patient. The use of low energy focused or un-focused waves at the target site enables multiple sequential treatments.
[0075] The present method does not rely on precise site location per se. The physician's general understanding of the anatomy of the patient should be sufficient to locate the target area to be treated. This is particularly true when the exposed organ is visually within the surgeon's line of sight and this permits the lens or membrane 3 of the emitting shock wave applicator 2 to impinge on the organ tissue directly during the shockwave treatment. The treated area can withstand a far greater number of shock waves based on the selected energy level being emitted. For example at very low energy levels the stimulation exposure can be provided over prolonged periods as much as 20 minutes if so desired. The number of shock waves could be from 10 to a few hundred or a few thousand within one treatment. The repletion frequency of shock waves per second could be from 0.5-20 per second. At higher energy levels the treatment duration can be shortened to less than a minute, less than a second if so desired. The limiting factor in the selected treatment dosage is avoidance or minimization of cell hemorrhaging and other kinds of damage to the cells or tissue while still providing a stimulating stem cell activation or a cellular release or activation of VEGF and other growth factors.
[0076] The underlying principle of these shock wave therapy methods is to stimulate the body's own natural healing capability. This is accomplished by deploying shock waves to stimulate strong cells in the tissue to activate a variety of responses. The acoustic shock waves transmit or trigger what appears to be a cellular communication throughout the entire anatomical structure, this activates a generalized cellular response at the treatment site, in particular, but more interestingly a systemic response in areas more removed from the wave form pattern. This is believed to be one of the reasons molecular stimulation can be conducted at threshold energies heretofore believed to be well below those commonly accepted as required. Accordingly not only can the energy intensity be reduced but also the number of applied shock wave impulses can be lowered from several thousand to as few as one or more pulses and still yield a beneficial stimulating response.
[0077] The use of shock waves as described above appears to involve factors such as thermal heating, light emission, electromagnetic field exposure, chemical releases in the cells as well as a microbiological response within the cells. Which combination of these factors plays a role in stimulating healing is not yet resolved. However, there appears to be a commonality in the fact that growth factors are released which applicants find indicative that otherwise dormant cells within the tissue appear to be activated which leads to the remarkable ability of the targeted organ or tissue to generate new growth or to regenerate weakened vascular networks in for example the cardio vascular system.
[0078] The use of shock wave therapy requires a fundamental understanding of focused and unfocused shock waves, coupled with a more accurate biological or molecular Focused shock waves are focused using ellipsoidal reflectors in electromechanical sources from a cylindrical surface or by the use of concave or convex lenses. Piezoelectric sources often use spherical surfaces to emit acoustic pressure waves which are self focused and have also been used in spherical electromagnetic devices.
[0079] The biological model proposed by co-inventor Wolfgang Schaden provides a whole array of clinically significant uses of shock wave therapy.
[0080] Accepting the biological model as promoted by W. Schaden, the peak pressure and the energy density of the shock waves can be lowered dramatically. Activation of the body's healing mechanisms will be seen by in growth of new blood vessels and the release of growth factors.
[0081] The biological model motivated the design of sources with low pressure amplitudes and energy densities. First: spherical waves generated between two tips 11 , 13 of an electrode; and second: nearly even waves generated by generalized parabolic reflectors. Third: divergent shock front characteristics are generated by an ellipsoid behind F2. Unfocused sources are preferably designed for extended two dimensional areas/volumes like skin. The unfocused sources can provide a divergent wave pattern or a nearly planar wave pattern and can be used in isolation or in combination with focused wave patterns yielding to an improved therapeutic treatment capability that is non-invasive with few if any disadvantageous contraindications. Alternatively a focused wave emitting treatment may be used wherein the focal point extends preferably beyond the target treatment site, potentially external to the patient. This results in the reduction of or elimination of a localized intensity zone with associated noticeable pain effect while providing a wide or enlarged treatment volume at a variety of depths more closely associated with high energy focused wave treatment. The utilization of a diffuser type lens or a shifted far-sighted focal point for the ellipsoidal reflector enables the spreading of the wave energy to effectively create a convergent but off target focal point. This insures less tissue trauma while insuring cellular stimulation to enhance the healing process.
[0082] This method of treatment has the steps of, locating a treatment site, generating either convergent diffused or far-sighted focused shock waves or unfocused shock waves, of directing these shock waves to the treatment site; and applying a sufficient number of these shock waves to induce activation of one or more growth factors thereby inducing or accelerating healing.
[0083] The unfocused shock waves can be of a divergent wave pattern or near planar pattern preferably of a low peak pressure amplitude and density. Typically the energy density values range as low as 0.000001 mJ/mm 2 and having a high end energy density of below 1.0 mJ/mm 2 , preferably 0.20 mJ/mm 2 or less. The peak pressure amplitude of the positive part of the cycle should be above 1.0 and its duration is below 1-3 microseconds.
[0084] The treatment depth can vary from the surface to the full depth of the treated organ. The treatment site can be defined by a much larger treatment area than the 0.10-3.0 cm 2 commonly produced by focused waves. The above methodology is particularly well suited for surface as well as sub-surface soft tissue organ treatments.
[0085] The above methodology is valuable in generation of tissue, vascularization and may be used in combination with stem cell therapies as well as regeneration of tissue and vascularization.
[0086] The methodology is useful in (re)vascularization of the heart, brain, liver, kidney and skin.
[0087] The methodology is useful in stimulating enforcement of defense mechanisms in tissue cells to fight infections from bacteria and can be used germicidally to treat or cleanse wounds or other target sites.
[0088] Conditions caused by cirrhosis of the liver can be treated by reversing this degenerative condition.
[0089] The implications of using the (re)generative features of this type of shock wave therapy are any weakened organ or tissue even bone can be strengthened to the point of reducing or eliminating the risk of irreparable damage or failure.
[0090] The stimulation of growth factors and activation of healing acceleration is particularly valuable to elderly patients and other high risk factor subjects.
[0091] Similar gains are visualized in organ transplant and complete organ regeneration, wherein a heart, liver, kidney, portions of the brain or any other organ or portions thereof of a human or animal may be transplanted into a patient, the organ being exposed to shock waves either prior to or after being transplanted.
[0092] With reference to FIGS. 7 and 8 the organ 100 shown is a heart. In FIG. 7 a frontal view of the heart is shown wherein the frontal region is being bombarded with exemplary shock waves 200 wherein the shockwave applicator 2 is shown unobstructed to the tissue of the heart. The shockwave applicator 2 is connected through the cable 1 back to a control and power supply 41 , as shown in FIG. 12 . As illustrated the exemplary shock waves 200 emanate through the tissue of the heart providing a beneficial regenerating and revascularization capability that heretofore was unachieved. The beneficial aspects of the present methodology are that the heart 100 as shown fully exposed in the views FIGS. 13 and 14 can be partially exposed or have an access portal such that the shock wave head 2 can be inserted therein and directed to contact or be in near contact to the heart tissue is such a way that the admitted exemplary shock waves 200 can most directly and in the most unobstructed way be transmitted to the region needing treatment. The heart itself can be lifted in the myocardial cavity and the applicator 2 positioned beneath the heart and firing the wave pattern upwardly into the tissue as shown in FIG. 8 . While the use of the shock wave applicator 2 in this fashion is clearly invasive it also has the beneficial aspects of providing a direct treatment to the cardiovascular area in need of regenerative or revascularization enhancement.
[0093] With reference to FIG. 9 , the organ 100 is a brain. As shown the brain and brain stem are completely exposed, however, normally only a small portion of the cranial cavity would be open such that the shockwave applicator 2 can be inserted therein to provide therapeutic shock wave treatments preferably of very low amplitude for stimulating certain regions of the brain for regenerative purposes.
[0094] In FIG. 10 a liver 100 is shown. In addition to the liver 100 , the stomach 102 , spleen 104 and duodenum 106 are also shown. The shock wave applicator 2 is in contact with the liver 100 and is providing a therapeutic shock wave treatment as illustrated wherein the exemplary shock waves 200 are being transmitted through the tissue of the liver. It is believed that the use of such exemplary shock waves 200 can help in enhancing liver regeneration particularly those that have been degenerative and in conditions that might be prone to failure. Again the liver 100 is shown fully exposed, however, in normal procedure only an access portal or opening may be needed such that the shock wave applicator 2 can be inserted there through and provide a direct unobstructed path to deliver shockwave treatments to this organ as well.
[0095] In FIG. 11 a pair of kidneys 100 is shown as the organ 100 being treated. In this fashion the kidneys similar to the liver, brain or heart can be treated such that the shock wave applicator 2 can be in direct or near contact in an unobstructed path to admit shock waves 200 to this organ. This has the added benefit of generating maximum therapy to the afflicted organ in such a way that the healing process can be stimulated more directly. Again in each of these procedures as shown there is an invasive technique requiring the shock wave applicator 2 to enter either an access portal or an opening wherein the organ 100 is at least partially exposed to the exemplary shock waves 200 as can either be accomplished by a surgical procedure or any other means that would permit entry of the shock wave applicator 2 to the afflicted organ.
[0096] In each of the representative treatments as shown in FIGS. 7 through 11 the shockwave applicator 2 when used within a sterile sleeve or covering 70 as shown in FIG. 6 or 22 may simply be disinfected using a suitable antimicrobial disinfecting agent prior to use. Alternatively the applicator 2 may be sterilized when used without a sterile sleeve. As shown the sleeves or coverings 70 are preferably disposable and should be discarded after use. When treating any tissue or organ 100 the sterile sleeve 70 holding the applicator 2 or in the case of using the applicator 2 without a sleeve the tissue contacting surface should be coupled acoustically by using known means such as sterile fluids or viscous gels like ultrasound gels or even NaCl solutions to couple the transmitted shock wave into the organ in an aseptic sterile fashion.
[0097] In FIGS. 7-11 exemplary shock waves 200 are illustrated, it must be appreciated that any of the recognized shock wave patterns exhibited in FIGS. 13-17 can be used in the shock wave treatment of the various organs 100 .
[0098] Heretofore such invasive techniques were not used in combination with shock wave therapy primarily because the shockwaves were believed to be able to sufficiently pass through interfering body tissue to achieve the desired result in a non-invasive fashion. While this may be true, in many cases if the degenerative process is such that an operation is required then the combination of an operation in conjunction with shockwave therapy only enhances the therapeutic values and the healing process of the patient and the organ such that regenerative conditions can be achieved that would include not only revascularization of the heart or other organs wherein sufficient or insufficient blood flow is occurring but also to enhance the improvement of ischemic tissue that may be occupying a portion of the organ. This ischemic tissue can then be minimized by the regenerative process of using shock wave therapy in the fashion described above to permit the tissue to rebuild itself in the region that has been afflicted.
[0099] As used throughout this application wherein the use of exemplary shock waves 200 in an unobstructed path has been described unobstructed path means that there is no or substantially no interfering tissue or bone skeletal mass between the shock wave applicator 2 and the treated organ. It is believed that the elimination of such interfering masses greatly enhances the control and the efficiency of the emitted exemplary shock waves 200 to create the desired beneficial healing effects and regenerative process needed for the organ to be repaired.
[0100] Furthermore such acoustic shock wave forms can be used in combination with drugs, chemical treatments, irradiation therapy or even physical therapy and when so combined the stimulated cells will more rapidly assist the body's natural healing response.
[0101] The present invention provides an apparatus for an effective treatment of indications, which benefit from low energy pressure pulse/shock waves having nearly plane or even divergent characteristics. With an unfocused wave having nearly plane wave characteristic or even divergent wave characteristics, the energy density of the wave may be or may be adjusted to be so low that side effects including pain are very minor or even do not exist at all.
[0102] In certain embodiments, the apparatus of the present invention is able to produce waves having energy density values that are below 0.3 mJ/mm2 or even as low as 0.000 001 mJ/mm2. In a preferred embodiment, those low end values range between 0.1-0.001 mJ/mm2. With these low energy densities, side effects are reduced and the dose application is much more uniform. Additionally, the possibility of harming surface tissue is reduced when using an apparatus of the present invention that generates waves having nearly plane or divergent characteristics and larger transmission areas compared to apparatuses using a focused shock wave source that need to be moved around to cover the affected area. The apparatus of the present invention also may allow the user to make more precise energy density adjustments than an apparatus generating only focused shock waves, which is generally limited in terms of lowering the energy output.
[0103] The treatment of the above mentioned indications are believed to be a first time use of acoustic shock wave therapy invasively. None of the work done to date has treated the above mentioned indications with convergent, divergent, planar or near-planar acoustic shock waves of low energy or focused shock waves in a direct unobstructed path from the emitting source lens or cover using the soft fluid filled organ as a transmitting medium directly. As is the use of acoustic shock waves for germicidal wound cleaning or preventive medical treatments.
[0104] With reference to FIGS. 13-17 the applicator 2 of the present invention can be provided with a reflector cavity 30 shaped or contoured to reflect the generated wave pattern 200 in a variety of shapes or geometric forms. In each of the following figures the wave pattern 200 includes a geometric pattern specific subset 200 A through 200 E.
[0105] FIG. 13 is a simplified depiction of the pressure pulse/shock wave (PP/SW) generator, such as the shock wave applicator 2 showing focusing characteristics of transmitted acoustic pressure pattern 200 A. The pattern as illustrated has waves that are converging as shown.
[0106] This converging wave pattern 200 A is commonly used in focused shock wave treatments wherein the focal point F 2 is targeted at a specific point in the tissue mass 100 . Alternatively the wave pattern can be used off target to avoid the high energy focal region if so desired. These wave patterns 200 A are most commonly produced by using an ellipsoidal shaped reflector surface in the cavity 30 .
[0107] FIG. 14 is a simplified depiction of a pressure pulse/shock wave generator, such as a shock wave head, with plane wave characteristics. Numeral 2 indicates the position of a pressure pulse applicator 2 according to the present invention, which generates a pressure pulse wave pattern 200 B which is leaving the housing at the membrane or lens position 3 , which may be a water cushion or any other kind of exit window. Somewhat even (also referred to herein as “disturbed”) wave characteristics can be generated, in case a paraboloid is used as a reflecting element, with a point source (e.g. electrode) that is located in the focal point of the paraboloid. The waves will be transmitted into the patient's body via a coupling media such as, e.g., ultrasound gel or oil and their amplitudes will be attenuated with increasing distance from the exit window or membrane 3 .
[0108] FIG. 15 is a simplified depiction of a pressure pulse shock wave generator (shock wave head) with divergent wave characteristics. The divergent wave fronts 200 C may be leaving the exit window 3 at point 201 where the amplitude of the wave front is very high. This point 201 could be regarded as the source point for the pressure pulses 200 C. In FIG. 1 c the pressure pulse source may be a point source, that is, the pressure pulse may be generated by an electrical discharge of an electrode under water between electrode tips. However, the pressure pulse may also be generated, for example, by an explosion.
[0109] FIG. 16 is a simplified depiction of the pressure pulse/shock wave generator (shock wave head) having as a focusing element an paraboloid (y 2 =2px). Thus, the characteristics of the wave fronts 200 D generated behind the exit window 3 are disturbed plane (“parallel”), the disturbance resulting from phenomena ranging from electrode burn down, spark ignition spatial variation to diffraction effects. However, other phenomena might contribute to the disturbance. This is common in so called planar patterns.
[0110] FIG. 17 is a simplified depiction of the pressure pulse/shock wave generator (shock wave head) having as a focusing element a generalized paraboloid (y n =2px, with 1,2<n<2,8 and n≠2). Thus, the characteristics of the wave fronts 200 E generated behind the exit window or membrane 3 are, compared to the wave fronts generated by a paraboloid (y 2 =2px), less disturbed, that is, nearly plane (or nearly parallel or nearly even). Thus, conformational adjustments of a regular paraboloid (y 2 =2px) to produce a generalized paraboloid can compensate for disturbances from, e.g., electrode burn down. Thus, in a generalized paraboloid, the characteristics of the wave front may be nearly plane due to its ability to compensate for phenomena including, but not limited to, burn down of the tips of the electrode and/or for disturbances caused by diffraction at the aperture of the paraboloid. For example, in a regular paraboloid (y 2 =2px) with p=1.25, introduction of a new electrode may result in p being about 1.05. If an electrode is used that adjusts itself to maintain the distance between the electrode tips (“adjustable electrode”) and assuming that the electrodes burn down is 4 mm (z=4 mm), p will increase to about 1.45. To compensate for this burn down, and here the change of p, and to generate nearly plane wave fronts over the life span of an electrode, a generalized paraboloid having, for example n=1.66 or n=2.5 may be used. An adjustable electrode is, for example, disclosed in U.S. Pat. No. 6,217,531.
[0111] Various wave patterns 200 A- 200 E are by no means intended to be more than exemplary and any such wave pattern or type may be used at the surgeon's discretion. Accordingly the depiction 200 in FIGS. 7-12 are intended to mean any style of wave pattern emitted including, but not limited to the subset 200 A- 200 E.
[0112] It will be appreciated that the apparatuses and processes of the present invention can have a variety of embodiments, only a few of which are disclosed herein. It will be apparent to the artisan that other embodiments exist and do not depart from the spirit of the invention. Thus, the described embodiments are illustrative and should not be construed as restrictive.
[0113] Variations in the present invention are possible in light of the description of it provided herein. While certain representative embodiments and details have been shown for the purpose of illustrating the subject invention, it will be apparent to those skilled in this art that various changes and modifications can be made therein without departing from the scope of the subject invention. It is, therefore, to be understood that changes can be made in the particular embodiments described which will be within the full intended scope of the invention as defined by the following appended claims.
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The system for treating an internal organ has a generator source for producing a shock wave connected to a portable shock wave applicator device, wherein the shock wave applicator device has a side-firing shock wave head having a variable angle adjustment relative to a release and lock connected handle or holder means for holding said device. The inclination of the shock wave head can be set to a fixed inclination to reach the organ at various locations or surfaces or can be pivotally inclined continuous to vary the treatment surfaces area.
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PRIORITY TO RELATED APPLICATION(S)
This application is a continuation-in-part of U.S. patent application Ser. No. 12/581,192, filed Oct. 19, 2009, now pending, which is a continuation of U.S. patent application Ser. No. 12/277,326, filed Nov. 25, 2008, now U.S. Pat. No. 7,618,973 which claims the benefit of European Patent Application No. 07122271.5, filed Dec. 4, 2007. Each of these applications is hereby incorporated by reference in their entirety.
BACKGROUND OF THE INVENTION
Receptors for the major inhibitory neurotransmitter, gamma-aminobutyric acid (GABA), are divided into two main classes: (1) GABA A receptors, which are members of the ligand-gated ion channel superfamily and (2) GABA B receptors, which are members of the G-protein linked receptor family. The GABA A receptor complex, which is a membrane-bound heteropentameric protein polymer composed principally of α, β and γ subunits.
Presently a total number of 21 subunits of the GABA A receptor have been cloned and sequenced. Three types of subunits (α, β and γ) are required for the construction of recombinant GABA A receptors which most closely mimic the biochemical, electrophysiological and pharmacological functions of native GABA A receptors obtained from mammalian brain cells. There is strong evidence that the benzodiazepine binding site lies between the α and γ subunits. Among the recombinant GABA A receptors, α1β2γ2 mimics many effects of the classical type-I BzR subtypes, whereas α2β2γ2, α3β2γ2 and α5β2γ2 ion channels are termed type-II BzR.
It has been shown by McNamara and Skelton in Psychobiology, 21:101-108 that the benzodiazepine receptor inverse agonist β-CCM enhance spatial learning in the Morris watermaze. However, β-CCM and other conventional benzodiazepine receptor inverse agonists are proconvulsant or convulsant which prevents their use as cognition enhancing agents in humans. In addition, these compounds are non-selective within the GABA A receptor subunits, whereas a GABA A α5 receptor partial or full inverse agonist which is relatively free of activity at GABA A α1 and/or α2 and/or α3 receptor binding sites can be used to provide a medicament which is useful for enhancing cognition with reduced or without proconvulsant activity. It is also possible to use GABA A α5 inverse agonists which are not free of activity at GABA A α1 and/or α2 and/or α3 receptor binding sites but which are functionally selective for α5 containing subunits. However, inverse agonists which are selective for GABA A α5 subunits and are relatively free of activity at GABA A α1, α2 and α3 receptor binding sites are preferred.
SUMMARY OF THE INVENTION
The present invention provides isoxazolo-pyrazine derivatives and their pharmaceutically acceptable salts having affinity and selectivity for the GABA A α5 receptor binding site, their manufacture, and pharmaceutical compositions containing them. The invention also provides methods for enhancing cognition and for treating cognitive disorders like Alzheimer's disease. The most preferred indication in accordance with the present invention is Alzheimer's disease.
In particular, the present invention is concerned with isoxazolo-pyrazine derivatives of formula I
wherein R 1 , R 2 , R 3 , R 4 and X are as described hereinbelow.
DETAILED DESCRIPTION OF THE INVENTION
The following definitions of the general terms used in the present description apply irrespective of whether the terms in question appear alone or in combination. It must be noted that, as used in the specification and the appended claims, the singular forms “a”, “an,” and “the” include plural forms unless the context clearly dictates otherwise.
As used herein, the term “alkyl” denotes a saturated straight- or branched-chain hydrocarbon group containing from 1 to 7 carbon atoms, for example, methyl, ethyl, propyl, isopropyl, n-butyl, iso-butyl, sec-butyl, tert-butyl and the like. Preferred alkyl groups are groups with 1 to 4 carbon atoms.
The term “halo-C 1-7 -alkyl”, “C 1-7 -haloalkyl” or “C 1-7 -alkyl optionally substituted with halo” denotes a C 1-7 -alkyl group as defined above wherein at least one of the hydrogen atoms of the alkyl group is replaced by a halogen atom, preferably fluoro or chloro, most preferably fluoro. Examples of halo-C 1-7 -alkyl include but are not limited to methyl, ethyl, propyl, isopropyl, isobutyl, sec-butyl, tert-butyl, pentyl or n-hexyl substituted by one or more Cl, F, Br or I atom(s), in particular one, two or three fluoro or chloro, as well as those groups specifically illustrated by the examples herein below. Among the preferred halo-C 1-7 -alkyl groups are difluoro- or trifluoro-methyl or -ethyl.
The term “hydroxy-C 1-7 -alkyl”, “C 1-7 -hydroxyalkyl” or “C 1-7 -alkyl optionally substituted with hydroxy” denotes a C 1-7 -alkyl group as defined above wherein at least one of the hydrogen atoms of the alkyl group is replaced by a hydroxy group. Examples of hydroxy-C 1-7 -alkyl include but are not limited to methyl, ethyl, propyl, isopropyl, isobutyl, sec-butyl, tert-butyl, pentyl or n-hexyl substituted by one or more hydroxy group(s), in particular with one, two or three hydroxy groups, preferably with one hydroxy group, as well as those groups specifically illustrated by the examples herein below.
The term “cyano-C 1-7 -alkyl”, “C 1-7 -cyanoalkyl” or “C 1-7 -alkyl optionally substituted with cyano” denotes a C 1-7 -alkyl group as defined above wherein at least one of the hydrogen atoms of the alkyl group is replaced by a cyano group. Examples of hydroxy-C 1-7 -alkyl include but are not limited to methyl, ethyl, propyl, isopropyl, isobutyl, sec-butyl, tert-butyl, pentyl or n-hexyl substituted by one or more cyano group(s), preferably by one, two or three, and more preferably by one cyano group, as well as those groups specifically illustrated by the examples herein below.
The term “alkoxy” denotes a group —O—R wherein R is alkyl as defined above.
The term “aryl” denotes a monovalent aromatic carbocyclic ring system, preferably phenyl or naphthyl, and more preferably phenyl. Aryl is optionally substituted as described herein.
The term “aromatic” means aromatic according to Hückel's rule. A cyclic molecule follows Hückel's rule when the number of its π-electrons equals 4n+2 where n is zero or any positive integer.
The term “halo” or “halogen” denotes chloro, iodo, fluoro and bromo.
The term “C 1-7 -haloalkoxy” or “halo-C 1-7 -alkoxy” denotes a C 1-7 -alkoxy group as defined above wherein at least one of the hydrogen atoms of the alkoxy group is replaced by a halogen atom, preferably fluoro or chloro, most preferably fluoro. Examples of halo-C 1-7 -alkoxy include but are not limited to methyl, ethyl, propyl, isopropyl, isobutyl, sec-butyl, tert-butyl, pentyl or n-hexyl substituted by one or more Cl, F, Br or I atom(s), in particular one, two or three fluoro or chloro atoms, as well as those groups specifically illustrated by the examples herein below. Among the preferred halo-C 1-7 -alkoxy groups are difluoro- or trifluoro-methoxy or -ethoxy substituted as described above, preferably —OCF 3 .
The term “cycloalkyl” refers to a monovalent saturated cyclic hydrocarbon radical of 3 to 7 ring carbon atoms, preferably 3 to 6 carbon atoms, such as cyclopropyl, cyclobutyl, cyclopentyl, or cyclohexyl.
The term “heterocycloalkyl” refers to a monovalent 3 to 7 membered saturated monocyclic ring containing one, two or three ring heteroatoms selected from N, O and S. One or two ring heteroatoms are preferred. Preferred are 4 to 6 membered heterocycloalkyl or 5 to 6 membered heterocycloalkyl, each containing one or two ring heteroatoms selected from N, O and S. Examples for heterocycloalkyl moieties are tetrahydrofuranyl, tetrahydropyranyl, pyrrolidinyl, morpholinyl, thiomorpholinyl, piperidinyl, or piperazinyl. A preferred heterocycloalkyl is tetrahydropyranyl. Heterocycloalkyl is a subgroup of “heterocyclyl” as described below. Heterocycloalkyl is optionally substituted as described herein.
The term “heteroaryl” refers to a monovalent aromatic 5- or 6-membered monocyclic ring containing one, two, or three ring heteroatoms selected from N, O, and S, the remaining ring atoms being C. Preferably, the 5- or 6-membered heteroaryl ring contains one or two ring heteroatoms. 6-membered heteroaryl are preferred. Examples for heteroaryl moieties include but are not limited to thiophenyl, furanyl, pyridinyl, pyrimidinyl, pyrazinyl, pyrazolyl, imidazolyl, oxazolyl, isoxazolyl, thiazolyl, isothiazolyl, triazolyl, 1,2,4-oxadiazolyl, or 1,3,4-oxadiazolyl.
The term “heterocyclyl” or “heterocyclyl moiety” refers to a monovalent saturated or partially saturated 3- to 7-membered monocyclic or 9- to 10-membered bicyclic ring system wherein one, two, three or four ring carbon atoms have been replaced by N, O or S, and with the attachment point on the saturated or partially unsaturated ring of said ring system. Such bicyclic heterocyclyl moieties hence include aromatic rings annelated to saturated rings. Where applicable, “heterocyclyl moiety” further includes cases where two residues R′ and R″ together with the nitrogen to which they are bound form such a heterocyclyl moiety. Examples for heterocyclyl include but are not limited to tetrahydrofuranyl, tetrahydropyranyl, pyrrolidinyl, morpholinyl, thiomorpholinyl, piperidinyl, piperaziny, or hexahydrothiopyranyl, as well as their corresponding partially unsaturated derivatives.
The term “oxo” when referring to substituents on heterocycloalkyl, heterocyclyl or on a heterocycle means that an oxygen atom is attached to the ring. Thereby, the “oxo” can either replace two hydrogen atoms on a carbon atom, or it can simply be attached to sulfur, so that the sulfur exists in oxidized form, i.e. bearing one or two oxygens.
When indicating the number of substituents, the term “one or more” means from one substituent to the highest possible number of substitution, i.e. replacement of one hydrogen up to replacement of all hydrogens by substituents. Thereby, one, two or three substituents are preferred.
“Pharmaceutically acceptable,” such as pharmaceutically acceptable carrier, excipient, etc., means pharmacologically acceptable and substantially non-toxic to the subject to which the particular compound is administered.
The term “pharmaceutically acceptable salt” or “pharmaceutically acceptable acid addition salt” embraces salts with inorganic and organic acids, such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, citric acid, formic acid, fumaric acid, maleic acid, acetic acid, succinic acid, tartaric acid, methanesulfonic acid, p-toluenesulfonic acid and the like.
“Therapeutically effective amount” means an amount that is effective to prevent, alleviate or ameliorate symptoms of disease or prolong the survival of the subject being treated.
In detail, the present invention relates to compounds of formula (I)
wherein
X is O or NH; R 1 is phenyl or pyridin-2-yl, each of which is optionally substituted with one, two or three halo, R 2 is H or C 1-4 alkyl; R 3 and R 4 each are independently
H, C 1-7 alkyl, optionally substituted with one or more halo, cyano, or hydroxy, C 1-7 alkoxy, optionally substituted with one or more halo, CN, halo, NO 2 , —C(O)—R a , wherein R a is hydroxy, C 1-7 alkoxy, C 1-7 alkyl, phenoxy or phenyl, —C(O)—NR b R c , wherein R b and R c are each independently
H, C 1-7 alkyl, optionally substituted with one or more halo, hydroxy, or cyano, —(CH 2 ) z —C 3-7 cycloalkyl, optionally substituted by one or more B,
and z is 0, 1, 2, 3 or 4,
—(CH 2 ) y -heterocyclyl, wherein y is 0, 1, 2, 3 or 4, and wherein heterocyclyl is optionally substituted by one or more A R b and R c together with the nitrogen to which they are bound form a heterocyclyl moiety, optionally substituted with one or more A, or
or R 3 and R 4 together form an annelated benzo ring, the benzo ring is optionally substituted by one or more E,
A is hydroxy, oxo, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, halo, or CN, B is halo, hydroxy, CN, C 1-4 alkyl, or C 1-4 haloalkyl, E is halo, CN, NO 2 , hydroxy, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, C 1-7 cyanoalkyl, C 1-7 haloalkoxy, or C 3-7 cycloalkyl,
or a pharmaceutically acceptable salt thereof.
In certain embodiments of the compound of formula I, X is O or NH. Each of these alternatives can be combined with any other embodiment as disclosed herein.
Further, it is to be understood that every embodiment relating to a specific residue R 1 to R 4 as disclosed herein can be combined with any other embodiment relating to another residue R 1 to R 4 as disclosed herein.
In certain embodiments of the compound of formula I, R 1 is phenyl, optionally substituted with one, two or three halo. Preferred halo substituents are chloro and fluoro. In case phenyl is substituted, preferably one or two optional halo substituents selected from chloro and fluoro are chosen.
In certain embodiments of the invention, R 2 is C 1-4 alkyl. Preferably, R 2 is methyl.
In certain embodiments of the compound of formula I, R 3 and R 4 are as defined above.
In certain embodiments of the compound of formula I, R 3 is H or R 3 and R 4 together form an anellated benzo ring, i.e. a benzo ring anellated to the pyrazin moiety, whereby benzo is optionally substituted as defined herein.
In certain embodiments of the compound of formula I, R 4 is as described above.
In certain embodiments of the compound of formula I, R 4 is
H, —C(O)—R a , wherein R a is hydroxy, C 1-7 alkoxy, C 1-7 alkyl, phenoxy or phenyl, —C(O)—NR b R c , wherein R b and R c are each independently
H, C 1-7 alkyl, optionally substituted with one or more halo, hydroxy, or cyano, —(CH 2 ) z —C 3-7 cycloalkyl, optionally substituted by one or more B, and z is 0, 1, 2, 3 or 4, preferably 0 or 1, —(CH 2 ) y -heterocyclyl, wherein y is 0, 1, 2, 3 or 4, preferably 0, and wherein heterocyclyl is optionally substituted by one or more A
or R 3 and R 4 together form an annelated benzo ring, the benzo ring is optionally substituted by one or more E, A is hydroxy, oxo, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, halo, or CN, B is halo, hydroxy, CN, C 1-4 alkyl, or C 1-4 haloalkyl, E is halo, CN, NO 2 , hydroxy, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 hydroxyalkyl, C 1-7 cyanoalkyl, C 1-7 haloalkoxy, or C 3-7 cycloalkyl.
In certain embodiments of the compound of formula I, R 4 is
H, —C(O)—R a , wherein R a is hydroxy, or C 1-7 alkoxy, —C(O)—NR b R c , wherein R b and R c are each independently
H, C 1-7 alkyl, optionally substituted with one or more halo, hydroxy, or cyano, —(CH 2 ) z —C 3-7 cycloalkyl, optionally substituted by one or more B,
and z is 0, 1, 2, 3 or 4, preferably 0 or 1,
(CH 2 ) y -heterocyclyl, wherein y is 0, 1, 2, 3 or 4, preferably 0, and wherein heterocyclyl is tetrahydropyranyl optionally substituted by one or more A
or R 3 and R 4 together form an annelated benzo ring, the benzo ring is optionally substituted by one or more E, A is hydroxy, oxo, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, halo, or CN, B is halo, hydroxy, CN, C 1-4 alkyl, or C 1-4 haloalkyl, E is halo, CN, NO 2 , hydroxy, C 1-7 alkyl, C 1-7 alkoxyl, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, C 1-7 cyanoalkyl, C 1-7 haloalkoxy, or C 3-7 cycloalkyl.
A certain embodiment of the invention comprises the compound of formula I
wherein
X is O or NH; R 1 is phenyl or pyridin-2-yl, each of which is optionally substituted with one, two or three halo, R 2 is C 1-4 alkyl; preferably methyl; R 3 is H; R 4 is H,
—C(O)—R a , wherein R a is hydroxy, C 1-7 alkoxy, C 1-7 alkyl, phenoxy or phenyl, —C(O)—NR b R c , wherein R b and R c are each independently
H, C 1-7 alkyl, optionally substituted with one or more halo, hydroxy, or cyano, —(CH 2 ) z —C 3-7 cycloalkyl, optionally substituted by one or more B,
and z is 0, 1, 2, 3 or 4, preferably 0 or 1,
—(CH 2 ) y -heterocyclyl, wherein y is 0, 1, 2, 3 or 4, preferably 0, and wherein heterocyclyl is optionally substituted by one or more A
or R 3 and R 4 together form an annelated benzo ring, the benzo ring is optionally substituted by one or more E, A is hydroxy, oxo, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, halo, or CN, B is halo, hydroxy, CN, C 1-4 alkyl, or C 1-4 haloalkyl, E is halo, CN, NO 2 , hydroxy, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 hydroxyalkyl, C 1-7 cyanoalkyl, C 1-7 haloalkoxy, or C 3-7 cycloalkyl,
or a pharmaceutically acceptable salt thereof.
A certain embodiment of the invention comprises the compound of formula I
wherein
X is O or NH; R 1 is phenyl or pyridine-2-yl, wherein the rings may be optionally substituted with halogen; R 2 is H or C 1-4 alkyl;
R 3 and R 4 each are independently
H, —C(O)—R a , wherein R a is hydroxy, C 1-7 alkoxy or C 1-7 alkyl, —C(O)—NR b R c , wherein R b and R c are each independently
hydrogen, C 1-7 alkyl, optionally substituted with one or more halogen or hydroxy, or are independently from each other —(CH 2 ) z —C 3-7 cycloalkyl, optionally substituted by one or more halogen for z being 0 or 1, or are independently from each other heterocyclyl,
or R 3 and R 4 together form an annelated benzo ring,
or a pharmaceutically acceptable salt thereof.
In detail, the present invention relates to compounds of formula (I)
wherein
X is O or NH; R 1 is pyridine-2-yl optionally substituted with one, two or three halo, R 2 is H or C 1-4 alkyl; R 3 and R 4 each are independently
H, C 1-7 alkyl, optionally substituted with one or more halo, cyano, or hydroxy, C 1-7 alkoxy, optionally substituted with one or more halo, CN, halo, NO 2 , —C(O)—R a , wherein R a is hydroxy, C 1-7 alkoxy, C 1-7 alkyl, phenoxy or phenyl, —C(O)—NR b R c , wherein R b and R c are each independently
H, C 1-7 alkyl, optionally substituted with one or more halo, hydroxy, or cyano, —(CH 2 ) z , —C 3-7 cycloalkyl, optionally substituted by one or more B,
and z is 0, 1, 2, 3 or 4,
—(CH 2 ) y -heterocyclyl, wherein y is 0, 1, 2, 3 or 4, and wherein heterocyclyl is optionally substituted by one or more A R b and R c together with the nitrogen to which they are bound form a heterocyclyl moiety, optionally substituted with one or more A, or
or R 3 and R 4 together form an annelated benzo ring, the benzo ring is optionally substituted by one or more E,
A is hydroxy, oxo, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, halo, or CN, B is halo, hydroxy, CN, C 1-4 alkyl, or C 1-4 haloalkyl, E is halo, CN, NO 2 , hydroxy, C 1-7 alkyl, C 1-7 alkoxy, C 1-7 haloalkyl, C 1-7 hydroxyalkyl, C 1-7 cyanoalkyl, C 1-7 haloalkoxy, or C 3-7 cycloalkyl,
or a pharmaceutically acceptable salt thereof.
Preferred compounds of formula I of present invention are
5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid methyl ester, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylmethyl-amide, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid isopropylamide, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid tert-butylamide, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylamide, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (4,4-difluoro-cyclohexyl)-amide, 2-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-quinoxaline, 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid isopropylamide, 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid cyclopropylamide, 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide, 5-[3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid cyclopropylmethyl-amide, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid isopropylamide, 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid isopropylamide, 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid ((S)-2-hydroxy-1-methyl-ethyl)-amide, 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid ((R)-2-hydroxy-1-methyl-ethyl)-amide, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid isopropylamide, and 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylamide.
The present compounds of formula I (X═O) and their pharmaceutically acceptable salts can be prepared by a process comprising:
a) reacting a compound of formula II:
with hydroxylamine hydrochloride in a suitable solvent, such as ethanol and water in the presence of a base, such as aqueous sodium hydroxide, to give a compound of formula III:
b) reacting the compound of formula III with a chlorinating agent, such as N-chlorosuccinimide, in a suitable solvent, such as DMF, to give a compound of formula IV:
c1) and then either reacting the compound of formula IV with a compound of formula V:
in the presence of a suitable base, such as triethylamine, in a suitable solvent, such as chloroform, or alternatively
c2) reacting the compound of formula IV with a compound of formula VI:
in the presence of a suitable base, such as triethylamine, in a suitable solvent, such as diethylether, to give a compound of formula VII:
d) reacting a compound of formula VII with a reducing agent, such as lithiumaluminiumhydride, in a suitable solvent, such as THF, to give a compound of formula VIII:
i) with a compound of formula IX:
in the presence of a suitable base, such as sodium hydride, in a suitable solvent, such as THF, to give a compound of formula I:
The present compounds of formula I (X═NH) and their pharmaceutically acceptable salts can be prepared by a process comprising:
j) reacting a compound of formula VIII:
with phthalimide in the presence of triphenylphosphine and diethylazodicarboxylate, in a suitable solvent, such as THF to give a compound of formula X:
g) reacting the compound of formula X with hydrazine, to give a compound of formula XI:
with a compound of formula IX:
in the presence of a suitable base, such as sodium hydride, in a suitable solvent, such as THF to give a compound of formula I:
The following scheme describes the processes for preparation of compounds of formula I (X═O and NH) in more detail.
In accordance with Scheme 1, compounds of formula I can be prepared following standards methods.
As mentioned earlier, the compounds of formula I and their pharmaceutically usable salts possess valuable pharmacological properties. The compounds of the present invention are ligands for GABA A receptors containing the α5 subunit and are therefore useful in the therapy where cognition enhancement is required.
The compounds were investigated in accordance with the test given hereinafter:
Membrane Preparation and Binding Assay
The affinity of compounds at GABA A receptor subtypes was measured by competition for [3H]flumazenil (85 Ci/mmol; Roche) binding to HEK293 cells expressing rat (stably transfected) or human (transiently transfected) receptors of composition α1β3γ2, α2β3γ2, α3β3γ2 and α5β3γ2.
Cell pellets were suspended in Krebs-tris buffer (4.8 mM KCl, 1.2 mM CaCl2, 1.2 mM MgCl 2 , 120 mM NaCl, 15 mM Tris; pH 7.5; binding assay buffer), homogenized by polytron for ca. 20 sec on ice and centrifuged for 60 min at 4° C. (50000 g; Sorvall, rotor: SM24=20000 rpm). The cell pellets were resuspended in Krebs-tris buffer and homogenized by polytron for ca. 15 sec on ice. Protein was measured (Bradford method, Bio-Rad) and aliquots of 1 mL were prepared and stored at −80° C.
Radioligand binding assays were carried out in a volume of 200 μL (96-well plates) which contained 100 μL of cell membranes, [3H]flumazenil at a concentration of 1 nM for α1, α2, α3 subunits and 0.5 nM for α5 subunits and the test compound in the range of 10-10 −3 ×10 −6 M. Nonspecific binding was defined by 10 −5 M diazepam and typically represented less than 5% of the total binding. Assays were incubated to equilibrium for 1 hour at. 4° C. and harvested onto GF/C uni-filters (Packard) by filtration using a Packard harvester and washing with ice-cold wash buffer (50 mM Tris; pH 7.5). After drying, filter-retained radioactivity was detected by liquid scintillation counting. Ki values were calculated using Excel-Fit (Microsoft) and are the means of two determinations.
The compounds of the accompanying examples were tested in the above described assay, and the preferred compounds were found to possess a Ki value for displacement of [3H]flumazenil from α5 subunits of the rat GABA A receptor of 100 nM or less. Most preferred are compounds with a Ki (nM)<35. In a preferred embodiment the compounds of the invention are binding selective for the α5 subunit relative to the α1, α2 and α3 subunit.
Representative test results are shown in the table below:
TABLE 1
Example
hKi (nM)
1
29
2
3.1
3
1.2
4
10.8
5
1.9
6
1.2
7
10.6
8
7.4
9
9.6
10
10.4
11
12.1
12
0.3
13
24
14
21
15
11
16
11.6
17
32
18
7.4
19
14.3
20
9.6
21
13.7
“h” in “hKi” means “human”.
The present invention also provides pharmaceutical compositions containing compounds of the invention, for example, compounds of formula I or pharmaceutically acceptable salts thereof and a pharmaceutically acceptable carrier. Such pharmaceutical compositions can be in the form of tablets, coated tablets, dragées, hard and soft gelatin capsules, solutions, emulsions, or suspensions. The pharmaceutical compositions also can be in the form of suppositories or injectable solutions.
The pharmaceutical compositions of the invention, in addition to one or more compounds of the invention, contain a pharmaceutically acceptable carrier. Suitable pharmaceutically acceptable carriers include pharmaceutically inert, inorganic or organic carriers. Lactose, corn starch or derivatives thereof, talc, stearic acid or its salts etc can be used as such excipients e.g. for tablets, dragées and hard gelatine capsules. Suitable excipients for soft gelatine capsules are e.g. vegetable oils, waxes, fats, semisolid and liquid polyols etc. Suitable excipients for the manufacture of solutions and syrups are e.g. water, polyols, saccharose, invert sugar, glucose etc. Suitable excipients for injection solutions are e.g. water, alcohols, polyols, glycerol, vegetable oils etc. Suitable excipients for suppositories are e.g. natural or hardened oils, waxes, fats, semi-liquid or liquid polyols etc.
Moreover, the pharmaceutical compositions can contain preservatives, solubilizers, stabilizers, wetting agents, emulsifiers, sweeteners, colorants, flavorants, salts for varying the osmotic pressure, buffers, masking agents or antioxidants. They can also contain still other therapeutically valuable substances.
The present invention also provides a method for the manufacture of pharmaceutical compositions. Such process comprises bringing one or more compounds of formula I and/or pharmaceutically acceptable acid addition salts thereof and, if desired, one or more other therapeutically valuable substances into a galenical administration form together with one or more therapeutically inert carriers.
The compounds and compositions of the present invention can be administered in a conventional manner, for example, orally, rectally, or parenterally. The pharmaceutical compositions of the invention can be administered orally, for example, in the form of tablets, coated tablets, dragées, hard and soft gelatin capsules, solutions, emulsions, or suspensions. The pharmaceutical compositions also can be administered rectally, for example, in the form of suppositories, or parenterally, for example, in the form of injectable solutions.
The dosage at which compounds of the invention can be administered can vary within wide limits and will, of course, be fitted to the individual requirements in each particular case. In general, in the case of oral administration a daily dosage of about 0.1 to 1000 mg per person of a compound of general formula I should be appropriate, although the above upper limit can also be exceeded when necessary.
The following examples illustrate the present invention without limiting it. All temperatures are given in degrees Celsius.
Example A
Tablets of the following composition can be manufactured in the usual manner:
mg/tablet
Active substance
5
Lactose
45
Corn starch
15
Microcrystalline cellulose
34
Magnesium stearate
1
Tablet weight
100
Example B
Capsules of the following composition can be manufactured:
mg/capsule
Active substance
10
Lactose
155
Corn starch
30
Talc
5
Capsule fill weight
200
The active substance, lactose and corn starch can be firstly mixed in a mixer and then in a comminuting machine. The mixture can be returned to the mixer, the talc can be added thereto and mixed thoroughly. The mixture can be filled by machine into hard gelatine capsules.
Example C
Suppositories of the following composition can be manufactured:
mg/supp.
Active substance
15
Suppository mass
1285
Total
1300
The suppository mass can be melted in a glass or steel vessel, mixed thoroughly and cooled to 45° C. Thereupon, the finely powdered active substance can be added thereto and stirred until it has dispersed completely. The mixture can be poured into suppository moulds of suitable size and left to cool. The suppositories then can be removed from the moulds and packed individually in wax paper or metal foil.
The following examples 1-11 are provided for illustration of the invention. They should not be considered as limiting the scope of the invention, but merely as being representative thereof.
Example 1
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid methyl ester
To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (1.24 g, 6.55 mmol) in THF (12 mL) was added sodium hydride (55% dispersion in mineral oil, 0.31 g, 7.2 mmol) at 0° C. The reaction mixture was stirred for 30 min while it was allowed to warm up to room temperature. Methyl 5-chloropyrazine-2-carboxylate (1.36 g, 7.86 mmol) was added and stirring was continued for 2 h. Water (10 mL) was added and the mixture was extracted with ethyl acetate (40 mL). The combined organic layers were washed with brine (10 mL) and dried over sodium sulfate. Concentration and purification of the residue by chromatography (SiO 2 , heptane:ethyl acetate=80:20 to 50:50, 1.00 g, 47%) which was obtained as a light yellow oil. MS: m/e=326.2 [M+H] + .
Example 2
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylmethyl-amide
a) 5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid
To a solution of 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid methyl ester (1.00 g, 3.07 mmol) (1.0 g, 1.69 mmol) in ethanol (10 mL) was added aqueous sodium hydroxide (1 N, 6.2 mL). After heating at 60° C. for 30 min it was cooled to ambient temperature and aqueous sodium carbonate (2 M, 50 mL) added. Addition of aqueous sodium hydroxide (1 M, 50 mL) was followed by extraction with tert-butylmethylether. The aqueous phase was acidified with aqueous hydrogen chloride (25%) to pH=2 and extracted with tert-butylmethylether and ethyl acetate. The combined organic layers were dried over sodium sulfate and concentration afforded the title compound (450 mg, 86%) as a white foam. MS: m/e=310.5 [M−H] − .
b) 5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylmethyl-amide
To a solution of 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (150 mg, 0.48 mmol) in DMF (2 mL) were added 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (170 mg, 0.55 mmol), N,N-diisopropyl ethyl amine (410 μL, 2.4 mmol) and aminomethylcyclopropane (41 mg, 0.58 mmol). The resulting reaction mixture was stirred for 30 min at room temperature and diluted with water. The mixture was then extracted with ethyl acetate and the combined organic layers washed with aqueous sodium carbonate (saturated) and dried over sodium sulfate. Concentration and purification by chromatography (SiO 2 , heptane:ethyl acetate=90:10 to 60:40) (117 mg, 67%) which was obtained as an off-white solid. MS: m/e=365.3 [M+H] + .
