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BACKGROUND OF THE INVENTION
This invention relates generally to improvements in electronic thermometer devices, and more particularly to electronic thermometers which will provide accurate and reliable temperature measurements which may be obtained without waiting for the temperature sensing unit to reach its stabilization point.
One of the primary measurements made in medicine is the measurement of the body's temperature. This measurement was historically made using a glass bulb mercury thermometer which is still used extensively despite obvious drawbacks. More recently, however, with the advent of sophisticated electronics, electronic thermometers have been developed. These instruments use thermocouples or thermistors as the temperature sensing device and then amplify and otherwise process the signal to provide an analog or digital readout. These devices have generally been rather bulky and cumbersome. Furthermore, they have been rather slow. This is due to the fact that temperature sensing unit require a rather long time to stabilize at the final temperature. Attempts have been made to alleviate this problem by using various schemes involving the anticipation of the final stabilized temperature.
It is therefore an object of the present invention to provide an electronic temperature measuring device which will accurately predict a stabilized temperature in a relatively short period of time.
It is a further object of the invention to provide a rapid output electronic temperature sensing instrument for use in the medical arts.
It is still a further object of the invention to provide a digital temperature display at a time prior to the temperature sensing instrument stabilization time.
It is another object of the present invention to provide apparatus producing a digital time display followed by a digital temperature display which is in anticipation of the final stabilized temperature.
SUMMARY OF THE INVENTION
The present invention provides apparatus to rapidly and accurately measure temperature without the necessity of waiting for a sensing instrument to reach a stabilized state. In order to accomplish such rapid temperature measurements, it is desirable to take the fewest possible sensor temperature samples. Obviously, one sensor temperature measurement representing a given instant will not be sufficient to predict a final stabilized sensor temperature. The present invention provides an algorithm and attendant computing apparatus sufficient to require that only two sensor temperature measurements to be taken. The algorithm of the invention recognizes that the response curve of a temperature sensing unit such as a thermistor as it gains or loses heat may be expressed as an exponential function in terms of the initial and final temperature values. This algorithm is useful generally because manufacturers of thermistors try very hard to obtain the exact resistance response curve for all devices of the same type. Upon solution of the algorithm of the present invention it is found that only two thermistor temperature measurements which represent instantaneous resistance are required. These two samples or measurements, however, must be made precisely at specified times, these times are determined by the thermal time constant of the particular type of thermistor in use. Once it is recognized that only two temperature measurements need be made, and the exact timing of these measurements is known then this information may be fed to a special purpose computer. Such computer, provided by the invention, then processes the measurement signals and produces a digital readout of the exact final temperature the thermistor will attain at a time well before the thermistor has actually stabilized.
As is well known, a thermistor presents a varying resistance when confronted with a varying temperature. A varying resistance, however, is not the most convenient signal with which to work. Therefore, the invention provides an analog to digital convertor which receives the varying resistance signal as measured by voltage from a thermistor circuit or the like and converts it to a frequency varying signal as required by the algorithm components. This is accomplished by utilizing the resistance of the sensing instrument as a component of a resistor-capacitor controlled oscillator. In this way, as the resistance varies so will the frequency of oscillation of the oscillator. Furthermore, by choosing the frequency of oscillation such that it will be a multiple of the actual temperature under measurement then the predicted temperature may be more easily obtained. This frequency varying temperature-dependent signal is then processed according to the mathematical equation, which was devised by the algorithm as previously discussed. Upon solution of this equation the actual temperature measurement may be easily displayed digitally by use of light emitting diodes or the like. In accomplishing this signal processing and timing operation a second oscillator is required; this oscillator may then be used with the display devices already incorporated to display a timing signal which could be used for obtaining a patient's pulse. Thus the patient's pulse rate may be determined simultaneously with the same patient's temperature.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a characteristic curve of the temperature response of a typical thermistor temperature sensing unit.
FIG. 2 is a block diagram of a preferred embodiment of electronic temperature measurement apparatus according to the present invention.
FIG. 3 is a schematic diagram of analog to digital converter as used in the preferred embodiment of the invention as shown in FIG. 2.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, a typical response curve of a temperature measuring instrument which utilizes a thermistor type sensing unit is shown. The ordinate axis T represents temperature. This response curve 10 is well known and is generally described as an exponential curve. A temperature at which the thermistor will be at rest is denoted as T R , a first measured temperature is T 1 , a second measured temperature T 2 and a final temperature T F . The response curve will theoretically approach this T F value asymptotically and hence the time that this temperature (T F ) will be reached will be infinity. The time of the at rest temperature T R is denoted as t o , while t 1 corresponds to the occurrence of the first temperature measurement T 1 and t 2 corresponds to the occurrence of the second temperature measurement T 2 .
Any temperature T along the response curve 10, at some time t, will be given by the equation:
T = T.sub.R + (T.sub.F -T.sub.R) (1 - e .sup.-.sup.t/.sup.τ) 1.
where τ represents the thermal time constant of the particular thermistor under consideration. If we write this equation (1) for the two temperature measurements T 1 , and T 2 , then solve for the final temperature T F , we have: ##EQU1##
by allowing (t 2 - t 1 ) to be represented by Δt, as shown in FIG. 1, equation (2) becomes: ##EQU2##
Since it is an objective of the invention to obtain a final temperature, without waiting for the sensing unit to stabilize, in the simplest manner possible, equation (3) should be solvable in the simplest manner also.
If we arbitrarily choose a value of ##EQU3## in order to allow equation (3) to be in its simplest form, we might choose 0.5, then: ##EQU4##
Having thus chosen the value in equation (4) we can then rewrite equation (3) as:
T.sub.F = 2T.sub.2 - T.sub.1 5.
rewriting equation (4) in different form yields ##EQU5## and solving for t,
Δt = t.sub.2 -t.sub.1 = τ ln 2 7.
Δ typical value for τ in a conventional thermistor might be 19 seconds. It is a simple matter to obtain the natural logarithm of 2 using tables, and then solving equation (7) for Δt we have:
Δt = 0.693 (19 sec.)≈13 sec. 8.
This means that the invention only requires a delay of 13 seconds between the first temperature measurement T 1 , and the second temperature measurement T 2 . Since the invention is intended for practical use, it has been found that upon the insertion of the thermistor probe into the patients body, the tissue surrounding the probe may be lowered in temperature momentarily by the lower temperature of the probe. Because of this it is advantageous to delay taking the first temperature measurement