Example 3
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid isopropylamide
As described for example 2b, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (100 mg, 0.32 mmol), was converted, using isopropylamine instead of aminomethylcyclopropane, to the title compound (SiO 2 , heptane:ethyl acetate=90:10 to 60:40, 37 mg, 33%) which was obtained as an off-white solid. MS: m/e=353.2 [M+H] + .
Example 4
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid tert-butylamide
As described for example 2b, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (100 mg, 0.32 mmol) was converted using tert-butylamine instead of aminomethylcyclopropane, to the title compound (SiO 2 , heptane:ethyl acetate=90:10 to 60:40, 24 mg, 20%) which was obtained as a colorless gum. MS: m/e=367.2 [M+H] + .
Example 5
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylamide
As described for example 2b, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (100 mg, 0.32 mmol) was converted, using cyclopropylamine instead of aminomethylcyclopropane, to the title compound (SiO 2 , heptane:ethyl acetate=90:10 to 60:40, 32 mg, 28%) which was obtained as a white solid. MS: m/e=351.3 [M+H] + .
Example 6
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
As described for example 2b, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (125 mg, 0.40 mmol) was converted, using 4-aminotetrahydropyran instead of aminomethylcyclopropane to the title compound (SiO 2 , heptane:ethyl acetate=70:30 to 40:60, 73 mg, 46%) which was obtained as a white solid. MS: m/e=395.1 [M+H] + .
Example 7
5-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (4,4-difluoro-cyclohexyl)-amide
As described for example 2b, 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (100 mg, 0.32 mmol) was converted, using 4,4-difluorocyclohexylamine instead of aminomethylcyclopropane to the title compound (SiO 2 , heptane:ethyl acetate=90:10 to 60:40, 37 mg, 27%) which was obtained as a white solid. MS: m/e=429.2 [M+H] + .
Example 8
2-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-quinoxaline
To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (100 mg, 0.53 mmol) in THF (6 mL) was added 2-hydroxyquinoxaline (77 mg, 0.53 mmol) and tributyl phosphine (206 μL, 0.79 mmol) at ambient temperature under an argon atmosphere. After cooling to 0° C., N,N,N′,N′-tetramethylazodicarboxamide (137 mg, 0.79 mmol) was added. The resulting orange solution was stirred for 16 h at ambient temperature followed by 2.5 h at 50° C. Then triphenylphosphine (208 mg, 0.79 mmol), 2-hydroxyquinoxaline (77 mg, 0.53 mmol) and diethyl azodicarboxylate (127 μL, 0.79 mmol) were added and the reaction mixture was stirred for 4 h at 50° C. The reaction mixture was then evaporated. Purification by chromatography (SiO 2 , heptane:ethyl acetate=95:5 to 0:100) afforded the title compound (67 mg, 40%) as a white solid. MS: m/e=318.2 [M+H] + .
Example 9
5-[(5-Methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid isopropylamide
a) 5-[(5-Methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester
A solution of (5-methyl-3-phenyl-4-isoxazolyl)methylamine (2.4 g, 12.7 mmol) and 5-chloro-pyrazine-2-carboxylic acid methyl ester (2.2 g, 12.7 mmol) in DMSO (15 mL) was heated with microwave irradiation to 160° C. for 30 min. After cooling to room temperature the reaction mixture was extracted with ethyl acetate, and the combined extracts were washed with water. The organic phase was dried over sodium sulfate, concentrated and chromatographed (SiO 2 , heptane:ethyl acetate=100:0 to 20:80). The oily product obtained was triturated with diisopropylether and ethyl acetate to afford the title compound (3.5 g, 84%) as an off-white solid. MS: m/e=325.4[M+H] + .
b) 5-[(5-Methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid isopropylamide
To a solution of isopropylamine (0.69 mL, 8 mmol) in dioxane (5 mL) was added dropwise trimethylaluminum solution (2M solution in hexane, 4 mL, 8 mmol). After stirring for 1 h at room temperature a suspension of 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester (650 mg, 2 mmol) in dioxane (5 mL) was added. The reaction mixture was stirred at 90° C. for 90 min, cooled to room temperature and poured into water. Extraction with ethyl acetate and washing with saturated aqueous Seignette salt solution was followed by drying of the organic phase over sodium sulfate and evaporation which afforded an oil. Purification by chromatography (SiO 2 , heptane:ethyl acetate=100:0 to 20:80) afforded the title compound (600 mg, 85%) as a white solid MS: m/e=352.3 [M+H] + .
Example 10
5-[(5-Methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid cyclopropylamide
As described for example 9b, 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester (650 mg, 2 mmol) was converted, using cyclopropylamine instead of isopropylamine, to the title compound (600 mg, 86%) which was obtained as a white solid. MS: m/e=394.3 [M+H] + .
Example 11
5-[(5-Methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
As described for example 9b, 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester (650 mg, 2 mmol) was converted, using 4-aminotetrahydropyran instead of isopropylamine, to the title compound (640 mg, 81%) which was obtained as a white solid. MS: m/e=350.4 [M+H] + .
Example 12
5-[3-(5-Fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
a) 5-Fluoro-pyridine-2-carbaldehyde oxime
To a solution of 5-fluoro-2-formylpyridine (5.0 g, 41 mmol) and hydroxylamine hydrochloride (3.06 g, 44 mmol) in ethanol (3.2 mL) and water (9.6 mL) was added ice (18.6 g). Then a solution of NaOH (4.0 g, 100 mmol) in water (4.6 mL) was added dropwise over 10 min keeping the temperature between −5° C. and 5° C. The reaction mixture was then stirred at room temperature for 30 min. Then HCl (4 N) was added to acidify the mixture and the resulting precipitate was filtered off and washed with water to afford the title compound (4.41 g, 79%) as a light brown solid. MS: m/e=141.0 [M+H] + .
b) 3-(5-Fluoro-pyridin-2-yl)-5-methyl-isoxazole-4-carboxylic acid ethyl ester
To a suspension of N-chlorosuccinimide (4.63 g, 35 mmol) in chloroform (21 mL) was added pyridine (0.28 mL, 3.5 mmol) and a solution of 5-fluoro-pyridine-2-carbaldehyde oxime (4.86 g, 35 mmol) in chloroform (110 mL) during 15 min at room temperature. After stirring for 30 min at this temperature a solution of ethyl (E)-3-(1-pyrrolidino)-2-butenoate (6.36 g, 35 mmol) in chloroform (4.4 mL) was added. The resulting suspension was warmed to 50° C. and a solution of triethylamine (4.83 mL, 35 mmol) in chloroform (4.4 mL) was added dropwise over a period of 30 min. Stirring was continued for 1.5 h at 50° C. and then cooled to ambient temperature. The solution was then diluted with ice-water (200 mL) and the aqueous layers were extracted with dichloromethane (50 mL) and dried over sodium sulfate and evaporation to give a dark brown oil. Purification by chromatography (SiO 2 , heptane:ethyl acetate=100:0 to 20:80) afforded the title compound (5.83 g, 67%) as yellow oil. MS: m/e=251.1 [M+H] + .
c) [3-(5-Fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-methanol
To a solution of 3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazole-4-carboxylic acid ethyl ester (2.5 g, 10 mmol) in dry THF (34 mL), cooled to 0° C., was added lithiumaluminumhydride (209 mg, 2.3 mmol) portionwise. After allowing to warm up to room temperature over 1 h, the mixture was cooled to 0° C. and water (0.2 mL) was added carefully followed by aqueous sodium hydroxide (15%, 0.2 mL) and water (0.6 mL). The resulting suspension was stirred for 4 h at ambient temperature and filtered over Hyflo®. The filtrate was then concentrated and purification by chromatography (SiO 2 , heptane:ethyl acetate=50:50 to 0:100) afforded the title compound (1.47 g, 71%) as a light yellow solid. MS: m/e=209.1 [M+H] + .
d) 5-[3-(5-Fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid
As described for example 1, [3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-methanol (1.0 g, 4.8 mmol), instead of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol, was converted to 5-[3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (667 mg) which was obtained as an ˜1:1 mixture with the starting alcohol after purification by chromatography (SiO 2 , heptane:ethyl acetate=50:50 to 0:100) as a light yellow solid. MS: m/e=345.2 [M+H] + . To a solution of the product mixture (655 mg, 0.86 mmol) in THF (2.2 mL), water (2.2 mL) and methanol (0.4 mL) was added lithium hydroxide monohydrate (72 mg, 1.7 mmol) and the resulting mixture stirred at room temperature for 72 h. The mixture was then evaporated and aqueous sodium hydroxide (1 N) added and a white precipitate formed which was filtered off (25 mg) and the filtrate was extracted with ethyl acetate. The aqueous phase was then acidified with HCl (4 N) and the precipitate was filtered off (39 mg). The combined precipitates were combined to afford the title compound (64 mg, 23%) which was obtained as an off-white solid. MS: m/e=329.2 [M−H] − .
e) 5-[3-(5-Fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
As described for example 2b, 5-[3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (44 mg, 13.3 mmol), instead of 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid, was converted, using 4-aminotetrahydropyran instead of aminomethylcyclopropane, to the title compound (SiO 2 , ethyl acetate then DCM:MeOH=90:10, 31 mg, 56%) which was obtained as a white solid. MS: m/e=414.2 [M+H] + .
Example 13
5-[3-(4-Fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide
a) (E)- and/or (Z)-4-Fluoro-benzaldehyde oxime
As described for example 12a, 4-fluorobenzaldehyde (24.8 g, 200 mmol) was converted, instead of 5-fluoro-2-formylpyridine, to the title compound (23.3 g, 84%) which was obtained as a white solid. MS: m/e=139.1 [M] + .
b) (E)- and/or (Z)-N-Hydroxy-4-fluoro-benzenecarboximidoyl chloride
To a solution of (E)- and/or (Z)-4-fluoro-benzaldehyde oxime (100 g, 719 mmol) in DMF (500 mL) was added N-chlorosuccinimide (110 g, 791 mmol) portionwise keeping the temperature below 70° C. The reaction mixture was stirred at room temperature for 2.5 h and then extracted with tert-butyl methyl ether to afford the title compound (125 g, 100%) which was obtained as a yellow oil. MS: m/e=173.1 [M] + .
c) 3-(4-Fluoro-phenyl)-isoxazole-4-carboxylic acid ethyl ester
To a solution of (E)- and/or (Z)-N-hydroxy-4-fluoro-benzenecarboximidoyl chloride (50 g, 241 mmol) in diethylether (1 L) was added a solution of ethyl 3-(N,N-dimethylamino)acrylate (87 mL, 601 mmol) and triethylamine (49 mL, 349 mmol) in diethylether (1 L). The resulting mixture was then stirred for 14 h at room temperature and evaporated. Purification by chromatography (SiO 2 , heptane:ethyl acetate=100:0 to 4:1) afforded the title product (50.2 g, 88%) which was obtained as a light yellow solid. MS: m/e=236.1 [M+H] + .
d) 3-(4-Fluoro-phenyl)-isoxazole-4-carboxylic acid
To a solution of 3-(4-fluoro-phenyl)-isoxazole-4-carboxylic acid ethyl ester (849 g, 208 mmol) in ethanol (215 mL) was added aqueous sodium hydroxide (2 N, 161 mL, 323 mmol) and the resulting mixture stirred overnight at room temperature. The mixture was then acidified with HCl solution (4 N, 85 mL) to pH 2-3. The precipitate was then filtered off and dissolved in THF (700 mL) and then washed with saturated sodium chloride solution. The aqueous phase was then extracted with ethyl acetate and THF (1:1, 300 mL) and the combined organic phases dried over sodium sulfate and evaporated to afford the title compound (40.8 g, 94%) which was obtained as an orange solid. MS: m/e=206.1 [M−H] − .
e) [3-(4-Fluoro-phenyl)-isoxazol-4-yl]-methanol
To a solution of 3-(4-fluoro-phenyl)-isoxazole-4-carboxylic acid (40 g, 193 mmol) in THF (400 mL) at −10° C. was added triethylamine (27.1 mL, 193 mmol) and then a solution of ethylchloroformate (18.8 mL, 193 mmol) in THF (120 mL) added keeping the temperature below −5° C. After 1 h the mixture was filtered and the filtrate cooled to −10° C. and a suspension of sodiumborohydride (19 g, 483 mmol) in water (120 mL) added over 15 minutes keeping the temperature below −5° C. The mixture was then allowed to warm up to room temperature over 2 h and diluted with aqueous sodium hydroxide (1 N, 700 mL) and extracted with tert-butylmethylether. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated. Purification by chromatography (SiO 2 , heptane:ethyl acetate=1:1) afforded the title product (20.1 g, 54%) which was obtained as white solid. MS: m/e=194.1 [M+H] + .
f) 5-[3-(4-Fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester
As described for example 1, [3-(4-fluoro-phenyl)-isoxazol-4-yl]-methanol (150 mg, 0.78 mmol), instead of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol, was converted to the title compound (153 mg, 60%) which was obtained as a white solid. MS: m/e=388.1 [M+OAc] + .
g) 5-[3-(4-Fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (2,2,2-trifluoro-ethyl)-amide
As described for example 9b, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (75 mg, 0.23 mmol), instead of 5-[(5-methyl-3-phenyl-isoxazol-4-ylmethyl)-amino]-pyrazine-2-carboxylic acid methyl ester, was converted, using 2,2,2-trifluoroethylamine instead of isopropylamine, to the title compound (64 mg, 71%) which was obtained as a light yellow solid. MS: m/e=397.2 [M+H] + .
Example 14
5-[3-(4-Fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid cyclopropylmethyl-amide
As described for example 13 g, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (75 mg, 0.23 mmol) was converted, using aminomethylcyclopropane instead of 2,2,2-trifluoroethylamine, to the title compound (44 mg, 52%) which was obtained as a light yellow solid. MS: m/e=427.0 [M+OAc] + .
Example 15
5-[3-(4-Fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid isopropylamide
As described for example 13 g, 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (100 mg, 0.3 mmol) was converted, using isopropylamine instead of 2,2,2-trifluoroethylamine, to the title compound (81 mg, 75%) which was obtained as a light yellow solid. MS: m/e=415.1 [M+OAc] + .
Example 16
5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid isopropylamide
a) (E)- and/or (Z)-4-Chloro-benzaldehyde oxime
As described for example 13a, 4-chlorobenzaldehyde (25.0 g, 178 mmol) was converted, instead of 4-fluorobenzaldehyde, to the title compound (27.0 g, 97%) which was obtained as an off-white solid. MS: m/e=155.1 [M] + .
b) (E)- and/or (Z)-N-Hydroxy-4-chloro-benzenecarboximidoyl chloride
As described for example 13b, (E)- and/or (Z)-4-chloro-benzaldehyde oxime (27.0 g, 173 mmol) was converted, instead of (E)- and/or (Z)-4-fluoro-benzaldehyde oxime, to the title compound (28.4 g, 86%) which was obtained as a light yellow solid. MS: m/e=189.1 [M] + .
c) 3-(4-Chloro-phenyl)-isoxazole-4-carboxylic acid ethyl ester
As described for example 13c, (E)- and/or (Z)-N-hydroxy-4-chloro-benzenecarboximidoyl chloride (58.0 g, 250.3 mmol) was converted, instead of (E)- and/or (Z)-N-hydroxy-4-fluoro-benzenecarboximidoyl chloride, to the title compound (57 g, 91%) which was obtained as a white solid. MS: m/e=252.1 [M+H] + .
d) 3-(4-Chloro-phenyl)-isoxazole-4-carboxylic acid
As described for example 13d, 3-(4-chloro-phenyl)-isoxazole-4-carboxylic acid ethyl ester (57.0 g, 226.5 mmol) was converted, instead of 3-(4-fluoro-phenyl)-isoxazole-4-carboxylic acid ethyl ester, to the title compound (50.7 g, 92%) which was obtained as a light yellow solid. MS: m/e=222.3 [M−H] − .
e) [3-(4-Chloro-phenyl)-isoxazol-4-yl]-methanol
As described for example 13e, 3-(4-chloro-phenyl)-isoxazole-4-carboxylic acid (40.0 g, 178.9 mmol) was converted, instead of 3-(4-fluoro-phenyl)-isoxazole-4-carboxylic acid, to the title compound (17.3 g, 46%) which was obtained as a light green solid. MS: m/e=210.1 [M+H] + .
f) 5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester
As described for example 1, [3-(4-chloro-phenyl)-isoxazol-4-yl]-methanol (1.5 g, 7.2 mmol), instead of [3-(4-fluoro-phenyl)-isoxazol-4-yl]-methanol, was converted to the title compound (1.7 g, 68%) which was obtained as a white solid. MS: m/e=404.1 [M+OAc] + .
g) 5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid isopropylamide
As described for example 15, 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (100 mg, 0.29 mmol), instead of 5-[3-(4-fluoro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester, was converted to the title compound (1.3 mg, 1%) which was obtained as a light yellow solid. MS: m/e=431.1 [M+OAc] + .
Example 17
5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid ((S)-2-hydroxy-1-methyl-ethyl)-amide
a) 5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid
To a solution of 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester (1.0 g, 2.89 mmol) in THF (6.3 mL), water (6.3 mL) and methanol (1.75 mL) was added lithium hydroxide monohydrate (141.4 mg, 5.78 mmol) and the resulting mixture stirred at room temperature for 2 h and then acidified with HCl (4 N) and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated to afford the title product (360 mg, 38%) which was obtained as white solid. MS: m/e=330.0 [M−H] − .
b) (5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid ((S)-2-hydroxy-1-methyl-ethyl)-amide
To a solution of 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (80 mg, 0.24 mmol) and D-alaninol (22.8 □L, 0.29 mmol) in THF (7 mL) was added 1-hydroxybenzotriazole hydrate (37.3 mg, 0.24 mmol), N-ethyldiisopropylamine (105.2 □L, 0.60 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (47.1 mg, 0.24 mmol) at room temperature under nitrogen. The reaction mixture was stirred at room temperature for 72 h. Then the reaction mixture was diluted with water (10 mL), and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated. Purification by chromatography (SiO 2 , heptane:ethyl acetate=1:1 to 2:3) afforded the title product (39 mg, 42%) which was obtained as white solid. MS: m/e=389.0 [M+H] + .
Example 18
5-[3-(4-Chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid ((R)-2-hydroxy-1-methyl-ethyl)-amide
As described for example 17b, 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid (80 mg, 0.24 mmol) was converted, using L -alaninol instead of D -alaninol, to the title compound (44 mg, 47%) which was obtained as a white solid. MS: m/e=389.0 [M+H] + .
Example 19
5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
a) 3-Pyridin-2-yl-isoxazole-4-carboxylic acid ethyl ester
To a solution of N-chlorosuccinimide (54.7 g, 409 mmol) in DMF (1 L) was added pyridine-2-carbaldoxime (50 g, 409 mmol) portionwise and the resulting mixture was then stirred for 64 h at room temperature. To this solution was then added ethyl 3-(N,N-dimethylamino)acrylate (58.6 g, 409 mmol) and triethylamine (82.9 mL, 819 mmol) in chloroform (10 mL) and the resulting mixture was then stirred for 14 h at room temperature and poured onto a mixture of ice water and HCl (4 N, 100 mL) and extracted with ethylacetate. The organic extract was then washed with water, saturated aqueous sodium hydrogen carbonate solution, brine, dried with sodium sulfate, filtered and evaporated. Purification by distillation afforded the title product (58.9 g, 66%) which was obtained as a light brown liquid. Bp 125-127° C. at 0.4 mbar. MS: m/e=219.2 [M+H] + .
b) 3-Pyridin-2-yl-isoxazole-4-carboxylic acid
As described for example 17a, 3-pyridin-2-yl-isoxazole-4-carboxylic acid ethyl ester (9.6 g, 44 mmol), instead of 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester, was converted to the title compound (6.5 g, 79%) which was obtained as an off-white solid. MS: m/e=189.3 [M−H] − .
c) (3-Pyridin-2-yl-isoxazol-4-yl)-methanol
As described for example 13e, 3-pyridin-2-yl-isoxazole-4-carboxylic acid (39.0 g, 200 mmol) was converted, instead of 3-(4-fluoro-phenyl)-isoxazole-4-carboxylic acid, to the title compound (26.8 g, 76%) which was obtained as a white solid. MS: m/e=177.2 [M] + .
d) 5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid methyl ester
As described for example 1, (3-pyridin-2-yl-isoxazol-4-yl)-methanol (1.0 g, 5.7 mmol), instead of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol, was converted to the title compound (584 mg, 32%) which was obtained as a white solid. MS: m/e=313.1 [M+H] + .
e) 5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid
As described for example 17a, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid methyl ester (432 mg, 1.4 mmol), instead of 5-[3-(4-chloro-phenyl)-isoxazol-4-ylmethoxy]-pyrazine-2-carboxylic acid methyl ester, was converted to the title compound (285 mg, 71%) which was obtained as a white solid. MS: m/e=297.1 [M−H] − .
f) 5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (tetrahydro-pyran-4-yl)-amide
As described for example 2b, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (75.4 mg, 2.5 mmol), instead of 5-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid, was converted, using 4-aminotetrahydropyran instead of aminomethylcyclopropane, to the title compound (SiO 2 , heptane:ethyl acetate 1:1 to 0:1, 83.8 mg, 87%) which was obtained as a white solid. MS: m/e=382.2 [M+H] + .
Example 20
5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid isopropylamide
As described for example 19f, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (83.6 mg, 2.8 mmol) was converted, using isopropylamine instead of 4-aminotetrahydropyran, to the title compound (SiO 2 , heptane:ethyl acetate 4:1 to 3:7, 65 mg, 68%) which was obtained as a white solid. MS: m/e=340.2 [M+H] + .
Example 21
5-(3-Pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid cyclopropylamide
As described for example 19f, 5-(3-pyridin-2-yl-isoxazol-4-ylmethoxy)-pyrazine-2-carboxylic acid (84.7 mg, 2.8 mmol) was converted, using cyclopropylamine instead of 4-aminotetrahydropyran, to the title compound (SiO 2 , heptane:ethyl acetate 7:3 to 2:8, 78 mg, 81%) which was obtained as a white solid. MS: m/e=338.3 [M+H] + .
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The invention relates to isoxazolo-pyrazine derivatives and their pharmaceutically acceptable salts having affinity and selectivity for the GABA A α5 receptor binding site, their manufacture, and pharmaceutical compositions containing them. The compounds of the present invention are inverse agonists of GABAAα5. The invention also relates to methods for enhancing cognition and for treating cognitive disorders like Alzheimer's disease.
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FIELD OF THE INVENTION
[0001] This invention relates to a semi-solid composition containing antioxidants and urea for treating and protecting the skin.
BACKGROUND OF THE INVENTION
[0002] As the outermost layer of skin, the stratum corneum (SC) is continuously exposed to an oxidative environment, including air pollutants, ultraviolet radiation, chemical oxidants, and aerobic microorganisms. Human SC reveals characteristic antioxidant and protein oxidation gradients with increasing antioxidant depletion and protein oxidation towards the outer layers. SC antioxidants, lipids, and proteins are oxidatively modified upon treatments with ultraviolet A/ultraviolet B, ozone, and benzoyl peroxide. Thiele J. J., Schroeter C., Hsieh S. N., Podda M., Packer L., Curr Probl Dermatol. 2001;29:26-42.
[0003] Furthermore, the skin is increasingly exposed to ambient UV-irradiation thus increasing its risk for photooxidative damage with long term detrimental effects like photoaging, which is characterized by wrinkles, loss of skin tone, and resilience. Scharffetter-Kochanek K, Brenneisen P, Wenk J, et al., Exp Gerontol. 2000; 35:307-316
[0004] The importance of antioxidants is their role in scavenging free radicals, which are created by natural oxidative process occurring in the environment.
[0005] There is a need for topical products with antioxidant formulations to prevent UV-induced carcinogenesis and photoaging as well as to modulate desquamatory skin disorders.
SUMMARY OF THE INVENTION
[0006] Accordingly, the present invention includes an improved treatment for the care and protection of the skin, particularly severely dry skin, using a combination of about 21 to about 40 wt-% of urea and about 0.1 to 20 wt-% of an antioxidant in a suitable defined formulation.
[0007] Thus, one aspect of the present invention is a dermatological composition including from about 21 to about 40 wt-% urea, from about 0.1 to 20 wt-% of an antioxidant, and the balance being dermatologically acceptable excipients.
[0008] The use of such high concentrations of urea combined with antioxidant skin protectants have been found to provide added efficacy and suitability for treating and protecting skin, and, particularly for treating icthyosis, xerosis, severely dry skin, dermatitis, eczema, debridement and tissue softening as well as other skin conditions.
[0009] Still another aspect of the present invention is a method of treating xerosis, ichthyosis, severe dry skin, dermatitis, and eczema by applying to skin in need of treatment an effective amount of a semi-solid dermatological composition containing about 21 to about 40 wt-% urea and about 0.1 to 20 wt-% of an antioxidant.
DETAILED DESCRIPTION
[0010] The dermatological composition of the present invention is a semi-solid at room temperature but is easily absorbed into the stratum corneum. A preferred application of the formulation is a cream which contains a petroleum based liquid and solid fraction as skin protectants.
[0011] The cream composition has advantageous properties for the treatment of severe dry skin clinically characterized as xerosis and for the temporary relief of itching associated with various pathological dermatological conditions. The formulation produces a keratolytic action found beneficial in the treatment of icthyosis, atopic dermatitis. The formulation also produces added protection against debridement and tissue suffering from oxidative events. Application of the cream to the skin as needed provides relief of the conditions.
[0012] In addition to containing about 21 to about 40 wt-% of urea, the composition of the present invention includes an effective amount of antioxidant skin protectants, for example, from about 0.1 to about 20 wt-% based on the total weight of the composition.
[0013] Antioxidants include, but are not limited to, tocopherols (vitamin E), tocopherol derivatives, tocotrienols, ascorbic acid (vitamin C), ascorbic acid derivatives, carotenoids, vitamin A or derivatives thereof, butylated hydroxytoluene, butylated hydroxyanisole, gallic esters, flavonoids such as, for example, quercetin or myricetin, selenium, grape seed extract, catechins such as, for example, epicatechin, epicatechingallate, epigallocatechin or epigallocatechingallate, sulfur-containing molecules such as, for example, glutathione, cysteine, lipoic acid, N-acetylcysteine, chelating agents such as, for example, ethylenediamine tetraacetic acid or other customary antioxidants.
[0014] One antioxidant, vitamin E, is of particular interest. The term “vitamin E” includes tocopherol (vitamin E) and derivatives thereof such as, for example, α-, β-, γ-, δ-, ε-, ζ 1 , ζ 2 , and η-tocopherol, and α-tocopherol acid succinate. Vitamin E is known as an antioxidant and protective vitamin for phospholipids of the cell membrane. It maintains the permeability and stability of the cell membrane, Lucy. Annals N. Y Academy of Science 203, p. 4 (1972). It further has been known that vitamin E has a membrane-sealing effect. In erythrocytes, the simplest cells of the human body, there has been found that vitamin E provides a protective effect for the cell membrane. As with all antioxidants, vitamin E protects cells, including, epidermal cells which are susceptible to a wide range of oxidating events.
[0015] The cream composition also includes a combination of semi-solid and liquid petroleum fractions. The semi-solid skin protectant is contained in about 5.5 to about 20 wt-% and includes petrolatum or a synthetic or semi-synthetic hydrocarbon of the same nature as petrolatum. Mixtures of such ingredients can also be used. The preferred semi-solid material is petrolatum, commercially available from a wide variety of sources.
[0016] The liquid portion skin protectant is a liquid petrolatum and contained in the composition in about 10 to about 20 wt-%. This material can include any synthetic or semi-synthetic oleaginous liquid fraction. A preferred embodiment is mineral oil which is a liquid mixture of hydrocarbons obtained from petroleum.
[0017] Another preferred ingredient encompassed in the composition of the present invention is propylene glycol which may be contained up to about 5 wt-% in the composition, preferably in the range of from about 1 to about 5 wt-%.
[0018] In addition to the above embodiments, the present composition also contains dermatologically acceptable excipients, such as for example emulsifiers and thickeners. Among these are for example a C 16 to C 18 straight or branched chain fatty alcohols or fatty acids or mixtures thereof. Preferably these include cetyl alcohol, stearyl alcohol, stearic acid, palmitic acid, or mixtures thereof. Fatty acids or fatty alcohols may be present in from about 0.25 to 2 wt-%.
[0019] Another ingredient useful in the composition of the present invention may be glyceryl stearate, which is a monoester of glycerine and stearic acid, or other suitable forms of glyceryl stearate for example glyceryl stearate SE, which is a commercially available self-emulsifying grade of glycerol stearate that contains some sodium and/or potassium stearate. Glyceryl stearate may be in the composition anywhere from about 1 to about 3 wt-%.
[0020] Xanthan gum is another ingredient which may be used in the present invention. Xanthan gum is a high molecular weight heteropolysaccharide gum produced by pure-culture fermentation of a carbohydrate with Xanthomonas campestris . The gum is also commercially available from various sources.
[0021] As part of the dermatologically acceptable excipients, the composition includes thickeners which provide a high viscosity cream designed to remain in place upon application to the skin. Preferred thickeners include a mixture of a carbomer and triethanolamine. The mixture is combined together and added to the composition in an amount totaling anywhere from about 0.05 to 5 wt-%. Triethanolamine is purchased as Trolamine NF from BASF. The carbomers come in various molecular weights and identified by numbers. These are otherwise known as Carbopol. A preferred embodiment of the present invention is Carbopol 940. The carbomer or Carbopols are resins which are known thickening agents. They are homopolymers of acrylic acid crosslinked with an allyl ether of pentaerythritol, an allyl ether of sucrose or an allyl ether of propylene. The carbomer is present in the composition as a thickener and also is used to suspend and stabilize the emulsion. Although Carbopol 940 is preferably used in the present invention, other analogs may also be used such as carbomer 910, 2984, 5984, 954, 980, 981, 941 and 934. Carbopol ETD 2001, 2020, and 2050 and Ultrez 20 are also commercially available and can be used since they are similar in chemistry and function.
[0022] A typical formulation representing the particular and most preferred embodiment of the present invention is illustrated as follows:
Ingredient % W/W Anti-oxidant 5.0 Urea USP 40 Carbopol 940 0.20 Petrolatum 6.00 Mineral oil 7.1 Glyceryl stearate 1.86 Cetyl alcohol 0.63 Propylene glycol 3.00 Xanthan gum 0.05 Trolamine 0.15 Purified water Q.S. 100.00.
Glossary of Ingredients
[0023] The formulation of the present invention has been defined above and more specifically exemplified in the following examples. Since the formulation employs various ingredients, some of the ingredients have been defined generically and by common name. In addition, the following is a glossary of technical names and trade names with manufacturing sources for some of the ingredients employed in the formulation of the present invention.
[0024] Mineral Oil
[0025] Definition
[0026] Mineral oil is a liquid mixture of hydrocarbons obtained from petroleum.
[0027] Technical Names
[0028] Heavy Mineral Oil
[0029] Light Mineral Oil
[0030] Liquid Paraffin
[0031] Paraffin Oil
[0032] Trade Names
[0033] Benol White Mineral Oil (Witco/Sonneborn)
[0034] Blandol White Mineral Oil (Witco/Sonneborn)
[0035] Britol 6 (Witco Corporation)
[0036] Britol 7 (Witco Corporation)
[0037] Britol 9 (Witco Corporation)
[0038] Britol 20 (Witco Corporation)
[0039] Britol 24 (Witco Corporation)
[0040] Britol 35 (Witco Corporation)
[0041] Britol 50 (Witco Corporation)
[0042] Carnation White Mineral Oil (Witco/Sonneborn)
[0043] Crystosol NF 70 (Witco Corporation)
[0044] Crystosol NF 90 (Witco Corporation)
[0045] Crystosol U.S. Pat. No. 200 (Witco Corporation)
[0046] Crystosol U.S. Pat. No. 240 (Witco Corporation)
[0047] Crystosol U.S. Pat. No. 350 (Witco Corporation)
[0048] Drakeol 5 (Penreco)
[0049] Drakeol 6 (Penreco)
[0050] Drakeol 7 (Penreco)
[0051] Drakeol 8 (Penreco)
[0052] Drakeol 9 (Penreco)
[0053] Drakeol 10 (Penreco)
[0054] Drakeol 13 (Penreco)
[0055] Drakeol 15 (Penreco)
[0056] Drakeol 19 (Penreco)
[0057] Drakeol 21 (Penreco)
[0058] Drakeol 32 (Penreco)
[0059] Drakeol 34 (Penreco)
[0060] Drakeol 35 (Penreco)
[0061] Draketex 50 (Penreco)
[0062] Ervol White Mineral Oil (Witco/Sonneborn)
[0063] GloriaWhite Mineral Oil (Witco/Sonneborn)
[0064] Kaydol White Mineral Oil (Witco/Sonneborn)
[0065] Klearol White Mineral Oil (Witco/Sonneborn)
[0066] Parol 70 (Penreco)
[0067] Parol 80 (Penreco)
[0068] Parol 100 (Penreco)
[0069] PD-23 White Mineral Oil (Witco/Sonneborn)
[0070] Peneteck (Penreco)
[0071] Protol White Mineral Oil (Witco/Sonneborn)
[0072] Superla Mineral Oil #5 NF (Amoco Lubricants)
[0073] Superla Mineral Oil #6 NF (Amoco Lubricants)
[0074] Superla Mineral Oil #7 NF (Amoco Lubricants)
[0075] Superla Mineral Oil #9 NF (Amoco Lubricants)
[0076] Superla Mineral Oil #10 NF (Amoco Lubricants)
[0077] Superla Mineral Oil #13 NF (Amoco Lubricants)
[0078] Superla Mineral Oil #18 USP (Amoco Lubricants)
[0079] Superla Mineral Oil #21 USP (Amoco Lubricants)
[0080] Superla Mineral Oil #31 USP (Amoco Lubricants)
[0081] Superla Mineral Oil #35 USP (Amoco Lubricants)
[0082] Uniwhite Oil 55 (UPI)
[0083] Uniwhite Oil 70 (UPI)
[0084] Uniwhite Oil 85 (UPI)
[0085] Uniwhite Oil 130 (UPI)
[0086] Uniwhite Oil 185 (UPI)
[0087] Uniwhite Oil 205 (UPI)
[0088] Uniwhite Oil 350 (UPI)
[0089] Glyceryl Stearate
[0090] Empirical Formula
C 21 H 42 O 4
[0091] Definition
[0092] Glyceryl stearate is the monoester of glycerin and stearic acid. It conforms generally to the formula:
[0093] Technical Names
[0094] 2,3-Dihydroxypropyl octadecanoate
[0095] Glyceryl monostearate
[0096] Monostearin
[0097] Octadecanoic acid, 2,3-dihydroxypropyl ester
[0098] Octadecanoic acid, monoester with 1,2,3-propanetriol
[0099] Trade Names
[0100] Aldo HMS (Lonza Inc./Lonza Ltd.)
[0101] Aldo MS (Lonza Inc./Lonza Ltd.)
[0102] Aldo MSLG (Lonza Inc./Lonza Ltd.)
[0103] Alkamuls GMS (Rhone-Poulenc)
[0104] Arlacel 129 (ICI)
[0105] Atmos 150 (ICI)
[0106] Atmul 84 (ICI)
[0107] Atmul 124 (ICI)
[0108] Capmul GMS (Karishamns Lipid Specialties)
[0109] Ceral MN (Fabriquimica)
[0110] Ceral MNT (Fabriquimica)
[0111] Cerasynt GMs (ISP Van Dyk)
[0112] Cerasynt SD (ISP Van Dyk)
[0113] Cithrol GMS N/E (Croda Surfactants Ltd.)
[0114] CPH-53-N (Hall)
[0115] CPH-144-N (Hall)
[0116] Cutina GMS (Henkel)
[0117] Cutina MD (Henkel)
[0118] Cutina MD-A (Henkel)
[0119] Dimodan PM (Grinsted)
[0120] Dimodan PM 300 (Grinsted)
[0121] Elfacos GMS (Akzo BV)
[0122] Emerest 2400 (Henkel/Organic Products)
[0123] Empilan GMS NSE (Albright & Wilson)
[0124] Emuldan FP 40 (Grinsted)
[0125] Emuldan HA 60 (Grinsted)
[0126] Emuldan HLT 40 (Grinsted)
[0127] ESTOL GMS90 1468 (Unichema)
[0128] ESTOL GMSveg 1474 (Unichema)
[0129] Geleol (Gattefosse)
[0130] Grillomuls S 40 (Grillo-Werke)
[0131] Grillomuls S 60 (Grillo-Werke)
[0132] Grillomuls S 90 Grillo-Werke)
[0133] Hefti GMS-33 (Hefti)
[0134] Hefti GMS-99 (Hefti)
[0135] Hodak GMS (Calgene)
[0136] Imwitor 191 (Huls AG/Huls America)
[0137] Imwitor 900 (Huls AG/Huls America)
[0138] Kemester 5500 (Witco)
[0139] Kemester 6000 (Witco)
[0140] Kessco GMS (Akzo BV)
[0141] Lanesta 24 (Lanaetex)
[0142] Lasemul 92 AE (Industrial Quimica)
[0143] Lasemul 92 AE/A (Industrial Quimica)
[0144] Lasemul 92 N 40 (Industrial Quimica)
[0145] Lexemul 503 (Inolex)
[0146] Lexemul 515 (Inolex)
[0147] Lexemul 55G (Inolex)
[0148] Lipo GMS 410 (Lipo)
[0149] Lipo GMS 450 (Lipo)
[0150] Lipo GMS 600 (Lipo)
[0151] Nikkol MGS-DEX (Nikko)
[0152] Norfox GMS (Norman, Fox & Co.)
[0153] Norfvox GMS-SE (Norman, Fox & Co.)
[0154] Prodhybase GLA (Prod'Hyg)
[0155] Protachem 26 (Protameen)
[0156] Protachem G 5509 (Protameen)
[0157] Protachem G-5566 (Protameen)
[0158] Protachem GMS-540 (Protameen)
[0159] Protachem HMS (Protameen)
[0160] Sterol GMS (Auschem)
[0161] Tegin 90 (Goldschmidt)
[0162] Tegin 515 (Goldschmidt)
[0163] Tegin 4011 (Goldschmidt)
[0164] Tegin 4100 (Goldschmidt)
[0165] Tegin GRB (Goldschmidt)
[0166] Tegin ISO (Goldschmidt)
[0167] Tegin M (Goldschmidt)
[0168] Tegin MAV (Goldschmidt)
[0169] Unitina MD (UPI)
[0170] Unitina MD-A (UPI)
[0171] Unitolate GS (UPI)
[0172] Witconol 2400 (Witco)
[0173] Witconol 2401 (Witco)
[0174] Witconol MST (Witco SA)
[0175] Witconol MST (Witco)
[0176] Zohar GLST (Zohar)
[0177] Glyceryl Stearate SE
[0178] Definition
[0179] Glyceryl stearate SE is a self-emulsifying grade of glyceryl stearate (q.v.) that contains some sodium and/or potassium stearate.
[0180] Trade Names
[0181] Aldo MSD (Lonza Inc./Lonza Ltd.)
[0182] Ceral ME (Fabriquimica)
[0183] Ceral MET (Fabriquimica)
[0184] Ceral TN (Fabriquimica)
[0185] Cerasynt Q (ISP Van Dyk)
[0186] Cithrol GMS S/E (Croda Surfactants Ltd.)
[0187] Cutina KD-16 (Henkel)
[0188] Dermalcare GMS/SE (Rhone-Poulenc)
[0189] Dracorin GMS SE O/W 2/008475 (Dragoco)
[0190] Emerest 2407 (Henkel/Organic Products)
[0191] Empilan GMS SE (Albright & Wilson)
[0192] Emuldan HA 32/S3 (Grinsted)
[0193] ESTOL BMSse 1462 (Unichema)
[0194] Hefti GMS-33-SES (Hefti)
[0195] Hodag GMS-D (Calgene)
[0196] Imwitor 960 (Huls Ag/Huls America)
[0197] Kemester 6000 SE (Witco)
[0198] Lamecreme KSM (Grunau)
[0199] Lanesta 40 (Lanaetex)
[0200] Lexemul 530 (Inolex)
[0201] Lexemul T (Inolex)
[0202] Lipo GMS 470 (Lipo)
[0203] Mazol GMSD-K (PPG)
[0204] Prodhybase GLN (Prod'Hyg)
[0205] REWOMUL MG SE (Rewo Chemische)
[0206] Tegin (Goldschmidt)
[0207] Tegin Spezial (Goldschmidt)
[0208] Tegin V (Goldschmidt)
[0209] Unitolate GMS-D (UPI)
[0210] Witconol 2407 (Witco)
[0211] Cetyl Alcohol
[0212] Empirical Formula
C 16 H 34 O
[0213] Definition
[0214] Cetyl alcohol is the fatty alcohol that conforms generally to the formula:
CH 2 (CH 2 ) 14 CH 2 OH
[0215] Technical Names
[0216] 1-Hexadecanol
[0217] n-Hexadecyl alcohol
[0218] Palmityl alcohol
[0219] Trade Names
[0220] Adol 52 (Witco)
[0221] Adol 520 (Witco)
[0222] Adol 52-NF (Witco)
[0223] Adol 520-NF (Witco)
[0224] Cachalot C-50 (Michel)
[0225] Cachalot C-51 (Michel)
[0226] Cachalot C-52 (Michel)
[0227] Cetaffine (Laserson & Sabetay)
[0228] Cetal (Amerchol)
[0229] Cetyl alcohol (Rhone-Poulenc)
[0230] CO-1695 (Procter & Gamble)
[0231] Crodacol C-70 (Croda, Inc.)
[0232] Crodacol C90 (Croda Chemicals Ltd.)
[0233] Crodacol C-95 (Croda, Inc.)
[0234] Fancol CA (Fanning)
[0235] Hyfatol 16-95 (Aarhus)
[0236] Hyfatol 16-98 (Aarhus)
[0237] Lanette 16 (Henkel)
[0238] Lanol C (SEPPIC)
[0239] Laurex 16 (Albright & Wilson)
[0240] Lipocol C (Lipo)
[0241] Stearic Acid
[0242] Empirical Formula
C 18 H 36 O 2
[0243] Definition
[0244] Stearic acid is the fatty acid that conforms generally to the formula:
CH 2 (CH 2 ) 16 COOH
[0245] Trade Names
[0246] Crosterene SA4310 (Croda Universal Ltd.)
[0247] Dar-Chem 14 (Darling)
[0248] Emersol 120 (Henkel/Emery)
[0249] Emersol 132 (Henkel/Emery)
[0250] Emersol 150 (Henkel/Emery)
[0251] Glycon DP (Lonza Inc./Lonza Ltd.)
[0252] Glycon P-45 (Lonza Inc./Lonza Ltd.)
[0253] Glycon S-65 (Lonza Inc./Lonza Ltd.)
[0254] Glycon S-70 (Lonza Inc./Lonza Ltd.)
[0255] Glycon S-90 (Lonza Inc./Lonza Ltd.)
[0256] Glycon TP (Lonza Inc./Lonza Ltd.)
[0257] Hy-Phi 1199 (Darling)
[0258] Hy-Phi 1303 (Darling)
[0259] Hy-Phi 1401 (Darling)
[0260] Hystrene 4516 (Witco)
[0261] Hystrene 5016 (Witco)
[0262] Hystrene 7018 (Witco)
[0263] Hystrene 9718 (Witco)
[0264] Industrene 5016 (Witco)
[0265] Industrene 7018 (Witco)
[0266] Kartacid 1890 (Akzo BV)
[0267] Neo-Fat 18 (Akzo)
[0268] Neo-Fat 18-54 (Akzo)
[0269] Neo-Fat 18-55 (Akzo)
[0270] Neo-Fat 18-61 (Akzo)
[0271] Pearl Stearic (Darling)
[0272] PRIFAC 2981 (Unichema)
[0273] Pristerene 4900 (Unichema)
[0274] Pristerene 4901 (Unichema)
[0275] Pristerene 4902 (Unichema)
[0276] Pristerene 4904 (Unichema)
[0277] Pristerene 4905 (Unichema)
[0278] Pristerene 4910 (Unichema)
[0279] Pristerene 4911 (Unichema)
[0280] Pristerene 4915 (Unichema)
[0281] Pristerene 4921 (Unichema)
[0282] Pristerene 4968 (Unichema)
[0283] Pristerene 9550 (Unichema)
[0284] Safacid 18 (Pronova)
[0285] Safacid 16/18 CR (Pronova)
[0286] Unifat 54 (UPI)
[0287] Unifat 55L (UPI)
[0288] Stearyl Alcohol
[0289] Empirical Formula
C 18 H 38 O
[0290] Definition
[0291] Stearyl alcohol is the fatty alcohol that conforms generally to the formula:
CH 3 (CH 2 ) 16 CH 2 OH
[0292] Technical Name
[0293] 1-Octadecanol
[0294] Trade Names
[0295] Adol 63 (Witco)
[0296] Adol 61-NF (Witco)
[0297] Adol 62-NF (Witco)
[0298] Adol 620-NF (Witco)
[0299] Cachalot S-53 (Michel)
[0300] Cachalot S-54 (Michel)
[0301] Cachalot S-56 (Michel)
[0302] CO-1895 (Procter & Gamble)
[0303] Crodacol S-70 (Croda, Inc.)
[0304] Crodacol S-95 (Croda, Inc.)
[0305] Crodacol S-95 (Croda Chemicals Ltd.)
[0306] Fancol SA (Fanning)
[0307] Hyfatol 18-95 (Aarhus)
[0308] Hyfatol 18-98 (Aarhus)
[0309] Lanette 18 (Henkel)
[0310] Lanol S (SEPPIC)
[0311] Laurex 18 (Albright & Wilson)
[0312] Lipocol S (Lipo)
[0313] Stearal (Amerchol)
[0314] Stearyl Alcohol (Rhone-Poulenc)
[0315] Steraffine (Laserson & Sabetay)
[0316] Unihydag WAX-18 (UPI)
[0317] Palmitic Acid
[0318] Empirical Formula
C 16 H 32 O 2
[0319] Definition
[0320] Palmitic acid is the fatty acid that conforms generally to the formula:
CH 3 (CH 2 ) 14 COOH
[0321] Technical Name
[0322] n-Hexadecanoic acid
[0323] Trade Names
[0324] Crodacid PD3160 (Croda Universal Ltd.)
[0325] Edenor L2SM (Henkel)
[0326] Emersol 142 (Henkel/Emery)
[0327] Emersol 144 (Henkel/Emery)
[0328] Hystrene 7016 (Witco)
[0329] Hystrene 9016 (Witco)
[0330] Kartacid 1692 (Akzo BV)
[0331] Neo-Fat 16 (Akzo)
[0332] Neo-Fat 16-54 (Akzo)
[0333] Neo-Fat 16-56 (Akzo)
[0334] Neo-Fat 16-S (Akzo)
[0335] PRIFAC 2962 (Unichema)
[0336] Prifrac 2690 (Unichema)
[0337] Trade Name Mixture
[0338] N.S.L.E. (Sederma)
[0339] Propylene Glycol
[0340] Empirical Formula
C 3 H 8 O 2
[0341] Definition
[0342] Propylene glycol is the aliphatic alcohol that conforms generally to the formula:
[0343] Technical Name
[0344] 1,2-Propanediol
[0345] Trade Names
[0346] Lexol PG-865 (855) (Inolex)
[0347] 1,2-Propylene Glycol USP (BASF)
[0348] Xanthan Gum
[0349] Definition
[0350] Xanthan gum is a high molecular weight hetero polysaccharide gum produced by a pure-culture fermentation of a carbohydrate with Xanthomonas campestris.
[0351] Technical Names
[0352] Corn sugar gum
[0353] Xanthan
[0354] Trade Names
[0355] Kelgum CG (Calgon)
[0356] Keltrol (Kelco)
[0357] Keltrol CG (Calgon)
[0358] Keltrol CG 1000 (Calgon)
[0359] Keltrol CG BT (Calgon)
[0360] Keltrol CG F (Calgon)
[0361] Keltrol CG GM (Calgon)
[0362] Keltrol CG RD (Calgon)
[0363] Keltrol CG SF (Calgon)
[0364] Keltrol CG T (Calgon)
[0365] Keltrol CG TF (Calgon)
[0366] Kelzan (Kelco)
[0367] Merezan 8 (Meer)
[0368] Merezan 20 (Meer)
[0369] Rhodigel (Vanderbilt)
[0370] Rhodigel (Rhone-Poulenc)
[0371] Rhodopol SC (Rhone-Poulenc)
[0372] Xanthan gum (Jungbunzlauer)
[0373] Triethanolamine
[0374] Empirical Formula
C 6 H 15 O 3 N
[0375] Definition
[0376] Triethanolamine is an alkanolamine that conforms generally to the formula:
N(CH 2 CH 2 OH) 3
[0377] Technical Names
[0378] Ethanol, 2,2′,2″-Nitrilotris-2,2′,2″-Nitrilotris[Ethanol]
[0379] TEA
[0380] Trolamine
[0381] Trade Name
[0382] Triethanolamine Pure C (BASF)
EXAMPLE
[0383] The typical formulation illustrated above is prepared commercially as follows:
# Ingredient Batch Units 1 Purified water 1084.47 Gm 2 Vitamin E 150.00 Gm 3 Urea USP 1200.00 Gm 4 Carbopol 940 4.50 Gm 5 Petrolatum 178.20 Gm 6 Mineral oil 211.80 Gm 7 Glyceryl stearate 56.25 Gm 8 Cetyl alcohol 18.78 Gm 9 Propylene glycol 90.00 Gm 10 Xanthan gum 1.50 Gm 11 Trolamine NF 4.50 Gm 12 Purified Water Q.S. 3000.00 Gm
[0384] The above product was manufactured as follows:
[0385] Step 1
[0386] Place #1 in Tank A (water phase) and sprinkle in #4 in Tank A and mix to disperse. After uniformly dispersed, heat contents of Tank A to about 75° C. while mixing.
[0387] Step 2
[0388] Add #3 to Tank A and mix to dissolve.
[0389] Step 3
[0390] In a separate tank add #2, 5, 6, 7, 8. Heat to about 75° C. with mixing (oil phase).
[0391] Step 4
[0392] In a separate container disperse uniformly #10 in #9. Add this to Tank A and continue to mix.
[0393] Step 5
[0394] Add the oil phase (step 3) to the water phase in Tank A with mixing.
[0395] Step 6
[0396] Add #11 to Tank A and mix. Slowly cool the batch.
[0397] Step 7
[0398] Add #12 to Q.S. the batch to final weight.
[0399] The bulk product is then packaged into conventional containers for use as a cream.
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Enhanced dermatological compositions are described herein using from about 21 to about 40 wt-% urea with antioxidant skin protectants suitable for the treatment of icthyosis, xerosis, severely dry skin, dermatitis, eczema, debridement and tissue suffering and other similar skin conditions.
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RELATED APPLICATIONS
[0001] This nonprovisional patent application is a continuation-in-part application of, and claims priority to co-pending, non-provisional patent application U.S. Ser. No. 12/842,558, filed on Jul. 23, 2010, and provisional patent application U.S. Ser. No. 61/453,329, filed on Mar. 16, 2011, both of which are hereby incorporated by reference in their entireties.
TECHNICAL FIELD OF THE INVENTION
[0002] The present invention relates to a process for improving oil recovery in carbonate reservoirs. More specifically, embodiments of the present invention utilize sequential salinity reduction waterflooding in conjunction with dilute surfactant flooding.
BACKGROUND OF THE INVENTION
[0003] The petroleum industry has recognized for decades that only a portion of original oil in place (OOIP) in oil-bearing reservoirs is produced by natural mechanisms. It is also well-known that conventional methods of supplementing natural recovery are relatively inefficient. Typically, a reservoir may retain half of its original oil in place even after the application of currently available methods of secondary recovery. Accordingly, there is a continuing need in improving recovery methods, which will substantially increase the ultimate petroleum recovery of subterranean reservoirs.
Waterflooding
[0004] Waterflooding is a method of secondary recovery in which water is injected into a reservoir formation to displace mobile oil within the reservoir formation. The water from injection wells physically sweeps the displaced oil to adjacent production wells, so that the oil can be collected from the production wells. Generally, the water used in a waterflooding process is taken from nearby water sources, which is usually either seawater or produced water.
[0005] It is known that a reduction in salinity values of the injected water can increase oil production for sandstone reservoirs. However, the low salinity floods have only been shown to work if the reservoir contains clays and with water having salinity values that are less than 5,000 ppm.
[0006] Carbonate reservoirs do not contain such clays. As such, the low salinity water flooding teachings known heretofore specifically teach away from the successful use of low salinity water for carbonate reservoirs. See A. Lager et al., “ Low Salinity Oil Recovery—An Experimental Investigation ,” paper presented at the Society of Core Analysts, September 2006 (“Finally it explains why LoSal™ does not seem to work on carbonate reservoirs.”). See also A. R. Doust et al., “ Smart Water as Wettability Modifier in Carbonate and Sandstone ,” paper presented at 15 th European Symposium on Improved Oil Recovery, April 2009 (“The wettability modification in carbonates can take place at high salinities, i.e. SW salinity. If SW is diluted by distilled water to a low saline fluid, ˜2000 ppm, the oil recovery will decrease due to a decrease in the active ions.”).
Surfactant Flooding
[0007] It is known to add aqueous surfactants to injection water in order to lower the oil-water interfacial tension and/or alter the wettability characteristics of reservoir rocks. However, the previously known methods involved the injection of an aqueous surfactant solution in high surfactant concentration known as micellar or microemulsion flooding. The objective was to displace residual oil and water miscible by a mutually soluble solvent using an injected slug of micellar solution (containing a mixture of a surfactant, a co-surfactant, brine and oil), so that an oil bank was formed in the subterranean formation before its production started. This art is commonly used in tertiary recovery mode with a high surfactant concentration of 1 wt % to 10 wt % (10,000 ppm to 100,000 ppm).
[0008] The high costs associated with classical surfactant flooding techniques described above have inhibited the implementation of this technique, particularly in harsh environments. Non-limiting examples of harsh environments include reservoirs with high reservoir temperatures, high brine salinities, and fractured carbonate. As a consequence, research into surfactant flooding has been focused on using dilute surfactant solutions in an attempt to reduce costs.
[0009] The use of high salinity water, particularly at elevated temperatures, presents a major challenge for dilute surfactant flooding. For example, high salinity causes low efficiency of surfactants in several ways, including high interfacial tension between the dilute surfactant solution and crude oil, high adsorption onto the reservoir rock surface, and precipitation of white, cloudy, solid materials.
[0010] Therefore, it would be desirable to have an improved process for waterflooding carbonate reservoirs that was simple and efficient. Preferably, it would be desirable to have a process that did not require the use of complicated chemicals or gases such as carbon dioxide, polymers, or the like. Preferably, it would be desirable to have a process that did not use a substantial amount of surfactant, thereby allowing the process to be more economical. Additionally, it would be beneficial if the process for an improved waterflooding could be implemented with existing infrastructure.
SUMMARY OF THE INVENTION
[0011] The present invention is directed to a process that satisfies at least one of these needs. In one embodiment, the process for recovering hydrocarbons in carbonate reservoirs includes the steps of introducing a first saline solution into the carbonate reservoir, recovering an amount of hydrocarbon from the carbonate reservoir, introducing a second saline solution into the carbonate reservoir, introducing a third saline solution into the carbonate reservoir, and recovering a second amount of hydrocarbon from the carbonate reservoir. The first saline solution has a first salt concentration, the second saline solution has a second salt concentration that is lower than the first salt concentration, and the third saline solution has a third salt concentration that is lower than the first salt concentration. The first saline solution includes water, salt, and an absence of a surfactant. The second saline solution includes water, salt, and a surfactant. The third saline solution includes water and salt. In one embodiment, the third saline solution is substantially free of a surfactant. In another embodiment, the third saline solution consists essential of water and salt.
[0012] In one embodiment, the first saline solution, the second saline solution, and the third saline solution further include an absence of a polymer. In another embodiment, the second saline solution has a surfactant concentration in an amount at about a critical micelle concentration of the second saline solution, such that a microemulsion is not formed when the second saline solution is injected into the carbonate reservoir. Those of ordinary skill in the art will recognize that the critical micelle concentration can be determined by a surface tension measurement known in the art. In one embodiment, the second saline solution has a surfactant concentration in an amount within the range of about 300 ppm and about 1000 ppm by weight. In another embodiment, the second saline solution has a surfactant concentration of about 500 ppm by weight.
[0013] In one embodiment, the ratio of the second salt concentration to the first salt concentration is in a range from about 1:10 to 9:10, more preferably from about 1:10 to 1:2, and more preferably, about 1:2.
[0014] In an embodiment, the first salt concentration is within a range of 35,000 to 70,000 ppm by weight. In another embodiment, the second salt concentration is within a range of 3,500 to 60,000 ppm by weight. In another embodiment, the second salt concentration is within a range of 17,500 to 52,500 ppm by weight. In another embodiment, the second salt concentration is within a range of 17,500 to 35,000 ppm by weight. In another embodiment, the process is conducted at a reservoir temperature of not less than about 70° C. and not more than about 120° C., more preferably about 100° C.
[0015] In one embodiment, the first saline solution can include at least two ions selected from the group consisting of sulfate ions, calcium ions, magnesium ions, and combinations thereof. In another embodiment, the first saline solution can include sulfate ions, calcium ions, and magnesium ions.
[0016] In one embodiment, the surfactant of the second saline solution is an amphoteric surfactant. Amphoteric surfactants are a type of surfactants that have two function groups, one anionic and one cationic. Non-limiting examples of amphoteric surfactants include sulfonates, carboxylates, and phosphates. In one embodiment, the surfactant can include sulfonate betaine having a C 12 to C 24 hydrophobic tail or carboxyl betaine having a C 12 to C 24 hydrophobic tail. In another embodiment, the surfactant may also include a co-surfactant, for example, ethylene glycol mono butyl ether
[0017] In one embodiment, the ratio of the third salt concentration to the first salt concentration can be in a range from about 1:10 to 9:10. In another embodiment, the third salt concentration is not greater than the second salt concentration. In another embodiment, the third salt concentration is within a range of 1,750 to 7,000 ppm by weight. In another embodiment, the third salt concentration is within a range of 3,500 to 7,000 ppm by weight.
[0018] In one embodiment, the recovering step is continued until the second amount of hydrocarbon recovered provides at least a 9% improvement in incremental oil recovery. In another embodiment, the recovering step is continued until the second amount of hydrocarbon recovered provides at least a 15% improvement in incremental oil recovery.
[0019] In one embodiment, the carbonate reservoir is substantially free of clay; more preferably, the carbonate reservoir has an absence of clay. In one embodiment, the carbonate reservoir has an absence of sandstone rock.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] These and other features, aspects, and advantages of the present invention will become better understood with regard to the following description, claims, and accompanying drawings. It is to be noted, however, that the drawings illustrate only several embodiments of the invention and are therefore not to be considered limiting of the invention's scope as it can admit to other equally effective embodiments.
[0021] FIG. 1 shows data collected from an experiment in accordance with an embodiment of the present invention.
[0022] FIG. 2 shows data collected from an experiment in accordance with the prior art.
DETAILED DESCRIPTION
[0023] While the invention will be described in connection with several embodiments, it will be understood that it is not intended to limit the invention to those embodiments. On the contrary, it is intended to cover all the alternatives, modifications and equivalence as may be included within the spirit and scope of the invention defined by the appended claims.
[0024] In one embodiment, the process for improving tertiary hydrocarbon recovery in carbonate reservoirs includes the steps of introducing a first saline solution into the carbonate reservoir, recovering an amount of hydrocarbon from the carbonate reservoir, introducing a second saline solution into the carbonate reservoir, introducing a third saline solution into the carbonate reservoir, and recovering a second amount of hydrocarbon from the carbonate reservoir. The first saline solution has a first salt concentration, and the second saline solution has a second salt concentration that is lower than the first salt concentration. In one embodiment, the first saline solution has an ion composition that includes at least two ions selected from the group consisting of sulfate, calcium, magnesium, and combinations thereof. The second saline solution includes water, salt, and a surfactant. The third saline solution preferably excludes a surfactant, and has a salt concentration that is lower than the first salt concentration.
[0025] The present invention is illustrated by the following examples, which are presented for illustrative purposes, only, and are not intended as limiting the scope of the invention which is defined by the appended claims:
Example 1
[0026] A coreflooding study was conducted to demonstrate an embodiment of the invention. The experimental parameters and procedures were designed to reflect the initial conditions commonly found in carbonate reservoirs, as well as the current field injection practices.
[0027] The core material was selected from a carbonate reservoir in Saudi Arabia. Core plugs (1-inch in diameter, and 1.5-inch in length) were cut from whole cores. One composite core was selected for the coreflood experiments. Table I shows the petrophysical properties of the selected cores. The average porosity and liquid permeability are 25% and 2.4 Darcy, respectively.
[0000]
TABLE I
Basic Petrophysical Properties for Core Plugs
Irreducible
Pore Volume
Liquid
Water
by Routine
Sample
Length
Dia.
Permeabil-
Saturation
Porosity
Core analy-
#
(cm)
(cm)
ity (D)
(%)
(%)
sis (cc)
124
3.44
3.80
2.4
20.34
23.6
5.15
148
4.25
3.81
2.35
19.68
26.7
5.24
Total
7.69
3.80
2.38
20.01
25.15
10.39
[0028] The most predominant mineral in the selected carbonate cores is calcite (more than 90 wt %). Other minerals are dolomite (trace up to 9 wt %), and a minor amount (<1 wt %) of quartz.
[0029] Two brines were primarily used in this study, including field connate water, to establish initial or irreducible water saturation (Swi) for composite cores, and to use as injected waters for different salinity slugs of seawater to displace oil out of the cores. All brines were prepared from distilled water and reagent grade chemicals, based on geochemical analysis of field water samples. Table II depicts the geochemical analysis and the corresponding chemicals concentration for each type of brine. For the experiments described below, the seawater had a salinity of about 57,700 ppm by weight. Initial connate water had a much higher salinity of 214,000 ppm by weight.
[0000]
TABLE II
Geochemical Analysis and Salt Concentrations
for Major Sources of Water
Field Connate
Ions
Water
seawater
Sodium
59,491
18,300
Calcium
19,040
650
Magnesium
2,439
2,110
Sulfate
350
4,290
Chloride
132,060
32,200
Carbonate
0
0
Bicarbonate
354
120
TDS
213,734
57,670
The salt recipes for major sources of water
UTMN Connate
Qurayyah
Salts
Water
seawater
NaCl, g/L
150.446
41.041
CaCl 2 •2H 2 O, g/L
69.841
2.384
MgCl 2 •6H 2 O, g/L
20.396
17.645
Na 2 SO 4 , g/L
0.518
6.343
NaHCO 3 , g/L
0.487
0.165
[0030] Twice diluted seawater was also prepared by mixing an equal volume of deionized water with the seawater. The surfactant used for this experiment was SS-887, provided by Oil Chem. This particular surfactant is an amphoteric surfactant having ethylene glycol mono butyl ether as a co-surfactant. Surfactant was added to the twice diluted seawater such that the resulting mixture contained approximately 300 ppm to 1000 ppm by weight surfactant. The density of the mixture was 1.001 g/ml at 185° F. The viscosity was measured to be 0.338 cP at 185° F. The interfacial tension (IFT) between oil and mixture was 0.0834 dynes/cm and 0.0301 dynes/cm at concentrations 500 ppm and 1000 ppm, respectively.
[0031] Reservoir oil samples were collected from the same carbonate reservoirs. Crude oil filtration was conducted to remove solids and contaminants to reduce any experimental difficulties during coreflood experiments. In order to increase the accuracy of the experiment, live oil (e.g., oil which was recombined from an oil/gas separator) was used such that the experimental conditions more closely resembled reservoir conditions. As used herein, live oil is oil containing dissolved gas in solution that can be released from solution at surface conditions. Oil in reservoirs usually contains dissolved gas, and once it reaches the surface, gas tends to evolve out due to the lower pressures at the surface as compared to within the reservoir. As used herein, dead oil is oil at sufficiently low pressure that it contains no dissolved gas. Total acid number and other oil properties are listed in Table III.
[0000]
TABLE III
Reservoir Oil Properties for Collected Oil Samples
Component
Amount
Saturates, %
40.57
Aromatics, %
51.75
Resins, %
5.55
Asphaltenes, %
2.03
Total Acid Number, mg KOH/g oil
0.05
Saturation pressure, psia @ 212° F.
1804
Gas oil ratio, SCF/STB
493
Stock tank oil gravity °API @ 60° F.
30.0
Dead oil density at room temperature, lb/ft 3
54.50
Dead oil viscosity at room temperature, cp
14.59
Dead oil density at 185° F., lb/ft3
51.81
Dead oil viscosity at 185° F., cp
2.807
[0032] The pore volume of cores, original oil in place, and connate water saturation of selected composite core plugs were determined using a centrifuge apparatus. The procedure for preparation of each core was as follows:
1. Measure dry weight. 2. Saturate core plug under vacuum for 5-7 days with field connate water to achieve ionic equilibrium with the core samples. 3. Measure wet weight. 4. Determine pore volume using weight difference and the density of field connate water at room temperature. 5. Centrifuge each core plug at 5000 rpm for 12 hrs to drain the water in the pores and establish the initial water saturation. 6. Measure weight of centrifuged core sample. 7. Determine the original oil in place (OOIP) and initial water saturation by weight difference—prior and post centrifuge—and the density of field connate water.
[0040] Table 4 shows the pore volume calculation results using the centrifuge method with the initial water saturation for core plugs used in coreflood experiment. The total pore volume for the composite was 10.39 cc, and original oil in place (OOIP) was 8.31 cc. The average initial water saturation for the composite was 20%. The position of each core plug in the composite sample is ordered by a harmonic arrangement. The plugs are organized in Table IV as the first plug from the inlet to the last plug from outlet of the coreholder.
[0000]
TABLE IV
Pore Volume Determination and Swi %
Results for Coreflooding Experiment
Pore
Post
Sample
Dry
Wet
Liquid
Volume,
Wet
Wet wt
#
wt, g
wt, g
wt, g
cc
wt, g
diff., g
S wi
124
80.16
86.07
5.91
5.15
81.54
4.53
0.2034
148
83.41
89.43
6.02
5.24
84.77
4.66
0.1968
10.39
0.2001
[0041] A coreflooding apparatus was then used to mimic reservoir conditions during a waterflood experiment. The experimental procedure followed is described below:
[0042] Each plug used in a composite was saturated with connate water by introducing degassed brine into an evacuated vessel containing the dry plugs. After obtaining saturated weights, the plugs were centrifuged to connate water saturation, Swi, followed by a dead oil flush. Core plugs were aged in crude oil (dead oil) for 4 weeks. The composite now replicates the carbonate reservoir in terms of fluid saturations, reservoir temperature and pressure, as well as wettability status.
[0043] During the water flooding, the amount of oil produced, pressure drop across the composite, and injection rate were all monitored. Water was injected at constant rate of 1 cc/min until no more oil was produced. The injection rate was increased up to 8 pore volumes of composite cores to ensure that all mobile oil was produced. Another practice implemented to make sure that mobile oil was produced is that the injection rate is first raised to 2 cc/min and then to 4 cc/min, and the injection rate is dropped back to 1 cc/min, at the end of this phase. This practice takes another 2 pore volumes.
[0044] The composite cores were then injected with one pore volume of 1000 ppm surfactant solution in a twice diluted seawater (i.e., salinity of 28,800 ppm). The objective of this slug is to determine the impact of the surfactant solution on oil recovery process. The coreflood was resumed by injection of twice diluted seawater as a succeeding waterflood. This third injection did not contain any appreciable amounts of surfactants. The effluent brine was collected in aliquot and brine ion analyses were performed to see the changes of ion concentrations in the effluent.
[0045] At the end of coreflood experiment, the composite was allowed to equilibrate at ambient conditions and the individual core plug sample removed. After the experiment, the composite core was put in the Dean-Stark extraction device to verify the oil recovery. The results from this experiment are shown in FIG. 1 .
[0046] FIG. 1 displays an oil recovery curve expressed in percentage of oil recovered. The oil recovery by seawater flooding is about 69% in terms of original oil in place (OOIP); this targets mobile oil in the cores, and represents the secondary oil recovery. The additional oil recovery (i.e., that over secondary recovery) was about 15.5% of OOIP with twice diluted seawater.
[0047] FIG. 2 displays an oil recovery curve expressed in percentage of oil recovered for a similar setup but without the surfactant injection. The oil recovery by seawater flooding is about 67% in terms of OOIP. Therefore, the additional oil recovery (i.e., that over secondary recovery) was about 7% of OOIP with twice diluted seawater. As such, embodiments of the present invention that include a surfactant injection can help to increase the recovery of the OOIP over methods known heretofore.
[0048] While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications, and variations as fall within the spirit and broad scope of the appended claims. The present invention may suitably comprise, consist or consist essentially of the elements disclosed and may be practiced in the absence of an element not disclosed.
|
A method for increasing oil production in a carbonate reservoir by incorporating a diluted surfactant injection in conjunction with conducting a step-wise reduction of salinity of the injected salt water that is injected into the carbonate reservoir. The method provides for increased oil production as compared to conventional waterflooding techniques.
| 2
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CROSS REFERENCE TO RELATED APPLICATION
This is a continuation of application Ser. No. 312,880, filed Dec. 7, 1972, now abandoned, which in turn is a continuation of our prior copending application Ser. No. 851,081, filed Aug. 18, 1969, and now abandoned.
SUMMARY OF THE INVENTION
The present invention involves new industrial compounds or products complying with the general formula:
[C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SO.sub.2 --Z].sub.d M
wherein: C n F 2n+1 represents a straight or ramified branched perfluorinated chain; n represents a number between 1 and 20, b is a whole number between 2 and 20, preferably equal to 2 or 4, Z represents a chlorine, bromine or an oxygen atom (when Z is a chlorine or a bromine atom, M is nothing and d is equal to 1), when Z is an oxygen atom: M is a hydrogen atom and in which case, d is equal to 1 or M is a metal of the Groups I A , II A , I B , II B , VIII of the periodic table, the ammonium radical, the aluminum or the lead radical and in which case d represents the valence of this metal. The novel compounds are prepared as illustrated by the following representative reactions:
C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SCN+3Cl.sub.2 +2H2O→C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SO.sub.2 Cl+CNCl+4HCl (1)
CnF.sub.2n+1 --CH.sub.2 --.sub.b Y+Na.sub.2 SO.sub.3 →C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SO.sub.3 Na+NaY (2)
wherein Y=Br or I
C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SO.sub.2 Cl+2NaOH→C.sub.n F.sub.2n+1 --CH.sub.2 --SO.sub.3 Na+NaCl+H.sub.2 O (3)
wherein n and b are as represented above.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The preparation of polyfluorinated sulphocyanides C n F 2n+1 --CH 2 -- b SCN used in reaction (1) has been described in the French patent application PV.138.101 of Jan. 31, 1968, in the applicant's name. The oxidation of a polyfluorinated sulphocyanide having the formula C n F 2n+1 --CH 2 -- b SCN by the chlorine or the bromine is easily carried out when the sulphocyanide is dissolved in a suitable solvent as a reaction medium. It is preferred to use as a solvent a water-acetic acid mixture containing between 5 and 25% of the water by volume.
A reaction temperature between about 15° and 120° C. can generally be used but it is preferred to use a reaction temperature between 15° and 75°.
During the reaction (1) a by-product is obtained, namely the polyfluoroalkane halide, whose formula is C n F 2n+1 --CH 2 -- b X wherein X is the chlorine or the bromine. The polyfluorinated sulphocyanide can be regenerated by reaction with an alkaline sulphocyanide according to the reaction:
C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b X+SCN.sup.- →C.sub.n F.sub.2n+1 --CH.sub.2).sub.b SCN+X.sup.- ( 4)
The following table indicates the boiling and the melting points of some products forming the subject of the invention. Owing to the reactivity of these products, the indicated values may show some inaccuracy.
______________________________________ PE °C. PF °C.______________________________________C.sub.2 F.sub.5 --C.sub.2 H.sub.4 --SO.sub.2 Cl 97°/100 mmC.sub.4 F.sub.9 --C.sub.2 H.sub.4 --SO.sub.2 Cl 94°/20 mmC.sub.6 F.sub.13 --C.sub.2 H.sub.4 --SO.sub.2 Cl 118-120°/20 mmC.sub.8 F.sub.17 --C.sub.2 H.sub.4 --SO.sub.2 Cl 141°/20 mm 62.3C.sub.10 F.sub.21 --C.sub.2 H.sub.4 --SO.sub.2 Cl -- 97-8______________________________________
The action of a mineral sulphite on a polyfluoroalkane halide C n F 2n+1 --CH 2 -- b Y (Y being the iodine or the bromine) as whown in equation (2) above is carried out under the classicial conditions of the Strecker's reaction. The reaction can be carried out in the presence of many solvents such as water, an alcohol (preferably ethanol), a ketone (preferably acetone), or an aprotic solvent (preferably dimethylformamide or dimethylsulphoxide). A mixture of solvents falling in the above classes can be used. It is preferred however, to use a mixture of water and ethanol, volume per volume.
The applicants have also discovered that the addition of a small quantity of copper turnings aids in the nucleophile attack of the polyfluoroalkane halide C n F 2n+1 --CH 2 -- b Y by the sulphite ion.
The reaction can be carried out at a temperature between about 20° and 250° C., preferably between 50° and 150°. If the reaction temperature is above the boiling point of the reaction mixture or one of its constituents, it can be carried out in an autoclave (See Example 9).
The polyfluorinated sulphonates [C n F 2n+1 --CH 2 -- b SO 3 ]d M, as set forth in equation (3) above, may also be obtained by neutralizing the halides of polyfluorinated sulphonic acids C n F 2n+1 --CH 2 -- b SO 2 Z with the aid of a base of the formula M (OH) d where M and d have the meanings designated above. This neutralizing is carried out under the usual conditions for this kind of reaction. The reaction can be carried out in the presence of many solvents, such as water, an ether (such as isopropyl ether), a ketone (such as acetone) or their mixtures. It is preferred, however, to operate in the presence of water. The reaction temperature can be between about 10° and 100° C. but prefereably at about 20° C. An increase in the reaction temperature, although it is not necessary, may accelerate the reaction owing to the solubility.
The new compounds of this invention are useful in the textile industry, and in the leather and paper industries. They can also be employed as corrosion inhibitory agents, surface active agents and levelling agents. The compounds can thus be incorporated in waxes, greases, varnishes and paints to improve the spreading out and levelling of such viscous products.
The following examples illustrate the invention. In all the examples, when a fraction contains several constituents the mentioned percentages are molar percentages of the various compounds and the yields are referred to the starting fluorinated material.
EXAMPLE 1
Chlorine was bubbled to 20°, for 3 h, at the rate of 4 l/h, through a mixture of C 2 F 5 --C 2 H 4 --SCN (20.5 g; 0.1 mole), ice acetic acid (100 cm3) and water (12 cm3 at 20° C. for 3 hours at the rate of 4 l/hour. After 1 hour and 45 minutes, the temperature rose to 61° C. in 15 minutes. It remained at this value for 15 minutes and then it gradually went down to the ambient temperature. The chlorine output was then stopped and the apparatus surged with a nitrogen flow for 30 minutes. A solid (4.1 g) was then filtered from the reaction mixture the main constituent or which was ammonium chloride. The filtrate was distilled and 4 fractions and one residue was obtained as follows:
a-Fraction 54°-60°/100 mm, 5.81 g was composed of water and acetic acid
b-Fraction 62°-5°/100 mm. Water (100 cm3) was added to this fraction, and a dense phase was decanted (7.6 g) composed of water (2.4%), acetic acid (11.6%) and C 2 F 5 --C 2 H 4 --SO 2 Cl (85.8%; 29.6 mmole)
c-Fraction 62°-92°/100 mm; 4.8 g was composed of C 2 F 5 --C 2 H 4 --Cl (1%), acetic acid (70%) and C 2 F 5 --C 2 H 4 --SO 2 Cl (29%; 12 mmole)
d-Fraction 92°-7°/100 mm; 6.5 g was composed of C 2 F 5 --C 2 H 4 --Cl (2.8%), C 2 F 5 --C 2 H 4 --SO 2 Cl (92.4%; 24.7 mmole) and three unidentified compounds (4.8%)
e-Solid residue, 3.2 g unidentified solid. C 2 F 5 --C 2 H 4 --SO 2 Cl was obtained with a conversion rate of 66.5%.
EXAMPLE 2
Chlorine, at the rate of 4 l/hour, was bubbled at 50° C. for 3 hours and 30 minutes through a mixture of C 4 F 9 --C 2 H 4 --SCN (30.5 g; 0.1 mole), icy acetic acid (100 cm3) and water (12 cm3). After 30 minutes, the temperature rose to 75° C. and remained at this value for 30 minutes before gradually going down to the ambient temperature. After stopping the chlorine output, the apparatus was purged with a nitrogen flow for 30 minutes. A solid (3.9 g) was then filtered from the mixture, the main constituent of which was ammonium chloride. The filtrate was distilled two fractions and one residue were obtained:
a-Fraction 50°-64°/100 mm, constituted of water and acetic acid
b-Fraction 90°-95°/20 mm; 27.4 g composed of C 4 F 9 --C 2 H 4 --Cl (3.4%), C 4 F 9 --C 2 H 4 --SCN (12.3%/10 mmole) and C 4 F 9 --C 2 H 4 --SO 2 Cl (84.3%; 23.6 mmole)
c-Solid residue 4.6 g unidentified solid C 4 F 9 --C 2 H 4 --SO 2 Cl was obtained with a conversion rate of 65% and a yield of 75.5%.
EXAMPLE 3
Chlorine, at the rate of 5 l/hour, was bubbled for 2 hours through a mixture of C 6 F 13 --C 2 H 4 --SCN (40.5 g; 0.1 mole), icy acetic acid (100 cm3) and water (12 cm3). The reaction vessel was maintained at 63° C. The introduction of the chlorine caused a rise in the temperature to 72° C. after 30 minutes. This temperature remained stable for 30 minutes, then gradually went down to 63° C. The chlorine output was stopped and the apparatus purged with a nitrogen flow for 30 minutes. A mineral solid (4.9 g) was removed from the mixture by filtering, the main component was ammonium chloride. The filtrate was distilled and 4 fractions and one residue were obtained as follows:
a-52°-60°/100 mm; composed of water and acetic acid
b-62°-6°/100 mm; 61 g. 50 cm3 of water was added to this fraction, and a dense phase (1.5 g) decanted composed of C 6 F 13 --C 2 H 4 --SO 2 Cl (68%; 2.4 mmole) and C 6 F 13 --C 2 H 4 --Cl (32%)
c-38°-105°/20 mm; 9.2 g; C 6 F 13 --C 2 H 4 --Cl (51% C 6 F 13 --C 2 H 4 --SO 2 Cl (7% 12.6 mmole)
Monochloracetic acid (9.2%), acetic acid (31%)
d-108°-115°/20 mm; 33.4 g; C 6 F 13 --C 2 H 4 --SO 2 Cl (85.4%; 65 mmole), C 6 F 13 --C 2 H 4 --Cl (14.6%; 11 mmole)
e-Residue 1.5 g unidentified. C 6 F 13 --C 2 H 4 --SO 2 Cl was obtained with a conversion rate of 70% and a yield of 78.5%.
EXAMPLE 4
Chlorine, at the rate of 4 l/hour, was bubbled for 4 hours through a mixture of C 8 F 17 --C 2 H 4 --SCN (50.5 g; 0.1 mole), icy acetic acid (100 cm3) and water (12 cm3). The reaction vessel was maintained at 50° C. 15 minutes after introducing chlorine, the temperature rose to 62° C. This temperature remained stable for 1 hour, and gradually went down to 50° C. The chlorine output was then stopped and the apparatus purged with a nitrogen flow for 30 minutes. A solid (52.8 g) was filtered from the reaction mixture and recrystallized in 90 cm3 of carbon tetrachloride. A mineral solid (4 g) was removed by filtration in a hot state and the filtrate cooled down to 20° C., and a solid A (37.2 g) filtered therefrom The last filtrate was concentrated to 20 cm3, which resulted in the precipitation of a solid B (7.4 g) which was filtered therefrom. The solids A and B are identical and comply with the formula C 8 F 17 --C 2 H 4 --SO 2 Cl. C 8 F 17 --C 2 H 4 --SO 2 Cl was obtained with a conversion rate of 81.5%.
EXAMPLE 5
Chlorine at the rate of 4 l/hour, was bubbled at 75° C. for 2 hours through a mixture of C 10 F 21 --C 2 H 4 --SCN (30.3 g; 0.05 mole), water (6 cm3) and icy acetic acid (50 cm3). After 30 minutes, the temperature rose to 80° C., and it remained at this value for 45 minutes and then gradually went down to 75° C. After stopping the chlorine output, the apparatus was purged with a nitrogen flow for 30 minutes. A solid (34 g) was filtered from the reaction mixture and recrystallized in 200 cm3 of carbon tetrachloride The solid was collected (29.3 g) which was composed of C 10 F 21 --C 2 H 4 --SO 2 Cl (83%; 38 mmole) and of C 10 F 21 --C 2 H 4 --SCN (17% 17.8 mmole) C 10 F 21 --C 2 H 4 --SO 2 Cl was obtained with a conversion rate of 76% and a yield of 90%.
EXAMPLE 6
A mixture of C 2 F 5 --C 2 H 4 --I (27.4 g; 0.1 mole), Na 2 SO 3 (25 g; 0.2 mole), water (50 cm3), ethanol (50 cm3) and a turning of copper (1 g) was maintained at a temperature of 78° C. for 48 hours.
The reaction mixture formed was a liquid and a solid. A solid A (26 g) was obtained therefrom by filtration and washed with 25 cm3 of water. A solid B (17 g) remained. The filtrate was distilled and two fractions and one residue were obtained as follows:
a-49°/200 mm: ethanol
b-60°/200 mm: water
c-residue
This residue was washed with 10 cm3 of water and separated by filtering a solid C (6 g). The solids B and C were collected and recrystallized in a water-ethanol mixture (50 cm3 per 100 cm3). 20.1 g of C 2 F 5 --C 2 H 4 --SO 3 N a were collected which corresponds to a conversion rate of 80%.
EXAMPLE 7
It has been kept to 78° C. for 48 hours. A mixture of C 4 F 9 --C 2 H 4 --I (37.4 g; 0.1 mole), Na 2 SO 3 (25 g; 0.2 mole), water (50 cm3), ethanol (50 cm3) and a turning of copper (1 g) were maintained at 78° C. for 48 hours in a suitable vessel. The reaction mixture was composed of a liquid and a solid. The solid was filtered therefrom (34.2 g) and washed with 100 cm3 of water before being recrystallized in water (50 cm3). The recrystallization solid was polyfluorinated sulphonate C 4 F 9 --C 2 H 4 --SO 3 Na, which after drying at 120° C. weighed 17.2 g.
The filtrate was distilled and three fractions were obtained as follows:
a-Fraction 60°/400 mm. This fraction was composed of two phases, they were stirred with 50 cm3 of water and the two phases collected, by decanting, the densest phase (16.2 g) was composed of C 4 F 9 --C 2 H 4 --I (98%; 0.041 mole and ethanol (2%).
b-Fraction 65°/400 mm: ethanol
c-Fraction 80°/400 mm: water and few ethanol. C 4 F 9 -C 2 H 4 -SO 3 Na was thus recovered with a conversion rate of 49% and a yield of 83%.
EXAMPLE 8
A mixture of C 6 F 13 --C 2 H 4 --I (47.4 g; 0.1 mole), Na 2 SO 3 (25 g; 0.2 mole), water (50 cm3) and ethanol (50 cm3) was maintained at 78° C. for 48 hours in a suitable reaction vessel. The reaction mixture resulting was a liquid and a solid. The solid was filtered therefrom and washed with 100 cm3 of water, and after filtering, the solid was dried in a drying vessel at 120° C., 20 g of C 6 F 13 --C 2 H 4 --SO 3 Na were thus obtained.
The filtrate was distilled and one fraction and one residue were obtained as follows:
a-Fraction 49°/200 mm: ethanol
b-Residue. This residue contained water and a solid. The solid (0.9 g) was filtered and was the sulfonate C 6 F 13 --C 2 H 4 --SO 3 Na. The filtrate was evaporated and a solid (4.1 g) whose origin is mainly mineral was obtained.
C 6 F 13 --C 2 H 4 --SO 3 Na was thus obtained with a conversion rate of 46.5%.
EXAMPLE 9
A mixture of C 6 F 13 --C 2 H 4 --I (47.4 g: 0.1 mole), Na 2 SO 3 (25 g: 0.2 mole), water (50 cm3), ethanol (50 cm3) and a turning of copper (1 g) was maintained at 120° C. for 48 hours in an autoclave. The maximum pressure was 3 bars. After cooling down the autoclave to 20° C., the reaction mixture was composed of a liquid and a solid. The solid was filtered and weighed 53 g. The solid was washed with 100 cm3 of water and after filtering, it was recrystallized in one liter of water. The solid collected (35 g) was the polyfluorinated sulphonate C 6 F 13 -C 2 H 4 -SO 3 Na; the conversion rate amounted to 78%.
EXAMPLE 10
A mixture of C 6 F 13 --C 2 H 4 -- 2 I (25 g; 0.05 mole), Na 2 SO 3 (12.5 g; 0.1 mole), water (25 cm3), ethanol (25 cm3) and a turning of copper (0.5 g) was maintained at 85° C. for 48 hours. The reaction mixture was composed of a liquid and a solid, and the solid was filtered therefrom. The solid weighed 28 g and was washed with 50 cm3 of water and recrystallized in ethanol (300 cm3). The solid collected (19.2 g) was the polyfluorinated sulphonate C 6 F 13 --C 2 H 4 --SO 3 Na the conversion rate was 80%.
EXAMPLE 11
20 cm3 of NaOH (10N) were rapidly added to C 8 F 17 --C 2 H 4 --SO 2 Cl (10.93 g; 0.02 mole). During this addition, the temperature rose from 20° to 45° C. The mixture was then brought to and maintained at 100° C. for 4 hours. A solid was recovered therefrom by filtering. This solid was washed with water (3×20 cm3), dried and collected. This solid (10.9 g) was the polyfluorinated sulphonate C 8 F 17 --C 2 H 4 --SO 3 Na. The conversion rate amounted to 99%.
EXAMPLE 12
A mixture of C 6 F 13 --C 2 H 4 --SO 2 Cl (11.16 g; 0.025 mole), water (40 cm3) and sulphuric acid at 66° C. B (12 g) was maintained at 100 C. for 8 hours. The mixture was then extracted with ethyl ether (4×50 cm3) and the ether eliminated or removed by distillation. The resulting residual solid was dried under vacuum. The dry solid obtained (8.8 g) was the sulphonic acid C 6 F 13 --C 2 H 4 --SO 3 H melting between 73° and 79° C. The conversion rate was 82.5%.
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New products and compositions of matter complying with the general formula:
[C.sub.n F.sub.2n+1 --CH.sub.2 --.sub.b SO.sub.2 --Z].sub.d M
wherein: C n F 2n+1 represents a straight or ramified branched perfluorinated chain: n represents a whole number between 1 and 20, b is a whole number between 2 and 20, preferably equal to 2 or 4, Z represents a chlorine, bromine or an oxygen atom (when Z is a chlorine or a bromine atom, M is nothing and d is equal to 1), when Z is an oxygen atom: M is a hydrogen atom in which case, d is equal to 1, M is a metal of the Groups I A , II A , I B , II B , VIII of the periodic table, the ammonium radical, the aluminum or the lead radical, and in which case d represents the valence of this metal and methods for preparing new products as illustrated by the following representative reactions.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and device for mechanically forming a hollow vessel body and more particularly relates to an effective method and device for mechanically and automatically forming a hollow vessel even when a viscosity of a raw material thereof is considerably low, and a hollow vessel body thus formed.
2. Prior Art
Waste recycling has been considered as an important issue in order to save resources, preserve living surroundings and prevent environmental pollution. One of the most familiar and urgent issues is a reuse of waste paper such as news paper, magazine, etc.
Waste paper is typically reused as regenerated paper, while a paper regeneration process has various industrial problems caused by waste paper treatment to prepare the starting material, residues thereof, relatively high production cost, etc. It is therefore desirable to recycle waste paper as simply as possible without troublesome treatment and addition of additives.
A cost-saving recycle process of waste paper is, for example, to simply slurry paper in water, which is used to form a vessel body such as flowerpots or a block body such as brick. The thus water-slurried waste paper, however, is not useful at all as a starting material to form the above mentioned vessel body because of a poor viscosity although it might sometimes be used for production of paper brick and the like. One of important factors for producing the waste paper vessel body such as flowerpots that the vessel can be formed on a large scale at a low cost while quality thereof is not necessarily high-grade. It seems possible to use a conventional device comprising a jigger, a negative mold and a forming attachment provided with a trowel (hereinafter simply referred to as a jigger unit) for mass-production of waste paper flowerpots, etc. Such a waste paper material, however, can not be shaped into a vessel body by conventional jigger units because of an excessively low viscosity thereof.
When the waste paper material is applied to the surface of a negative mold by means of a trowel, the material is easily repelled from or hardly stuck on the mold so that no shape is formed thereon.
When a vessel body is formed by means of a conventional jigger unit an applicable material is a pottery clay which is freely and easily transformed and water content thereof has been adjusted to appropriate hardness (or softness) enough to keep a vessel shape to be formed. Thus, such a pottery clay can be formed by the conventional jiggler unit without trouble. Conversely, it might be said that the above mentioned jigger unit has been developed only for forming the pottery clay.
However, it is impossible to obtain quality similar to the pottery clay even if a water content of the waste paper material is carefully controlled when the material is prepared by simply slurrying waste paper in water. The slurried waste paper is hardly used as a starting material at a higher water content while it becomes rather dry and decreases a viscosity impracticably at a lower water content.
A slurry of waste paper is sometimes mixed with a solidifying agent or a glue to improve properties of the material, however, such a mixture is different from the environmentally desirable reuse of waste paper as it is and what is worse, the thus mixed material still shows a relatively low viscosity and keeps a rather dryish state.
Although waste paper may be chemically treated to yield a starting material which has similar properties as a pottery clay, the present invention intends to reuse waste paper as it is without adding any chemical agent.
A material of waste paper is conventionally formed by means of press molding. It is necessary to finely distribute the material on the mold surface due to poor flowability thereof, while water extracted therefrom should be released by means of, for example, a partially meshed mold. The product thus formed under such a complicated condition looks quite poor and, in addition, should be reinforced by wax finishing, etc.
According to the present invention, a method and a device for mechanically and automatically forming a vessel body even when a material has low viscosity such as waste paper of lower water content prepared by simply slurrying it in water, the thus formed product looking reasonably good and having sufficient strength, are provided.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a method for forming a vessel body in which a material is charged in a negative mold, pressed to and spread on a mold surface by means of a rotating cylindrical rotary trowel to form a vessel body.
Another object of the present invention is to provide a device for forming a vessel body which comprises an open top negative mold, a ring-like lid member of a negative mold, which inside diameter is smaller than an open top diameter of the mold, a cylindrical rotary trowel which is mechanically fixed to move against an inner surface of the mold within a predetermined range and is at least longer than height of an inner wall surface of the vessel body to be formed, and a trowel drive.
Yet another object of the present invention is to provide a vessel body formed by a method stated above in which there is used a material of extremely low viscosity such as that prepared by slurring waste paper in water.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic side view of a vessel body forming devise of the present invention.
FIG. 2 is a perspective view of a rotary trowel and a driving motor used in a vessel body forming devise of the present invention.
FIG. 3 is a perspective view of a rotary trowel and a driving motor used in another vessel body forming devise of the present invention.
FIG. 4 is a vertical center-section of a vessel body forming devise of the present invention provided with a shave stand, a negative mold and a lid.
FIG. 5 is an enlarged vertical center-section of a vessel body forming devise of the present invention provided with a shave stand, negative mold, a lid and a rotary trowel when a material is formed.
FIG. 6 is a perspective view of a flower pot formed by the present invention.
FIG. 7 is a vertical sectional view of a double-layered flower pot formed by the present invention.
FIG. 8 is a perspective view of a half of split type negative mold.
DETAILED DESCRIPTION
The negative mold may be a rotatable type and be forcibly rotated in the same rotating direction of the rotary trowel at a surface rotational speed lower than that of the rotary trowel so as to form a vessel body.
When such a negative mold of rotatable type is used, the mold per se can be rotated by means of the rotary trowel, while formation of a vessel body is conducted successfully as a result of different rotation of the mold and the trowel. It is an important feature of the present invention that rotation of the negative mold is slower than that of the rotary trowel. The negative mold may also be forcible rotated by means of a drive such as a motor.
Further, the negative mold used in the present invention may be a split type. A ring-like lid member may be integrally formed on such a negative mold of split type. The ring-like lid member may be integrally formed either on each split half as a part thereof or on one of the split halves as a whole if the ring-like lid member is not split. The split type mold may be a rotatable type.
The negative mold may be combined with a shave stand for fitting the mold and a turn table for supporting the shave stand.
There may be used a drive which rotates the negative mold in the same rotating direction as the rotary trowel at a surface rotational speed lower than that of the trowel.
The rotary trowel may have a shape of a right cylinder or cone, while thickness thereof may be partially increased or decreased.
The rotary trowel may be moved in close to the inner surface of the negative mold at a certain space to give the thickness of a vessel body to be formed.
The rotary trowel is preferably rotated at high speed of, for example, 1,000 r.p.m. Although rotational speed less than 1,000 r.p.m. is also effective, it takes a long time to conduct a smooth forming process at relatively low speed.
The negative mold may be fixed directly to a support such as a rotatable shaft in an undetachable or detachable situation. As the negative mold should be changed depending on a type or kind of vessel bodies to be formed, the mold is replaced together with the above mentioned support, shave stand and/or turntable unless otherwise the mold is fixed undetachably.
A combination of each negative mold, shave stand and turn table is necessarily fixed rotatably around the axial center while drive for the shave stand is not necessary in general because the shave stand is forcibly rotated through a forming material with the force of the rotary trowel during the forming process. When a large vessel body is formed, however, a torque of the rotary trowel is not enough to rotate the shave stand and the negative mold with a large amount of material. A drive may be used in such a case to rotate a combination of the negative mold, shave stand and turn table.
The negative mold may be made of plastics, metal and the like, rigidity thereof being preferably high.
A relative arrangement of the negative mold and the shave stand and/or the turn table may be similar to that of conventional jiggers.
A mold lid may be detachably fitted to the negative mold by conventional means such as screws. The mold lid is formed as a ring-like disc by cutting off around the central part thereof and protruded inward like a flange on the negative mold, protruded width thereof corresponding to thickness of the top surface of the vessel body. The lid is put on the mold during the forming process and taken off when the formed vessel body is taken out therefrom. In the case of a particular mold type, such as a negative mold separable into two parts for easier ejection of the product, the lid may be fixed to the mold undetachably.
The method or device of the present invention is most effectively used to form materials of extremely low viscosity, and is also usefully applicable to conventional materials such as porcelain clay as a matter of course.
The material used in the present method or device is prepared by simply slurring waste paper in water.
Further, it is quite easy for the present invention to form a multilayered vessel body by using a mixture of different materials.
Materials of extremely low viscosity which can be used to form a vessel body by the present invention include not only waste paper itself but a mixture of waste paper and one of more materials selected from powdery or particulate charcoal, solid fertilizer, enzyme containing particles and mineral such as cullet. Using the above mentioned mixture, a desirable vessel body can be formed by the present invention.
Charcoal particles, wood chips and leaf mold may be used as a material of the present vessel body independently or in the form of mixture thereof.
Further it is possible to use waste wire coil as a useful material of the present invention, which is prepared by removing thermoplastic cover such as polyvinyl chloride therefrom, finely cutting wire and coil paper to form particle and slurring with water.
A multi-layer vessel body is easily formed by the present invention by using a mixture of different materials.
A vessel body formed by the present invention includes products such as a flower pot, trash box, etc., but is not limited to a specific product.
According to the present invention, any of the above mentioned material can be used to form a uniform vessel body of high quality without skilled technique.
The present device may be built in an on-line mass production system.
The thus formed vessel body of waste paper alone or a mixture thereof exhibits excellent appearance and strength which has never been achieved by similar products.
According to the present invention, it is not necessary to add any glue or adhesive to the material nor to reinforce the product by waxing, etc.
As has been described above, the present invention provides quite a novel and excellent method and device for forming a vessel body, while there may be used some unexpected materials other than those materials as disclosed herein.
The material is kept between the rotary trowel and the inner surface of the negative mold, and pressed to and extended along the surface by means of the trowel which rotates faster than the negative mold.
Because of characteristic features of the present invention as described above, even a material of extremely low viscosity can be formed mechanically and automatically as a vessel body. It is possible to easily produce uniform vessel bodies of high quality without any skilled technique.
The vessel bodies produced by the present invention are far more excellent in appearance and shape than those of conventional products. In addition, they are strong enough to leave out any reinforcing process such as waxing.
EMBODIMENTS
Referring now to the attached drawings, the present invention will be detailed in the following.
EXAMPLE 1
FIG. 1 is a schematic side view of the vessel body forming device. FIG. 2 is a perspective view of a rotary trowel and a driving motor. FIG. 3 is a vertical sectional view of the vessel body forming device provided with a shave stand, a negative mold and a lid, FIG. 4 is an enlarged vertical sectional view of the vessel body forming device provided with a shave stand, negative mold, a lid and a rotary trowel when a material is formed, and FIG. 5 is a perspective view of a flower pot formed by the present invention. In FIG. 1, 1 , 2 and 3 designate a rotary trowel, a drive motor and a manipulating arm, respectively, and 4 designates a shave stand. 5 and 6 designate a negative mold and a ring-like lid portion, respectively. And further, 7 and 8 designate a turn table and a shaft, respectively.
The shave stand is additionally used together with the turn table in this example.
The rotary trowel 1 is a stainless steel right cylinder of 3 cm in diameter and chamfered to form a moderate and spherical tip. The rotary trowel 1 is co-axially attached to a shaft of the drive motor 2 , and turned around and stopped when the drive motor 2 is turned on and off. An on-off switch 9 of the motor 2 is fixed on a joint portion of the arm 3 so as to switch on when a supporting portion of the arm moves downward to a predetermined position, i.e., the position just before a point where the rotary trowel 1 begins to form a material on the negative mold.
The rotary trowel 1 is conventionally fixed to the arm by a pair of screws and nuts while the arm is adjusted to move within a predetermined range so that the rotary trowel 1 does not move downward over the above mentioned position in the shave stand 4 and also keeps a certain space to the inner surface of the negative mold.
The negative mold has a hollow portion on the center of the bottom where a protrusion 10 of the shave stand 4 is fitted to form a draining hole of flower pot to be prepared. The protrusion 10 of the shave stand shoots upward from the bottom surface of the mold to an extent equal to thickness of the bottom of the flower pot.
The negative mold 5 is made of plastics and not necessarily water absorbable. A gypsum negative mold used for a jigger tends to absorb too much water from the material to form a vessel body of the present invention and is not preferable from a standpoint of strength because the material is strongly pressed thereto by means of the rotary trowel.
The negative mold is detachably fitted to the shave stand 4 as a matter of course.
The ring-like lid 6 protrudes inward as a flange having width equal to top thickness of the flower pot and is fitted detachably on the negative mold by means of conventional screws.
The shave stand 4 is arranged co-axially and detachably on the turn table 7 which is rotatably fixed on a the shafts 8 . As the turn table 7 functions as a flywheel, it is preferable to turn around the table 7 by hand before it is rotated by force of the rotary trowel. It is also preferable to use a drive unit to rotate the turn table at lower surface velocity of the mold 5 than that of the rotary trowel when a large vessel body is formed.
It is convenient to use a stop means to kill rotation soon after the forming process finishes. When such a stop means is not used, the turntable may be stopped by holding a periphery thereof by hand or allowed to turn around until it stops naturally.
EXAMPLE 2
FIG. 7 shows a forming device of the present invention in which the shave stand and the turn table used in Example 1 are removed. The forming process is conducted by this device basically in a similar manner as described in Example 1. A rotary trowel may also be the same as used in Example 1.
EXAMPLE 3
Using the forming device described in Example 1, a flower pot as shown in FIG. 5 was prepared.
The negative mold 5 was fitted to the shave stand 4 followed by putting the lid 6 thereon.
A forming material 11 was prepared by finely cutting 10 kg of news paper by means of a shredder, soaking the bulk of cut paper in 30 litter, of water, stirring the paper-water mixture by means of a stirrer to completely dissolve paper in water and wringing water from the mixture to yield about 33 kg of slurried paper (water content thereof being about 70%)
The thus prepared material 11 in an amount of about 500 g was charged in the negative mold 5 and subjected to the next step by controlling the arm 3 to move the rotary trowel 1 downward into the mold 5 so that the material 11 is pressed to the mold surface. The switch 9 was turned on by the jointing portion of the arm 3 during a downward movement thereof to automatically rotate the trowel 1 in the mold 5 .
The turn table 7 was slowly turned around by hand before the forming process was started. Then, the shave stand 4 and the negative mold 5 began to rotate by force of the rotary trowel 1 together with the turn table 7 . The material 11 was extended with the aid of rotation of the trowel 1 and that of the mold 5 to finally form the flower pot 12 between the trowel 1 and the surface of the mold 5 under the lid 6 .
The thus extended material was raised from the bottom along the mold surface. The following process was continued by pressing and extending the material by means of the rotary trowel until the material reached the ring-like lid 6 as a flange, thereby the top surface of the flower pot being formed.
Overflowing of the material from the lid 6 was not observed because an amount required to form the flower pot was determined in advance and, at the same time, the process was carefully conducted to prevent such overflowing by controlling the rotary trowel. It should be noted, however, that the material in relatively larger or smaller amount in certain extent does not cause overflowing nor affect the forming process but yields a vessel body of relatively higher or lower density.
When the material 11 was pressed by the rotary trowel 1 , water was wrung therefrom but immediately absorbed in the surrounding material, which did not affect the forming process because only a part of the material was pressed just for a moment to result in a slight amount of water.
The wet flower pot thus prepared and shown in FIG. 5 was exposed under the sun for two days to completely dry and harden. The thus prepared flower pot was practically useful and was not deformed nor damaged by repeated watering.
The flower pot exhibited sufficiently high density and excellent appearance of inner and outer surfaces thereof compared with that of a conventional product made mainly of waste paper. The flower pot was so strong that no additional reinforcement such as waxing was necessary.
Each vessel body formed by the present invention may be dried naturally or by means of a conventional dryer although a drying manner is different depending on a specific material to be formed.
EXAMPLE 4
Using the same device and material of the Example 3, a thinner flower pot as an outer layer 14 was prepared. The outer layer was dried and again put in the negative mold while the material was homogeneously mixed with about 3 parts by volume of charcoal particles of at most 5 mm in diameter, which was applied to the inner surface of the dried one as an inner layer 15 to form a double-layered flower pot as shown in FIG. 6 .
A flower pot comprising a mono-layer of charcoal mixed material has a coarse outer surface where charcoal particles are exposed, which tends to come off and soil a user's hands. On the other hand, the double-layered product formed by the present invention has no such defect and keeps a useful effect of the charcoal mixture for a long time.
It is important for preparing a multi-layered vessel body to form layers in the outer-to-inner order, that is, the outermost layer is formed at first and dried, then the second one is formed and dried and such a process may be repeated. For example, the outer layer is completed and then the second layer of the charcoal mixture is formed followed by drying the double-layered product as a whole, as described above. If the second layer is formed before the first layer is not dried charcoal particles are allowed to invade into the first layer during the forming process and are finally cropped out of the outer surface, which is inconvenient similar to the mono-layer product of charcoal mixture.
EXAMPLE 5
A half of a negative mold is shown in FIG. 8, which structure is quite different from that used in the above Examples. This split type mold consists of two completely symmetrical halves thereof to be combined into one and is supported by a shave stand (not shown). Using the split type mold, a vessel body is formed similarly as described above. After the forming process is completed, the negative mold is removed from the shaving stand and split into two to take out a vessel body.
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A device, for forming a vessel body, which has an open top negative mold, a ring-like lid member for the negative mold with an inside diameter which is smaller than an open top diameter of the mold, a cylindrical rotary trowel which is mechanically fixed to move against an inner surface of the mold within a predetermined range and is at least longer in length than a height of an inner wall surface of the vessel body to be formed, and a trowel drive for rotating the rotary trowel.
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FIELD OF THE INVENTION
[0001] The present invention relates to a method for treating wastewater containing hydrogen peroxide, and particularly to a method for treating wastewater containing hydrogen peroxide with activated carbon.
BACKGROUND OF THE INVENTION
[0002] Hydrogen peroxide is an oxidant commonly used in semiconductor processes. For example, industry names of cleaning solutions for washing wafers include SPM (with a composition of H 2 SO 4 :H 2 O 2 of 1:4), HPM (with a composition of HCl:H 2 O 2 : DIW (deionized water) of 1:2:5), SC1 (with a composition of NH 4 OH: H 2 O 2 :DIW of 0.25:1:5). Wastewater discharged after receiving treatment with one of these cleaning solutions contains a high concentration of hydrogen peroxide. Furthermore, the quantity of such wastewater is rather large—about ⅓ of the total wastewater discharged in a semiconductor process. At present, most plants directly discharge this type of wastewater to a wastewater treatment plant without recovery. In recent years, however, due to an ever increasing threshold on the water recovery ratio required by law, and a constant increase in the frequency of the occurrences of water shortages, a semiconductor plant needs to recover this type of acidic wastewater containing a high concentration of oxidant in the future in order to comply with the law and meet the plant's demand for water.
[0003] In a typical water treatment process, a water recovery system commonly consisted of an activated carbon tower, together with other units, such as a membrane filtration unit, an ion exchange resin tower, etc. The main purpose for installing the activated carbon tower is to remove the suspension solids (SS) and to absorbe total organic contaminants (TOC). The main purpose for installing an ion exchange tower is to eliminate the electrical conductivity in water caused by anions and cations. A membrane filtration unit includes a unit, such as an ultrafiltration (UF) unit, a reverse osmosis (RO) unit, etc., for removing dissolved TOC, SiO 2 , F − , TDS (total dissolved solids), etc., and obtaining recycled water at a desired quality.
[0004] Therefore, though commonly used in the typical water treatment process, activated carbon can also produce a partial removal effect of hydrogen peroxide. However, removing hydrogen peroxide is not a main objective in the use of activated carbon, and activated carbon has a limited effect in removing hydrogen peroxide, and does not effectively remove hydrogen peroxide at high concentrations in water. Thus, in the typical techniques of removing hydrogen peroxide from water, the following conventional methods have been used to reduce the damage to a recovery system caused by hydrogen peroxide:
Using a redox potential measurement to control the redox potential of wastewater to less than 175 mV in order to reduce the oxidation power of an oxidant on the treatment system; Adding sodium sulfite to reduce the number of H 2 O 2 molecules, H 2 O 2 +Na 2 SO 3 →H 2 O+Na 2 SO 4 Increasing the pH value of wastewater to reduce the oxidation power of H 2 O 2 : Because H 2 O 2 is a weak acid, when the pH=11.5, 50% of H 2 O 2 will be converted into ionic (H 2 O 2 ) − that is without oxidation power, which reduces the overall oxidation power of H 2 O 2 ; Using activated carbon to adsorb H 2 O 2 ; Reducing the content of heavy metals in acidic wastewater: The presence of heavy metals promote the conversion of H 2 O 2 into hydroxyl radicals, leading to a large increase of the oxidation power and an increase of damage to the RO membrane, etc.
[0010] Research has shown that an ion exchange resin will dissolve within 24 hours when the concentration of hydrogen peroxide reaches 500 ppm or higher. More data indicates that the functions of an ion exchange resin is affected when the concentration of hydrogen peroxide in water exceeds ppm. Therefore, there is a need to remove hydrogen peroxide from wastewater before wastewater can be further recycled.
[0011] Prior art in using activated carbon for removing H 2 O 2 from water includes, for example, Taiwan Patent No. 197382 (1993), which discloses an activated carbon filter for removing hydrogen peroxide from a fluid. The activated carbon filter includes a gravel bed located on a first end thereof, an activated carbon bed located on a second end thereof, an inlet device, and an outlet device. The inlet device distributes a hydrogen peroxide-containing fluid to contact in succession the gravel bed and the activated carbon bed; subsequently, the fluid flows out of the filter through the outlet device. Japan Patent Laid-Open No. 7-171561 discloses a wastewater treatment method for removing hydrogen peroxide by using a packed tower loaded with a granular activated carbon. Two serially connected front and rear section packed towers loaded with a granular activated carbon are used. The above-mentioned two patents are both related to the hardware design of a packed tower loaded with activated carbon, and do not mention the use of controlling the pH value of wastewater to increase the efficiency and operational lifespan of the activated carbon.
SUMMARY OF THE INVENTION
[0012] A major objective of the present invention is to provide a method and a system for treating wastewater containing hydrogen peroxide by using activated carbon.
[0013] Another objective of the present invention is to provide a method and a system for treating acidic wastewater containing hydrogen peroxide by using activated carbon.
[0014] In order to accomplish the aforesaid objectives a method for treating wastewater containing hydrogen peroxide provided according to the invention of the present application comprises the following steps: (a) controlling the wastewater containing hydrogen peroxide to a H value of 4 or higher; and (b) contacting the wastewater having a pH value of 4 or higher from step (a) with an activated carbon bed to reduce the content of hydrogen peroxide in the wastewater.
[0015] Preferably, the control of the pH value in step (a) enables the activated carbon bed in step (b) to contact wastewater with a pH value of 4 to 7.
[0016] Preferably, the control of the pH value in step (a) comprises introducing the wastewater containing hydrogen peroxide into a pH adjustment unit, measuring the pH value of the wastewater in the pH adjustment unit, and adding an alkali or an acid into the wastewater in the pH adjustment unit according to the variation of the pH value with time.
[0017] Preferably, the method of the present invention further comprises using a membrane to filter wastewater having a reduced hydrogen peroxide content from the activated carbon bed in step (b) in order to filter out solid particles therein. More preferably, the method of the present invention further comprises contacting the filtered wastewater with an ion exchange resin in order to remove charged ions therein.
[0018] Preferably, the method of the present invention further comprises using a reverse osmosis membrane to further purify the filtered wastewater.
[0019] Preferably, the wastewater containing hydrogen peroxide has a pH value less than 4, and the pH value control in step (a) comprises adding an alkali into the wastewater containing hydrogen peroxide.
[0020] The present invention also dislcoses a system for treating wastewater containing hydrogen peroxide, which comprises:
[0021] a pH adjustment unit for controlling the pH value of a wastewater containing hydrogen peroxide to a value of 4 or higher; and
[0022] an activated carbon bed for receiving a discharged wastewater with a pH value of 4 or higher from the pH adjustment unit in order to reduce the content of hydrogen peroxide in the wastewater.
[0023] Preferably, the pH adjustment unit includes a pH adjustment tank and a chemical addition device control unit, wherein the pH adjustment tank is used to mix the wastewater containing hydrogen peroxide with an alkali or acid, and the chemical addition device control unit is used to measure the pH value of the wastewater in the pH adjustment unit and add an alkali or an acid into the wastewater in the pH adjustment unit according to the variation of the pH value with time.
[0024] Preferably, the treatment system of the present invention further comprises a membrane filtration unit, which receives the wastewater having a reduced content of hydrogen peroxide from the activated carbon bed to filter out solid particles therein. More preferably, the treatment system of the present invention further comprises an ion exchange resin adsorption unit, which receives the filtered water from the membrane filtration unit to remove charged ions therein; or further comprises a reverse osmosis unit, which receives the filtered water from the membrane filtration unit to obtain purified water.
[0025] The present invention controls the pH value of wastewater to a suitable range for inducing activated carbon to impair the catalytic function of hydrogen peroxide, thereby increasing the treatment efficiency of activated carbon in removing hydrogen peroxide in water. Thus, the removal ratio of hydrogen peroxide by activated carbon is increased, and the activated carbon has a longer operational lifespan in environments having high concentrations of hydrogen peroxide (>400 ppm). In comparison with a method without using activated carbon according the present invention, a method according to the present invention can effectively increase the operational lifespan of activated carbon by more than 10 fold.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] FIG. 1 is a block diagram of a method for treating wastewater containing hydrogen peroxide according to a preferred embodiment of the present invention.
[0027] FIG. 2 is a graph of experimental results of using an activated carbon column in treating wastewater with pH values of 2, 4, 8, and 10.
[0028] FIG. 3 is a block diagram of a system for treating wastewater containing hydrogen peroxide according to an embodiment of the present invention.
[0029] FIG. 4 is a graph of experimental results of wastewater containing hydrogen peroxide with pH values of 2 and 6 continuously treated by the system of FIG. 3 .
DETAILED DESCRIPTION OF THE INVENTION
[0030] The present invention discloses a method for increasing the power of activated carbon in removing hydrogen peroxide from water. Thus, a high concentration of hydrogen peroxide can be removed from acidic wastewater according to a technique of the present invention without damaging downstream membranes, resin units, etc., for the convenience of recovery of the wastewater and conservation of water resources. The technical means in achieving the above objectives mainly adopts a control of the pH value of the wastewater prior to entering an activated carbon treatment unit for controlling the pH value of the wastewater to a desired range (pH≧4) in order to induce the activated carbon to produce a catalytic function in breaking up hydrogen peroxide, thereby prolonging the operational lifespan of the activated carbon.
[0031] A method for treating wastewater containing hydrogen peroxide according to a preferred embodiment of the present invention is explained in the following with reference to FIG. 1 .
[0032] Acidic wastewater 20 containing a high concentration of hydrogen peroxide is adjusted to a pH value greater than or equal to 4 by the addition of an alkali solution from a pH adjustment unit 21 prior to entering an activated carbon bed (tower) 23 .
[0033] The activated carbon in the activated carbon bed (tower) 23 is induced by the adjusted pH value of the wastewater to generate a catalytic function in breaking up hydrogen peroxide. Experimental results indicate that more than 99% of hydrogen peroxide can be removed from wastewater that is adjusted to a pH value larger than 4 and that contains 348 ppm of hydrogen peroxide (as shown in Table 1). Thus, a high concentration of hydrogen peroxide passing through the activated carbon bed (tower) 23 and oxidizing a subsequent treatment unit (membrane 24 , ion exchange resin 25 , or reverse osmosis membrane 26 ) is avoided.
[0034] After the above-mentioned step of removing high concentrations of hydrogen peroxide, the acidic wastewater enters a membrane filtration unit 24 for the removal of fine particles in the water or fine carbon particles caused by the decomposition of hydrogen peroxide in order to protect a subsequent treatment unit. The membrane filtration unit 24 can be a micro filter (MF) or an ultra filter (UF) membrane.
[0035] A large quantity of ions in the acidic wastewater can be removed by an ion exchange resin 25 or a reverse osmosis membrane (RO) 26 or a combination of the two to increase the removal effect of soluble ions or organic contaminants. After undergoing the above-mentioned treatment steps, water can be used as reprocessed water 27 and recycled.
[0036] As shown in the process of FIG. 1 , the pH adjustment unit 21 performs a pH measurement step, an alkali solution addition step according to the pH value and the quantity of water, and a mixing step of the alkali solution and the acidic wastewater. When a plurality of parallel activated carbon beds (towers) 23 are used, the pH adjustment unit 21 further performs a step of switching the pH-adjusted acidic wastewater into different activated carbon beds (towers) 23 . The pH adjustment unit 21 can use a conventional chemical engineering process method (e.g. a PID method) to control the pH value.
[0037] A person skilled in the art can alter, modify or omit the membrane filtration unit 24 , the ion exchange resin 25 or the reverse osmosis 26 , and/or additional auxiliary wastewater treatment units in FIG. 1 to meet the requirements of different wastewater sources.
EXAMPLE
[0038] This example used acidic wastewater from a semiconductor plant to verify the effectiveness of the invention method. The objective of the treatment was to obtain treated water in compliance with a next-generation water quality standard.
[0039] The acidic wastewater from a semiconductor plant had a pH value of about 1˜3, and a concentration of hydrogen peroxide of about 100˜400 ppm. In order to determine the treatment power of the activated carbon for designing an activated carbon tower, a batch experiment and a continuous column experiment were conducted to obtain the required parameters, and then a test was conducted on the actual plant system.
[0000] (a) Batch Experiment
[0040] According to a jar-test design, 500 mL of tap water was prepared to contain 350 ppm H 2 O 2 , and adjusted to a pH value of 2 by H 2 SO 4 to simulate the acidic wastewater of an actual plant. Next, different wastewaters with pH values of 4, 8 and 10 were separately prepared by using NaOH. 50 g of activated carbon was separately added into different cups containing different wastewater with a specific pH value. Next, the wastewater in each cup was agitated at 130 rpm, and the results were recorded in Table 1.
[0041] From the experiment, wastewater with a pH value of 2 contained 38.0 ppm H 2 O 2 after receiving treatment for 60 minutes, and 9.00 ppm H 2 O 2 after receiving treatment for 90 minutes. However, if the wastewater had a pH value of larger than 4, a vigorous reaction between the highly concentrated hydrogen peroxide in the wastewater and the activated carbon was observed, and the hydrogen peroxide decomposed, resulting in the formation of oxygen bubbles, thereby increasing the hydrogen peroxide removal power of the activated carbon—only 2.40 ppm H 2 O 2 remained after receiving treatment for 60 minutes, and only 0.14 ppm H 2 O 2 remained after receiving treatment for 90 minutes. This experiment also indicated that the activated carbon maintained a substantially equal hydrogen peroxide removal power after a number of repetitive experiments when the pH value of the wastewater was adjusted to 4, 8, or 10.
TABLE 1 Effect of pH variation on removal of hydrogen peroxide pH = 2 pH = 4 Time Conductivity H 2 O 2 Conductivity H 2 O 2 (min) pH (μS/cm) (ppm) pH (μS/cm) (ppm) 0 2.01 9600 354 4.09 3660 348 15 2.20 6460 197 7.84 3620 100 30 2.25 5850 107 8.03 3630 25.6 60 2.36 5500 38.0 8.07 3630 2.40 90 2.28 5350 9.00 8.11 3660 0.14 pH = 8 pH = 10 Time Conductivity H 2 O 2 Conductivity H 2 O 2 (min) pH (μS/cm) (ppm) pH (μS/cm) (ppm) 0 8.04 3740 342 10.01 4120 336 15 8.33 3700 98.8 8.98 4010 80.0 30 8.34 3730 30.2 8.86 4010 18.0 60 8.32 3740 3.40 8.80 4040 1.20 90 8.42 3750 0.22 8.90 4040 0.06
(b) Continuous Column Experiment
[0042] In an actual plant application, the treatment performance of activated carbon was influenced by the properties and retention time of the wastewater, etc., thereby altering the retention time of hydrogen peroxide in the activated carbon tower. Thus, a continuous column experiment was used to investigate the continuous treatment performance of an activated carbon tower.
[0043] A small column (with an internal diameter of 6.8 cm, and a height of about 20 cm) was used in the experiment. The column was packed with about 430 g of activated carbon for performing a continuous fluid test. Wastewater was prepared by using tap water containing 200 ppm of hydrogen peroxide, and was adjusted to a pH value of 2 by H 2 SO 4 to simulate the acidic wastewater from an actual plant. Next, NaOH was used to prepared different wastewaters with pH values of 4, 8, and 10. The wastewater flowed through the activated carbon column at a flowrate of 150 mL/min; after a continuous fluid test of 25 hours, the results are shown in FIG. 2 . Experimental results indicated that hydrogen peroxide could be effectively removed from water when the experiment was conducted in conditions where the pH value of the water exceeded or equaled 4, with a hydrogen peroxide removal ratio exceeding 95%.
[0000] (c) Test on an Actual Plant System
[0044] A process design shown in FIG. 1 was used to design a wastewater treatment system used by this example, as shown in FIG. 3 , wherein the design parameters of the activated carbon tower were obtained from the laboratory column test data.
[0045] The wastewater from the actual plant had a pH value of about 1˜3, a H 2 O 2 concentration of about 200 ppm (sometimes exceeding 400 ppm), and a conductivity of 5,000˜8,000 S/cm.
[0046] The process for treating the wastewater from an actual plant comprised: introducing the acidic wastewater into a pH adjustment tank 10 , using a pH meter to measure the pH value of the acidic wastewater, using a chemical addition control unit 16 to control the addition of NaOH in order to control the pH value of the acidic wastewater to be ≧4 (weakly acidic˜neutral), then introducing the wastewater into an activated carbon tower 11 . After receiving treatment from the activated carbon tower 11 , the wastewater was introduced into a temporary storage tank 12 , and from the temporary storage tank 12 was then introduced into a micro-filtration system (MF) 13 for the removal of the fine carbon particles produced during the hydrogen peroxide decomposition process. After receiving treatment from the micro-filtration system (MF) 13 , the wastewater was introduced into another temporary storage tank 14 . After reaching a sufficient water level, the wastewater was introduced to a reverse osmosis unit 15 for receiving further purification in order to remove soluble ions and organic contaminants. After receiving treatment from the reverse osmosis unit 15 (RO), the purified water was used as next level water and recycled. The concentrated wastewater produced by the reverse osmosis unit 15 and the backwash waste solution produced by the micro-filtration system 13 were all introduced downstream to a conventional treatment unit for further treatment, or discharged directly.
[0047] For the above-mentioned wastewater treatment process of an actual plant, the test results of removal of hydrogen peroxide by the activated carbon 11 are shown in FIG. 4 . The acidic wastewater was adjusted to a pH value of about 6, and the hydrogen peroxide removal ratio was greater than 99% over long term monitoring. In another control experiment, the raw water was not adjusted for its pH value and was directly introduced into the activated carbon tower. The initial measurements indicated that the H 2 O 2 removal ratio was about 83% (within 10 days). However, after continuous operation for 30 days, the removal ratio dropped to 77%, and the concentration of hydrogen peroxide after passing through the activated carbon tower was more than 40 ppm, thereby causing oxidation losses on a subsequent treatment unit (RO). Thus, this experiment indicated that if the acidic wastewater was not adjusted for its pH value (thus having a pH value in the range of 1˜3) and a continuous test was carried out, the H 2 O 2 removal efficiency of the activated carbon decreased gradually with the progress of the operation. However, if the pH value of the wastewater was adjusted to about 6, the operational lifespan and the H 2 O 2 removal efficiency of the activated carbon were significantly increased.
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The present invention provides an improvement for H 2 O 2 -containing wastewater treatment, wherein activated carbon for reducing the hydrogen peroxide content in the wastewater has an enhanced efficiency and a longer useful lifetime. The method of the present invention monitors a pH value of the H 2 O 2 -containing wastewater, and adjusts the pH value to 4 or higher by adding a base, when the pH is lower than 4, prior to causing the wastewater to contact activated carbon.
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BACKGROUND OF THE INVENTION
This invention relates to a display placard, and in particular to a point-of-purchase display placard for ladders.
It is particularly difficult to put informational or advertising displays on ladders, because a ladder's open configuration makes it difficult to attach signage, and a ladder's size usually makes it impractical to put the ladder in a container or box. Thus, information and advertising displays for ladders are generally secured to the styles, or some other part of the ladder. Such displays can be cumbersome and time consuming to apply. Such displays are generally small, and are often not clearly visible when the ladder is on display.
SUMMARY OF THE INVENTION
The present invention is a point-of-sale display placard that is of simple and inexpensive construction, and which can be quickly and easily secured to a ladder. The placard provides a large, visible display surface, that is both securely attached to the ladder, and held in position so that it remains visible during the transportation, storage, display, and sale of the ladder. The display placard can be formed from a blank having a portion that be manually folded around a portion of the ladder and secured, without the need for special tools or separate fasteners.
Generally, the display placard of the present invention is formed from a blank having first and second ends. At least two segments are formed in the blank at the first end by at least two fold lines to permit the segments to be folded around the rung of a ladder and secured to the placard to encircle the rung of the ladder, thereby securing the placard to the ladder. There is preferably a tab on the first end of the blank, and a slot in the blank adapted to receive and engage the tab on the first end, to secure the placard around the rung. In the preferred embodiment there are three segments at the first end of the blank, which when folded around the rung of ladder form an enclosure of rectangular cross section around the rung of the ladder.
The display placard is secured to a rung or step of the ladder with the enclosure formed by the segments surrounding the rung or step. The second end of the blank engages some other portion of the ladder, such as an adjacent rung or step, the stiles of the ladder, or perhaps gussets, to hold the panel portion generally in the plane of the ladder, so that it remains visible to someone looking at the front of the ladder.
Thus the display placard of the present invention provides a simple and inexpensive point-of-purchase display that can be quickly installed on the ladder, which remains securely on the ladder while the ladder, is transported, stored, displayed, and sold, but which can be easily removed by the consumer after purchase. The display placard is configured to remain prominently in view in the front elevation of the ladder, so that the information on the placard is and remains readily visible. The placard can be provided in the form of an inexpensive blank that is easy to fabricate, and compact for storage. These and other features and advantages will be in part apparent and in part pointed out hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front elevation of a first embodiment of a blank for a point-of-sale display placard constructed according to the principles of the present invention;
FIG. 2 is a front elevation view of the placard shown as it would be secured on the rung or step of a conventional ladder;
FIG. 3 is a vertical cross-sectional view of the placard, taken along the plane of line 3 — 3 in FIG. 2;
FIG. 4 is a front elevation view of the placard shown as it would be secured on the rung or step of a stepladder;
FIG. 4 a is a front elevation view of the placard on a stepladder, showing an alternate method of the securing placard;
FIG. 5 is a vertical cross-sectional view of the placard shown as it would be secured on an extension ladder;
FIG. 5 a is a vertical cross-sectional view of the placard on an extension ladder, showing an alternate method of securing the placard; and
FIG. 6 is a front elevation view of a second embodiment of a blank for a point-of-sale placard constructed according to the principles of this invention.
Corresponding reference numerals indicate corresponding parts throughout the several views of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
A blank for a point-of-sale display placard constructed according to the principles of the present invention is indicated generally as 20 in FIG. 1 . The blank has a front face 22 , and a back face, a first end 24 and a second end 26 , and left and right side edges 28 and 30 . The blank includes a panel portion 32 onto which information and illustrations can be printed or affixed. The blank 20 is preferably made from a flat, relatively rigid material such as a corrugated cardboard. There are at least two segments 34 formed at the first end 24 of the blank 20 by at least two fold lines 36 . In the preferred embodiment shown and described herein, there are three segments 34 a , 34 b , and 34 c , formed by fold lines 36 a , 36 b , and 36 c . The fold lines 36 can be, for example, creases pre-formed in the material of the blank so that the blank is pre-disposed to fold in a straight line along the crease. Thus the segments can be wrapped around the rung or step of a ladder, and once secured to the placard, encircle the rung or step, securing the placard to the ladder.
In the preferred embodiment there is a tab 38 on the first end 24 of the blank 20 , that is adapted to fit in a slot 40 in the panel portion 32 of the blank so that the segments 34 and a portion of the panel 32 form an enclosure around the rung or step of the ladder. As shown in FIG. 1, the tab 38 has barbs 42 on each side to help retain the tab in the slot 40 . The tab 38 further has an opening 44 , which is adapted to be engaged by a tooth 46 in the slot 40 , to further secure the tab in the slot. Thus the blank 20 can be formed into a placard that remains secured on the rung or step of a ladder without the need for tools or separate fasteners. The tab 38 and slot 40 help retain the placard on the ladder during shipment, storage, and sale, yet the placard can be easily removed by the ultimate consumer.
The completed placard made from the blank 20 is shown in FIGS. 2 and 3 as it would be secured on a conventional ladder 44 having stiles 46 and 48 , and rungs or steps 50 extending therebetween. As shown in FIG. 3, the segments 34 a , 34 b , and 34 c and the portion of the panel 32 between the slot 40 and the fold line 36 c , form an enclosure having a generally rectangular cross-section around a rung or step 50 . The first end of the blank is secured to the panel portion of the placard by the tab 38 that extends through the slot 40 .
The placard, and in particular the panel portion 32 of the placard is preferably sized and shaped for the particular ladder 44 , so that the second end (i.e. the end opposite from the end secured to a rung or step of the ladder, engages and is supported by the ladder, holding the placard in position generally in the plane of the ladder, so that the placard stays visible from the front of the ladder. For example, as shown in FIGS. 2 and 3, in the case of ladder 44 , the second end of the panel is supported by an adjacent rung 50 .
The placard of the present invention is shown in FIGS. 4 and 4 a as it would be secured on a stepladder 52 . The stepladder 52 has converging stiles 54 and 56 , and a plurality of rungs or steps 58 , supported by gussets 60 . As shown in FIG. 4 the placard is secured on a rung with the panel 32 depending downwardly and supported by an adjacent rung and gussets. As shown in FIG. 4 a the placard is secured on a rung with the panel 32 extending upwardly and supported by an adjacent rung and gussets.
The placard of the present invention is shown in FIG. 5 as it would be secured on an extension ladder 62 . The extension ladder 62 comprises first and second ladder sections 64 and 66 . Each ladder section comprises stiles 68 and 70 , with rungs or steps 72 extending therebetween. The enclosure formed by the segments on the first end of the placard surrounds a rung or step 72 on the first ladder section 64 , and the second end of the placard is sized and configured so that it extends between, and is thereby supported by adjacent rungs 72 on the first and second ladder sections 64 and 66 . Thus the placard is supported generally in the plane of the ladder 62 , so that its panel portion 20 remains visible at substantially all times from the front of the ladder. As shown in FIG. 5 the placard is secured on a rung with the panel 32 depending downwardly. As shown in FIG. 5 a the placard is secured on a rung with the panel 32 extending upwardly.
A second embodiment of a blank constructed according to the principles of this invention is indicated generally as 20 ′ in FIG. 6 . The blank 20 ′ is similar to blank 20 , and corresponding reference numerals indicate corresponding parts. However, unlike blank 20 , in blank 20 ′ the segments 34 a ′, 34 b ′, and 34 c ′ are not of equal size. Thus, when the segments are founded around the rung or step of a ladder, they form a more rectangular and less square enclosure around the rung. This is particularly desirable for stepladders, which typically have flat steps with more elongate cross sections, as compared to a round or nearly round rungs found on conventional ladders.
While both the blanks 20 and 20 ′ of the first and second embodiments are shown with three segments, which together with a portion of the panel form a four sided enclosure, the blanks could have been provided with as few as two segments, which would form an enclosure with a triangular cross section, or more than three segments, which would form an enclosure with a polygonal cross-section such as a pentagon, hexagon, etc.
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In combination with a ladder that comprises a pair of stiles connected by a plurality of spaced steps or rungs, a point of sale display placard is secured on the one of the steps or rungs. The placard includes a panel having first and second ends. A plurality of segments are formed at the first end, connected by folds to form an enclosure surrounding the rung. The portion of the placard adjacent the second end engages a portion of the ladder so that the panel remains generally parallel to the plane of the ladder.
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TECHNICAL FIELD
[0001] The invention relates to a valve assembly with a vent flow bypass for a fuel tank.
BACKGROUND OF THE INVENTION
[0002] Fuel tank valve assemblies that control the fluid level within the tank and provide nozzle shutoff are known. The fuel tanks must include vapor venting ability for gasses within the tank to maintain balanced pressure as the fuel levels within the tank change. Additionally, these valve assemblies often provide protection from liquid escaping during roll over conditions. However it is also desirable to prevent liquid from escaping due to sloshing of the liquid under normal conditions.
SUMMARY OF THE INVENTION
[0003] A valve assembly for a fuel tank is provided. The valve assembly includes a housing. A portion of the housing is located at least partially outside of the fuel tank. The housing also defines a vapor passage. A membrane is supported by the housing such that the membrane covers the vapor passage. The membrane allows the passage of vapor through the membrane and prevents the passage of liquid through the membrane. A flow control feature is supported by the housing to assist in controlling flow of a vapor through the membrane and the vapor passage. The flow control feature assists in controlling flow by providing variable flow through the vapor passage. A splash guard is useful in reducing the amount of liquid that comes in contact with the membrane
[0004] The housing includes a vapor recovery housing portion located at least partially outside of the fuel tank and a fuel tank housing portion located at least partially within the fuel tank.
[0005] Additionally, a carrier may be secured to the housing. The membrane is attached to the carrier such that the membrane covers the vapor passage and a carrier opening is defined by the carrier to allow the passage of vapor and prevent the passage of liquid.
[0006] The above features and advantages and other features and advantages of the present invention are readily apparent from the following detailed description of the best modes for carrying out the invention when taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 is a schematic fragmentary cross-sectional illustration of a valve assembly mounted to a fuel tank;
[0008] FIG. 2 is a schematic cross-sectional illustration of a membrane carrier for the valve assembly of FIG. 1 ;
[0009] FIG. 3 is a schematic end view illustration of the membrane carrier for the valve assembly of FIGS. 1 and 2 ;
[0010] FIG. 4 is a schematic cross-sectional illustration of another embodiment of a valve assembly;
[0011] FIG. 5 is a schematic cross-sectional illustration of third embodiment of a valve assembly; and
[0012] FIG. 6 is a schematic cross-sectional illustration of a fourth embodiment of a valve assembly.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0013] Referring to the drawings, wherein like reference numbers refer to like components, FIG. 1 shows a valve assembly 10 mounted to a fuel tank 12 . The valve assembly 10 has a housing 14 . A first housing portion 16 is located primarily within the fuel tank 12 . A second housing portion 18 is located primarily outside of the fuel tank 12 . The housing 14 also defines a vapor passage 20 , also referred to as a vent opening, which is in fluid communication with a vapor outlet 22 . The vapor outlet 22 leads to a vapor recovery canister (not shown) or other destination outside of the tank 12 .
[0014] The first housing portion 16 is inserted within a tank hole 24 in the fuel tank 12 . The first housing portion 16 could also be mounted externally with a passageway that allows communication with the interior of the tank. The first housing portion 16 includes a flange 26 which is located outside of the fuel tank 12 to prevent the valve assembly 10 from passing entirely through the tank hole 24 and into the fuel tank 12 . The second housing portion 18 is sometimes referred to as the vapor recovery side of the housing 14 . The second housing portion 18 is secured to the first housing portion 16 at the flange 26 . A carrier 28 is located between the first housing portion 16 and the second housing portion 18 . Securing the second housing portion 18 on the first housing portion 16 retains the carrier 28 to the housing 14 .
[0015] FIG. 2 illustrates an enlarged cross-sectional view of the carrier 28 and FIG. 3 illustrates a bottom view of the carrier 28 of FIG. 1 . The carrier 28 is generally annular in shape having a main body 30 . At least one finger 32 protrudes upwardly from the main body 30 . The finger 32 corresponds to indentations 34 (shown in FIG. 1 ) on the second housing portion 18 when the carrier 28 is assembled with the housing 14 . As discussed above, and illustrated in FIG. 1 , the main body 30 is secured between the first housing portion 16 and the second housing portion 18 when the valve assembly 10 is assembled. The annular shape of the carrier 28 defines a carrier opening 36 through which vapor within the fuel tank 12 can vent through to the vapor vent passage 20 (shown in FIG. 1 ). A membrane 38 is secured to the carrier 28 and extends over the entire carrier opening 36 . The membrane 38 is of a material that allows vapor to pass through the membrane 38 but prohibits liquid from passing through. The membrane may be secured to the carrier 28 by weld, adhesive, heat sealing, insert molding, or other methods. One skilled in the art would know the appropriate attachment required for a particular carrier 28 and membrane 38 arrangement.
[0016] The carrier 28 includes at least one flow control feature 39 . In the embodiment shown the flow control feature 39 is a deflector 40 . As the membrane 38 is exposed to liquid, the liquid may slow the flow rate of the vapor through the membrane. Thus, the deflector 40 deters liquid from reaching the membrane 38 to help maintain the vapor flow rate through the membrane 38 at a predetermined level.
[0017] The deflector 40 extends downwardly and inwardly from the main body 30 of the carrier 28 . The deflector 40 defines at least one deflector opening 42 and may define a plurality of deflector openings. The deflector 40 would assist in directing liquid away from the membrane 38 and the vapor vent passage 20 while the deflector opening 42 allows vapor to pass the deflector 40 and exit the fuel tank 12 through the membrane 38 . The size and number of deflector openings 42 may be set to control the maximum amount of vapor that may pass through at one time. Additionally, the deflector 40 may include several layers of material with deflector openings 42 at various locations on each layer of the deflector 40 . This would create a tortuous flow path further assisting in deflecting liquid away from the membrane 38 .
[0018] The carrier 28 may also include a plurality of ribs 44 extending upwardly from the deflector 40 . The ribs 44 are arranged radially on the deflector 40 and provide support for the membrane 38 and assist in stiffening the deflector 40 . Additionally, the flow control feature 39 may include optimizing the size of the carrier opening 36 to control the maximum flow rate of the vapor that may exit the fuel tank 12 at one time.
[0019] FIG. 4 illustrates a second embodiment of a valve assembly 110 having a carrier 128 for use with a fuel tank 12 (shown in FIG. 1 ). The carrier 128 is mounted to a housing 114 . The carrier 128 includes a main body 130 . At least one finger 132 protrudes upwardly from the carrier 128 to assist in securing the carrier 128 to the housing 1 14 . The main body 130 defines a carrier opening 136 . A membrane 138 is secured to the main body 130 to cover at least the carrier opening 136 . The membrane 138 may be larger in size than the carrier opening 136 . The size of the carrier opening 136 may be determined based upon the maximum desired vapor flow through the housing 114 to a vapor vent passage 120 .
[0020] The membrane 138 is illustrated in as a generally flat membrane. However, the membrane 138 may also be a cylinder or may be pleated to increase the surface area of the membrane 138 . One skilled in the art would know the proper shape for a membrane 138 for a particular valve assembly 110 arrangement.
[0021] A flow control feature 139 for the valve assembly 110 is a head valve. The flow control feature 139 includes a disc (or plate) 146 . The disc 146 is located above the carrier 128 within the vapor vent passage 120 . The disc 146 defines a disc opening 148 through which vapor may exit the fuel tank 12 (shown in FIG. 1 ). The disc opening 148 is smaller in diameter than the carrier opening 136 and is sized to control the amount of flow at a given pressure inside the tank. When the vapor pressure within the fuel tank 12 reaches a sufficient level the disc 146 is lifted off the carrier 138 , as shown. The vapor may exit through the disc opening 148 and around the sides of the disc 146 , as illustrated by arrows V. The finger 132 assists in guiding the disc 146 in the proper position with respect to the carrier 128 . As the vapor escapes the fuel tank 12 the pressure within the fuel tank 12 decreases and the disc 146 returns to the resting position on the carrier 128 . Vapor may still exit the fuel tank through the disc opening 148 but will not exit around the disc 146 until the pressure again increases to a level that will raise the disc 146 off the carrier 128 .
[0022] The carrier 128 may also include flange protrusions 150 extending downward from the main body 130 . The flange protrusions 150 assist in attaching the membrane 138 to the carrier 128 . The membrane 138 may be attached by weld, adhesive, heat sealing, insert molding, or other methods. One skilled in the art would know the appropriate attachment required for a particular carrier 128 and membrane 138 arrangement.
[0023] FIG. 5 illustrates another embodiment of a valve assembly 210 . The valve assembly 210 has a housing 214 . The valve assembly 210 has a housing 214 with features that define at least one passageway 242 A and 242 B for vapor flow. The housing 214 interfaces with the fuel tank (not shown).
[0024] A membrane 238 is secured to the housing 214 to cover at least the first housing opening 242 A and the second housing opening 242 B. The size of the first housing opening 242 A and of the second housing opening 242 B may be determined based upon the maximum desired vapor flow through the housing 214 to a vapor passage 220 also defined by the housing. The membrane 238 is illustrated in as a generally flat membrane. However, the membrane 238 may also be a cylinder or may be pleated to increase the surface area of the membrane 238 . One skilled in the art would know the proper shape for a membrane 238 for a particular valve assembly 210 arrangement.
[0025] A flow control feature 239 for the valve assembly 210 is a head valve which includes a ball 246 located within the second housing opening 242 B. The ball 246 is located above the housing 214 partially within the vapor vent passage 220 and the second housing opening 242 B. The second housing opening 242 B may have an enlarged or tapered portion 244 for guiding and supporting the ball 246 . Vapor may exit the fuel tank 212 through the first housing opening 242 A which includes an orifice limiting the flow. When the vapor pressure within the fuel tank reaches a sufficient level the ball 246 is lifted off the housing 214 , as shown. The vapor may exit through the first housing opening 242 A and the second housing opening 242 B around the sides of the ball 246 , as illustrated by arrows V. The tapered portion 244 assists in guiding the ball 246 in the proper position with respect to the housing 214 . As the vapor escapes the fuel tank the pressure within the fuel tank decreases and the ball 246 returns to the resting position on the housing 214 . Vapor may still exit the fuel tank through the first housing opening 242 A but will not exit through the second housing opening 242 B until the pressure within the fuel tank again increases to a level that will raise the ball 246 off the housing 214 .
[0026] FIG. 6 illustrates another embodiment of a valve assembly 310 . The valve assembly 310 has a housing 314 . A first housing portion 316 is located primarily within the fuel tank 312 and a second housing portion 318 is located primarily outside of the fuel tank 312 . The housing 314 also defines a vapor vent passage 320 , also referred to as a vent opening, which is in fluid communication with a vapor outlet 322 . The vapor outlet 322 leads to a vapor recovery canister (not shown) or other destination outside of the tank 312 .
[0027] The first housing portion 316 is inserted within a tank hole 324 in the fuel tank 312 . The housing 314 includes a flange 326 which is located outside of the fuel tank 312 to prevent the valve assembly 310 from passing entirely through the tank hole 324 and into the fuel tank 312 . The second housing portion 318 is sometimes referred to as the vapor recovery side of the housing 314 .
[0028] The housing 314 includes a carrier 328 . A membrane 338 is secured to the carrier 328 by weld, adhesive, heat sealing, insert molding, or other methods. One skilled in the art would know the appropriate attachment required for a particular membrane 338 .
[0029] The membrane 138 is illustrated in as a generally flat membrane. However, the membrane 138 may also be a cylinder, may be spirally wound, or may be pleated to increase the surface area of the membrane 138 . One skilled in the art would know the proper shape for a membrane 138 for a particular valve assembly 110 arrangement.
[0030] The carrier 328 and housing 314 defines a housing opening 348 through which vapor within the fuel tank 312 can vent through to the vapor vent passage 320 . The membrane 338 is secured to the carrier 328 and extends over the entire housing opening 348 . The membrane 338 is of a material that allows vapor to pass through the membrane 338 but prohibits liquid from passing through.
[0031] The carrier 328 includes at least one flow control feature 339 . In the embodiment shown, the flow control feature 339 is a restriction in the size of the housing opening 348 to control the amount of vapor that may exit the fuel tank 312 at one time.
[0032] Additionally the flow control feature 339 may include a soft shut off feature on the first housing portion 316 . The first housing portion 316 , in this instance, is often referred to as a dip tube. The first housing portion 316 extends downward within the fuel tank 312 . As is known to those skilled in the art the first housing portion 316 may provide an air pocket to control shut off of a fuel pump when filling the fuel tank. In the embodiment shown, the first housing portion 316 has a tapered edge 350 around at least a portion of the first housing portion 316 . Additionally, the first housing portion 316 defines a fuel shut off aperture 352 . The tapered edge 350 and the fuel shut off aperture 352 provide for restricted vapor flow as the fuel tank 312 is filled with fluid. Therefore, this will accommodate for sloshing as the fuel tank is filled, by minimizing the amount of liquid from the sloshing that reaches the membrane 338 . The tapered edge 350 and fuel shut off aperture 352 can be used together or individually to restrict vapor flow into the housing as the liquid level rises until the tapered edge 350 and the fuel shut off aperture 352 are completely submerged.
[0033] Alternatively to a dip tube, the flow control feature 339 may include a float located within the first housing portion 316 which may also be used to control fuel shut off at a fuel pump, as is known in the art.
[0034] While the best modes for carrying out the invention have been described in detail, those familiar with the art to which this invention relates will recognize various alternative designs and embodiments for practicing the invention within the scope of the appended claims.
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A valve assembly for a fuel tank includes a housing. A membrane supported by the housing such that the membrane covers a vapor passage defined by the housing. The membrane allows the passage of vapor through the membrane and prevents the passage of liquid through the membrane. A flow control feature is supported by the housing to assist in controlling flow of a vapor through the membrane and the vapor passage. The flow control feature assists in controlling flow by one of shielding liquid from the membrane and providing variable flow through the vapor passage.
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This is a divisional of application Ser. No. 09/382,161 filed Aug. 24, 1999, which is a divisional of Ser. No. 08/798,320, filed on Feb. 10, 1997, which issued as U.S. Pat. No. 5,989,698 on Nov. 23, 1999.
FIELD OF THE INVENTION
This invention relates to coated porous materials that exhibit air permeability and repellency to liquids having a surface tension at least equal to or greater than 20 dynes/cm.
BACKGROUND OF THE INVENTION
Films, fabrics, and fibrous substrates including textiles have been treated with fluorochemical uncrosslinked urethanes to impart water and soil repellency.
Microporous films prepared by thermally-induced phase separation (TIPS) methods are known. U.S. Pat. No. 4,539,256 (Shipman), U.S. Pat. Nos. 4,726,989 and 5,120,594 (Mrozinski) and U.S. Pat. No. 5,260,360 (Mrozinski et al.) describe such films containing a multiplicity of spaced, randomly dispersed, equiaxed, nonuniform shaped particles of a thermoplastic polymer, optionally coated with a liquid that is immiscible with the polymer at the crystallization temperature of the polymer. Micropores allow permeability to gases, including moisture vapor, but can be impermeable to high surface tension liquids such as water.
Microporous membranes have been coated with a urethane such that the pores are filled and the membrane is impervious to passage of gases. On the other hand, U.S. Pat. No. 5,286,279 describes a gas permeable membrane coated with a fluorochemical urethane wherein the urethane is prepared from either 1,4-cyclohexane diisocyanate or methane 4,4,′-diphenyl diisocyanate.
SUMMARY OF THE INVENTION
The present invention fills a need by employing a precursor fluorocarbon urethane composition or curable coating composition to coat a porous material, e.g. a microporous polyolefin membrane. The urethane precursors are crosslinked in situ, upon drying, in such a way that the pathways through the membrane are not blocked or plugged with a coating. As a result, resistance to airflow and bubble point pore size values are retained after coating. Because the coated membrane is highly breathable, durable, and has a low surface energy, it is useful for making ileostomy vent filters, transdermal drug substrates, agricultural and medical apparel, as well as paint and chemical protective garments.
Accordingly, the present invention in its first aspect is a curable coating composition for a porous material containing fluorocarbon urethane precursors including:
(a) a polyisocyanate;
(b) a polyhydric alcohol; wherein at least one member of (a) or (b) has a functionality of greater than 2, and
(c) a perfluoroalkyl alcohol of the formula
R—(CH 2 ) x —OH, (I)
in which R is C n F 2n+1 or
where x is 1-12; n is 3-20, and R 1 is H, alkyl of 1-4 carbon atoms or —(CH 2 ) x —OH, wherein said composition is capable of crosslinking.
A second aspect of the present invention is a coated porous material which includes a porous material and a curable coating composition applied to said material which includes the following fluorocarbon urethane precursors:
(i) a polyisocyanate;
(ii) a polyhydric alcohol; wherein at least one member of (i) or (ii) has a functionality of greater than 2, and
(iii) a perfluoroalkyl alcohol of the formula
R—(CH 2 ) x —OH, (I)
in which R is C n F 2n+1 or
where x is 1-12; n is 3-20, and R 1 is H, alkyl of 1-4 carbon atoms or —(CH 2 ) x —OH.
Another aspect of the present invention is a process or method of making a coated porous material which includes the following steps:
applying a curable coating composition which includes the above defined fluorocarbon urethane precursor on an organic solvent, on a porous material to cover the material, and
drying the resulting coating sufficiently to remove the solvent and promote cross-linking or curing, to produce the coated membrane which exhibits air permeability and repellency to liquid having a surface tension at least equal to or greater than 20 dynes/cm.
The inventive porous materials having a cured coating, which include non-woven, woven materials, perforated films and microporous membranes retain their liquid repellency and moisture vapor permeability properties for extended periods in all types of applications.
The microporous polyolefin materials may contain a compatible liquid or diluent such as mineral oil along with the fluorocarbon urethane coated material and are referred to as (oil-in) materials. Such a fluorocarbon urethane coating on an oil-in polyolefin membrane provides the membrane the ability to resist wetting by fluids like alcohols, toluene, mineral oil, water-surfactant solutions and ethylene glycol even though the membrane's pore walls are coated with approximately 35-40 wt-% mineral oil or another diluent. The same coating on a polyolefin membrane having no diluent (oil-out) or on other membranes or materials not prepared by thermally induced phase separation (TIPS) provides materials displaying even more repellency such that the coated materials resist wetting by all of the above-mentioned fluids as well as chlorohydrocarbons such as trichloroethane, and hydrocarbons such as decane, octane, heptane and hexane.
The present coated porous materials having a cured coating are repellent to a wide variety of fluids including the above organic fluids and are much more repellent than membranes containing prior fluorocarbon coatings such as the fluorocarbon oxazolidinone coatings on polyolefin membranes described in U.S. Pat. No. 5,260,360.
DETAILED DESCRIPTION
Coated and cured porous materials, e.g. microporous polyolefin membrane materials, of the present invention, exhibit significant air permeability properties and repel aqueous-based as well as non-aqueous based liquids including a wide variety of non-aqueous liquids having a surface tension at least equal to or greater than 20 dynes/cm.
Porous materials of the present invention having a cured coating exhibit durability of their fluid repellency properties when subjected to rubbing, touching, folding, flexing or abrasive contact. They also display oleophobic properties, resisting penetration by oils and greases and some (eg. those made from polyethylene (PE), polypropylene (PP) or PE/PP blends) may be heat sealable. For the oil-in version of the invention, the oleophobicity and heat sealing properties of the membrane materials are most surprising since the membrane materials contain an oily, oleophoic processing compound which is a priori, one would expect, would promote wetting by other oleophilic materials and which also would inhibit heat sealing.
Transport of a liquid challenge through most porous materials or fabrics occurs because the liquid is able to wet the material. A possible route through the material is for the liquid to initially wet the surface of the material and to subsequently enter pore openings at the surface of the material followed by a progressive wetting of and travel through interconnected pores until finally reaching the opposite surface of the material. If the liquid has difficulty wetting the material, liquid penetration into and through the material will, for the most part, be reduced. A similar phenomenon occurs in the pores, where reduced wetability, in turn, reduces pore invasion. Generally the greater the numerical difference between the liquid surface tension of the liquid and the surface energy of the porous material (the latter being lower), the less likely it is that the liquid will wet the porous material.
In the case of aqueous solutions containing surface active agents (eg. surfactants) the wetting of the porous materials is usually time-dependent, controlled by the slow diffusion and absorption of surfactants onto the surface of the porous materials.
In the present invention, the extent of barrier protection may be described by four levels, of which the first two describe existing levels and the last two describe levels of protection as a result of the coatings presented by this invention.
Level 1 TIPS membranes without diluents (polypropylene (PP), or high density polyethylene (HDPE)) TIPS membranes with diluents, particle-filled membranes, and polytetrafluoroethylene (PTFE) membranes. In terms of repellency beyond water, these materials immediately wet through with a 0.1 wt. % surfactant, Triton X-1000/water solution with a surface tension of 30 dynes/cm under a constant pressure of 69 kpa (10 psi). These microporous materials also wet easily with mineral oil and solvents like alcohol, toluene, methylethyl ketone (MEK) and the like.
Level 2 TIPS oil-in PP membranes containing fluorocarbon oxazolidinone (FCO) as a melt additive or a topical coating. These membranes prevent penetration of the above surfactant/water solution for 32 minutes at 69 kpa (10 psi). They also resist wetting by methyl alcohol and water/isopropyl alcohol mixtures (IPA) (up to 80% IPA), but are wetted by pure IPA, toluene, MEK, and other solvents.
Level 3 TIPS oil-in PP membranes with a fluorocarbon-urethane coating presented by this invention. These materials do not allow flow of the above surfactant/water solution through the membrane in over three days of continuous testing under a constant pressure of 69 kpa (10 psi). In addition, these materials resist wetting by any alcohol, toluene, ethylene glycol, ethyl acetate, and by a number of concentrated surfactants.
Level 4 TIPS diluent-free (or oil-out) membranes, PTFE, particle-filled membranes, polyamides and other polymer membranes with a fluorocarbon-urethane coating of the present invention. These materials resist wetting (except under high pressure) by surfactants, alcohol, MEK, toluene, dodecane, decane, octane, heptane, and hexane.
The oleophobic, hydrophobic, moisture permeable, air permeable, coated porous materials of the present invention may be prepared by topically applying a fluorocarbon urethane precursor, the curable coating composition, to a porous material through spray or roll-on application, through dip coating or transfer coating techniques. Following the application, the coating is dried sufficiently to remove solvent and to promote cross-linking or curing of the fluorocarbon urethane coating membrane.
By porous material, it is meant that a material has a pore size less than about 250 micrometers. Preferably the pore size is from about 0.01 to about 250 micrometers. The materials include non-woven and woven materials and perforated films. Porous polymeric materials include polyurethane, polyesters, polycarbonates, polyamides, and preferably polytetrafluoroethylene (PTFE) and polyolefins. The polymeric materials may also be referred to as microporous membranes.
Examples of membranes which are made by thermally induced phase separation include crystalline or crystallizable polyolefin membranes described, for example, in U.S. Pat. No. 4,539,256 (Shipman), U.S. Pat. No. 4,726,989 (Mrozinski), U.S. Pat. No. 4,863,792 (Mrozinski), U.S. Pat. No. 4,824,718 (Hwang), U.S. Pat. No. 5,120,594 (Mrozinski) and U.S. Pat. No. 5,260,360 (Mrozinski) each of which is incorporated herein by reference.
An example of a perforated films is the plain surface, polycarbonate, Track-etch membrane filter screens available from Poretics Corporation, of Livermore, Calif.
Further, the curable coating compositions can be topically applied to materials such as stretched PTFE, as mentioned above, or particle loaded films which do not contain a diluent or compatible liquid (oil-out). The compatible liquid may be removed from the microporous polyolefin sheet material, either before or after orientation, to form a diluent-free microporous polymeric material. The compatible liquid can be removed by, for example, solvent extraction, volatilization, or any other convenient method.
Crystallizable olefin polymers suitable for use in the preparation of coated microporous membrane materials of the present invention are melt processable under conventional processing conditions. That is, on heating, they will easily soften and/or melt to permit processing in conventional equipment, such as an extruder, to form a sheet, tube, filament or hollow fiber. Upon cooling the melt under controlled conditions, suitable polymers spontaneously form geometrically regular and ordered crystalline structures. Preferred crystalizable olefin polymers for use in the present invention have a high degree of crystallinity and also possess a tensile strength of at least about 689 kpa (100 psi).
Examples of suitable commercially available crystallizable polyolefins include polypropylene, block copolymers or other copolymers of ethylene and propylene, or other polymers, such as polyethylene, polypropylene and polybutylene polymers which can be used singularly or in a mixture.
Materials suitable as processing compounds for blending with the crystallizable polymer to make the microporous membrane materials of the present invention are liquids or solids which are not solvents for the crystallizable polymer at room temperature. However, at the melt temperature of the crystallizable polymer the compounds become good solvents for the polymer and dissolve it to form a homogeneous solution. The homogeneous solution is extruded through, for example, a film die, and on cooling to or below the crystallization temperature of the crystallizable polymer, the solution phase separates to form a phase separated film.
Preferably, these second phase compounds have a boiling point at atmospheric pressure at least as high as the melting temperature of the polymer. However, compounds having lower boiling points may be used in those instances where superatmospheric pressure may be employed to elevate the boiling point of the compound to a temperature at least as high as the melting temperature of the polymer. Generally, suitable compounds have solubility parameter and a hydrogen bonding parameter within a few units of the values of these same parameters for the polymer.
Some examples of blends of olefin polymers and processing compounds which are useful in preparing microporous materials in accordance with the present invention include; polypropylene with mineral oil, dibenzylether, dibutyl phthalate, dioctylphthalate, or mineral spirits; polyethylene with xylene, decalin, decanoic acid, oleic acid, decyl alcohol, diethyl phthalate, dioctyl phthalate, mineral oil or mineral sprits, and polyethylene-polypropylene copolymers with mineral oil or mineral spirits. Typical blending ratios are 20 to 80 weight percent polymer and 20 to 80 weight percent blending compound.
A particular combination of polymer and processing compound may include more than one polymer, i.e., a mixture of two or more polymers, e.g. polypropylene and polybutylene, and/or more than one blending compound. Mineral oil and mineral spirits are examples of mixtures of processing compounds, since they are typically blends of hydrocarbon liquids. Similarly, blends of liquids and solids may also serve as the processing compound.
The curable coating composition or fluorocarbon urethane precursors include a combination of polyisocyanate, a polyhydric alcohol and a perfluoroalkyl alcohol as above defined. These components are mixed in an organic solvent and the resulting solution is applied as above described to the polyolefin membrane. The composition contains at least equimolar amounts of polyisocyanate and alcohol. Preferably, an excess of polyisocyanate may be used.
As the polyfunctional isocyanate component employed in the curable coating composition of the present invention, various compounds may be employed without any particular restrictions, so long as they are bifunctional or of higher functionality. Preferred polyisocyanates are di or tri-functional isocyanates. For example, di-functional isocyanate compounds may include aromatic isocyanates such as 2,4-toluenediisocyanate, 4,4′-diphenylmethanediisocyanate, tolidinediisocyanate and dianisidinediisocyanate; alicyclic diisocyanates such as 2-methyl-cyclohexane-1,4-diisocyanate, isophoronediisocyanate and hydrogenated MDI
and aliphatic diisocyanates such as hexamethylenediisocyanate and decamethylenediisocyanate. These compounds may be represented by the formula OCN—Y—NCO. When two OCN—Y—NCO are reacted in the presence of water, a dimer of the formula OCN—Y—NHCONH—Y—NCO will be formed. The difunctional isocyanate compounds include such dimers. Another difunctional isocyanate is
In addition to the difunctional isocyanate compounds, polyfunctional isocyanate compounds such as trifunctional, tetrafunctional or pentafunctional isocyanate compounds may be mentioned. Specific examples of trifunctional isocyanate compounds include, in addition to the after-mentioned compounds, a trimer of the formula
obtained by reacting the above-mentioned dimer of the formula OCN—Y—NHCONH—Y—NCO with a monomer of the formula OCN—Y—NCO. Examples of other tri-functional isocyanate compounds include:
The polyhydric alcohol includes any multifunctional monomer alcohol having at least two hydroxyl groups. Preferred polyhydric alcohols are those having 2 to 8 carbon atoms and preferably being a diol or triol. Particularly useful are, for example, 1,4-butane diol, neopentyl glycol or trimethylol propane.
Preferred perfluoroalkyl alcohols are those of formula I, defined above,
wherein R is
in which x is 1-4, and R 1 is methyl, ethyl or —CH 2 OH.
Most preferred is the alcohol of formula I wherein R is C n F 2n+1 SO 2 —N—R 1 in which n is 8, and x is 2 and R 1 is methyl.
The above components of the curable coating composition are combined in a solvent in which the solution contains from about 2 to about 40 wt-% solids, preferably from about 5-10 wt-% solids. A most preferred composition-contains about 7 wt-% solids. This solution is applied as described above to the porous material.
An optional ingredient to enhance the crosslinking of the components of the curable coating composition is a catalyst. Such catalysts are well-known in the art and may include
(a) tertiary amines;
(b) tertiary phosphines;
(c) strong bases;
(d) acidic metal salts of strong acids;
(e) chelates of various metals;
(f) alcoholates and phenolates of various metals;
(g) salts of organic acids with a variety of metals such as alkali metals, alkaline earth metals;
(h) organometallic derivatives of tetravalent tin, trivalent and pentavalent As, Sb, and Bi and metal carbonyls of iron and cobalt.
Organotin compounds deserve particular mention as catalysts for catalyzing the urethane forming reaction. These compounds include the dialkyltin salts of carboxylic acids, e.g., dibutyltin diacetate, dibutyltin dilaurate, dibutyltin maleate, dilauryltin diacetate, dioctyltin diacetate, dibutylin-bis(4-methylaminobenzoate), dibutyltin-bis(6-methylaminocaproate), and the like. Similarly, there may be used a trialkyltin hydroxide, dialkytin oxide, dialkytin dialkoxide or dialkyltin dichloride. Examples of these compounds include trimethyltin hydroxide, tributyltin hydroxide, trioctyltin hydroxide, bitutyltin oxide, dioctyltin oxide, dilauryltin oxide, dibutyltin-bis(isopropoxide), dibutyltin-bis(2-dimethylaminopentylate), dibutyltin dichloride, dioctyltin dichloride, and the like. Particularly useful for the present invention is dibutyltin dilaurate.
As an organic solvent used to facilitate the application of the precursors, the following may be used: an ether such as dioxane, tetrahydrofuran, ethyl propyl ether; an amide such as formamide, dimethylformamide or acetamide; ketones such as acetone, methyl ethyl ketone, methyl isopropyl ketone or methyl isobutyl ketone; and esters such as methyl acetate, ethyl acetate, propyl acetate or butyl acetate. Such an organic solvent is added usually in an amount of from about 60 to about 98 wt-%, preferably about 90-95 wt-%. The most preferred amount of solvent is about 93 wt-% of the total of coating precursors, and the preferred solvent employed is a ketone such as methyl ethyl ketone.
Certain conventional additive materials may also be blended in limited quantities with the curable coating composition. Additive levels should be chosen so as not to interfere with the formation of the microporous membrane material or to result in unwanted exuding of the additive. Such additives may include, for example, dyes, pigments, plasticizers, UV absorbers, antioxidants, bactericides, fungicides, ionizing radiation resistant additives, and the like. Additive levels should typically be less than about 10% of the weight of the polymer component, preferably less than about 2% by weight.
An additional aspect of the present invention is the use of at least one surfactant which may be applied onto the porous material as a precoat or made part of the curable coating composition.
The surfactant adds hydrophilic character to the porous material and decreases the interfacial tension of a liquid or liquid system against the surface of the pores within a porous material. Normally any surfactant used will be a wetting agent which will facilitate the surface of the pores within a membrane being wetted by water. If desired, a mixture of different wetting agents may be employed in any specific application.
Accordingly, any surfactant which, when applied to the porous material (i.e., in the absence of the coating polymer), lowers the surface tension thereof to the extent that the substrate will exhibit a contact angle with water of less than about 80°, preferably less than about 60°, will render said substrate hydrophilic and can be employed in conjunction with the coating polymer.
Surfactants used may be a nonionic, cationic, or anionic type, or a combination of two or more of these surfactants.
Examples of nonionic surfactants are: polyol fatty acid monoglyceride, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl allyl ether, and polyoxyethylene alkylether phosphate.
Examples of cationic surfactants are: quaternary ammonium salts, polyoxyethylene alkylamines, and alkylamine oxides.
Examples of anionic surfactants are: alkylsulphonates, alkylbenzene sulphonates, alkylnaphthalene sulphonates, alkylsulphosuccinates, alkylsulphonate ester salts, polyoxyethylene alkyl sulphonate ester salts, alkyl phosphates, and polyoxyethylene alkyl phosphates.
A preferred nonionic surfactant is, for example, polyethylene glycol monostearate. A preferred anionic surfactant is dioctyl sodiumsulfosuccinate.
In the following non-limiting examples, all parts and percentages are by weight unless otherwise indicated. In evaluating the materials of the invention and the comparative materials, the following test methods are used.
EXAMPLES
Test Methods
“Gurley time” is measured by means of densometer number (i.e., flow-through time) of at least 2 seconds for 50 cc of air at 124 mm (4.88 in.) H 2 O pressure to pass through a sample of the web having a circular cross-sectional area of approximately 645 mm 2 (1 square inch). A temperature of approximately 23°-24° C. (74°-76° F.) and 50 percent relative humidity are maintained for consistent measurements. The “Gurley” densometer or flow-through time may be measured on a densometer of the type sold under the trade designation “Model 4110” densometer by W. & L. E. Gurley of Troy, N.Y., which is calibrated and operated with a Gurley Teledyne sensitivity meter (Cat. No. 4134/4135). The “Gurley” densometer time is determined in a manner similar to a standard test of the Technical Association of the Pulp and Paper Industry of Atlanta, Ga., for measuring the air resistance of paper (TAPPI Official Test Method T 460 om-B3 (which is incorporated herein by reference). Gurley time is inversely related to void volume of the test specimen of web. Gurley time is also inversely related to average pore size of the test specimen.
Example 1
A coating solution was prepared by mixing 38.5 g 1,6-hexane diisocyanate biuret (Desmodur™ N-75, Bayer, Philadelphia, Pa.), 56.8 g N-methyl-N-2-hydroxyethyl-perfluorooctylsulfonamide (available from Minnesota Mining and Manufacturing Company (3M), St. Paul, Minn.) and 4.7 g 1,4-butanediol (Aldrich Chemical Co., Milwaukee, Wis.) in 1390 g methyl ethyl ketone (MEK, Aldrich) to make a 7.0 weight percent solids solution. The solution was stirred and mixed with 0.5 g dibutyltin dilaurate (Aldrich), then applied to two different microporous membranes using a rotogravure coating process and a gravure roll having small indentations in its surface shaped like inverted pyramids. There were approximately 35 lines (of inverted pyramids) per inch (14 lines per cm) each pyramid being about 0.25 mm deep and having an internal tooth angle (angle between two edges of pyramid measured in the plane of one pyramid surface at the apex) of 90°, and the land area between inverted pyramids comprised about 50% of the gravure roll surface. The membranes were conveyed through the gravure roll apparatus at a rate of 3 m/min. Membrane 1A was a 0.04 mm thick polypropylene membrane (“oil-in” KN 9400™ porous film, 3M) and membrane 1B was a 0.05 mm thick polyethylene membrane (“oil-out” Cotran™ membrane, 3M) supported on a silicone release liner. After coating, each membrane was dried in an oven at 99° C. to remove MEK solvent and crosslink the urethane coating. Properties of the coated membranes are shown in Table 1.
TABLE 1
Oil/
Coating
Gurley
Pore size
Water/IPA
Heptane
Add-On,
No.,
micro-
resistance
resistance
Example
wt %
sec/50 cm 3
meters
A
B
1A Comp
0
56
0.26
2
0
1A
15
60
0.25
10
2-3
1B Comp
0
12
0.34
1
0
1B
30
17
0.32
10
6
A values range from 1-10, where 1 means a membrane resisted wetting by a 10 wt. % aqueous solution of isopropyl alcohol (IPA) for 30 seconds and 10 means a membrane resisted wetting by pure IPA
B values range from 0-8. 1 means the membrane resisted wetting by 100% mineral oil for 30 seconds, 2 means a membrane resisted wetting by a 65:35 oil:hexadecane mixture, and 8 means a membrane resisted wetting by 100% heptane for 30 seconds.
Table 1 shows that a fluorourethane coating of the invention increases membrane resistance to wetting by both water and oil, whether the membrane is “oil-in” (i.e., Example 1A) or “oil-out” (Example 1B) without reducing breathability (Gurley Number) too much and without filling pores of the membrane. In addition, the table shows that coatings of the invention are effective on both polypropylene and polyethylene membranes.
Example 2
A coating solution was prepared as described in Example 1 by mixing 35.1 g 1,6-hexane diisocyanate biuret (Desmodur N-75, Bayer) diisocyanate, 51.3 g N-methyl-N-2-hydroxyethyl-perfluorooctylsulfonamide, 12.2 g polyethylene glycol 400 monostearate (Aldrich) and 1.4 g 1,4-butanediol in 1329 g methyl ethyl ketone to make a 7.0 weight percent solids solution. The solution was stirred and mixed with 0.5 g dibutyltin dilaurate then applied to a 0.05 mm thick polyethylene membrane (“oil-out” Cotran™ membrane, 3M Co.) supported on a silicone release liner, dried and crosslinked. Coating weight was approximately 30 wt. %. Properties of the coated membrane are shown in Table 2.
TABLE 2
Gurley No.,
Pore size
Water/IPA
Oil/Heptane
Example
sec/50 cm 3
micrometers
resistance A
resistance B
2 Comp
12
0.34
1
0
2
17
0.32
10
8
A,B as described in Table 1
The data of Table 2 show that a chain-extended fluorourethane provided increased oil/heptane resistance (compared to Example 1B) over that provided by a non-chain extended fluorourethane.
Example 3
A solution of 44 g polyhydroxyl polyether (Pluracol™ PEP 550, BASF Corp., Mt. Olive, N.J.), 94 g N-methyl-N-2-hydroxyethyl-perfluorooctylsulfonamide and 150 g Desmodur™ N-75 diisocyanate in 2212 g methyl ethyl ketone was stirred and mixed with 2.5 g Irganox™ 1010 antioxidant (Ciba-Geigy, Ardsley, N.Y.) and 2.5 g dibutyltindilaurate to make a 10% by weight solution of isocyanate/polyol. The solution was coated onto porous polyethylene membrane (3M, St. Paul, Minn.) from a dip pan onto a trihelical gravure cylinder (40 lines/2.54 cm) having a volume factor of 51 micrometers and a tooth angle of 135°. Coating speed was 3.65 m/min after which the saturated membrane was heated in three successive ovens at 104° C. (total residence time 4 minutes) to complete the polyurethane formation. Initial membrane weight was 4.5 g/m 2 and final, cured coated membrane weight was 6.75 g/m 2 .
The coated membrane had a moisture vapor transmission rate (MVTR) that was 95% of the original uncoated film. Gurley porosity of the uncoated film was 14 sec/50 cc, and that of the coated film was 142 sec/50 cc. The coated film was not wet by toluene, octane, ethyl acetate and isopropyl alcohol, and it was wet by heptane, ethylether and Freon™ 113.
Example 4
Effect of Various Formulations on Performance
In order to evaluate certain polyurethane formulations, several isocyanates, aliphatic diols, and fluorocarbon alcohols were formulated into coatings for oil-in, oil-out and laminated porous membranes. The results are shown in Table 4. In Table 4:
D-75N was Desmodur 75N™, the trifunctional biuret of hexane diisocyanate (Bayer corp., Pittsburgh, Pa.)
D-I was Desmodur I™, toluene diisocyanaate (Bayer Corp.)
D-W was Desmodur W™, methane bis(4,4′-isocyanatocyclohexane) (Bayer Corp.)
MDI was methane bis(4,4′-isocyanatobenzene)
D-H was Desmodur H™, 1,6-hexanediisocyanate (Bayer Corp.)
BDO was 1,4-butane diol
TMP was trimethylolpropane
N-MeFOSE was N-methyl-N-(2-hydroxyethyl)perfluorooctane sulfonamide (3M, St. Paul, Minn.)
Zonyl Ba-N™ was perfluoroalkyl ethyl alcohol (DuPont Chemical Co., Wilmington, Del.)
Oil-out PP film was prepared according to U.S. Pat. No. 5,120,594, Example 1, incorporated by reference; precoating Gurley=10-12; W=3; O=0 Oil-in PP film was KN 9400™ microporous film (3M Company); precoating Gurley=80-125; W=3; O=0 Gurley numbers were as described supra, in units of sec/50 cc
O and W refer to resistance to Oil and Water, respectively, as described for Table 1, supra Laminate refers to a single-ply oil-in KN 9400™ film laminated with a 1 ounce polypropylene spunbonded web (Polybond, Inc., Waynesboro, Va.) as described in U.S. Pat. No. 5,260,360, Example 17, incorporated by reference;
for formulation 4B Laminate, Gurley=439
for formulation 4B Laminate, coated twice, W=10, O=4, Gurley=1140
for formulation 4I Laminate, Gurley=336
for formulation 4I Laminate, coated twice, W=10, Gurley=1403
Data in Table 4 shows that post-coating resistance was approximately the same for almost every formulation, and it was improved significantly over pre-coated values. In one example each, both N-ethyl FOSE and Zonyl™ BA-N appeared to provide slightly less post-coating resistance than precoated or uncoated films, for both oil and water on both oil-in and oil-out films.
TABLE 4
EFFECT OF VARIOUS FORMULATIONS ON PERFORMANCE
Films, After Coating
Oil-out PP
Oil-in PP
Aliphatic
Fluoroalcohol, g
Resist-
Resist-
Lami-
Isocyanate, g
Diol, g
N-Me
N-Et
Zonyl ™
ance
ance
nate
Sample
D-75N
D-I
D-W
MDI
D-H
BDO
TMP
FOSE
FOSE
BA-N
Gurley
W
O
Gurley
W
O
W
O
4A
825
67
838
12.6
10
6
128
10
3
4B
825
68
838
12.0
10
6
84.5
10
3
10
3
4C
383
67
838
12.2
9
6
157
9
3
4D
396
67
838
12.6
9
6
156
9
3
4E
429
67
838
25.1
10
8
1048
10
3
4F
252
67
838
20.3
10
8
235
10
3
4G
504
203
838
37.3
10
8
1200
10
3
4H
825
68
860
12.9
6
6
209
5
2
4I
577.5
68
838
13.0
10
6
180
10
2
10
2
4J
825
68
771
22.0
10
6
180
5
1
4K
1650
68
838
12.3
10
6
170
10
2
4L
275
45
559
12.8
10
6
170
10
2
Example 5
Effect of Coating on Various Substrates
In order to demonstrate the effectiveness of fluorourethane coatings on a number of microporous membranes, a standard mixture of 3.0 equivalents Desmodur N-75™ (Bayer Corp.), 1.5 equivalents N-methyl FOSE (3M), and 1.5 equivalents 1,4-butanediol (Aldrich Chemical Co.) in methyl ethyl ketone solvent, at the percent solids shown in Table 5, was prepared, and membranes were coated as described in Example 1. In some cases (5F, 5M-O, 5R) a surfactant was added to the coating solution, which generally increased wetting of the membrane, increasing coating effectiveness. Samples 5P and 5Q describe a membrane prepared by melt-blending a waxy surfactant with the polypropylene/mineral oil nucleating agent mixture to prepare a hydrophilic membrane prior to solution-coating the polyurethane precursor solution. Samples 5G and 5H were coated with the urethane precursor solution, dried, then re-coated (hence the designation “2X.” In Table 5:
Oil-in PP refers to KN 9400™ microporous film (3M Company);
Oil-out PP refers to microporous film prepared according to U.S. Pat. No. 5,120,594, Example 1;
PEGML 200 refers to poly(ethylene glycol) monolaurate surfactant of MW 200 (Aldrich);
Laminate refers to a single-ply oil-in KN 9400™ film laminated with a 1 ounce polypropylene spunbonded web (Polybond, Inc., Waynesboro, Va.) as described in U.S. Pat. No. 5,260,360, Example 17;
PEGMS 400 refers to a poly(ethylene glycol)monostearate surfactant of MW 400 (Aldrich);
TYVEK™ refers to a spunbonded polyethylene material (DuPont Co.);
EXXAIRE™ refers to a particle-filled polyethylene membrane (Exxon Chemical Co.);
SONTARA™ refers to a woven fabric comprising cellulose and poly(ethylene terphthalate) fibers (DuPont)
Porous PTFE refers to a poly(tetrafluoroethylene) membrane, Gurley=5 sec/50 cc, (Tetratec Corp., Feasterville, Pa.).
DOS 3 refers to dioctyl sodiumsulfosuccinate (Aldrich)
The data in Table 5 show that, for essentially any type of surfactant, using a surfactant in the urethane-precursor coating solution or coating on an oil-out membrane prior to treating with urethane-precursor solution improves wetting, hence improves oil and water resistance of the coated membrane over membranes coated in the absence of a surfactant. For oil-in membranes, melt blending a surfactant in the extrusion formation process (rather than coating with a surfactant on an oil-in membrane prior to treating with urethane precursor solution) results in improved water and oil resistance, compare Sample 50 (melt) to 5G (topical).
TABLE 5
Effect of Coating on Various Substrates
Min. Oil,
Gurley
% +
Solution
Before
Gurley After
W/IPA
W/IPA
Oil/Hept
Oil/Hept
Sample
Description
additive %
Solids, %
cm/50 cc
cm/50 cc
Before
After
Before
After
5A
Oil-in PP (3M)
27
7
80
85
3
10
0
3
5B
″
27
7
120
213
3
10
0
3
5C
″
27
20
120
450
3
10
0
3
5D
″
27
40
120
>5000
3
10
0
4
5E
″
27
2
120
125
3
10
0
1
5F
Oil-in PP (3M) 2X
27
7
295
510
3
10
0
2
5G
Oil-in PP (3M) + PEGML 200
27
7
120
300
3
9
0
1
5H
Oil-out PP (3M)
0
7
12
12
3
10
0
6-7
5I
″
0
20
12
20
3
10
0
6-7
5J
″
0
40
12
240
3
10
0
6-7
5K
″
0
2
12
12
3
8
0
4
5L
Oil-out PP (3M) + FC-13876
0
7
12
13
3
10
0
8
5M
Oil-out PP (3M) + PEGML 200
0
7
12
13
3
10
0
7-8
5N
Oil-out PP (3M) + PEGMS 400
0
5
12
15
3
10
0
8
5O
Oil-in PP + PEGML
37 + 3
7
25
47
0
10
0
2
200 melt
5P
Oil-in PP + PEGMS
27
5
125
155
3
10
0
2
400
5Q
TYVEK ™ (DuPont)
0
7
5
3
1
7
0
6
5R
EXXAIRE ™ (Exxon)
0
7
185
950
3
10
0
6-7
5S
SONTARA ™ (Dupont)
0
7
<1
<1
8
10
5
6-7
5T
Porous PTFE
0
7
5
4
4
10
0
8
(Tetratech)
5U
Oil-out PP +
0
7
12
15
3
10
0
B
DOS 3 before
urethane coating
5V
Oil-out PP +
0
7
12
15
3
10
0
8
DOS 3 in urethane
precursor coating
The above specification, examples and data provide a complete description of the manufacture and use of the composition of the invention. Since many embodiments of the invention can be made without departing from the spirit and scope of the invention, the invention resides in the claims hereinafter appended.
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Coated porous materials that exhibit air permeability and repellency to liquids having a surface tension at least equal to or greater than 20 dynes/cm which are suitable for making ileostomy vent filters, transdermal drug substrates, agricultural and medical apparel, as well as paint and chemical protective garments. The coating for the porous material is applied as a curable composition containing fluorocarbon urethane precursors which are cross-linked in situ.
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This invention relates to an adaptive brake system control.
BACKGROUND OF THE INVENTION
In a conventional hydraulic brake system, front to rear brake proportioning is typically fixed by the hydraulic design of the brakes and proportioning valves in the brake system.
More recently, there have been proposals for various drive-by-wire brake systems in which front to rear proportioning need not be fixed by system hydraulics and can be controlled instead by an electronic controller operating on one or more brake actuators. Such systems allow dynamic front to rear brake proportioning, that is, brake proportioning that is not fixed, but can be adjusted during vehicle driving and/or braking to achieve a desired result.
SUMMARY OF THE INVENTION
An adaptive brake system control in accordance with the present invention is characterized by the features specified in claim 1.
Advantageously, this invention provides a motor vehicle adaptive brake system control with dynamic front to rear brake proportioning.
According to one example of this invention, brake system control is implemented by an electronic controller that receives a brake command from a brake pedal and develops a front brake command. A rear brake command is developed through position control of rear brake actuators through a rear brake command table. The function of the rear brake command table and the rear brake command output in relation to the front brake command is the proportioning between the front and rear brakes. The front to rear brake proportioning may be made dependent on various factors including vehicle speed so that, during any given stop, the front to rear proportioning at different points during the stop vary in a desired manner. Thus, a given dynamic proportioning function can be programmed into the controller through the rear brake table in its relationship to the front brake command control to provide a programmed-in dynamic proportioning result.
In yet a further advantage according to this invention, during a braking maneuver, various vehicle parameters, including the vehicle wheel speeds, are monitored and the monitored information is used to adaptively update the rear brake command tables so that the rear brake command table achieves, in relation to the front brake control structure, a desired front to rear proportioning result. Thus, advantageously, this invention not only allows a desired dynamic proportioning control of the braking to be programmed into the braking controller, but adaptively updates the brake controller in response to actual vehicle performance to insure that the resulting brake response conforms to the response desired by the system designer.
Advantages gained by examples of this invention include the adaptive compensation of the brake control to various vehicle loading conditions, to tire wear and to tire type.
Advantageously, in an example according to this invention, an adaptive brake control method, for a motor vehicle with first and second front vehicle wheels and third and fourth rear vehicle wheels, is achieved according to the steps of: receiving an operator input brake command; responsive to a brake command function stored in memory and the operator input brake command, developing a rear brake position command; outputting the rear brake position command to a rear brake actuator; monitoring the first and second front wheel speeds and the third and fourth rear wheel speeds; responsive to the monitored first and second front wheel speeds and the monitored third and fourth rear wheel speeds, updating the brake command function stored in memory, wherein the brake position command table is adaptively updated and a front to rear brake proportioning of the vehicle is adaptively controlled to mimimize a difference between the front and rear wheel speeds during braking.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates, schematically, a vehicle with adaptive brake control according to this invention;
FIG. 2 illustrates schematically the flow of this invention;
FIG. 3 illustrates schematically the flow of this invention in braking mode;
FIG. 4 is an example graph of a rear brake command table; and
FIGS. 5A and 5B illustrate an example flow diagram implementing this invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, the example vehicle braking system illustrated includes left and right front driven wheels 10 and 12 and left and right rear non-driven wheels 14 and 16. The front and rear wheels 10, 12, 14 and 16 have respective hydraulic actuated brakes 18, 20, 34 and 36 actuated by hydraulic pressure generated via respective electrohydraulic actuators 22, 24 and 62 (for both rear brakes 34 and 36). Each of the hydraulic brakes 18, 20, 34 and 36 are further hydraulically coupled to a conventional master cylinder 26 through respective normally opened electromagnetic valves 28, 30 and 60. Actuators 22, 24, 62 include a working chamber hydraulically coupled to the wheel brakes 18, 20, 34 and 36 and the valves 28, 30 and 60. In the preferred form of the invention, the electrohydraulic actuators 22, 24 and 62 each take the form of a brushless dc motor driven actuator wherein a motor is operated to control a piston for regulating the braking pressure (the motor for actuator 62 drives two pistons in parallel, one for each rear brake 34, 36). The brake torque is established at each brake 18, 20, 34, 36 at a value proportional to the position of each actuator piston and is reflected through the torque and/or output of the respective motor. For example, the electrohydraulic brake actuators 22, 24, 62 may each take the general form of the electrohydraulic actuator as described in the U.S. Pat. No. RE 33,557, which issued Mar. 19, 1991, assigned to the assignee of this invention. With exception to the modifications discussed below, the actuators 22, 24 and 62 may be operated generally as described in U.S. patent application, Ser. No. 08/355,468, filed Dec. 14, 1994, now U.S. Pat. No. 5,558,409, assigned to the assignee of this invention, the disclosure of which is incorporated herein by reference.
The master cylinder 26 is operated by a conventional vehicle brake pedal 32 in response to the foot pressure applied by the vehicle operator.
While as illustrated in FIG. 1, the rear wheels are braked by electrohydraulic actuator 62, the rear wheels may alternatively be braked by means of a pair of electrically operated brakes 34 and 36. Such brakes 34 and 36 may each take the form of an electronically operated drum brake in which the braking torque is established by operation of a dc torque motor. One example of such a brake is illustrated in the U.S. Pat. No. 5,000,291, issued Mar. 19, 1991, assigned to the assignee of this invention.
The front and rear brakes 18, 20, 34 and 36 are operated to establish a desired braking condition by means of an electronic controller 38. In general, the electronic controller 38 senses a braking command input by the vehicle operator by sensing the state of a conventional brake switch 40 which provides a signal when the vehicle operator applies pressure to the brake pedal 32. When the brake switch input is sensed, the electronic controller 38 operates the electromagnetic valves 28, 30 and 60 to close off the hydraulic communication between the master cylinder and the electrohydraulic actuators 22 and 24. This effectively isolates the wheel brakes 18, 20, 34 and 36 from the master cylinder 26 such that the hydraulic pressures at the wheel brakes are controlled solely by means of the electrohydraulic actuators 22, 24 and 62. The degree of braking effort commanded by the vehicle operator is sensed by means of a pedal position sensor 41 and a pressure sensor 42 monitoring operator depression of pedal 32 and the hydraulic pressure output of master cylinder 26, respectively. As is well known, the hydraulic pressure output of the master cylinder 26 is directly proportional to the applied pressure to the brake pedal 32 controlling the position of the master cylinder 26 and the position output of sensor 41.
Both the pedal position and the pedal pressure may be used to determine the operator requested brake effort command. In response to the brake effort command, the electronic controller 38 provides for establishing a desired brake torque at each of the wheels 10, 12, 14 and 16 via the respective brakes 18, 20, 34 and 36 by commanding motor current to each actuator 22, 24 and 62 to establish the actuator position, and therefore the brake pressure, for each brake 18, 20, 34 and 36 at a desired level related to the brake effort command. The commands generated by electronic controller 38 implementing the adaptive brake control according to this invention are also responsive to the outputs of wheel speeds as measured by wheel speed sensors 48, 50, 52 and 54. The commands generated by electronic controller 38 may also be responsive to the output of throttle position sensor 84, which provides an output signal indicative of the position of engine throttle 82, controlled by accelerator pedal 80. The commands generated by electronic controller 38 may also be responsive to steering wheel angle sensor 88, which provides an output signal indicative of the angular displacement from straight ahead center of steering wheel 86.
The actuator position feedback provided by the actuators 22, 24 and 68 used in a standard commutation control to control the switching of the dc brushless motors provide closed-loop brake actuator position control in accordance with the like control described in the pending U.S. patent application, Ser. No. 08/355,468.
The electronic controller 38 has an internal microprocessor that runs a control routine stored in permanent memory to develop position commands for the front actuators 22, 24 and the rear actuator 62 to effect a desired adaptive front to rear brake proportioning according to this invention. The adaptive proportioning according to this invention results in the distribution of braking force between the front and rear wheels to match the normal (perpendicular to the road) forces on the front and rear wheels. The controller 38 achieves this control without the use of sensors to directly measure brake torque and normal force, implementing instead an advantageous use of wheel speed data.
More particularly, referring now also to FIG. 2, the controller 38 uses fie wheel speed data to adaptively control front to rear brake proportioning based on the assumption that two wheels, rotating at the tame speed on the same vehicle must, if they are slipping on the road surface, have the same mount of slip. To operate on this assumption according to this invention, the measured wheel speeds must be carefully normalized. Thus, in FIG. 2, the control of this invention, responsive to the system inputs, designated generally by block 100 to include all of the system inputs referred to herein, operates in two modes, non-braking mode 110, when the vehicle is not braking, and braking mode 112, when the vehicle is braking. A wheel speed normalization control 114 is run during the non-braking mode 110 and performs the normalization of the measured wheel speeds required to use the assumption that wheel speed information is representative of wheel slip.
More particularly, in the non-braking mode 110, the controller 38 continuously monitors and normalizes the wheel speed data to allow the front and rear wheel speed data to be compared. The normalization removes speed errors caused by tire pressure, tire wear, tire size and the tire style (including the presence of spare or mismatched tires). This calibration is done during periods of constant speed while the vehicle is traveling between predetermined minimum and maximum read speeds, i.e., between twenty and eighty miles per hour. A normalization factor for each wheel is established by dividing the sum of each individual wheel speed over a time period by the sum of all wheel speeds over the same time period. For example:
N.sub.i =ΣS.sub.i (t)/(Σ(S.sub.1 (t)+S.sub.2 (t)+S.sub.3 (t)+S.sub.4 (t))) for t=0 to T,
where T is the number of measurements summed and i equals 1, 2, 3, 4 for the left front right from, left rear and right rear wheels, respectively. In general, normalization of wheel speeds during non-braking vehicle operation for brake and/or traction control is known to those skilled in the art.
To avoid the effects of tire deformation, calibration of the normalization factors are performed only under ideal conditions. For example, the normalization does not take place if the brake switch is activated or if the vehicle is not traveling at a velocity constant within +/-Kvel, where Kvel is a predetermined constant. The normalization does not take place if the vehicle speed is not between a predetermined minimum and maximum, for example, 20 and 80 miles per hour. The normalization does not take place if the vehicle is in a turn that can induce the effects of vehicle lateral acceleration on the vehicle wheels. This can be determined by comparing the measured steering wheel angle to a calibratable limit, Kturn, or by detecting a difference between left and right wheel speeds of the undriven wheels greater than a predetermined threshold.
The normalization does not take place if any of the vehicle wheels are traveling over bumps that effect the wheel speed information. This can be determined by comparing, for each wheel, the present verses the immediately preceding wheel speed information to a calibratable threshold Kjitter*Vveh, where Kjitter is a constant or a table based value that increases with vehicle speed and Vveh is the vehicle velocity. The normalization does not take place if the vehicle is experiencing lateral acceleration that can effect wheel speed information. This is detected by determining the difference between the sum of the two left vehicle wheels and the sum of the two right vehicle wheels and comparing that difference to a threshold Klftrt*Vveh, where Klftrt is a predetermined constant. The normalization does not take place if the vehicle is experiencing longitudinal acceleration that can affect wheel speed information. This is detected by determining the difference between the sum of the front wheel speeds and the rear wheel speeds and comparing that difference to a threshold Kfrntrr*Vveh, where Kfrntrr is a predetermined constant. The normalization does not take place if the vehicle is traveling at a velocity near the upper velocity limit and accelerating or if the vehicle is traveling at a velocity near the lower velocity limit and decelerating. This is detected by comparing the throttle position to Kthrthi*Vveh and Kthrtlo*Vveh, respectively, where Kthrthi and Kthrtlo are predetermined constants. Also, the normalization does not take place if the vehicle traction control (to limit wheel slip during vehicle acceleration) or anti-lock brake control is active.
After the calibration is complete, the change in the normalization factor is compared to a maximum limit. If the change in the normalization factor exceeds the maximum limit, the new normalization factor is limited to the previous normalization factor plus or minus the maximum limit. This prevents the normalization factor from being changed too quickly by invalid data. After the normalization factor is determined, the process is repeated as long as the vehicle is in non-braking mode.
In addition to the assumption that the wheel speed velocity for front and rear wheels is the same for a given amount of slip, this invention also operates on the assumption that the coefficient of friction between front wheels and the road and the rear wheels and the road are the same. Since not all road conditions meet this criteria, the adaptive update of the brake control is performed only during select driving and road conditions, as will be explained below. When the vehicle is in the select driving and road conditions, the assumption that the coefficient of friction between each wheel and the road is the same as between the other wheels and the road is valid and leads to the conclusion that the amount of braking force at each wheel is directly proportional to the normal force between each wheel and the road. Stated in another way, with valid wheel speeds provided by the normalization routine, and with the select driving and road conditions, by forcing all of the wheel speeds to be identical during braking, the braking torque is proportioned so that each wheel is providing braking torque based on the normal force between that wheel and the road. In an example implementation, the system is calibrated to assure that the rear wheel speeds are slightly higher than the front wheel speeds.
Thus, in the braking mode 112, this invention uses a selection criteria and wheel speed information to adaptively proportion (block 116) the brake force distribution between the front and rear wheels so that brake force is proportioned according to the load on the vehicle wheels and so that wheel speeds are forced to be substantially identical, providing the maximum efficient brake force distribution.
Referring now to FIG. 3, the general operation of the braking mode 112 is shown. The braking mode 112 is responsive to the various system inputs discussed herein, including the wheel velocities, and develops a from brake command at block 130 responsive to the various inputs. An example position control of the front brakes and development of the commands thereof is set forth in pending U.S. patent application Ser. No. 08/355,468, filed Dec. 14, 1994, now U.S. Pat. No. 5,558,409. The rear brakes are operated responsive to a pedal command, PC, determined responsive to brake pedal travel and master cylinder pressure in the manner described in the above-mentioned copending patent application Ser. No. 08/355,468.
The pedal command is input to the rear motor position command table 132, which develops a rear motor position command used to control the rear brake actuator. The rear motor position command table is stored in EEPROM according to an initial table stored in ROM designed to provide, together with the front brake command control 130, the desired front to rear brake proportioning. The rear motor position table comprises, indexed in consecutive table positions, a series of motor position commands. The position commands are calibrated from a desired brake torque response through simple experimentation in a prototype vehicle in a manner within the level of those skilled in the an given the information within this specification. The shape of the calibrated table defines the predetermined table shape function used during the adaptive updating of the table according to this invention. During vehicle operations, the rear motor position command table is transferred from EEPROM to active RAM and is adaptively updated so that actual vehicle performance achieves the front to rear braking desired by the system designer. Thus, in addition to determining a rear motor position command at block 132, the rear brake control includes block 134, which, responsive to the various system inputs, determines if the vehicle operating conditions meet the criteria for adaptive modification to the rear motor position command table.
If the update criteria is passed at block 134, the rear brake control adaptively updates the rear motor position command table at block 136 to achieve the desired results of equal wheel speeds and equal slip of all vehicle wheels during non-ABS vehicle braking. Referring to FIG. 4, trace 150 illustrates an example table position versus motor position function of the rear brake position command table stored in ROM memory. Traces 152 and 154 illustrate possible adapted table position versus motor position functions laterally displaced from table 150 in response to the adaptive control according to this invention. As can be seen the curve fit operation of this invention ensures that traces 152 and 154 have substantially the same shape as trace 150.
The control according to this invention uses conditional normalization and acquisition steps to adaptively update the table that generates the front to rear proportioning commands. The control further uses predetermined brake table shaping to accelerate the correction of all table positions during adaptive updates and to guard against non-linearities and invalid table data. As will be appreciated by those skilled in the art having read this specification, variations in vehicle loading, such as due to changes in the number of vehicle passengers or the amount of cargo in the vehicle, can result in variations in the normal force loading of the vehicle wheels. By adaptively updating the rear brake command table responsive to the actual operating conditions, this invention adaptively controls the brakes to maintain the desired front to rear proportioning despite variations in loading of the individual vehicle wheels.
Referring now to FIGS. 5A and 5B, the example brake control according to this invention shown uses the normalized wheel speeds, determined during the non-braking mode and as further normalized responsive to vehicle load shift during braking as described in copending U.S. patent application, 08/513,192 filed concurrently with this invention, assigned to the assignee of this invention and having a disclosure incorporated herein by reference. The routine begins when the vehicle ignition is powered on and moves to block 202 where the system is initialized according to known techniques, the rear brake tables are loaded from EEPROM into RAM and the delta speed error dead band, DB, is increased by a constant Kfade. The delta speed error dead band, DB, is used to compensate for the variation of the coefficient of friction of the brake lining with brake lining temperature. The routine estimates the brake lining heat index by adding the term Kfade to DB.
Not shown in FIGS. 5A and 5B are the steps of determining the front brake commands and the pedal command PC. However, any suitable front brake control may be implemented, with the understanding that the function of the rear brake command table, in relation to the front brake control and command PC that is implemented, determines the default front to rear brake proportioning. A suitable example front brake control is set forth in the above mentioned pending U.S. patent application, Ser. No. 08/355,468.
At block 206, the routine checks whether the vehicle ignition has been powered off. If the vehicle ignition has been powered off, the routine moves to block 208, there the rear brake tables in the EEPROM are updated. The tables in the EEPROM are updated as follows. Each rear brake table value in RAM is compared to the previously stored value in EEPROM, values that are less than the corresponding EEPROM table values are stored into the EEPROM replacing the previous EEPROM table values, values that are greater than the corresponding EEPROM values are averaged with the corresponding EEPROM values and the result replaces the previous EEPROM value as the new EEPROM value. By averaging table values greater than the corresponding EEPROM values with the corresponding EEPROM values, the routine prevents brake fade or temporary heavy vehicle loading from creating a rear bias condition at the next vehicle start-up.
If, at block 206, the ignition is not off, then the routine moves to block 209 where various vehicle parameter data is input from the controller input circuitry or read from memory. This data includes the normalized wheel speeds of the four wheels, the brake pedal position, the brake pedal pressure, the steering wheel angle, the brake actuator motor positions, the vehicle deceleration rate and the pedal command, PC.
At block 210, the routine checks the signal from the brake pedal switch to determine if the vehicle operator is commanding a brake command. If there is no brake command, the routine proceeds through a series of operations that normalize the measured wheel speeds (block 211). This normalization of wheel speeds is done in the manner described above in reference to the non-braking mode.
If there is a brake pedal command at block 210, the routine moves to block 212 if the vehicle has rear drum brakes. At block 212, the pedal command, PC, for rear drum brakes is adjusted based on a velocity dependent compliance variation according to:
PC=PC+((Vveh*Kbrkfctr)*Kfluidvolume),
where Vveh is the vehicle velocity, Kbrkfctr is a constant for the drum brake and Kfluidvolume is a constant that represents the fluid volume of the particular drum brake used. The velocity dependent compliance variation is disclosed in Research Disclosure, No. 36801, published Dec. 10, 1994.
Also at block 212, the routine begins determining the motor position that achieves the required rear proportional brake line pressures by interpolating the rear brake table. The table position, Tpos, is obtained by dividing the pedal command by the factor Ktpos, which yields a number between zero and the highest table position at full pedal command. The relative percent between table positions is calculated by dividing the remainder of the equation PC/Ktpos by Ktpos to determine Rperc. The rear motor position command is formed by looking up from the rear brake table the motor position located at Tpos, Mpos(Tpos). Also the motor position Mpos(Tpos+1) is retrieved. The routine determines the difference between Mpos(Tpos+1) and Mpos(Tpos), multiplies that difference by Rperc and adds the result to Mpos(Tpos) to determine the position command MPOS.
At block 214, the routine determines, in a manner well known to those skilled in the art, if any of the four vehicle wheels are in an anti-lock brake (ABS) mode. In general, a wheel is controlled to be in ABS mode if its wheel slip is greater than a predetermined threshold. If none of the wheels are in ABS mode, then the routine continues to block 226. If at block 214 any of the wheels are in ABS mode, the routine continues to block 216 where it determines if either of the front wheels is in ABS mode. If at block 216 either of the front wheels is in ABS mode, the routine continues to block 224 where an ABS control routine of any suitable type known to those skilled in the art for performing anti-lock brake control of vehicle wheels is performed. If at block 216 neither of the front wheels is in ABS, then the routine continues to block 218 where the value Rabs, which tracks rear ABS only events, is incremented. At block 220, Rabs is compared to the predetermined constant Krabs and if Rabs is not greater than Krabs, then the routine continues to block 224. If at block 220, Rabs is greater than Krabs, it indicates that the rear brakes are entering ABS often and the rear brake tables are too "aggressive." In this event, the routine moves to block 222 where the rear tables are reinitiated from the ROM and sets the auto-calibration flag to false.
A constant Kdb is predetermined so that when DB equals Kdb, the brakes are thought to be operating at the nominal temperature. At block 226, the routine compares DB to Kdb and continues to block 230 if DB is less than or equal to Kdb. If, at block 226, Kdb is not less than or equal to Kdb, then the routine moves to block 228 where the product of Tpos (determined at block 212) multiplied by a predetermined heat nominalizing constant, Kheat, is subtracted from DB. This decreases DB back to the nominal value in steps with each brake apply.
At block 230, the routine begins a series of tests to determine if the rear brake table is to be adaptively modified. The rear brake table is adaptively modified only under select brake conditions. If the braking is not in the select conditions, the rear brake table adaptive modification is bypassed and the routine continues straight to the proportional/derivative control loop at block 362. At block 230, the routine checks the an auto-calibration flag, continues to block 362 if the auto-calibration flag is set to false and continues to block 232 if the auto-calibration flag is set to true. The auto-calibration flag is set to true when a successful wheel speed normalization calibration has occurred and is otherwise set to false.
At block 232 the normalized wheel speeds of each of the four vehicle wheels are updated responsive to the effects of vehicle weight shift during braking according to the method described in the copending application, 08/513,192.
Block 234 determines if the vehicle speed is in a predetermined range, for example, between 12 and 80 miles per hour, and, if not, continues to block 362. At block 236, the routine compares Tpos to the value of Tpos during the preceding loop of the control routine. If the values are not the same, the routine continues to block 238 where the values Wadj1 and Wadj2 are set to zero and then continues to block 362.
If at block 236, Tpos is the same as Tpos during the preceding loop of the routine, the routine moves to block 240 where it compares the steering wheel angle to a predetermined threshold, Kturn. If the steering angle is greater than Kturn, the routine moves to block 244 where it determines if the value Vdelta (computed at block 274) is negative to test for rear brake bias. Since the radius of travel around the center of a rum is smaller for the rear wheels than for the front wheels, rear brake torque is reduced if Vdelta is positive. Thus, if at block 244 Vdelta is negative, the routine continues to block 362. If at block 244, Vdelta is not negative, the routine continues to block 248, where the rear motor position command MPOS is reduced according to:
MPOS=MPOS-((Ksteer)*(Asteer*Vveh)),
where Ksteer is a constant representing a motor position reduction of the rear actuators as a function of steering angle and vehicle speed and Asteer is the steering wheel angle. This reduction in the rear motor position command leads to an elimination of steering-induced rear bias conditions. From block 248, the routine moves to block 362.
From block 240, if the steering wheel angle is not greater than Kturn, then the routine moves to block 252, where each of the wheel speeds is summed for three consecutive loops of the routine to determine Slfspd, Srfspd, Slrspd and Srrspd, which are the wheel speed sums for the left front, right front, left rear and right rear wheels, respectively. The routine then moves to block 254 where, for each wheel, the difference between the immediately preceding wheel speed sum and the current wheel speed sum is compared to the product of Kjitter*Vveh, where Kjitter is a constant. Block 254 tests to determine if the vehicle is on a bumpy road in which the suspension movement of the wheels interferes with the wheel speed information. The test at block 254 may also be responsive to deformable roads, such as gravel, sand, snow and puddles and to very low coefficient of friction surfaces such as ice. These road surface types also might interfere with wheel speed information for purposes of rear brake table calibration. If at block 254, for any of the vehicle wheels, the difference between the immediately preceding wheel speed sum and the current wheel speed sum is greater than the product Kjitter*Vveh, the routine continues to block 362, otherwise, the routine continues to block 258,
At block 258, the routine compares the sum of the left front and rear wheel speed sums to the sum of the right front and rear wheels speed sums and, if the difference between the two sums is greater than a product Klftrt*Vveh, where Klftrt is a constant, then the routine continues to block 362. Otherwise the routine continues to block 262. Step 258 tests whether the vehicle is undergoing lateral acceleration causing rolling radius change of the right and/or left vehicle wheels. Step 258 might also detect whether the vehicle is on a split coefficient of friction road surface, that is whether the left vehicle wheels are on one type of road surface while the right vehicle wheels are on another, which may interfere with wheel speed information for purposes of rear brake table calibration.
Step 262 compares the sum of the front wheel speed sums to the sum of the rear wheel speed sums and, if the difference between the two sums is greater than a product Kfrntrr*Vveh, where Kfrntrr is a constant, the routine continues to block 362. Otherwise the routine continues to block 266. This step tests whether the vehicle is experiencing longitudinal acceleration that causes a rolling radius change of front and/or rear vehicle wheels. Block 262 may also test whether the vehicle is experiencing a change of road surface, for example, from a high coefficient of friction road surface to a low coefficient of friction surface, such as may occur when the vehicle enters bumps, gravel, sand, snow, ice and puddles, which may also interfere with wheel speed information for purposes of updating the brake command table.
Beginning at block 270, the routine determines if the rear brake table is to be modified. In general the modification of the rear brake table occurs if wheel slip during braking is higher than the dead band DB and higher than an adaptive dead band DDB. At block 270, the routine determines a value Vdelta according to:
Vdelta=(Slfspd+Srfspd)-(Slrspd+Srrspd).
Block 274 compares Vdelta to DB and if Vdelta is not greater than DB, the routine continues to block 362. If at block 274, Vdelta is greater than DB, the routine moves to block 278, where it determines the wheel speed noise adaptive dead band, DDB, according to:
DDB=DB+(Kdb*Tpos),
where Kdb is a predetermined constant. The wheel speed noise adaptive dead band increases with higher vehicle decelerations. Block 282 compares Vdelta to the adaptive dead band DBB and if Vdelta is not greater than DBB, the routine continues to block 362. If at block 282 Vdelta is greater than DDB, the routine continues to block 286 where the adaptive update of the rear brake table begins.
Blocks 286 and 290 limit Vdelta, for purposes of table adaptive updating, to a predetermined value Kmaxdb. If at block 286 Vdelta is not greater than Kmaxdb, then the routine moves to block 294. If at block 286 Vdelta is greater than Kmaxdb, the routine moves to block 290 where Vdelta is limited to Kmaxdb.
Block 294 updates two accumulators Wadj1 and Wadj2 according to:
Wadj1=Vdelta*Rperc+Wadj1, and
Wadj2=Vdelta*(1-Rperc)+Wadj2.
The accumulators Wadj1 and Wadj2 control updating of the rear brake table in RAM. At block 298 if Wadj1 is not greater than or equal to 1, the update of the RAM table value Mpos(Tpos) is bypassed and the routine continues to block 306. If at block 298, Wadj1 is greater than or equal to 1 the routine continues to block 302 where the RAM table value Mpos(Tpos) is updated according to:
Mpos(Tpos)=Mpos(Tpos)+Wadj1.
At block 306, if Wadj2 is not greater than or equal to 1, the update of the RAM table value Mpos(Tpos+1) is bypassed and the routine continues to block 314. If at block 306, Wadj2 is greater than or equal to 1, the routine continues to block 310, where the RAM table value Mpos(Tpos+1) is updated according to:
Mpos(Tpos+1)=Mpos(Tpos+1)+Wadj2.
Beginning at block 314, the routine starts updating the remainder of the RAM table and tests the transfer function of the table versus a nominal table function, Knom, stored in memory. In updating the remainder of the table, the new motor position commands Mpos(Tpos) and Mpos(Tpos+1) are used as a point of reference and the nominal table function is used as a curve to fit or adjust the remainder of the table to the motor position commands that are the point of reference. The transfer function of Knom is that of either drum brakes or disc brakes, whichever is used for the rear brakes. The shape of a pressure versus position curve for a typical drum brake has the lowest pressure increase per position increase at the beginning of the curve. For example a change of one count at table position ten may be equivalent to a change of forty counts at table position one. The shape of pressure versus position for a typical disc brake is more aggressive than the typical drum brake. The table shaping starts at the table position Tpos+1 and compares the difference between each pair of consecutive table values to the nominal table Kcrv. Block 314 begins this by performing the comparison:
Mpos(Tpos+1)-Mpos(Tpos)>Knom(Tpos)*Kcrv?
where Kcrv is a predetermined constant. If the test not true at block 314, then the table does not need further adjustment at the position Tpos and the routine moves to block 322. If the test is true at block 314, the routine moves to block 318 where the RAM table is adjusted at position Tpos according to:
Mpos(Tpos)=Mpos(Tpos+1)-Knom(Tpos)*Kcrv.
Block 322 then subtracts one from Tpos and block 326 then returns the routine to block 314 if Tpos does not equal zero so that the remainder of the table below the original Tpos is updated.
Starting at block 330, the remainder of the table above the original Tpos is updated. Block 330 determines values Sep and Reasn according to:
Sep=Mpos(Tpos)+Knom(Tpos), and
Reasn=Mpos(Tpos)+Knom(Tpos)*Kreasn,
where Kreasn is a predetermined constant. Block 334 compares Tpos to Klast, which is the highest value Tpos can be (the highest table position). If Tpos is greater than or equal to Klast, then the routine continues to block 358. Otherwise the routine continues to block 338 where the value Sep is compared to Mpos(Tpos+1). If at block 338, Sep is greater than Mpos(Tpos+1), then block 342 sets Mpos(Tpos+1) to Sep. The routine then continues to block 346 where Mpos(Tpos+1) is compared to the value Reasn. If Mpos(Tpos+1) is greater than Reasn, then block 350 sets Mpos(Tpos+1) equal to Reasn. Block 354 then increments Tpos and the routine returns to block 330. The routine loops through blocks 330 to 354 until the entire table is updated, at which time the test at block 334 will be passed and the routine continues to block 358.
At block 358, the routine sets the table position zero, Mpos(0), which is the adaptive motor position offset. Block 358 computes Mpos(0) according to:
Mpos(0)=Mpos(1)*Konset,
where Konset is a value between zero and one set so that Mpos(0) is the approximate actuator position at which the application of brake torque begins.
Blocks 362 represents a standard proportional and derivative control loop of a type known to those skilled in the art for control of the actuator motor and block 366 outputs the motor current command to bring the actuator motor to the commanded position.
While the above described example uses three brake actuators to control the braking, one for each front wheel and one that simultaneously controls braking for both rear wheels, this invention may also be implemented in a vehicle with four brake actuators, one for controlling the brake of each wheel. The operation of the four brake actuator braking system, according to the invention, operates as described above with the exception that instead of a single command being developed for the rear wheels responsive to the sum of the rear wheel speed, a brake command is developed for each rear wheel responsive to that rear wheel's speeds and the average of the front wheel speeds. Those skilled in the art can readily adapt the above example described with respect to FIGS. 1-5B, according to the information provided herein, to implement the four brake actuator example of this invention. If four brake actuators are implemented, the control of U.S. patent application, Ser. No. 08/195,225, now U.S. Pat. No. 5,539,641, assigned to the assignee of this invention, may be used.
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An adaptive brake control method, for a motor vehicle with first and second front vehicle wheels and third and fourth rear vehicle wheels, is achieved according to the steps of: receiving an operator input brake command; responsive to a brake command function stored in memory and the operator input brake command, developing a rear brake position command; outputting the rear brake position command to a rear brake actuator; monitoring the first and second front wheel speeds and the third and fourth rear wheel speeds; responsive to the monitored first and second front wheel speeds and the monitored third and fourth rear wheel speeds, updating the brake command function stored in memory, wherein the brake position command table is adaptively updated and a front to rear brake proportioning of the vehicle is adaptively controlled to minimize a difference between the front and rear wheel speeds during braking.
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FIELD OF THE INVENTION
[0001] The invention relates to mail sorting machines and processes of the type currently carried out by the U.S. Postal Service (USPS).
BACKGROUND OF THE INVENTION
[0002] Barnum et al. U.S. Pat. No. 6,671,577, Dec. 30, 2003, describes a system and method for directly connecting an ISS advanced facer canceler system (IAFCS) to a DBCS/OSS. As noted in that patent, the contents of which are incorporated by reference herein, conventional mail systems now in use by the USPS process stamped mail through a plurality of separate machines, including an advanced facer canceler system/input subsystem (IAFCS), an optical character reader (OCR) machine, and a delivery bar code sorter/output subsystem (DBCS/OSS). IAFCS places incoming mail into a single file line in a pinch belt, checks for appropriate postage on mail, cancels the postage, and stacks the mail in bins. IAFCS positions the mail upright between a pair of pinch belts with either the stamp leading and the address on the front side or the stamp trailing and the address on the back side. IAFCS obtains a picture image of the stamped side of each piece of mail and prints a mail identifier (ID tag) on each mail piece on the side opposite the stamped side that is stored along with the image. The image is used to determine mail type such as printed address and script address. After canceling the postage, IAFCS sorts the mail into bins based on mail type. Each mail type has two bins, one for mail with the stamp leading and one for mail with the stamp trailing The machines that next process the mail, such as DBCS/OSS, require that all the mail be positioned with the stamp leading. An operator takes the stamp trailing mail from a bin of the IAFCS and places it in a stamp leading position to combine with the stamp leading mail before feeding into the DBCS/OSS. Based on the mail type, the operator then moves the mail to the next processing point. Mail that has been imprinted by the IAFCS with a UV bar code, ID tag, is taken directly to the DBCS/OSS. DBCS/OSS prints a bar code onto the mail by querying the IPSS system for the result of computer OCR or operator video coding associated with the ID tag of the mail. DBCS/OSS sorts the mail into a plurality of stackers based on the bar code data which reflects the mail destination.
[0003] A processing method according to the '577 patent processes mail through a postage verifier having an optical character reader, mail interface system, and a mail sorter. The mail interface system includes an upward module carrying mail up to an overhead transport positioned at a height above an output of the postage verifier, and a downward module carrying mail down from the overhead transport to the mail sorter. The method includes vearifying and canceling postage, positioning mail pieces in a same configuration in a single file line, directing mail pieces up the upward module, directing mail pieces through the overhead transport, directing mail pieces down the downward module to a mail sorter, and sorting the mail based on destination. The interface module referred to directly connects the IAFCS machine to the DBCS/OSS sorter, eliminating the need for manual transfer of mail between these machines.
[0004] Difficulties remain notwithstanding the potential improvement such a Direct Connect between the IAFCS machine and the sorter could provide. One such problem arises in connection with FIM (facing identification mark) mail. Facing identification marks are ⅝ inch tall vertical bars beginning at the top of the envelope near the stamp. There are 4 types of FIM:
[0005] FIM A: Courtesy reply and metered reply, Postnet bar code required
[0006] FIM B: Business reply mail, Postnet bar code not required
[0007] FIM C: Business reply mail, Postnet bar code required
[0008] FIM D: Non fluorescent IBI and PC postage, Postnet bar code not required
[0000] The most common usage is for “remittance” mail, FIM A and C that consists of bills being paid by customers of a utility company, for example.
[0009] Currently, FIM A and C are detected on the IAFCS and sorted out for special handling to reserved bins on the IAFCS. FIM A and C mail from multiple AFCS machines within a processing and distribution center, P&DC, is collected and funneled to a single DBCS machine for sorting due to the time critical nature of remittance mail. If Direct Connect is implemented and the FIM mail is passed on to the DBCS/OSS and not intercepted at the IAFCS, an additional processing step is added with respect to the existing method and a corresponding undesirable delay in processing of the FIM mail is incurred. If the FIM is pulled out at the IAFCS, this causes a loss of as much as 25% of the mail from the IAFCS machines. If the Direct Connect of the '577 patent is implemented under these circumstances, the DBCS/OSS sorting machine linked to the IAFCS machine becomes “starved”, that is, does not receive enough mail from the IAFCS machine to operate efficiently The present invention addresses this problem and opens up new sorting possibilities by providing a sorting machine that is in effect several sorting machines with the capability of passing mail to be sorted between them automatically. Consolidation of inputs from multiple front ends eliminates the need for secondary sorting operations to alleviate partial trays of mail.
[0010] Edmonds U.S. Patent Publication 20030208298, Nov. 6, 2003, describes a method and system for single pass letter and flat processing. As part of the process, the '298 publication notes that use of two interconnected OCR sorting machines expands the capacity of such machines over the two machines used separately. However, this publication provides no specific guidance as to how such capability should be implemented.
SUMMARY OF THE INVENTION
[0011] The present invention provides a sorting system using multiple sorters operating as part of a single, multi-sorting machine unified system or “supercell”. A sorting system according to the invention includes a plurality of input sections capable of operating in parallel, each including a feeder that takes in mail pieces one at a time and a scanner that scans each mail piece for destination indicia, a plurality of stackers each comprising at least one row of pockets, a control system that determines a destination pocket in the stacker for each mail piece based on a predetermined sort scheme and the destination indicia, and a routing system effective to route mail in accordance with the sort scheme from any input section to any pocket of a stacker. For purposes of the invention, “destination indicia” refers to an ID tag which is associated with stored address information, a bar code which gives the information, or a written address read using OCR.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] In the accompanying drawings, where like numerals denote like elements and letters (A, B, C, etc.) denote multiples of a component:
[0013] FIG. 1 is a perspective view of a known mail sorting machine;
[0014] FIG. 2 is a schematic diagram of a mail sorting machine according to the invention;
[0015] FIG. 3 is a three-dimensional representation of the machine of FIG. 2 ;
[0016] FIG. 4 is a plan view of the machine of FIG. 2 ;
[0017] FIG. 5 is a schematic diagram of a (2:4) merge used in the invention;
[0018] FIG. 6 is a schematic diagram of four (2:1) merges used in the invention;
[0019] FIG. 7 is a schematic diagram of a control system for the machine of the invention as shown in FIGS. 2-6 .
DETAILED DESCRIPTION
[0020] In a typical postal sorting machine as shown in FIG. 1 , the machine 10 includes a feeder/singulator 12 where an unordered stack 14 of mail pieces are loaded for sorting. Feeder 12 singulates and transfers or conveys the mail pieces to a scanner 18 such as a bar code scanner or an optical character recognition (OCR) apparatus. Scanner 18 reads destination information from the mail pieces and transmits the information to a control computer which stores the destination information and identifies the bin 22 where the mail piece is to be directed. One or more conveyors 16 convey the mail pieces to a plurality of diverters in a stacker section 24 which contains bins 22 . This type of sorting machine is well known in the art and comes in a variety of types, such as Delivery Bar Code Sorter (DBCS) and DIOSS. A DIOSS machine is a Delivery bar code sorter (DBCS) with an optical character reader Input/Output SubSystem (IOSS). The present invention involves physically separating the stacker 24 of each sorter from its upstream components, referred to herein as an input section that includes at least feeder 12 and scanner 18 .
[0021] The present invention exploits an aspect of the existing multi-level stacker designs in that any single level is capable of sorting mail at a rate equal to the feed rate of the front end. Thus, a stacker line with four stacker levels is theoretically capable of sorting mail at four times the rate of the feeder of an OSS or DIOSS front-end with randomly distributed mail. Statistically, a four times advantage is not achievable due to normal distributions, but a two times advantage is.
[0022] Referring to FIGS. 2, 3 and 4 , a mail sorting system 30 according to the invention receives mail from several (e.g. 2 to 4) IAFCS machines 31 that operate in parallel on incoming collection mail. Each IAFCS 31 is an Integrated Automated Facer-canceler System of a type now in use by the U.S. Postal Service that culls, faces, cancels, prints an ID tag and lifts a video image of the mail. Output from these machines 31 is transported to an associated input section 32 . Each input section 32 preferably includes both an OSS 33 and a DIOSS 34 which operate at the same time. OSS 33 receives canceled mail from IAFCS 31 either by means of a direct conveyor connection as described in Barnum et al. U.S. Pat. No. 6,671,577, Dec. 30, 2003, the contents of which are incorporated by reference herein, or by manual loading of an associated feeder. OSS 33 reads an ID tag put on by IAFCS 31 and sprays the corresponding Postnet bar code onto each mail piece, which is then sorted according to the sort scheme as explained further below. DIOSS 34 receives mail that does not require cancellation, primarily metered and permit mail, through its feeder 36 . DIOSS 34 prints an ID tag on each mail piece and, if resolved by the online encoding system, prints a Postnet bar code on the mail piece. The destination for each mail piece leaving each input section 32 is provided to a computerized control system 37 .
[0023] Mail from either source exits input section 32 and enters a routing section 40 that is interposed between input sections 32 and a series of stackers 41 . The specific design of routing section 40 will vary to some extent depending on the number of input sections and stackers associated with it. In this example, eight input machines 33 , 34 are linked to four 254 pocket stacker lines each having four rows of pockets at different elevations, but the number of components on each side of routing section 40 does not necessarily have to be 2:1 as discussed further below. Control system 37 operates the diverts of routing section 40 in a manner effective to direct each mail piece to any one of the stackers 41 , depending on the sort scheme.
[0024] While a variety of vertical and horizontal conveyor systems are known in the art, to create routing system 40 successfully, certain principles should be observed. First, the average volume of mail on any one section of transport cannot exceed the average output of one DIOSS or OSS input, assuming a random distribution at input. This may require adjustment of the pinch belt transport speeds, for example, using a faster belt speed at the takeaway portion of a merge. Second, mail held in pinch belts vertical to the earth may be turned or diverted along a horizontal plane, whereas this is difficult to do with mail held horizontally. Third, mail held in pinch belts horizontal to the earth may be turned or diverted in a vertical direction, i.e. can readily change elevation. The following description of routing section 40 illustrates these principles.
[0025] Mail entering routing section 40 from one of the input sections 32 first enters a 2 to 4 (2:4) merge section 42 . FIG. 5 illustrates one of the (2:4) merges 42 . Mail from a first OSS 33 travels along a vertical pinch belt conveyor to a first vertical divert 51 A where it is routed either straight ahead to a first merge 52 A or diverted to a second merge 52 B, depending on the ultimate destination. A vertical divert for purposes of the invention is one that diverts the mail while it is in a vertical position, and a horizontal divert is one which diverts the mail while the mail is in a horizontal position.
[0026] Mail from a first DIOSS 34 travels along a vertical belt conveyor to a divert 51 B where it is routed either straight ahead to second merge 52 B or diverted to first merge 52 A, again depending on the ultimate destination. For this purpose, although it could be avoided by designing OSS 33 and DIOSS 34 pairs at different elevations, the mail pieces pass through an intersection 53 where the conveyor paths pass through one another. For this purpose, (2:4) merges 42 are preferably each provided with input buffers 36 A, 36 B, which may for example be a feeder capable of holding 1 to 3 mail pieces in a vertical stack, taking them in on an input side and ejecting them on a output side after a short delay in first-in, first-out order. Buffers 36 A, 36 B are controlled as described hereafter to ensure that collisions between mail pieces passing through intersection 53 are avoided and each mail piece is diverted to its correct destination. Diverts 51 and merges 52 may be of types known in the mail sorting art. Shifting wedge-type diverts 51 may be used.
[0027] Mail conveyed from each merge 52 A, 52 B enters a pair of twist sections 56 A, 56 B wherein the belt path changes from vertical to horizontal as illustrated in the three-dimensional FIG. 3 . Twist sections as described herein are pinch (dual) belt conveyors wherein the orientation of the belts gradually changes due to the layout of the supporting rollers as the belts move along. Once horizontal, the mail stream from merge 52 A is taken to a different (in this case, higher) elevation than the mail stream from merge 52 B. A pair of horizontal diverts 57 A, 57 B then further divide the mail streams from twist sections 56 A, 56 B into four mail streams carried by horizontal pinch belt conveyors 58 A 1 , 58 A 2 , 58 B 1 and 58 B 2 , each at a different elevation. Conveyors 58 A 1 , A 2 , B 1 , B 2 then each enter a second twist section 59 wherein each conveyor assumes a vertical orientation.
[0028] In the embodiment shown, the inputs for the entire system 30 are divided into two sections 59 A, 59 B each receiving input from 2 OSS and 2 DIOSS machines. Sections 59 A, 59 B each have two 2:4 merges 42 A, 42 B and 42 C, 42 D which are essentially identical as shown in FIGS. 2-4 . The mail streams from left and right merges 42 A, 42 B and 42 C, 42 D must next be merged such that all mail from any one of the OSS or DIOSS machines in that section 59 A or 59 B intended for a specific sorter 41 A-D is brought together. Four (2:1) vertical merges 60 A- 60 D per section are provided for this purpose as shown in FIGS. 4 and 6 .
[0029] Each (2:1) merge section 60 A- 60 D receives one mail stream from section 42 A and a matching mail stream merge 42 B destined for the same stacker 41 . For this purpose, each merge 60 includes a pair of buffers 61 A- 61 D which feed mail pieces to path merges 62 A- 62 D, respectively. The conveyors leading away from path merges 62 then comprise a 4-level vertical transport section 63 of the routing system. In transport section 63 , mail pieces from each section 59 A, 59 B destined for the same stacker 41 are brought together at four (2:4) merges 71 A-D. This requires, in the case of mail pieces needing to cross the system from one side to the other, relatively long lateral conveyor spans 66 that are spaced apart vertically as shown in FIG. 3 . For this purpose, “crossing the system” means, for example, a mail piece entering from leftmost input section 32 that must be routed to rightmost stacker 41 .
[0030] Merges 71 A-D may be functionally the same as merges (2:4) merges 42 shown in FIG. 5 , but with differences in the layout of the conveyor pathways as shown in FIG. 3 . The output from merges 71 A-D is at four different elevations corresponding to each level of the associated stacker 41 A- 41 D. Preferably, each (2:4) merge 71 A- 71 D has associated buffers 72 A, 72 B capable of holding from 1 to 3 mail pieces at a time. Buffers 72 are operated by control system 37 to ensure that jams do not occur at (2:4) merges 71 A- 71 D.
[0031] Mail entering one of stackers 41 A-D enters at one of the four levels and is sorted to the pocket assigned by the sort scheme. The system of the invention is intended for use at postal P&DC's for sorting according to high level sort schemes, e.g. by 3 or 5 digit zip codes. However, with a larger number of pockets available, more refined sort schemes become possible wherein fewer sorts to the 3-digit level need to be made. As such, mail sorted using the system of the invention is well suited for use with a single pass sorting system that sorts to carrier sequence order, such as the one disclosed in Pippin et al. U.S. Patent Application 20030038065, published Feb. 27, 2003, the contents of which are incorporated by reference herein.
[0032] FIM mail from all eight input machines is preferably funneled to one stacker or stacker row(s), where some of the pockets are assigned to specific high volume FIM recipients, some national and some local. As a result, FIM mail is handled in a manner which causes no delay in operations and does not “starve” a sorter directly connected to an IAFCS machine, as may happen in the system described Barnum et al. U.S. Pat. No. 6,671,577.
[0033] Stackers 41 may be of the conventional type which must be swept manually by postal workers during and after sorting. The stacks of mail are then loaded into trays for transport at a nearby traying station. In the alternative, the stackers may use cartridges in the manner described in U.S. Pat. Nos. 6,390,756, 6,183,191, 6,135,697, 6,026,967, 5,993,132, 5,947,468, 5,857,830 and 5,833,076, the contents of which patents are incorporated by reference herein. The mail cartridges are not used for two pass sorting, but instead are removed by a robot 91 and transported to a storage rack 92 and ultimately to an unloading table or machine which unloads the mail into a postal tray. Such an unloading machine is described in Isaacs U.S. Pat. No. 6,238,164, May 29, 2001, the contents of which are incorporated by reference herein.
[0034] Control system 37 according to the invention could comprise a single computer that reads all the incoming mail pieces and determines respective sorting destinations, as well as controls all buffers, sorting gates and diverts in order to conducting each mail piece through the routing system to the correct stacker pocket. However, referring to FIG. 7 , it is preferable that such a system comprise several computers, including a set of processors 81 for each OSS or DIOSS machine that are programmed to determine the sorting destination and transmit that information to a master control computer 82 . In lieu of attempting to track the movements of the entire mail stream moving through the routing system at any given time, it is preferred that each mail piece be tracked by its ID tag at certain strategic locations in the system. Each IAFCS and DIOSS machine applies an ID tag, such as an ultraviolet-detectable bar code, onto all mail pieces passing through, and computer 82 maintains a table of ID numbers and associated destination pockets according to the sort scheme.
[0035] Each buffer 36 , 72 has associated therewith a local controller 83 which controls the operation of the buffer and the immediately downstream diverters that act in coordination with the buffer to ensure that each mail piece is diverted in the correct direction. Each buffer 36 , 72 also has a tag reader 84 that reads the ID tag on each mail piece entering the buffer, sends the number to master computer 82 , and receives back instructions on how to divert that mail piece. By this means, it does not matter in what order mail pieces arrive at each buffer 72 , as long as each piece is diverted to the correct destination. A mail piece that reaches a buffer 72 in error is directed by master computer 82 to a special reject pocket on that stacker for later re-processing. Buffers 61 A- 61 D, which are not associated with any diverts, need not have a tag reader or computerized controller beyond what is needed to avoid jams in the downstream merges 62 .
[0036] In variations of the system according to the invention, the number of input feeders and stackers may be varied to some extent. For purposes of designing the routing system, it is much preferred that the number of input sorters be twice the number of stackers, and that this number be an even number, 2, 4, or 8 being most likely for practical purposes. In a system with only 2 input sorters, e.g., one OSS and one DIOSS operating in parallel, the routing system can be simplified to include only the first 2:4 merge which feeds directly to each level of a single stacker. A system twice the size of the illustrated embodiment would be possible, but the routing system would become much more complex, with sufficient diverts and merges to take a mail piece to any one of 32 levels in eight stackers. A system missing one input, i.e. 7 inputs for 8 stackers, or where one of eight inputs is out of service, could operate using the same routing system as described above or simplified for the portion of the routing system connected to the single input. For practical purposes, the preferred number of input sorters is between 6 and 8, with a corresponding number of stackers. These and other variations will occur to those skilled in the art and are within the scope of the claims presented hereafter.
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A sorting system using multiple sorters operating as part of a single, multi-sorting machine unified system. The system according to the invention includes a plurality of input sections capable of operating in parallel, each including a feeder that takes in mail pieces one at a time and a scanner that scans each mail piece for destination indicia, a plurality of stackers each comprising at least one row of pockets, a control system that determines a destination pocket in the stacker for each mail piece based on a predetermined sort scheme and the destination indicia, and a routing system effective to route mail in accordance with the sort scheme from any input section to any pocket of a stacker.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates in general to a leveling device and in particular to a novel tool which can be attached to a machine to adjust the output spindle to a level position and which can also be connected to a workpiece so as to adjust the workpiece to a level position for machining and drilling and other procedures.
2. Description of the Prior Art
The alignment of a workpiece with drilling, grinding and other tools is often times done by visually aligning the surface or bore of the workpiece to the tool. Such alignment is often inaccurate and results in excessive grinding and/or cutting.
SUMMARY OF THE INVENTION
The present invention provides a novel leveling device which is generally cylindrical-shaped and which has dowels or pins which extend from opposite ends such that the upper pin can be inserted into a grinding or cutting tool. The lower pin can be attached to a grinder or cutter and can be inserted into an opening or into the planar surface of a workpiece. The device is provided with a mercury switch which when level provides an open circuit, but which when tilted closes the circuit. Indicating lights are connected in circuit with the mercury switch so as to indicate that the device is tilted in one of two directions.
A second embodiment includes a pendulum and a fiber optic light indicating means so as to indicate when the pendulum is in the centered position.
Other objects, features and advantages of the invention will be readily apparent from the following description of certain preferred embodiments thereof taken in conjunction with the accompanying drawings although variations and modifications may be effected without departing from the spirit and scope of the novel concepts of the disclosure, and in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front plan view of the invention mounted on a flat surface;
FIG. 2 is a front plan view of the invention mounted to a grinding or drilling tool spindle;
FIG. 3 is a perspective view of the invention mounted to a tool which fits within the bore of a workpiece;
FIG. 4 is a sectional view of the invention illustrated in FIG. 3;
FIG. 5 is an exploded view of the invention;
FIG. 6 illustrates the electrical circuit of the invention;
FIG. 7 illustrates a modification of the invention in sectional view; and
FIG. 8 is a perspective view of the modification illustrated in FIG. 7.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1-5 illustrate a first embodiment of the invention which comprises a quick level device 10 of generally cylindrical-shape which has a first extending dowel 11 from one end 52. The outer portion of the level 10 is surrounded by a cylindrical shell 26 which joins a conical portion 24 which has an end 23. A drill bushing 25 can be received in an opening in the end 23. As shown in FIG. 2, the leveling device 10 is used to assure alignment of a drill 13 mounted on a head 14 which extends from a base 16. FIG. 1 illustrates a workpiece 30 which has an upper surface 31 which is to be ground or otherwise machined. A flat plate 21 is formed with an opening 40 into which a pin 22 can be inserted. Pin 22 is also inserted into the opening in the end 23 of the leveling device 10. Thus, in the usage shown in FIG. 1, the leveling device 10 can be utilized to level an upper surface 31 of a workpiece 30. As shown in FIG. 3, the base 16 carries a workpiece 32 which is held by clamps 35 and 35' to the bed 38 of the base 16. A leveling device 10 is provided with a grinding tool 36 which has a stem 34 that can be received into the opening in the end 23 and the grinding tool 36 can be placed into the opening 33 of the workpiece 32 to grind it.
Exploded view FIG. 5 illustrates the construction of the leveling device 10. A planar member 51 is formed with a horizontal opening 57. A mercury switch 58 is attached to a clamp 50 which can be received in the opening 57 to support the mercury switch 58. As is shown in the sectional view of FIG. 6, the mercury switch 58 includes three electrodes 64, 67 and 62 and a quantity of mercury 61. When the mercury switch 58 is level, the mercury 61 engages the center contact 67, but it does not engage either of the contacts 62 or 64. This condition is illustrated in FIG. 6. It is to be noted that the electrical contact 62 has a curved portion 60 which terminates adjacent the right end of the switch 58 as shown in FIG. 6. The contact 64 terminates adjacent the left end of the switch 58. Conical member 24 is attached to the planar member 51 and is formed with an opening 23 which is adaptable to receive different size drill bushings 25 therein, for example. An upper end 52 is formed with an opening 53 for receiving a dowel pin 11 therein and also has openings 54, 55 and 56 for respectively receiving therein an LED light 91 which has an end 92 which is received in opening 54, a push button switch 79 which has a push button 81 which is received in opening 55 and an LED light 84 which has an illuminated end 86 which is received in the opening 56. A battery holder 73 is attached to the member 51 and has contacts for receiving batteries 71 and 72 therein. A cylindrical cover member 26 fits over the member 51 and a set screw 106 passes through an opening 103 in the cylindrical member 26 and is received in an opening 104 in the end member 52. The screw 106 also passes through an opening 102 in an indicator plate 101.
FIG. 6 illustrates the electrical circuit for the leveling device. The batteries 71 and 72 are connected in series and a first lead 78 extends from switch 79 to one end 76 of the battery 72. A jumper 74 extends from the other end of the battery 72 to one end of the battery 71. A lead 83 extends from the end 77 of battery 71 to one contact of the LED 84 and a lead 87 extends from the other contact of the LED 84 to contact 70, 62, 60. A lead 89 extends from the end 77 of the battery 71 to one contact of LED 91 and a second lead 93 extends from the other contact of LED 91 to contact 66 which is connected to contact 64. The second side of the switch 81 is connected to electrical contact 67 by lead.
In operation, a leveling device 10 can be placed in the chuck 13 of a tool by extending the dowel 11 into the tool and tightening the chuck thereon. The switch 81 is closed and if the tool 13 is not vertical, the mercury 61 will move to one of the ends of the mercury switch 58 so as to make electrical contact between contact 64 and 67 for example. When this occurs, the LED 92 will be illuminated to indicate that the left side of the mercury switch 58 is low which indicates a non-level condition. The tool 13 is then leveled until the LED 92 turns off which means that the mercury 61 has moved out of engagement with the contact 64. If on the other hand the mercury 61 moves to engage the contact 60, the LED 86 will be illuminated to indicate that the right side is low and the tool will be adjusted until the mercury 61 is in the center out of engagement with the contacts 60 and 64. The leveling device 10 would then be rotated 90° and releveled so as to assure that the tool is vertical in both planes.
The planar surface 31 can also be leveled using the tool as illustrated in FIG. 1
FIGS. 7 and 8 illustrate a modified form of the invention wherein outer case 122 supports a pendulum 126 on a pivot shaft 127. The pendulum 120 is formed with a central notch 128. A light and detector source 141 is connected to the case 122 and when turned on by an on-off switch 142 illuminates the pendulum such that if the slot 128 is centrally aligned then light will not be reflected to the detector. Magnetic switches 146 and 144 are connected to the case 122 so as to detect when the pendulum 126 moves from the center position toward the magnetic switches. The magnetic switch 146 is connected by a lead 148 to an indicator unit 149 which has a light 151 which is illuminated when the pendulum 126 is closely adjacent the magnetic switch 146. The magnetic switch 144 is connected by a lead 156 to the indicator unit 149 and to indicator light 157 so as to indicate when the pendulum 126 is closely adjacent the magnetic 144. A lead 161 is connected to an indicator light 162 in the indicator module 149 so as to indicate when the detector 141 indicates that the slot 128 is not centered relative to the detector 141. The dowel 125 and the dowel 123 allow the leveling device to be mounted in a manner similar to the leveling device 10 illustrated in FIGS. 1-5.
Although the invention has been described with respect to preferred embodiments, it is not to be so limited as changes and modifications can be made which are within the full intended scope of the invention as defined by the appended claims.
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A leveling device for leveling tools and workpieces which has extending shafts at opposite ends with one shaft being adapted to be inserted into a tool so as to adjust and indicate whether it is level and the other shaft being adjusted to receive a drilling or grinding tool or a flat plate such that the surface of a workpiece can be leveled.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to containers for storing and carrying snow skis and ski poles and more particularly to a ski and ski pole containment apparatus and method which provides ease in containment while minimizing the cross-section of the container.
2. Description of the Prior Art
The prior art indicates that several attempts have been made to provide for the storing and carrying of skis, ski poles and/or ski boots.
For example, U.S. Pat. No. 4,161,268, issued to C. W. Heil discloses a complicated structure comprising three telescoping body members which must be adjusted and locked into position to fit a particular pair of skis. The exterior surface has numerous depressions and ribs.
U.S. Pat. No. 3,767,036, issued to W. N. McLeod discloses a two-part hinged container, much like a typical suitcase, having rigid masses mounted therein to receive ski equipment. This design bends the skis to increase the rigidity of the case. It contains a set of ski boots. A rigid metallic lip is affixed to the perimeter of each case half. Furthermore, exterior briefcase-type locks are affixed.
U.S. Pat. No. 3,086,688, issued to M. A. Vikre discloses a ski carrier particularly adaptable for use with water skis. The Vikre device uses a complex support arm mechanism and does not include an exterior shell for protection.
U.S. Pat. No. 4,643,302, issued to E. W. Baumgardner discloses a multiple sports equipment container comprising an elongated tube substantially elliptical in shape but having truncations at opposite extremities of the major elliptical axis. The Baumgardner device uses end caps having deep means of closure and access to a cavity of adjustable length within the container. This design is of extruded plastic and is not optimized for carrying a given quantity of skis and ski poles. Many articles, such as golf clubs and boat paddles may be carried.
U.S. Pat. No. 3,837,548, issued to D. Nerger, discloses a substantially rigid ski carrying case having oppositely disposed case portions comprising components or segments also provided with one or more removable sections which may. be attached to, and between, the case portions for extending or reducing the length of the case. All sections are hinged. As a result, the design is structurally significantly weaker than an integral tube and has numerous exterior fittings.
U.S. Pat. No. 4,380,290, issued to R. A. Luebke, discloses a container for articles, particularly elongated articles such as snow skis. Slidably disposed within the container is an adjustable partition to provide various sizes of storage compartments, the size depending upon the length of the article being stored therein. The selective positioning of the partition provides a secondary storage compartment.
OBJECTS OF THE INVENTION
A principal object of the present invention is to provide a ski container with a minimal cross-section and minimal weight.
Another object is to provide a high level of protection against ski and binding damage.
Another object is to provide a method for easily packing the skis and ski poles into a ski container.
Still another object is to provide a weather-resistant ski container.
Yet another object is to provide a ski container which is low in cost.
Other objects, advantages and novel features of the present invention will become apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawing.
The aforementioned objects are achieved by the present apparatus and method for containing snow skis and ski poles. In its broadest aspects, the present invention comprises a rigid, integral elongated tube having two opposing, parallel flat surfaces with lengths, L, and widths equal to W L ; two opposing parallel, flat surfaces with lengths, L, and widths equal to W S ; and, four curved surfaces each curved surface having a radius of curvature, R, for joining the flat surfaces. The elongated tube therefore has a substantially rectangular cross-section but with curved surfaces at the corners of the cross-section. The geometrical dimensions of the cross-section of the elongated tube is defined by the relationships: ##EQU1## where n=the number of strapped pairs of skis to be inserted into the ski container, ##EQU2##
One end of the elongated tube is open and the other end is closed. An end cap is hingedly attached to the open end and may be locked in place to close the tube. The aforementioned geometry of the elongated tube provides a minimal cross-section for containing the unique geometries of the skis and poles. In order to fit properly within this geometry, the skis and poles must be strapped together in a specific manner prior to their insertion within the container. The skis are oriented in the tip-to-tail fashion with the bindings facing each other so that the tip of one ski is adjacent to the tail of its paired ski. Ski poles are located adjacent each other on one side of the skis between the edges of the skis.
The elongated tube is preferably formed of blowmolded plastic. Thus, by novel combination of the elongated tube and packed geometry of the skis and ski poles, an apparatus and method for containing skis is provided which is of low cost, is of minimal weight, minimal cross-section while not compromising the high level of protection needed to protect against ski and binding damage. Furthermore, this geometry results in a clean, pleasing, stream-lined appearance which compliments the sportsman-like nature of most skiers and current automobile design.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side perspective view of the ski container of the present invention.
FIG. 2 is a top perspective view of the ski container of the present invention, taken along line 2--2 of FIG. 1.
FIG. 3 is a side, partial cross-section of the ski container of the present invention, with the skis and poles contained therein, taken along line 3--3 of FIG. 2.
FIG. 4 is an end view of the ski container, taken along line 4--4 of FIG. 3.
FIG. 5 is an end view of the ski container, taken along line 5--5 of FIG. 3.
FIG. 6 is an end view of a ski container embodying the principals of the present invention which contains two pairs of skis and poles.
The same elements or parts throughout the figures are designated by the same reference characters, while equivalent elements bear a prime designation.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings and the characters of reference marked thereon, FIG. 1 illustrates a side perspective view of the ski container of the present invention, generally designated 10. The apparatus 10 comprises an elongated tube 12 of sufficient length to contain skis. Elongated tube 12 has one closed end 14 and an open opposite end with an end cap 16 attached thereon. The end cap 16 is secured to the elongated tube 12 by a hinge (designated 18 in FIG. 3) and locking means 20. Locking means 20 may comprise a cam-type lock or other conventional lock, preferably of the key or combination type. Carrying straps 22,24 are provided to conveniently carry the ski container 10 by the hand and/or shoulder.
As shown in FIG. 2, four indented locations 26 on the top surface of apparatus 10 provide access for attachment of the straps 22,24. Fasteners 28 may comprise, for example, standard heavy-duty plastic lips and D-rings. The straps 22,24 may be removable for auto and airline travel and stowed inside the tube.
Referring now to FIG. 3, a side partial cross-section of the apparatus 10 is shown with a pair of snow skis 30,30' and ski poles 32,32' located therein. As can be readily seen by this Figure, each ski 30 has a substantially flat portion 34 and tip 36 formed on the forward portion of the ski 30 and curved from the flat portion 34. The flat portion 34 terminates in a tail end 38. Each ski 30 further has a toe binding 40 for supporting the toe of the ski boot and a heel binding 42 for supporting the heel of the ski boot. The bindings 40,42 are each securely attached to the flat portion 34.
Each heel binding 42 includes a ski brake 44 attached thereto. In its normal position each ski brake 44 normally extends at a significant angle (i.e. approximately 45 ° from the plane of the flat portion 34 of the ski 30. However, the ski brake 44 may become depressable so as to change its angular orientation, and become substantially parallel to the plane of the flat portion 34 of ski 30.
Prior to being inserted into the elongated tube 12 a pair of skis 30,30' and a pair of ski poles 32,32' are strapped together as a single unit, generally designated 46. The formation of such a strapped unit 46 allows for convenient insertion and removal of the skis and poles from the ski container 12.
Prior to being strapped, the skis 30,30' are oriented in a tip-to-tail fashion, that is, so that the tip 36 of one ski 30 is adjacent to the tail 38' of the other paired ski 30'. A strap 48 is utilized with a rigid loop 50 attached to one end 52, as shown in FIG. 4. The strap 48 is wound around the pair of skis in a first direction at the location of the ski brake 44. The other end 54 of the strap 48 is directed through the loop 50 and pulled in a second direction opposite from the first direction and with sufficient tension to depress the ski brake 44 and to maintain the skis in close proximity.
The ski poles 32 are placed on one side of the skis 30, as shown in FIG. 4. Furtheraore, the ski poles 32 are disposed between the dges of the skis 30,30'. Thus, as the strap 48 is wound in the second direction it wraps around the ski poles 32,32' as well as the skis 30,30'. End 54 is then fastened to a fastening location on the strap 48. This is preferably accomplished by providing end 54 with a mating half 56 of adhesive strip of synthetic material of the type that adheres when pressed together with a corresponding mating strip 58 (commonly sold under the trademark "VELCRO"). The strap 48 is preferably formed of a webbed cloth, however other suitable materials such as nylon may be utilized. Fastened together as a compact unit 46 the skis 30,30' and poles 32,32' may be inserted into the novel elongated container 12 which is specially formed to contain the unit 46.
Referring now to FIG. 5, the elongated tube 12 has two opposing parallel flat surfaces 60,62 having lengths, L, and widths, W L . (The length, L, is designated in FIG. 1.) Two other opposing flat surfaces 64,66 are oriented perpendicular to surfaces 60,62 and have the same length, L as those two surfaces, but have shorter widths, W S . Four curved surfaces 68,70,72,74, each having a radius of curvature, R, join the flat surfaces. Thus, the elongated tube 12 has a substantially rectangular cross-section but has curved surfaces 68,70,72,74 at the corners of the cross-section. The geometrical dimensions of the cross-section of the embodiment illustrated in FIGS. 1-5 is defined by the relationships ##EQU3## Applicant has found that design adherence to these equations provides minimal cross-section resulting in minimal weight, minimal exterior size, and excellent bending strength and crush resistance.
A minimal side-to-side envelope is obtained by interlocking the ski bindings such that the tip and tail of opposing skis are on the same plane perpendicular to the ski axis. This configuration minimizes the lateral dimension by limiting the lateral variables to one ski tip height, H T , and one binding height, H B (see FIG. 3). Most common skis stored in this configuration have a total width of under seven inches. Vertical height is a function of ski brake width, ski width, binding height and ski pole handle 76 size. Stacking the ski poles on one side of the skis minimizes total ensemble height because the ski baskets 78 are flexible and are deflected by surface 60 and therefore allow the ski pole handles to be pivoted downward allowing a reduced total height.
The elongated tube is preferably formed of a blow-molded-type plastic, such as the product commonly sold under the trademark "GELOY". In its manufacture, a tube with two closed ends is first formed. After the blow-molding process is completed one of the closed ends is detached and reattached using a bonded hinge assembly and lock. The fittings for the straps may be bonded or riveted into blow-molded depressions. The mold for blowmolding may incorporate removable sections so as to provide variable-lengthed tubes.
As illustrated in FIG. 6, an elongated tube 80 may be utilized which contains two or even more strapped units 46,46'. The generalized geometric relationship that defines the dimensions of the tube is expressed as ##EQU4## where n=the number of strapped pairs of skis to be inserted into the ski container, ##EQU5##
Obviously, many modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described.
For example, it is understood that the values for K 1 , K 2 and R may differ from the above-described quantities by certain reasonable limits yet still embody the principals of the present invention. A reasonable range of values is listed below:
0.411<K 1 <0.503
0.549<K 2 <0.671
1.28<R<1.92
Furthermore, the thickness of the ski container may be increased near the open end to provide increased stiffness. Or, a doubler may be bonded to the inner surface of the tube along the perimeter of the cross-section to provide increased strength and stiffness.
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An apparatus and method for controlling snow skis and ski poles optimized for carrying selected quantities of pairs of skis and ski poles. The apparatus is characterized by a single, elongated tube with a hingedly attached lockable cap. Pairs of skis and ski poles are strapped together as a compact unit for convenient insertion in the small cross-sectioned tube. The tube cross-section incorporates large radius corners for increased crush-resistance.
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TECHNICAL FIELD
This invention relates to the optimization of computer software and hardware, and in particular to optimization according to user-specified preferences, databases, and dynamic monitoring of system behavior and performance.
BACKGROUND OF THE INVENTION
Computer operating systems include a large number of parameters, many of which may be queried, controlled, and changed in order to alter the characteristics of the computer system. Similarly, software applications running on computer systems also often include a large number of parameters, many of which may be controlled and changed to alter the characteristics of the application running on the computer system. As an example, in Microsoft's Windows NT operating system, the resolution and color characteristics of the computer system's display may be changed by selecting the “Control Panel” icon from a “Settings” menu item. When the control panel is displayed, a user is presented with a set of new icons, one of which (“Display Properties”) may be selected to bring up another panel containing a set of tabs. The “Settings” tab on the “Display Properties” panel may be selected which allows a user to manually change the number of colors, resolution, video refresh rate, font size, and related graphical characteristics. The user specifies the refresh frequency by selecting from a pull-down menu list of available settings (e.g. 60 Hz, 70 Hz, etc.). The user can specify the screen resolution by selecting a slider icon and moving it right or left to increase or decrease the screen resolution (e.g., from 1024×1280 pixels to 600×800 pixels). Some of these settings may affect the performance of applications running on the system. For example, decreasing the color resolution and screen resolution may increase the speed of some graphics applications.
This example focuses on system settings. When one also considers the numerous application settings and various different hardware configurations available to users, and the interaction of all of these settings and configurations, the control accessing of the plurality of settings and configurations can be cumbersome and often requires detailed knowledge on the part of computer users. The need for a dynamic, semi-automatic, consolidated, and rule-based system that changes such settings and other aspects of the computer system, and makes recommendations, becomes apparent. Although many graphical user interfaces exist to control various aspects of the system (such as the graphical slider which controls screen resolution for Windows platforms) and in applications, the need for improved graphical user interfaces becomes apparent as computer systems become more complex.
With reference now to the figures and in particular to FIG. 1 , there is illustrated a computer system in accordance with the method and system of the present invention. Typically the computer system 12 includes a computer 36 , a computer display 38 , a keyboard 40 , and multiple input pointing devices 42 . Those skilled in the art will appreciate that input pointing devices may be implemented utilizing a pointing stick 44 , a mouse 46 , a track ball 48 , a pen 50 , display screen 52 (e.g. a touch display screen 52 ), or any other device that permits a user to manipulate objects, icons, and other display items in a graphical manner on the computer display 38 . Connected to the computer system may also be audio speakers 54 and/or audio input devices 51 . (See for example, IBM's Voice Type Dictation system. “Voice Type” is a trademark of the IBM Corporation.) A graphical user interface may be displayed on screen 52 and manipulated using any input pointing device 42 . This graphical user interface may include display of an application 60 that displays information pages 62 using any known browser. The information pages may include graphical, audio, or text information 67 presented to the user via the display screen 52 , speakers 54 , or other output device. The information pages may contain selectable links 66 to other information pages, where such links can be activated by one of the input devices, like mouse 46 , to request the associated information pages. This hardware is well known in the art and is also used in conjunction with televisions (“web TV”) and multimedia entertainment centers. The system 12 contains one or more memories (See 65 of FIG. 2. ) where a remote computer 130 , connected to the system 12 through a network 110 , can send information. Here the network can be any known (public or privately available) local area network (LAN) or wide area network (WAN), e.g., the Internet. The display may be controlled by a graphics adaptor card such as an Intergraph Intense 3D,
Graphical user interfaces (GUIs) provide ways for users of computers and other devices to effectively communicate with the computer. In GUIs, available applications and data sets are often represented by icons 63 consisting of small graphical representations which can be selected by a user and moved on the screen. The data sets (including pages of information) and applications may reside on the local computer or on a remote computer accessed over a network. The selection of icons often takes the place of typing in a command using a keyboard in order to initiate a program or access a data set. In general, icons are tiny on-screen symbols that simplify access to a program, command, or data file. Icons are often activated or selected by moving a mouse-controlled cursor onto the icon and pressing one or more times on a mouse button.
GUIs include graphical images on computer monitors and often consist of both icons and windows. (GUIs may also reside on the screens of televisions, kiosks, personal digital assistants (PDAs), automatic teller machines (AIMs), and on other devices and appliances such as ovens, cameras, video recorders and instrument consoles.) A computer window is a portion of the graphical image that appears on the monitor and is dedicated to some specific purpose. Windows allow the user to treat the graphical images on the computer monitor like a desktop where various files can remain open simultaneously. The user can control the size, shape, and position of the windows.
Although the use of GUls with icons usually simplifies a user's interactions with a computer, GUIs are often tedious and frustrating to use. Icons must be maintained in a logical manner. It is difficult to organize windows and icons when many are similarly displayed at the same time on a single device.
In a drag-and-drop GUI, icons are selected 64 and moved 68 (i.e. “dragged”) to a target icon 69 to achieve a desired effect. For example, an icon representing a computer file stored on disk may be dragged over an icon containing an image of a printer in order to print the file, or dragged over an icon of a trash can to delete the file. An icon representing a page of information on the World Wide Web may be selected and dragged to a trash can to delete the link to the page of information. The page of information may be on the local machine or on a remote machine. A typical user's screen contains many icons, and only a subset of them will at anyone time be valid, useful targets for a selected icon. For example, it would not be useful to drag the icon representing a data file on top of an icon whose only purpose is to access an unrelated multimedia application.
Icons 63 could include static or animated graphics, text, multimedia presentations, and windows displaying TV broadcasts. Icons 63 could also include three dimensional images, for example, those used in virtual reality applications.
SUMMARY OF THE INVENTION
An object of this invention is a method and system for increasing the apparent speed of a computer by automatically optimizing software and hardware according to user-specified preferences.
Another object of this invention is to provide a method and system for increasing the apparent speed of a computer using a database.
Yet another object of this invention is to provide a method and system for effectively increasing the apparent speed of a computer based on results obtained by dynamically monitoring system behavior and performance.
This invention permits users to conveniently optimize software running on a computer. The term “optimize” refers to running of a computer system or software more efficiently, for example, by maximizing both the speed with which a software application runs and user satisfaction, and/or minimizing cost or resource use. “Optimization” includes the setting of various parameters in hardware, operating system software, or application software such that the system as a whole runs as efficiently as possible. These parameters might be set to optimize speed, system resource cost, or other variables corresponding to a user's satisfaction.
Accordingly, this invention provides for a method of enhancing, for example, program application performance on a computer system. With this invention configuration information and performance capabilities based on characteristics of the program/system are determined. Then, the configuration information and the performance capabilities are used to optimize configuration parameters of the program applications so as to enhance the performance of the workstation in running the program'system. Further, with this invention user preferences in the operation of the program are selected by, for example, dragging rule icons to a target optimizer icon to provide user selected rules of operation of the application program.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be further understood by reference to the following detailed description when read in conjunction with the accompanying drawings, wherein:
FIG. 1 depicts a pictorial representation of an example computer system that embodies the present invention.
FIG. 2 is a block diagram of the computer system architecture showing an optimization database.
FIG. 3 is a block diagram showing portions of a computer network wherein a local computer and a remote computer are both connected directly to the network.
FIG. 4 are example database records that may be used for optimization.
FIG. 5 is a flow chart depicting the steps performed in the optimization.
FIG. 6 is a schematic illustration display with an optimizer and rule icons thereon.
FIG. 7 is a flow chart showing the steps of one preferred method of the present invention pertaining to the use of iconic rules.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference now to FIG. 2 , there is illustrated a block diagram of the architecture of the computer system 12 in accordance with the present invention.
The core architecture includes a Central Processing Unit 165 , memory controller 162 , system memory 65 , disk storage 70 , disk storage controller 75 , and graphics subsystem 166 . The computer system 12 can be either a stand alone workstation or a server and a workstation connected to each other via a communications network such as the internet. A portion of the system memory is set aside for an optimizer-database cache 80 . Additionally, file space 85 on the disk storage unit 70 may be set aside for the optimizer database 140 . Generally speaking, a cache or buffer is a place where data (files, images, and other information) can be stored to avoid having to read the data from a slower device, such as a remote, network-attached computer disk. For instance, a disk cache can store information that can be read without accessing remote disk storage.
With reference now to FIG. 3 , there is illustrated a partial portion of a computer network in accordance with the method and system of the present invention. Computer system 12 connects to the network backbone 110 by means of a connecting device 100 . Also connected to the network 110 are one or more server computers 130 by means of their own connecting device 100 ′. Those skilled in the art will appreciate that these connecting devices 100 may take various forms, including modems, token-ring hubs, and other network-enabling devices depending on the capabilities and technology of the connecting devices. The remote computer 130 may include an area of system memory and/or disk storage space dedicated to storing and maintaining a optimization database table 140 (e.g. data file). The optimization database table 140 may reside on the local client or reside on both the client and remote computer. Portions of the optimizer program 136 may reside on the local computer and/or the remote computer. The optimizer program contains or accesses a dynamic monitor 137 of system and application activity. Various user applications 138 run on the remote or local computer. For example, these applications may be office productivity, scientific and engineering, finance, transaction processing, Internet, or any other software a user needs to run. Such applications may be controlled by a configuration file 141 or a central database that controls particular settings of the application that may affect application performance. The optimizer program 136 may contain a graphical user interface 139 , used to specify settings or provide information to the user. An operating system 150 runs on the local computer. The operating system, such as Windows NT, primarily provides an interface between the user application and the computer hardware. The operating system also provides services on behalf of the user and applications such as networking, file management, etc.
FIG. 4 includes example records 430 for optimizing system performance. The set of records comprise the database 140 . Application settings 420 may consist of a set of control parameters A 1 , A 2 , . . . , AN shown in this example in rows 430 and associated with a particular unique identifier 410 for a software application. The software application may be designated in the database 140 as an alphanumeric string 410 . By way of example, parameter A 1 may control the graphical quality of an engineering application's 3-D graphics. Lower graphical quality often implies faster use of an application. System settings 440 contain information usually relating to static qualities of the computer system such as the particular operating system, amount of memory, processor speed, graphics card name, and bios version. These values S 1 , S 2 , . . . , SN are static in the sense that they do not usually change during the operation of an application. Dynamic data 460 may contain current or prior reports of system behavior or performance. The dynamic data is generally dynamic information, such as current CPU, memory, and disk use, all of which change as an application performs operations, and reads and writes information to memory and disk. The values M 1 , M 2 , M 3 . . . for this dynamic data 460 may be obtained by a monitor program 137 which, for example, scans the system for CPU, memory, and disk use at specific increments of time. Suggestions 480 consist of alphanumeric information (R 1 , R 2 , R 3 , . . . ) that may be supplied to the user (e.g., recommendations or warning messages) for particular applications. The optimizer program 136 may scan a row or record 430 of database 400 to optimize a single, particular application, or it might join the results of numerous rows to optimize for a set of concurrently running applications designated by identifiers 410 . Note that in FIG. 4 , parameters A 1 , A 2 , A 3 . . . control application settings. Parameters S 1 , S 2 , S 3 . . . control system settings. Parameters M 1 , M 2 , M 3 . . . control dynamic settings. Parameters R 1 , R 2 , R 3 . . . are recommendations.
FIG. 5 comprises a flow chart for an optimization process 300 that the local computer 12 or server 130 uses to optimize software applications 138 and system response or utilization, or to provide recommendations 480 . In step 303 , the optimizer 136 gathers relevant system information including: operating system 150 version and release data, installed hardware components, hardware configuration, and software configurations. For example, the optimizer determines the size of RAM, BIOS level, installed options etc. This information gathering can be accomplished using standard operating system or other commands. For example, on Microsoft's Windows NT operating system, the “Winmsd/f” calls, the Win32 API, queries to the system registry, and other methods known to those skilled in the art, allow the optimizer to collect such information. In step 305 , the optimizer 136 gathers relevant application information, for example, release version, installed options, etc. In step 310 , the optimizer 136 reads records 430 from database 140 , that control various parameters 420 , associated with a particular application name 410 . The database 140 may reside on a remote computer or server 130 accessed over a network 110 or on the local computer 12 .
In step 320 , the optimizer 136 monitors system 12 behavior. For example, the optimizer may query the current CPU use, memory use, or other activity 321 using operating system commands known to those skilled in the art. Also, a monitor program 137 may use such commands to monitor such activity. This monitor program 137 may contain a graphical user interface 139 that displays such activity in graphical form, such as with bar graphs, pie carts, numerical indicators, gauges, etc. This activity 321 may be stored in the form of dynamic values M 1 , M 2 , . . . , MN in settings 460 and read by the optimizer program 136 . Alternatively, the values corresponding to system activity/use may be directly obtained using operating system commands. One benefit of storing the dynamic data is that the optimizer 136 may compare current to past system activity. In this step 320 , the optimizer also may perform performance measurements to “benchmark” the system by running built-in test routines. For example, the optimizer may time the rotation of a 3-D graphical object to assess the speed of the graphics subsystem 166 .
In step 325 , the optimizer 136 reads user input. For example, the user may enter text or data at the keyboard 40 (or with various input devices 46 , 48 , 50 , or by voice input using audio input device 51 ) that specifies a level of optimization 326 . This level of optimization may control which of the application settings 420 are used to optimize the application in step 330 or optimize the system 12 in step 340 . A user wishing to have maximum performance may, for example, sacrifice graphic quality controlled in applications settings 420 , that are generally read upon invocation of application 138 .
By way of example, the optimizer 136 can adjust the following parameter settings 420 , in the Unigraphics control file to adjust performance. (Unigraphics is an graphically-intensive engineering application created by EDS.) The values for each of these settings may be determined in step 325 and stored in record 430 .
Low Performance settings
*Ugraf130.realTimeDynamics: TRUE *Ugraf130.suppressAutoRefresh: FALSE *Ugraf130.backfaceCulling : FALSE *Ugraf130.depthSortedWireframe: TRUE *Ugraf130.lineAntialiasing: TRUE *Ugraf130.disableTranslucency: FALSE
High Performance settings
*Ugraf130.realTimeDynamics: FALSE *Ugraf130.suppressAutoRefresh: TRUE *Ugraf130.backfaceCulling: TRUE *Ugraf130.depthSortedWireframe: FALSE *Ugraf130.lineAntialiasing: FALSE *Ugraf130.disableTranslucency: TRUE
In this example, if a user sets suppressAutoRefresh to TRUE, the application performance can improve by reducing excess redrawing. “Low Performance” is generally correlated with higher graphical quality. The “level” of optimization 326 may correspond to the number of “high performance” settings selected. For example, highest performance (highest level of optimization) may correspond to the use of all the settings in their high performance states. Lower levels of optimization correspond to fewer of the high-performance settings being used. Those values that constitute high performance settings may be stored in application settings 420 .
Similarly, the optimizer also optimizes system settings 440 . These are settings independent of applications and generally associated with the computer or its hardware or software components. For example, the graphics card may have general settings that control the resolution, color depth, synchronization on vertical refresh, and other features. The disk may have a fragmentation state which may be altered. The size of “swap” spaces may be specified. These system settings are sometimes stored in the system registry or in initialization files which may be modified using methods known to those skilled in the art.
Returning to step 325 in FIG. 5 , as an alternative to text, a graphical user interface 139 may be used to provide input data. For example, a graphical depiction of a slider may be used to control the program optimization level by causing the optimizer 136 to optimize 330 the application by writing discrete records in an application configuration file 141 stored on disk. See step 330 . Such a file as the configuration file 141 is typically read by an application when the application starts and controls various performance characteristics of a particular application. The audio input device 51 also permits speech input in step 325 . Generally speaking, in steps 330 and 340 , the optimizer uses the information acquired in steps 303 , 305 , 310 , 320 , and 325 to adjust system or application parameters in order to optimize the operation of the application. For example, the ensemble of data from 310 , 320 , and 325 may cause the optimizer to not only specify settings to the application but also to the graphics card, or system to alter the speed of the application. In general, the optimizer adjusts system and application settings to best meet user-specified quality/performance trade-offs. The information gathered in steps 303 , 305 , and 320 may be stored in the database 140 maintained by the optimizer. The database can be helpful in determining changes to system and application configurations at different points in time, in evaluating the effects of changing application settings, and in comparing actual system/application settings with recommended settings.
In step 350 , the optimizer 136 may provide suggestions or recommendations 480 , for example, in the form of specific text that is output to the user. This output may appear in the optimizer's graphical user interface 139 , in a web browser 90 , or as audible sound played through speakers 54 another audio output device. These recommendations may be used to warn the user of various conditions (e.g. “disk space is low”), or give suggestions on how to improve performance (e.g. “purchase more memory”). The optimizer contains rules 331 , 341 , 351 that it uses to make such optimizations 330 , 340 and recommendations 350 . For example, a rule may be: If A 1 =yes, and S 1 =200 MHz, or M 1 =90%, then make suggestion and change (in step 340 ) the graphic card settings (e.g. 450 ) that control “synchronization on vertical refresh”. In this example, S 1 corresponds to the processor frequency, and M 1 corresponds to the percentage of memory used. A rule may consist of a set of conditionals and Boolean operations (e.g. if A and B are true and C is false then make suggestions and take action).
Note that the suggestions 480 , entire records 430 , and rules 331 , 341 , 351 may be segregated into different files in database 400 , stored at a local machine 12 or remote machine 130 . Users may view ( 360 ) the rules 331 , 341 , 350 , records 430 , and suggestions 480 using graphical user interface 53 , which may visually segregate these items based on origin of the suggestions (e.g. companies, individuals, etc.), severity, date, or other criteria. These rules and suggestions may be web accessible (using network 110 ) for dynamic optimization across the web using a propriety program product at the web server.
Referring to FIGS. 1 and 5 , note that the rules 331 , 341 , 351 may also be represented as icons 63 displayed on the graphics screen. (These icons representing rules are hereafter sometimes referred to as “iconic rules”.) Particular rules may be selected 64 from a set of available rules by the user and dragged 68 to an icon 69 representing the optimizer 136 so that the optimizer will implement 330 , 340 , 350 the rules. Additionally, the rules 331 , 341 , 351 may require password protection so that only certain users or classes of users have permission to implement the rules. In an example scenario, a user drags 68 an iconic rule 63 to optimizer icon 69 . This rule may require that the graphical quality be degraded for a model part if the model part consists of greater than 100,000 triangular facets. (This will enhance the display speed of the model part.) When the user drops the iconic rule on the optimizer icon, the user must enter a password (e.g. consisting of a keyboard entry, speech input, mouse swipes, a sequence of mouse key presses, a secret position on the optimizer icon, or by other means) before the rule is acted upon in steps 330 , 340 , or 350 . In another embodiment, the rules are dragged to a region 70 of the screen and not to the optimizer icon in order for the rules to take effect. Password protection may be useful in a variety of situations, for example, if certain rules are being tested by developers and administrators or if certain rules cause actions that should be restricted (e.g. access to confidential databases, CPU or cost-intensive jobs, the allocation of e-money and credit information, etc.)
The optimizer in steps 330 , 340 and 350 may learn 370 from a user's past activity. For example, if the user has always used an application with small files, and past CPU use has always been low (e.g. as stored in settings 470 ), the software optimizer can make suggestions ( 480 ), accordingly. Note that one benefit of having portions of the database 140 (e.g. the settings and suggestions) and rules 331 , 341 , and 351 on a remote machine 130 is that a company or system administrator can continually manage and update messages and rules as new information is provided by application vendors. When a user runs an application in 410 , the user can make use of the latest information in the database. If the database 140 resides on a remote machine 130 the optimization 330 , 340 , and 350 can be performed either on the local machine or the remote machine. If performed on a remote machine, messages and other parameters are fed from the remote server 130 to the client 12 using the network 110 .
FIG. 6 is a block diagram of a GUI 591 with rule icons 540 , 63 (See FIG. 1. ) including optimizer icons 69 , 510 , 511 . In the present invention, the user uses a selection device such as mouse 46 to select 512 an icon 540 and drags 550 the icon to optimizer icons 510 , 511 . If the icon 540 , representing a rule, is touching or close (within a threshold distance 590 ) to the optimizer icon 510 , then the rule 541 , 331 , 341 , 351 is applied. In other words, “closeness” of an icon is determined by computing the distances from the selected icon 540 to regions 520 of the optimizer icon displayed on the GUI. If the distance is smaller than a particular threshold 592 , the icon 540 is close to a region of the optimizer.
In one embodiment, the optimizer icon 510 consists of different regions 520 to which iconic rules 540 are dragged. The optimizer software determines near what location 520 icon is positioned using techniques which are well known to those skilled in the art of GUI interfaces. In addition to performing general optimization, the optimizer icons 510 may be used to specify the ‘nature’ of the update; for example, one optimizer icon 510 may be specified for optimization concerning graphics, while another icon 511 may be specific for controlling all aspects of memory and disk space. The optimizer icon may change its graphical attribute such as color or brightness 570 in response to the information gained when the optimizer software applies the rules 541 . For example, once a rule is successfully applied, then the optimizer region 520 may turn red 570 . The iconic rules 541 may also change graphical attributes in a similar manner. (Changes in graphical characteristics of the iconic rules and optimizer icons are carried out in step 670 in FIG. 7 ).
The rule application can be carried out by the optimizer software by comparing the position 585 of icon 540 to values stored in a position file 596 which may be stored on disk.
The optimizer icon 510 may also contain graphical indications of regions 520 , such as cutouts 530 , to which iconic rules 540 may be dragged. In this manner, when the icons are placed in the optimizer icon 510 there can be a graphical indication 551 of the binding to the user. Additionally, the area around the cutout may change color or brightness 570 once an icon 540 is located in the cutout. The use of discrete cutouts 530 may be useful when only a limited number of rules may be used. The rules may be evident to the user by text 560 written on the optimizer icon or by colors 570 .
FIG. 7 is a flow chart 600 showing the steps 600 performed for a preferred version of optimizer 163 executed by the system in FIG. 1 . In step 610 , a program checks if an icon 540 (e.g., if an iconic rule) is selected. The selected icon 540 may be selected by any selection method: e.g., pointing and clicking or by an application program If the icon is moved 620 , its new location is determined 630 . If the icon is near (within a threshold distance 590 from) an optimizer region 520 (step 640 ), then a visual indication 650 of placement such as changing color or brightness 570 of a region 520 optionally may be given. As stated in the description of FIG. 5 , the region 520 may be graphically depicted as cutouts 530 to help give users a graphical (visual) indication of the placement. Also as mentioned in the description for FIG. 5 , “nearness” or “closeness” is determined by computing the distances from the selected icon to all optimizer icons regions 520 on the GUI. In one preferred embodiment, distances are computed using known geometrical methods. For example, if (x 1 ,y 1 ) are the coordinates of an icon 540 and (x 2 ,y 2 ) are the coordinates of a region 520 , then the distance is d-sqrt ((x 2 −x 1 )**2+(y 2 −y 1 )**2). This formula may be extended to include additional variables for higher dimensional spaces, such as in a virtual reality or three-dimensional environment. An optimizer table (file) 596 on disk may store the x,y locations of regions 520 .
The rule 541 represented by an icon 540 is applied 660 . The icon 540 or optimizer icon 510 optionally may change color, brightness, texture, blink rate, shape, size, or other graphical attribute (see step 670 ). This graphical attribute may be a function of the nature of the rule. For example, an iconic rule that increases graphics quality may be red. An icon representing a rule that decreases graphics quality may be green. The optimizer icon may change colors when the rule is successfully applied or has a beneficial effect.
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A method of optimizing the operation of a computer system in running application programs in accordance with system capabilities, user preferences and configuration parameters of the application program. More specifically, with this invention, an optimizing program gathers information on the system capabilities, user preferences and configuration parameters of the application program to maximize the operation of the application program or computer system. Further, user selected rules of operation can be selected by dragging rule icons to target optimizer icon.
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BACKGROUND OF THE INVENTION
As is well known to those versed in the automotive service field, location of an ignition circuit defect is often tedious and time consuming, usually requiring disconnection and reconnection of parts which often results in damage, or removal and replacement of parts which may be expensive without remedying the problem.
While there are a number of prior art ignition circuit tester devices, such devices have not been found satisfactory and generally leave the practitioner to cope with the above-described difficulties. Applicant is aware of the below listed prior U.S. Pat. Nos.
2,701,335 Sargeant et al
3,452,270 Cook
3,603,872 Pelta
3,743,922 Festos
3,763,421 Glomski
3,811,089 Strzelewicz
SUMMARY OF THE INVENTION
Accordingly, it is an important object of the present invention to provide an ignition circuit tester for use with automotive and similar electric ignition type internal combustion engines, which enables a mechanic to simply, quickly, and easily manipulate a pick-up assembly or probe to selectively locate the probe along an element to be tested and observe the quality of the element by a corresponding meter reading.
More specifically, it is an object of the present invention to provide an ignition circuit tester wherein a coil assembly is adapted to be carried on the end of an elongate member or handle for convenient manual location in inductive coupling with a selected spark plug, ignition wire, distributor or corresponding part of an electronic ignition circuit, all without disconnection, removal, replacement, or other handling of ignition circuit elements, to effectively overcome the above-mentioned difficulties of the prior art.
Other objects of the present invention will become apparent upon reading the following specification and referring to the accompanying drawings, which form a material part of this disclosure.
The invention accordingly consists in the features of construction, combination of elements, and arrangements of parts, which will be exemplified in the construction hereinafter described, and of which the scope will be indicated by the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a rear prospective view showing a pick-up assembly of the present invention, broken away to conserve drawing space.
FIG. 2 is a front view of the assembly of FIG. 1.
FIG. 3 is a schematic representation of the electrical circuitry of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now more particularly to the drawings, and specifically to FIGS. 1 and 2 thereof, a pick-up or coil assembly is there generally designated 10, and may include a coil housing 11 carried by a straddling yoke 12. An elongate member or handle 13 includes a rod 14 having one end suitably fixed, as by welding 15 to the yoke or carrier 12, and the other end of rod 14 may be provided with a hand piece 16 for manual grasping by the user.
The housing 11 may be in the form of an enclosure, say of box-like configuration, having one side open, and fabricated of conductive, electronically shielding material, such as aluminum. Specifically, the housing 11 may include a generally rectangular rear wall or back 20, top and bottom walls 21 and 22 extending forwardly from upper and lower edges of the back wall 20, and opposite side walls 23 extending forwardly from opposite side edges of the back wall and between the top and bottom walls. The front of the rectangular or box-like enclosure or housing 11 may be open, as by the absence of a front wall.
Internally within the hollow or concavity of the housing 11 there is suitably mounted a helical coil 25 of conductive filament or wire having a suitable number of convolutions, 4500 turns of 149 ohm #38AWG magnet wire having been found satisfactory. The coil 25 is carried by a rod or core 26 extending between side walls 23, and end pieces or discs 27 are circumposed about the rod 26 at opposite ends of the coil 25, so that the rod 26 and ends 27 define a spool for the coil. Thus, the axis of the coil 25 extends laterally with respect to the housing 11, between opposite housing side walls 23.
The carrier or yoke 12 may be of generally U-shaped configuration, including an intermediate portion extending laterally across and rearward of the rear housing wall 20, and a pair of generally forwardly extending legs 31 projecting in general parallelism from opposite ends of the intermediate portion 30. The forward ends of the legs 31 terminate adjacent to and outward of respective housing side walls 23 and may be pivotally connected thereto, as by appropriate pivot means 32.
An electric wire or cord 35 may be of two-conductor shielded wire, extending from interiorly of the housing 11, having two conductors 36 and 37 respectively connected to opposite ends of coil 25, and the shield conductor 38 connected to the housing 11. The shielded conductor 38 may extend externally of the housing to terminate in a suitable connector or plug 39.
In practice, the coil 25 is preferably potted, or imbedded in potting material, such as transparent epoxy 40, which may substantially completely fill the interior of the housing 11. The potting material is of insulating characteristic, so as not to adversely affect a magnetic field being sensed, and effectively protects the coil from damage.
Considering now the circuitry of FIG. 3, the pick-up coil assembly includes the coil 25 on its core 26 and connected at its opposite ends to conductors 36 and 37, which are provided with a shield 38 connected interiorly of the housing 11 to the latter, as at 50, and connected adjacent to the plug 39, as at 51, to conductor 37. The conductor 37 is connected to ground, in the operative condition, as through conductor 52.
Through the cord 35, containing conductors 36 and 37, the coil 25 is connected to feed amplifier means 53, the output of which is fed to an indicating means or meter 54.
More specifically, the amplifier means 53 includes a plural stage transistor amplifier, including a pair of resistance coupled transistors, as at 55 and 56. The coil conductor 36 may feed through plug 39, shielded conductor 57, and filtering compacitor 58 to the base of n-p-n type transistor 55. The emitter of transistor 55 is biased to ground, and the collector of transistor 55 is resistance coupled to feed the base of p-n-p transistor 56. From the collector of transistor 56, an output conductor 59 feeds a transformer 60.
Specifically, the output conductor 59 of transistor amplifier means 53 is connected to the primary winding 61 of transformer 60, and the secondary winding 62 of the transformer is connected by conductor 63 and 64 to opposite sides of a rectifying bridge 70. A push-button switch 65 may be connected in conductor 64, being normally closed in the latter conductor, and depressible to connect the meter 54 on one side to a contact 66 connected through a rheostat 67 to the positive terminal of a battery 68.
The meter 54 is connected on one side to one bridge junction, as by conductor 71, and is connected on its other side by a conductor 72, and through resistor 73 to the opposite junction of bridge 70. A switch 74 is swingable to selectively bypass the resistor 73 to effectively change the calibration of meter 54, for purposes which will presently become apparent.
The battery 68 supplies power to the circuitry, having one side grounded, as at 75, and having its other side connected through a switch 76 to the input of two stage transistor amplifier 53, as through coupling resistor 77. The switch arm 76 is selectively swingable to contact 78 directly connected to the battery 68, and a contact 79 connected through a conductor 80 to the battery. The switch arms 76 and 74 may be combined as a single switch, as a two pole double throw switch.
In operation, the quality of the battery 68 may be tested by closing switch 65 to contact 66, which will place the battery across the meter 54. With the potentiometer 67 properly calibrated, a good battery may read full scale on the meter.
In testing ignition wires and spark plugs, the switch arms 74 and 76 may be swung leftward to, respectively, bypass the resistor 73 and engage the arm 76 with contact 78 for connecting power to the circuit. It is then necessary to locate the coil 25 along the several wires, with the coil axis extending transverse of the wire, such as a wire 81 shown in FIG. 3, to lie in the magnetic field of the wire with the coil inductively coupled with the magnetic field. A properly operating ignition wire with the probe or pick-up 10 located as described, will produce a known reading on meter 54. Similarly, the pick-up is successively located along and similarly in inductively coupled relation with the several spark plugs. Here also, properly operating spark plugs will produce a known reading at meter 54. Of course, inoperative ignition wires or plugs will be identified by the absence of the correct meter reading.
In testing the distributor, as higher voltage and stronger electromagnetic field is there produced, the switch arms 74 and 76 are swung rightward to, respectively, place the resistor 73 in series with the meter 54 and close arm 76 to contact 79 for connecting power to amplifier 53 through conductor 80 to battery 68. The pick-up assembly 10 is then located in inductively coupled relation with the distributor, to ascertain whether a predetermined signal is generated in the coil by observing the meter 54. That is, the meter 54, including the resistor 73, is known to produce a predetermined indication responsive to a properly operating distributor. This is also true when the testing device is used in association with the newer electronic or high energy ignition systems.
From the foregoing, it is seen that the present invention provides an ignition circuit testing apparatus which is extremely simple in construction, durable and reliable throughout a long useful life, and which otherwise fully accomplishes its intended objects.
Although the present invention has been described in some detail by way of illustration and example for purposes of clarity of understanding, it is understood that certain changes and modifications may be made within the spirit of the invention.
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An ignition circuit tester including a pick-up coil assembly for inductive coupling with and location closely along a circuit element to be tested, an amplifier circuit for amplifying a signal picked up by the coil assembly, and a meter to indicate the signal.
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BACKGROUND
[0001] 1. Technical Field
[0002] An improved frame assembly is provided, such as for a window or door frame assembly, which is often referred to as a “door lite.” The improved frame assembly has a component structure that provides an alignment guide for placing two halves of the frame assembly together during transport and final assembly. The improved frame assembly also has a robust and adjustable locking mechanism.
[0003] 2. Description of the Related Art
[0004] Frame assemblies for door lites are generally known in the art. These frame assemblies are typically pre-manufactured in several pieces and shipped to another destination for assembly. For example, door lite frame assemblies can come in two sub-parts, which are secured together with a piece of glass or other transparent or insulating material, such as a glazing panel, in-between the two sub-parts. There are many existing frame assemblies having different types of external clips or other external fasteners (such as screws) for securing the frame assembly together.
[0005] Unfortunately, installation of these existing door lite frames with external fasteners can be time consuming. For example, in prior art door lite frames, when the frame assembly arrives at the place of installation, the frame sub-parts typically are separated by removing fasteners that held the sub-parts together during transportation. Then during installation, the frame sub-parts are positioned and resecured together with fasteners. Each fastener that needs to be removed after shipment and resecured during installation, decreasing the efficiency of installation and increases costs.
[0006] Another drawback to the existing door lite frames is that any fasteners, or holes for the fasteners, that are visible from the exterior of the door lite can detract from its aesthetic appeal. Covering the visible ends of the fasteners or holes with a plug or putty, for example, requires additional costs and introduces more inefficiency during installation.
[0007] An example of a prior art door lite frame assembly is shown in FIG. 1 . The prior art door lite 1 has two frame sub-parts 2 and 3 that secure there-between a piece of glass 8 . When installed, threaded fasteners 5 are screwed into the threaded holes 6 and 7 , securing the glass 8 between the frame sub-parts 2 and 3 .
[0008] This prior art door lite 1 is not desirable for several reasons. For example, the door lite 1 does not have an efficient and simple way to be aligned or secured during transport from the manufacturing facility to the place of final installation. While the frame sub-parts 2 and 3 can be aligned and secured together with the threaded fasteners 5 before transport, this is undesirable because of the time involved securing the door lite 1 prior to transport, removing the threaded fasteners 5 at the place of installation, and then resecuring the threaded fasteners 5 during final installation. Moreover, the exposed holes 6 and 7 are undesirable.
[0009] Door lites without external threaded fasteners have been the subject of U.S. patents, but these door lites suffer from their own problems. For example, a “screwless” door lite is disclosed in U.S. Pat. No. 6,925,767 by Krochmal et al. and U.S. Pat. No. 7,010,888 by Tumlin et al., however these designs do not provide for a shipping orientation or integral parts necessary for alignment in a shipping orientation. Not having a shipping orientation that provides guided interconnection of matching frame assembly sub-parts is a major drawback to these designs. It is desirable to have two matching frame parts aligned together during shipping because this helps ensure that matching parts are transported and delivered together, and it allows a glass panel or glazing to be held in-between the matching frame parts during shipping.
[0010] Door lites with shipping and installation orientations have also been the subject of U.S. patents, but these door lites also suffer from their own shortcomings. For example, the door lites disclosed in U.S. Pat. No. 6,694,701 by Wang et al. and U.S. Pat. No. 7,386,959 by Ouellette are inadequate because neither provide for a guided interconnection of matching frame assembly sub-parts in both the shipping and installation orientations via parts formed on the door lite frame.
[0011] Rather, Ouellette describes clip structures that are separate components from the door lite frame, thus adding to the cost of manufacturing and increasing the complexity of installation. Similarly, the frame disclosed by Wang et al. suffers from multiple deficiencies. While the frame of Wang et al. provides a shipping and installation orientation, there is no provision for guided interconnection in the installation orientation, leading to misalignment during installation. Moreover, the frame of Wang et al. requires separate structures for orienting the frame during shipping and permanently coupling the frame halves together. These separate structures increase the manufacturing cost and multiply the complications for properly orienting the frame halves during shipping and installation.
[0012] Existing door lite frames with an installation alignment system have also proven difficult and cumbersome. For example, U.S. Pat. No. 7,331,142 by Gerard describes a connector system for the shipping and installation orientations, but the alignment system is inadequate and does not provide for minimization of localized torsion that can lead to misalignment during installation and permanent interconnection. The frame disclosed by Gerard is therefore difficult to properly align during installation, leading to problems from the frame halves being permanently connected out of alignment.
[0013] Moreover, many of the prior door lites, such as those disclosed by Gerard, Ouellette and Wang et al., do not provide interconnects that acceptably accommodate a wide range of varying thicknesses in the structure sandwiched between the two halves of the frame structure. For example, the two subparts of a door lite frame assembly typically need to be installed on outside portions of a door or frame that is supposed to be 1¾ inches, but the thickness of the door or frame may vary by as much as 0.06 to 0.09 inches. This variance is complicated by differences in thicknesses of other materials and structures that are often placed between the door lite frame and the structure therebetween, for example foam, seals or other gaskets, and panels such as glass or glazing.
[0014] Another complication during installation from inadequate provisions for thickness variations is that the door lite frame halves have inadequate connection and retention. For example, in the prior door lites, it is difficult to discern if all of the interconnects are properly connected. Due to the variances in thicknesses in the door lite materials, the opportunity of an improper connection during installation is magnified. Thus, these prior door lite frames may unintentionally separate and come apart after installation.
[0015] There is a need for a door lite frame system that provides an adjustable interconnect that can handle variations in thicknesses around the door lite frame. There is also a need for the door lite frame system to provide an alignment structure that is used in both shipping and installation orientations and can also minimize torsion and rotation during installation. Moreover, it is highly desirable for that frame system to be durable and easy to assemble. It is also desirable for that system to have a low cost production with the frame system providing a structure that is easily assembled both in the shipping and installation orientation. No prior art door lite frame system provides all of these desired features.
BRIEF SUMMARY
[0016] In embodiments of the present frame system, some to all of the aforementioned problems are overcome. For example, in certain embodiments, a frame assembly is provided that has orientation structures that substantially axially align in a geometrically congruent fashion two frame halves, with the orientation structures aligning the frame system in both a shipment and an installation orientation. In some embodiments, the orientation structures are configured to provide removable engagement in a shipping orientation so that the frame halves can be quickly and easily decoupled at the place of installation.
[0017] Moreover, the orientation structures are configured to provide, in embodiments, a rotational stiffness that substantially holds the two frame halves in alignment and substantially prevents axial rotation of the two frame halves out of alignment. Significantly, in some embodiments, even a single pair of orientation structures, including an orientation guide or pin on one frame half and an orientation receiver or aperture on the other frame half, provide this alignment and rotational stiffness.
[0018] Also, in certain embodiments of the present frame system, an interlocking structure is provided that is configured for progressive locking during installation that can accommodate various sizes of materials that may be installed between the two halves of the frame system. Thus, in embodiments having the progressive locking feature, various sizes of material, for example doors, walls, glass, glazing or other materials of substantially different thicknesses, can be installed within the same size framing system without having to change the dimensions of the framing system.
[0019] Significantly, in some embodiments, the orientation structures and the interlocking structures work in cooperation to provide a frame system that is robust and easy to align, assemble, and install. For example, the orientation structures cooperate to help ensure that the interlocking structures are aligned and actually lock together during installation, even for embodiments where only one pair of orientation structures is provided.
[0020] Also, in embodiments, interaction between the orientation structures and the interlocking structures provides added strength to the frame system. For example, even in embodiments where the orientation structures are separate and distinct from the interlocking structures, rotational stiffness from the orientation structures substantially prevents the two frame halves from axially rotating and the interlocking structures from slipping out of a locked interaction. Moreover, the orientation structures can be configured to absorb forces placed on the frame halves, thereby reducing any stress, force and torque that may act on the interlocking structures.
[0021] For example, in some embodiments, a frame assembly is provided that comprises a first frame structure with corresponding first interlocking members and first alignment members substantially parallel to each other and aligned in substantially a same plane. Also, in embodiments, a second frame structure is also provided that has second alignment members each having at least one second interlocking member formed thereon. In these embodiments, the first and second frame structures have a shipping and installation orientations with respect to one another separated by approximately 180 degrees, with the first and second alignment members configured to be engaged in both orientations. In the shipping orientation, the first and second alignment members are configured to be removably engaged, and in the installation orientation, are configured to be substantially permanently engaged by corresponding sets of first interlocking members and second interlocking members. In these embodiments, alignment in both the shipping and installation orientation is provided by the second alignment members each having an aperture that is substantially geometrically congruent with a shape of each of the first alignment members. Thus, even for embodiments having a single set of first and second alignment members, the frame system is aligned during shipping and installation.
[0022] These and many other embodiments of the present frame system are provided for and described in the accompanying drawings, detailed description, and claims. Moreover, methods of manufacturing the frame system as well as methods of assembling the frame system in the shipping and installation orientations are provided for and described in the accompanying drawings, detailed description, and claims.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0023] FIG. 1 is an isometric view of a prior art frame system;
[0024] FIG. 2 is an isometric view of an unassembled embodiment of the present frame system;
[0025] FIG. 3 is an isometric view of an embodiment of the present frame system assembled in an installation orientation;
[0026] FIG. 4 is an isometric view of a portion of FIG. 3 showing engaged alignment and locking mechanisms;
[0027] FIG. 5 is a side view of an embodiment of the present frame system in the installation orientation;
[0028] FIG. 6 is a side view of a portion of an embodiment of the present frame system in the installation orientation showing details of alignment and locking between the first and second halves with an embodiment of a progressive locking feature in a first locked position;
[0029] FIG. 7 is a cross-sectional view of FIG. 6 ;
[0030] FIG. 8 is a side view of a portion of an embodiment of the present frame system in the installation orientation showing details of alignment and locking between the first and second halves with an embodiment of a progressive locking feature in a second locked position;
[0031] FIG. 9 is a cross-sectional view of FIG. 8 ;
[0032] FIG. 10 is a side view of a portion of an embodiment of the present frame system in the installation orientation showing details of alignment and locking between the first and second halves with an embodiment of a progressive locking feature in a third locked position;
[0033] FIG. 11 is a cross-sectional view of FIG. 10 ;
[0034] FIG. 12 is a side view of an embodiment of the present frame system in a shipping orientation;
[0035] FIG. 13 is a side view of an embodiment of the present frame system in a shipping orientation showing details of alignment between the first and second halves;
[0036] FIG. 14 is a side view of an embodiment of a frame half of the present frame system showing orientation receivers and locking structures formed thereon;
[0037] FIG. 15 is an isometric view of an embodiment of a frame half of the present frame system showing orientation receivers and locking structures formed thereon;
[0038] FIG. 16 is bottom view of an embodiment of a frame half of the present frame system showing orientation receivers and locking structures formed thereon;
[0039] FIG. 17 is an isometric view of an embodiment of a frame half of the present frame system showing orientation guides and locking structures formed thereon;
[0040] FIG. 18 is a side view of an embodiment of a frame half of the present frame system showing orientation guides and locking structures formed thereon;
[0041] FIGS. 19A-19D are isometric views of alternative embodiments of the present frame system showing orientation guides, orientation receivers and locking structures formed thereon; and
[0042] FIG. 20 is a block diagram of methods of manufacturing and assembly of various embodiments of the present frame system.
DETAILED DESCRIPTION
[0043] Referring to FIGS. 2-4 , an embodiment of a frame system or frame assembly is illustrated. In FIG. 2 , an exemplary frame system 10 is shown unassembled in two parts or halves, with a first frame member 20 below a second frame member 30 . In an exemplary embodiment, the frame system 10 has a rectangular shape with a plurality of diametrically opposed straight sides. In other embodiments, the frame system 10 and frame halves 20 / 30 can be substantially larger or smaller than the illustrated structure and can have other shapes, such as other rectangular, oblong, elliptical, square, circular, or triangular shapes or a combination of shapes.
[0044] The frame system 10 and the first and second frame halves 20 / 30 , including all of the elements formed thereon, can be formed using known techniques, such as injection molding. Pliable materials, such as Acrylonitrile Butadiene Styrene (ABS), other plastics, or other pliable materials can be used to make the frame system 10 . Alternatively, rigid materials, such as nylon, metal, glass or other rigid materials, can be used to make the frame system 10 . In other embodiments, the frame system 10 can be made of multiple materials, including combinations of pliable and rigid materials.
[0045] In an exemplary embodiment, the first half 20 of the frame structure has a first alignment member and a first interlocking member. For example, in embodiments, first half 20 of the frame structure has an orientation guide 40 and a first locking structure 50 that are each a longitudinally projecting member formed on an inner portion of the first half 20 . In embodiments, the first locking structure 50 and the orientation guide 40 are separate and distinct structures spaced apart from one another, as depicted in FIG. 2 (or FIG. 18 ). In other embodiments, the first locking structure 50 and the orientation guide 40 can be formed together as one piece. Also, in embodiments, one or more of the orientation guides 40 and first locking structures 50 can be formed apart from the first half 20 of the frame system 10 and attached thereto.
[0046] In embodiments, the first locking structure 50 includes at least one ledge or arm 55 laterally extending from and formed on a portion of the first locking structure 50 . In embodiments, there are a plurality of ledges or arms 55 formed on the first locking structure 50 . In an exemplary embodiment, the arms 55 are formed on only one side of the first locking structure 50 . In embodiments, the arms 55 laterally project from the first locking structures 50 at an angle, such as 45 degrees.
[0047] In embodiments, there are a plurality of orientation guides 40 and a plurality of first locking structures 50 formed on the inner portion of the first frame member 20 and are separate components spaced apart from one another. One orientation guide 40 and one first locking structure 50 form a unit, with the orientation guide 40 and first locking structure 50 separate and distinct from one another but spaced proximately to one another. In embodiments, corresponding orientation guides 40 and first locking structures 50 are formed substantially parallel to one another and project from the first frame member 20 in substantially parallel planes. For each unit, the arms 55 laterally project into a space between the orientation guide 40 and first locking structure 50 . In embodiments, the orientation guides 40 and first locking structures are spaced evenly about an inner portion of the first half 20 of the frame system 10 .
[0048] In an exemplary embodiment, the second half 30 of the frame structure has a second alignment member and a second interlocking member. For example, in embodiments, the second half 30 of the frame structure 10 comprises an orientation receiver 60 that is a longitudinally projecting member formed on an inner portion of the second half 30 , with the orientation receiver 60 comprising a second locking structure 65 formed on an outer portion of the orientation receiver 60 . In other embodiments, one or more of the orientation receivers 60 and second locking structure 65 can be formed apart from the second half 30 of the frame system 10 and attached thereto.
[0049] In embodiments, the second locking structure 65 is at least one lateral projection or ledge, for example, an arm or other structure, or a plurality of such structures, such as a saw-tooth structure or serrated teeth. In this embodiment, there are a plurality of orientation receivers 60 , each having a second locking structure 65 formed thereon, and the orientation receivers 60 are spaced evenly about an inner portion of the second half 30 of the frame system 10 . In embodiments, the second locking structures 65 are a plurality of triangular saw tooth ledges extending from the side of the orientation receivers 60 with a flat top surface and an angled bottom surface, for example 45 degrees.
[0050] Although the frame assembly 10 is shown in embodiments having two frame halves 20 / 30 with different structures on each half, in alternative embodiments, the two frame halves can be similar or substantially identical. For example, instead of having the orientation guides 40 and first locking structures 50 only on the first frame half 20 and the orientation receivers 60 and second locking structures 65 only on the second frame half 30 , these various elements can be placed on both frame halves 20 / 30 providing identical frame halves 20 / 30 . In these alternative embodiments, the orientation guides 40 can be configured with corresponding orientation receivers 60 and the first locking structures 50 can be configured with corresponding second locking structures 65 to provide guided alignment of the two frame halves 20 / 30 for shipping and installation orientations and to provide interlocking of the first and second locking structures 50 / 65 during installation.
[0051] Referring to FIGS. 3-4 , an embodiment of the frame assembly 10 is shown in an installation orientation with the orientation guides 40 engaged with the orientation receivers 60 and the first locking structures 50 engaged with the second locking structures 65 . In certain embodiments, orientation guides 40 and orientation receivers 60 are means for aligning the first and second frame halves 20 / 30 during installation. In certain embodiments, the first locking structures 50 and the second locking structures 65 are means for coupling the first and second frame halves 20 / 30 during installation.
[0052] FIG. 4 shows in greater detail the engagement of the orientation guides and receivers 40 / 60 and first and second locking structures 50 / 65 . When the first and second locking structures 50 / 65 are engaged and the first and second halves 20 / 30 of the frame 10 are locked together, a piece of material, such as glass or glazing, can be held in place between an inner surface 90 of the first half 20 and an inner surface 95 of the second half 30 . The distance between the surfaces 90 / 95 is reflected in FIG. 5 by “d”, while the corresponding spacing about the perimeter of the frame 10 , where the frame sandwiches a door or other structure, is designated by “D”.
[0053] With reference to FIGS. 5-11 , engagement of the orientation guides and receivers 40 / 60 and first and second locking structures 50 / 65 will be explained in greater detail. FIG. 5 shows a side view of the frame system 10 with the first and second halves 20 / 30 engaged in an installation orientation. In certain embodiments, the first and second locking structures 50 / 65 are configured to provide a progressive locking mechanism wherein the first and second halves 20 / 30 are able to be locked together in an increasingly closer relationship.
[0054] Significantly, in embodiments having the first and second locking structures 50 / 65 , the progressive locking mechanism allows materials of various thicknesses to be installed between the same two frame halves 20 / 30 without having to change the dimensions of the first and second locking structures 50 / 65 . In some embodiments, the progressive locking feature is provided in part by a plurality of laterally extending arms 55 formed lengthwise on a portion of the first locking structure 50 that engage a plurality of second locking structures 65 formed lengthwise on a portion of the orientation receiver 60 .
[0055] For example, engagement of the orientation guides and receivers 40 / 60 and first and second locking structures 50 / 65 is shown in a progressive manner in FIGS. 6-11 . In FIG. 6 , the first and second halves 20 / 30 of the frame system are brought together, with the orientation guide 40 inserted into the orientation receiver 60 , thereby aligning the second locking structures 65 on the orientation guide 60 to be in substantially the same plane as the arms 55 on the first locking structure 50 before the arms 55 of the first locking structure 50 engage the second locking structure 65 on the orientation guide 60 . As the first and second halves 20 / 30 of the frame system are pushed together, a leading edge 70 of the orientation receiver 60 reaches a proximate edge 85 of a first arm 75 , pushing the first arm 75 down until it snaps into a crevice 80 of the second locking structure nearest the leading edge 70 of the orientation receiver 60 , thereby substantially permanently coupling or engaging the first and second frame members 20 / 30 . Then, as the first and second halves 20 / 30 of the frame system are pushed further together, the first and second locking structures 50 / 65 continue to engage and progressively lock or ratchet, with the arms 55 of the first locking structure 50 locking or ratcheting into crevices 80 of the second locking structure 65 .
[0056] In embodiments, the arms 55 of the first locking structure 50 are made of a material that allows the arms 55 to deflect as they are engaged by the second locking structures 65 , and also allows the arms 55 to snap back into or close to their original orientation as the arms 55 snap into the crevices 80 of second locking structures 65 . In alternative embodiments, the arms 55 can be made of a more resilient material and the second locking structures 65 can be made of a material that deflects when engaged by the arms 55 , which allows the second locking structures 65 to snap back into their original orientation as the second locking structures 65 lock with the arms 55 .
[0057] As shown in FIG. 6 , the first and second halves 20 / 30 of the frame system have been pushed together such that each of the arms 55 of the first locking structure 50 are in a crevice 80 of the second locking structure 65 . FIG. 7 is a cross-section of FIG. 6 , both showing a first distance d 1 between the inner surfaces 90 / 95 (and a corresponding distance D 1 ) of the respective frame halves 20 / 30 . FIG. 8 illustrates the first and second halves 20 / 30 of the frame system pushed together even further, with the leading edge 70 of the orientation receiver 60 proximate a distal end 100 of the orientation guide 40 . FIG. 9 is a cross-section of FIG. 8 , both showing a second distance d 2 /D 2 closer than the first distance d 1 /D 1 between the respective frame halves 20 / 30 . FIG. 10 illustrates the first and second halves 20 / 30 of the frame system pushed together even further, with the leading edge 70 of the orientation receiver 60 reaching substantially a same plane as a distal end 100 of the orientation guide 40 . FIG. 11 is a cross-section of FIG. 10 , both showing a third distance d 3 /D 3 closer than the second distance d 2 /D 2 between the respective frame halves 20 / 30 .
[0058] As can be appreciated from the progressive locking feature illustrated in FIGS. 5-11 , which can progressively decrease a distance between the first and second halves 20 / 30 of the frame system, the first and second halves 20 / 30 of the frame system can be locked together with a varying range of distance between the first half 20 and the second half 30 . This range of distance provided by the progressive locking feature allows for various widths or sizes of material that can be placed between the inner surface 90 of the first half 20 and the inner surface 95 of the second half 30 of the frame system, and can likewise accommodate for door or other structures of varying thicknesses.
[0059] Referring to FIGS. 2-4 and 12 - 13 , an embodiment of the present frame system 10 having a shipping and installation orientations will be discussed. An installation orientation of an embodiment of the frame system is shown in FIGS. 2-4 , with the first half 20 and second half 30 of the frame system 10 aligned such that when the two frame halves 20 / 30 are brought together, the orientation guides 40 engage the orientation receivers 60 . In embodiments, the orientation guides 40 have a greater height than the arms 55 of the first locking structure 50 so that the orientation guides 40 engage the orientation receivers 60 before the arms 55 of the first locking structure 50 engage the second locking structure 65 on the orientation receiver 60 . As a result, the interaction between the orientation guides 40 and the orientation receivers 60 helps ensure that the two frame halves 20 / 30 are properly aligned for installation prior to locking of the frame halves 20 / 30 together, with the outside perimeters of the first and second halves 20 / 30 of the frame assembly being substantially congruent. Once the geometry of the frame halves are properly aligned via the orientation guides 40 entering the orientation receivers 60 , the frame halves 20 / 30 can be pressed together, with the orientation guides 40 continuing to travel up into the orientation receivers 60 , and the first and second locking structures 50 / 65 engaging one another and substantially permanently locking the two frame halves together.
[0060] For shipping, however, it is desirable for the frame halves 20 / 30 to not be permanently locked together. Rather, it is desirable for the frame halves 20 / 30 to be easily separated just prior to installation. Also, it is desirable for the frame halves 20 / 30 to be aligned during shipment to keep matching frame halves 20 / 30 together and provide an efficient use of space during shipment, as well as to allow materials to be stored between the frame halves 20 / 30 during shipment. In certain embodiments, orientation guides 40 and orientation receivers 60 are means for aligning the first and second frame halves 20 / 30 during shipment.
[0061] In embodiments, the frame system 10 provides a shipping orientation by rotating one of the two frame halves 20 / 30 by 180 degrees axially from the orientation shown in FIGS. 2-4 . It can be appreciated, however, that rotation required between the shipping and installation orientations depends on the particular shape of the frame system 10 and frame halves 20 / 30 . For example, in embodiments where the frame system 10 or frame halves 20 / 30 have more than two axes of symmetry, such as circular, hexagonal, or square shapes, then rotation between shipping and installation orientations can be 90 degrees or less. In contrast, when the frame system 10 and frame halves 20 / 30 have only two axes of symmetry, such as an oblong, rectangle or elliptical shapes, then rotation between shipping and installation orientations will be 180 degrees.
[0062] Similar to the installation orientation, the orientation guides 40 and receivers 60 provide a guide to align the frame halves together in certain embodiments. In the shipping orientation, as shown in FIGS. 12-13 , the frame system 10 is aligned through engagement of the orientation guides 40 and orientation receivers 60 , while the second locking structures 65 do not engage the first locking structures 50 . Instead, the orientation guides 40 enter and engage the orientation receivers 60 , thereby providing alignment of the frame halves 20 / 30 during shipping with the outside perimeters of the first and second halves 20 / 30 of the frame assembly 10 being substantially congruent.
[0063] In embodiments, the orientation guides 40 and orientation receivers 60 are geometrically shaped such that when they engage one another, they are removably received or removably engaged. For example, in embodiments, a friction fit is provided between the orientation guides 40 and orientation receivers 60 when they are engaged. Thus, the friction fit between the orientation guides 40 and orientation receivers 60 hold the frame halves 20 / 30 together. The friction fit is also configured to be quickly and efficiently disengaged without having to release a locking structure. In alternative embodiments, however, the orientation guides 40 and orientation receivers 60 can be provided with a locking device or structure or wrapping material to provide greater strength in holding the frame halves 20 / 30 together during shipment.
[0064] In the embodiment shown in FIGS. 12-13 , the second locking structures 65 do not engage the first locking structures 50 in the shipping orientation because the second locking structures 65 are formed on one side of the orientation receiver 60 . The second locking structures 65 on the orientation receivers 60 are configured to be aligned and engage with the first locking structure when in the installation orientation (shown in FIG. 2 ), and in contrast, when one of the frame halves 20 / 30 is rotated 180 degrees axially, for example clockwise or counter-clockwise in a plane parallel with the installation orientation, until the frame halves are in a shipping orientation (shown in FIGS. 12-13 ).
[0065] In embodiments, one or both of the frame halves 20 / 30 can include fasteners, either as part of or separate from the frame system, to secure the frame halves together during shipping. For example, the frame halves 20 / 30 can be secured together with a fastener or wrapped with tape or plastic or a shipping material to hold the frame halves 20 / 30 together in the shipping orientation. Also, the orientation guides 40 and receivers 60 can be shaped such that when the guides 40 engage the receivers 60 , there is a friction fit holding the frame halves 20 / 30 together in the shipping orientation.
[0066] Embodiments of the orientation receiver 60 and second locking structure 65 will be discussed with reference to FIGS. 14-16 . In an embodiment, the orientation receivers 60 are formed on an inside portion of one of the two halves 20 / 30 of the frame system 10 with the orientation receivers evenly spaced around the frame half. In alternative embodiments, however, the orientation receivers 60 can be formed on the other frame half 20 , or alternatively, the orientation receivers 60 can be formed on both of the frame halves 20 / 30 . Moreover, in embodiments, the orientation receivers 60 can be unevenly spaced around one or more of the frame halves 20 / 30 , and the second locking structures 65 can be formed on only a portion of the total number of orientation receivers 60 , for example, on every other orientation receiver 60 or some other random or systematic selection.
[0067] As shown in FIG. 14 , in embodiments, the second engagement structures 65 are formed on the orientation receiver 60 such that when the frame halves 20 / 30 are aligned in the installation orientation (shown in FIGS. 2-4 ), the second locking structures 65 face the first locking structures 50 (i.e., the second locking structures 65 and the first locking structures face each other) and are therefore axially aligned with and capable of engaging each other when the orientation guide 40 is inserted and pushed into the orientation receiver 60 . In contrast, when one of the frame halves 20 / 30 is axially rotated 180 degrees with respect to the other, the second engagement structures 65 do not face the first locking structures 50 (i.e., the second locking structures 65 and the first locking structures face the same direction) and therefore not engage each other when the orientation guide 40 is inserted and pushed into the orientation receiver 60 , as shown in FIGS. 12-13 .
[0068] With reference to FIGS. 15-16 , in embodiments, the orientation receivers 60 each define a closed rectangular cavity, with the second locking structures 65 formed on only one side of each orientation receiver 60 . In alternative embodiments, the orientation receiver 60 can be other shapes, for example other rectangular, oblong, elliptical, square, circular, or triangular shapes or a combination of shapes. In alternative embodiments, the second locking structures 65 can be formed on more than one side of the orientation receiver 60 or can be absent from the orientation receiver 60 . In alternative embodiments, the orientation receiver 60 and second locking structures 65 can be separate structures formed on the same or different halves 20 / 30 of the frame system.
[0069] Referring to FIGS. 6 and 16 , in embodiments, the second locking structures 65 are a plurality of ridges formed on the orientation receiver 60 , where the ridges are configured to engage and provide a locking fit with at least a portion of the first locking structure 50 . In alternative embodiments, the second locking structures 65 can be any number of structures, such as another ledge, arm or saw tooth or a different structure having one or more segments configured to engage and lock with at least a portion of the first locking structure 50 .
[0070] Embodiments of the orientation guide 60 and first locking structure 50 having arms 55 will be discussed with reference to FIGS. 17-18 . In an embodiment, the orientation guides 40 and first locking structures 50 are formed on an inside portion of one of the two halves 20 / 30 of the frame system 10 with the orientation guides 40 and first locking structures 50 formed separately, evenly spaced around the frame half 20 in corresponding pairs. In alternative embodiments, however, the orientation guides 40 and first locking structures 50 can be formed on the other frame half 30 , or alternatively, the orientation guides 40 and first locking structures 50 can be formed on separate frame halves 20 / 30 or on both of the frame halves 20 / 30 . Moreover, in embodiments, either or both of the orientation guides 40 and first locking structures 50 can be unevenly spaced around one or more of the frame halves 20 / 30 , and in embodiments, the arms 55 of the first locking structures 50 can be formed on only a portion of the total number of first locking structures 50 , for example, on every other first locking structure 50 or some other random or systematic selection.
[0071] As shown in FIG. 18 , in embodiments, the arms 55 are formed on the first locking structure 50 such that when the frame halves 20 / 30 are aligned in the installation orientation (shown in FIGS. 2-4 ), the arms 55 face the second locking structures 65 (i.e., arms 55 and the second locking structures 65 face each other) and are therefore axially aligned and capable of engaging each other when the orientation guide 40 is inserted and pushed into the orientation receiver 60 . In contrast, when one of the frame halves 20 / 30 is axially rotated 180 degrees, the arms 55 do not face the second engagement structures 65 (i.e., the arms 55 and the second locking structures 65 face the same direction) and are therefore not axially aligned and do not engage each other when the orientation guide 40 is inserted and pushed into the orientation receiver 60 , as shown in FIGS. 12-13 .
[0072] In embodiments, the orientation guides 40 are formed in a geometric shape that is substantially congruent with a geometric shape of an aperture formed within the orientation receivers 60 . For example, in embodiments, the orientation guides 40 are each a closed rectangular structure formed on an inner surface of the frame half 20 with the rectangular structure having a rectangular shape substantially similar to the closed rectangular cavity of the orientation receivers 60 . In alternative embodiments, the orientation guide 40 and orientation receivers 60 can be other shapes, for example other rectangular, oblong, elliptical, square, circular, or triangular shapes or a combination of shapes. In alternative embodiments, the arms 55 can be formed on more than one side of the first locking structure 50 or can be absent from the first locking structure 50 . In alternative embodiments, the arms 55 and first locking structure 50 can be separate structures formed on the same or different halves 20 / 30 of the frame system.
[0073] Referring to FIGS. 6 and 18 , in embodiments, the arms 55 are a plurality of ledges formed on the first locking structure 50 , where the ledges are configured to engage and provide a locking fit with at least a portion of the second locking structures 65 . In alternative embodiments, the arms 55 can be any number of structures, such as another ledge, arm or saw tooth or another structure having one or more segments configured to engage and lock with at least a portion of the second locking structure 65 .
[0074] Referring to FIGS. 19A-19D , alternative embodiments of the orientation guide 40 , orientation receiver 60 , and first and second locking structures 50 / 65 will be discussed. As shown in FIGS. 19A and 19B , the orientation guides 40 and orientation receivers 60 each have corresponding tapered upper portions 40 A and 60 A leading to substantially similar rectangular cross-sections beyond the tapered portions. Likewise, in embodiments, the first locking structures 50 have a tapered upper portion 50 A. In these embodiments, misalignment or butting of the upper portions of the orientation guides and receivers 40 / 60 is less likely to occur because the upper tapered portions 40 A and 60 A have a tapered or curved cross-sectional area at the top for initial engagement, and then have increasing flat corresponding cross-sectional areas as the orientation guides and receivers 40 / 60 are engaged and aligned together.
[0075] In these embodiments, the tapered upper portions 40 A and 60 A facilitate alignment of the frame halves 20 and 30 in either the shipment or installation orientations. As the frame halves 20 and 30 are brought together, the uppermost tapered portions 40 A and 60 A of at least one pair of corresponding orientation guides 40 and orientation receivers 60 engage one another, thereby aligning at least a portion of the frame halves 20 and 30 , and also allowing some axial rotational movement between the frame halves 20 / 30 .
[0076] The axial rotational movement allowed by the engagement of the uppermost tapered portions 40 A and 60 A facilitates engagement and alignment of other corresponding orientation guides 40 and orientation receivers 60 . For example, variations in geometry of materials between the frame halves 20 / 30 and variations in tolerances of the frame halves 20 / 30 and their corresponding elements can be accommodated by limited axial rotation movement between the uppermost tapered portions 40 A and 60 A of engaged orientation guides 40 and orientation receivers 60 until the remaining orientation guides 40 and orientation receivers 60 are aligned and engaged.
[0077] In either the shipment or installation orientations, once the orientation guides 40 and orientation receivers 60 have been aligned and engaged by at least their uppermost tapered portions 40 A and 60 A, the orientation guides 40 and orientation receivers 60 can be pressed together until the orientation guides 40 are received by the orientation receivers 60 beyond the uppermost tapered portions 40 A and 60 A.
[0078] In embodiments, for example, with reference to FIGS. 6-11 and 19 A- 19 B, the tapered upper portion 40 A of the orientation guide 40 can be pressed into the corresponding orientation receiver 60 until the tapered upper portion 40 A of the orientation guide 40 rests upon a corresponding tapered portion of the second frame half 30 . Similarly, the tapered upper portion 60 A of the orientation receiver 60 can engage the corresponding orientation guide 40 until the tapered upper portion 60 A of the orientation receiver 60 rests upon a corresponding tapered portion of the first frame half 20 . In embodiments, where the tapered upper portions 40 A/ 60 A of the orientation guides and receivers 40 / 60 rest upon the frame halves 20 / 30 , the tapered upper portion 50 A of the first locking structures can also rest upon a corresponding tapered portion of the second frame half 30 .
[0079] In alternative embodiments, the upper portions of the orientation guides 40 , orientation receivers 60 and the first locking structures 50 can have cross-sectional areas different than that discussed above and depicted in the corresponding Figures. For example, in alternative embodiments depicted in FIGS. 19C and 19D , the upper portions of the orientation guides 40 , orientation receivers 60 and the first locking structures 50 are not tapered or curved, but rather each have flat upper portions.
[0080] In embodiments, the upper lip of the orientation guides 40 , orientation receivers 60 and the first locking structures 50 can be uniform and rectangular, without tapered or curved upper portions, as shown in FIGS. 19C and 19D . In these alternative embodiments, the orientation guides 40 and orientation receivers 60 can still engage one another and align the frame halves in the shipment and installation orientations 20 / 30 , and the first and second locking structures 50 / 65 can still engage one another in the installation orientation.
[0081] In these embodiments depicted in FIGS. 19C and 19D , the frame halves 20 / 30 can be adapted to have flat portions that correspond to the flat upper cross-sectional area of the orientation guides 40 , orientation receivers 60 and the first locking structures 50 . Thus, in embodiments, for example, the flat upper portion of the orientation guide 40 can be pressed into the corresponding orientation receiver 60 until the flat upper portion of the orientation guide 40 rests upon a corresponding flat portion of the second frame half 30 . Similarly, the flat upper portion of the orientation receiver 60 can engage the corresponding orientation guide 40 until the flat upper portion of the orientation receiver 60 rests upon a corresponding flat portion of the first frame half 20 . In embodiments where the flat upper portions of the orientation guides and receivers 40 / 60 rest upon the frame halves 20 / 30 , the flat upper portion of the first locking structures 50 can also rest upon a corresponding flat portion of the second frame half 30 .
[0082] In other embodiments, the frame halves 20 / 30 can be configured with one or more of the orientation guides 40 , orientation receivers 60 , and first and second locking structures 50 / 65 depicted in FIGS. 19A-19D . For example, in embodiments, a frame system can include orientation guides 40 , orientation receivers 60 , and first locking structures 50 both with tapered or curved upper ends and flat, non-tapered upper ends.
[0083] In embodiments having at least one half of the frame system with an orientation receiver defining a cavity having at least one flat portion, for example orientation receiver 60 , the orientation receiver can engage a corresponding orientation structure on the other half of the frame system, for example orientation guide 40 , or other orientation structures with a shape substantially similar to the shape of the orientation receiver's cavity or aperture. When the orientation receiver and corresponding flat outer portion(s) of the orientation guide engage each other, interaction between the flat inner portion(s) of the orientation receiver and corresponding flat outer portions of the orientation guide provide for alignment between the orientation receiver and orientation guide, and as a result, alignment between the first and second halves of the frame system. Thus, alignment between the first and second halves of the frame system can be provided for by a single orientation receiver on one frame half and a single orientation guide on the other frame half.
[0084] In embodiments having orientation receivers 60 and orientation guides 40 , it can be appreciated that once one pair of a corresponding orientation receiver 60 and guide 40 engage each other, the entire frame system 10 will be aligned in either the shipping orientation or the installation orientation.
[0085] Significantly, this relationship provides assurances during installation that when the orientation receivers 60 and orientation guides 40 are aligned, each of the first and second locking structures 50 / 65 will properly engage and substantially lock the two frame halves 20 / 30 together in proper alignment. Similarly, during shipment, when the orientation receivers 60 and orientation guides 40 are aligned, the frame halves 20 / 30 will be brought and held together in proper alignment in the shipping orientation.
[0086] In certain embodiments, interaction between the orientation guides 40 and orientation receivers 60 during alignment also restricts axial rotational movement between the two frame halves, resulting in a rotational stiffness with the first and second frame structures 20 / 30 being substantially rotationally fixed. For example, engagement of a single orientation guide 40 and orientation receiver 60 can substantially restrict the axial rotational movement of the two frame halves 20 / 30 from the flat surfaces of the orientation guide 40 and orientation receiver 60 pushing against each other. Accordingly, engagement of a single pair of a corresponding orientation guide 40 and orientation receiver 60 can result in both frame halves 20 / 30 being properly aligned, and moreover, can result in the frame halves 20 / 30 being substantially rotationally fixed, with axial rotational movement between the frame halves 20 / 30 being minimized or eliminated. In preferred embodiments, there are a plurality of orientation guides 40 , orientation receivers 60 , and first and second locking structures 50 / 65 to maximize the strength, flexibility, and ease of orientation and installation of the frame system.
[0087] Significantly, the added rotational stiffness from the orientation guides 40 and orientation receivers 60 provides added strength when the two frame halves 20 / 30 are in an installation orientation and the first and second locking structures 50 / 65 are engaged. Thus, in some embodiments, even though the orientation guide 40 is separate and distinct from the first and second locking structures 50 / 65 , the rotational stiffness from the orientation guides 40 and orientation receivers 60 substantially prevents the two frame halves 20 / 30 from axially rotating and the first and second locking structures 50 / 65 from slipping out of a locked interaction. Moreover, the first and second locking structures 50 / 65 can absorb forces placed on the frame halves 20 / 30 , thereby reducing any stress, force and torque that may act on the first and second locking structures 50 / 65 .
[0088] In embodiments having the progressive locking features provided by the first and second locking structures 50 / 65 , it can also be appreciated that as each arm 55 engages the second locking structures 65 , a greater force would be required to separate the two frame halves 20 / 30 . Accordingly, in these embodiments of the frame system 10 , flexibility is provided as to the force required to separate the two frame halves 20 / 30 once substantially permanently locked together in an installation orientation.
[0089] In certain embodiments, the interaction of the progressive locking mechanism of the first and second locking structures 50 / 65 along with the added rotational stiffness from the orientation guides 40 and orientation receivers 60 provides a significant improvement over other frame systems. For example, in tests of the first and second locking structures 50 / 65 and orientation guides 40 and orientation receivers 60 , there was a 50% greater strength than the locking features of the door lite frame described in U.S. Pat. No. 6,694,701.
[0090] In an exemplary embodiment, the frame assembly has two rectangular halves, forming a 15″×25″ door lite. First alignment members and first interlocking members are spaced equally around an inside perimeter of one of the frame halves, with spacing between adjacent first alignment members and first interlocking members being between approximately 25-28 mm, and the spacing between adjacent first alignment members and between adjacent first interlocking members being between approximately 150-160 mm. These dimensions and configurations are provided as an example only. One of ordinary skill in the art can use the present frame assembly and select dimensions and configurations appropriate for specific applications. Moreover, specific dimensions of the alignment and interlocking structures are dependant on the specific application and materials used. Thus, it is within the ordinary skill in the art to optimize particular dimensions for particular applications using the disclosed frame system.
[0091] Referring to FIG. 20 , and referencing embodiments found in FIGS. 2-19D , methods of manufacturing and assembling frame systems are described. For example, in embodiments, a frame system can be manufactured by the step 120 of providing a first frame member and a second frame member, for example first and second halves 20 and 30 of the frame system 10 . In an exemplary embodiment, the first frame member comprises one or more first longitudinally extending members for alignment, for example an orientation guide 40 , and one or more second longitudinally extending members having one or more ledges for interlocking, for example a first locking structure 50 with arms 55 . In an embodiment, one or more of the ledges of a second longitudinally extending member is within a space between corresponding first and second longitudinally extending members of the first frame member. In an exemplary embodiment, the second frame member comprises one or more third longitudinally extending members, for example orientation receiver 60 , having an aperture for alignment with a shape corresponding to the shape of the first longitudinally extending member and one or more ledges for interlocking, for example second locking structure 65 , formed on an outside portion of the third longitudinally extending member.
[0092] In embodiments, the frame system is manufactured in such a way as to provide the first and second frame members that are configured for a first shipping orientation, where at least one of the longitudinally extending members are able to be removably received by the apertures of at least one of the third longitudinally extending members. In the shipping orientation, the received first longitudinally extending members are substantially rotationally fixed to the corresponding third longitudinally extending members. Also, the frame system is manufactured to provide for a second installation orientation, where at least one of the first longitudinally extending members are received by the apertures of at least one of the third longitudinally extending members. In the installation orientation, at least one of the first set of ledges of the second longitudinally extending members engage at least one of the second set of ledges of the third longitudinally extending members, thereby substantially permanently coupling the received first longitudinally extending members and the corresponding third longitudinally extending members. In embodiments, the first and second orientations are approximately a 180 degree rotation from each other. Also, the frame assembly can be configured such that the first and second sets of ledges are only engaged in the installation orientation.
[0093] In some embodiments, the frame assembly is manufactured and configured to provide a frame assembly where at least one of the first and third longitudinally extending members are engaged in both the first and second orientations. This provides alignment of the frame system, with the outside perimeters of the first and second frame members being substantially congruent, in both the first and second orientations.
[0094] Once the frame assembly is manufactured, it can be assembled for shipment and for installation. For example, in embodiments, the first and second frame members provided in step 120 can be assembled for shipment by performing a step 140 of removably coupling the first and second frame members in a shipping orientation, with at least one of the first longitudinally extending members, for example orientation guide 40 , removably received within an aperture of at least one of the third longitudinally extending members, for example orientation receiver 60 , thereby substantially rotationally fixing the first and second frame members in a substantially geometric congruent alignment. In some embodiments, a panel, for example a piece of glass or glazing, can be inserted between the first and second frame members prior to the step 140 of removably coupling the frame members.
[0095] After shipping the frame assembly, a method of installation can be performed. For example, in embodiments, a step 160 of decoupling the first and second frame members from the shipment orientation is performed by removing at least one of the first longitudinally extending members from the aperture of at least one of the third longitudinally extending members, followed by rotating at least one of the first and second frame members approximately 180 degrees into an installation orientation. Then, a step 180 of inserting a gasket and a panel, for example glass or glazing, between the two frame members is performed. For example, placing the gasket and panel on an inside portion of one or more of the two frame members. The two frame members can then be assembled from opposing sides of a door or other structure by performing a step 200 of having at least one of the first longitudinally extending members, for example orientation guide 40 , received by at least one aperture of a third longitudinally extending member, for example orientation receiver 60 , such that at least one ledge of a second longitudinally extending member, for example first locking structure 50 and arm 55 , engage at least one ledge of a third longitudinally extending member, for example second locking structure 65 and orientation receiver 60 , thereby substantially permanently coupling the received first longitudinally extending member and the corresponding third longitudinally extending member. The two frame members can then be ratcheted together, via progressive engagement of the first and second sets of ledges, by pushing the two frame members together until a desired fit between the two frame members and the panel, door and/or other structures therebetween is achieved.
[0096] With respect to the various methods described, it is understood that other steps, techniques, configurations, components and processes are contemplated without departing from the subject matter contemplated herein. Moreover, while the invention has been described in connection with what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention is not to be limited to the disclosed embodiments, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
[0097] These and other changes can be made to the embodiments in lite of the above-detailed description. In general, in the following claims, the terms used should not be construed to limit the claims to the specific embodiments disclosed in the specification and the claims, but should be construed to include all possible embodiments along with the full scope of equivalents to which such claims are entitled. Accordingly, the claims are not limited by the disclosure.
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An improved frame assembly is provided, such as for a window or door frame assembly often referred to as a “door lite.” The improved frame assembly includes an integrally formed cooperative structure of interlocking members having a temporary transport alignment and an installation alignment. Significantly, the cooperative structure includes an alignment guide that engages in both the temporary transport alignment and installation alignment, and also includes an adjustable locking mechanism that engages in the installation alignment, wherein the adjustable locking mechanism can accommodate varying thicknesses of door lites.
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This application is a divisional application of our copending patent application Ser. No. 343,642, filed Jan. 28, 1982, abandoned.
BACKGROUND OF THE INVENTION
The catalytic pyrolysis of carbonaceous materials to produce carbon particles is well known. Many metal catalysts have been suggested for use in pyrolysis reactions. Group VIII metals, such as iron, cobalt, and nickel, are among the metals used.
THE INVENTION
It has been discovered that in the production of microfibrous carbon the action of the catalyst can be improved by the addition of a Group V element-containing substance.
OBJECTS OF THE INVENTION
It is an object of the invention to produce carbon fibers having high surface areas from oganic compounds at elevated temperatures.
It is another object of the invention to enhance the effectiveness of Group VIII metal catalysts in carbon fiber production by employing suitable quantities of one or more Group V substances.
It is another object of the invention to produce high surface area microfibrous carbon fibers using a catalyst combination containing a Group VIII metal oxide and phosphorus.
It is still another object of the invention to produce high surface area carbon fibers using a three component catalyst containing a Group VIII metal oxide, a Group III or IV metal oxide, and phosphorus.
DESCRIPTION OF THE INVENTION
The Carbon Containing Substance
Useful carbon sources or carbonaceous materials are organic compounds and oxides of carbon. The preferred organic compounds are hydrocarbons such as alkanes, alkenes, and alkynes, with butane, butadiene, and acetylene most preferred. The preferred oxide is carbon monoxide.
Mixtures of hydrocarbons, such as natural gas, can be employed as the carbon source.
In one embodiment of the invention, a hydrocarbon carbon source is diluted with a suitable quantity of inert gas, such as hydrogen or nitrogen. Useful dilution ratios include 0.5:1 to 15:1.
The Group VIII Metal Containing Substance
Useful Group VIII metal substances are free metals, and oxides or salts of these metals. Oxides are most preferred. Of the Group VIII metals--that is of metals having atomic numbers 26-28, 44-46, and 76-78--iron, cobalt, and nickel are preferred. Nickel is most preferred.
Mixtures of Group VIII metal containing substances can be used in the invention.
The concentration of Group VIII metal-containing substance used can vary from 1 to 100%. Preferably it will be 25-50%, based on total catalyst weight.
The Group III or IV Metal-Containing Substance
Of the Group III and IV elements, that is Group IIIa, IIIb, IVa, and IVb, those of Group IVb are preferred. Titanium and zirconium are favored. Titanium is most preferred.
Useful substances containing these metals are the free metals, their oxides, and their salts. Oxides are preferred.
Mixtures of metals from one or more of Group III and IV can be used in the invention. Normally, the concentration of Group III or IV metal-containing substance is between 0-99% based on the total weight of the catalyst, with 31% preferred.
One or more inert refractory materials can be substituted for all or part of the Group III or IV metal containing substances.
The Group V Element Containing Substance
Substances of both Group Va and Vb are contemplated for use. Of these, Group Va substances are preferred. Phosphorus and its compounds are most preferred.
The Group V substance can be an element, an oxide, or a salt. Phosphorus oxides, e.g., phosphates are highly preferred. Mixtures of Group V substances can be used.
The quantity of Group V metal substance employed will be between 0 and 10%, based on the total weight of catalyst, with 1-6% preferred.
Catalyst Preparation
In one embodiment, the catalyst composition of the invention is produced by the steps of:
(1) contacting a Group VIII metal containing substance with a Group III or IV metal containing substance;
(2) contacting the product of step (1) with a Group V element containing substance; and
(3) subjecting the product of step (2) to physical treatment such that a solid catalyst is produced.
Alternatively, steps (1) and (2) can be conducted simultaneously.
In another embodiment, the Group VIII metal containing substance is contacted with an inert support material and the resultant product is treated with a Group V element containing substance.
Step (3) will preferably comprise conventional operations, such as filtering, drying, and calcining.
While it is believed that the catalyst is operable in any physical form, it is preferred that the catalyst be in the form of granules.
If the catalyst is used in particulate or granular form, it is preferred that its particle size range from 10 to 300 mesh, preferably 50-100 mesh.
Reaction Conditions
The pyrolysis of the carbon containing substance takes place at elevated temperatures. Since pyrolysis, like destructive distillation, requires the breaking of covalent bonds, energy requirements are large.
The temperatures employed are usually between 500° C. to 1000° C., with preferred temperatures lying between 600° C. and 900° C. Operable pressures are those at which the carbon containing substance is gaseous.
The reaction takes place in any suitable apparatus designed for catalytic pyrolysis and carbon deposition. A non-static apparatus is preferred.
Typically, the carbon source is introduced at a GHSV of 1000 hr -1 to 7200 hr -1 , with 3600 hr -1 preferred. The "GHSV" (gas hourly space velocity) is the ratio of the gas volume to the catalyst volume per hour. Alternatively, the GHSV can be expressed as V/V/hr, indicating the ratio of gas volume to catalyst volume to unit time.
The Carbon Product
The carbon particles produced in accordance with the invention are smaller than conventional carbon fibers, i.e., those produced without a Group V element containing substance in the catalyst. Carbon particles produced in accordance with the invention have decreased average fiber diameters and average fiber lengths. The particles of the invention have average surface areas which are three to four times greater than those of conventional carbon particles. It is believed that the increased surface area of the product gives it good binding strength for reinforcement applications.
while generally fibrous in microstructure, the carbon particles produced in accordance with the invention can be characterized in bulk as granular or nodular. Their principal feature is their uniquely high surface area which ranges from 150 to 200 m 2 /g.
EXAMPLE I
(Production of Catalyst)
About 2.6 moles of KOH (85%) was dissolved in 400 ml of water. 1.3 moles of flame-hydrolyzed TiO 2 was slurried in 600 ml of water and the pH of the slurry was adjusted to 8 by adding a few drops of KOH solution. 1.3 moles of Ni (NO 3 ) 2 ×6H 2 O was dissolved in 1300 ml of water. A portion of the unused KOH solution and all of the Ni (NO 3 ) 2 solution were added simultaneously to the TiO 2 slurry at rates which maintained the pH at 8. The remaining KOH was added to raise the pH to 9.0 (i.e. an OH/Ni molar ratio of 2). The resultant precipitate is filtered and washed to a K level equal to 0.1%.
After filtration 1.9 grams of H 3 PO 4 is added to one 1/4 of the solid to give 1.0% phosphorus in the final product. Enough water is added to slurry the gel to a thick slurry. The mixture is dried at 110° C. over night and calcined for 3 hours at 800° C. The granular product is NiTiO 3 containing 1.0% phosphorus and is 20/40 mesh in size. Its composition, in calculated weight percentages is: 37.6% Ni, 30.7% Ti, 30.7% O, 1.0% P, and 0.1% K.
EXAMPLE II
(Production of Carbon)
230.2 mg. of a 40/50 mesh NiTiO 3 catalyst containing 1% phosphorus (analysis for P showed 1.2%) was used in a TGA (thermal gravimetric analysis apparatus) to produce carbon particles. The carbon source was butane diluted at a 1:10 volume ratio with nitrogen gas. The butane/nitrogen mixture was supplied to the catalyst at a range of 0.0012 moles/min. (30 cc/min) at a temperature of 600° C. Rapid carbon growth (15.3 mg/min) took place until 600 mg had been deposited and breakout occurred. "Breakout" is the point at which further carbon deposits can no longer be weighed using the microbalance of a TGA apparatus. Prior to breakout, the rate of carbon growth accelerated from 12.8 mg/min for 0-100 mg carbon to 17.2 mg/min for 400-500 mg. 5.7 grams of carbon was formed. The final carbon to catalyst ratio was 24.8 The carbon particles had a surface area of 179 m 2 /g.
EXAMPLE III
(Use of catalysts having varying P content)
Five runs were conducted with NiTiO 3 catalysts containing varying amounts of added phosphorus. Butane diluted with inert gas was passed over the catalysts at 600° C. and atmosphere pressure.
______________________________________ Carbon Fiber Fiber Phosphorus Surface Diameter.sup.a Length.sup.aRun No. Weight % Area (m.sup.2 /g) (10.sup.-6 m) (10.sup.-6 m)______________________________________1 0 54 0.06 22 0.2 55 .sup.b --3 1.2 179 .sup.c --4 3.0 178 0.045 0.65 5.6 181 0.023 0.4______________________________________ .sup.a measured by transmission electron microscopy .sup.b observed by scanning electronic microscopy, insufficient resolutio for accurate measurement, but appears close to run #1 in dimensions. .sup.c observed by scanning electronic microscopy, insufficient resolutio for accurate measurement, but appear close to runs 4 and 5 in dimensions.
As the above table indicates, an increase in phosphorus concentration produces a decrease in the diameter and the length of the carbon fibers produced. Correspondingly, as the phosphorus concentration increases, the surface area of the carbon product increases.
Reasonable variations and modifications which will become apparent to those skilled in the art can be made in the present invention without departing from the spirit and scope thereof.
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The production of microfibrous carbon by the catalytic pyrolysis of carbonaceous materials in the presence of metal containing catalysts is improved by the presence of a small quantity of a phosphorus-containing substance.
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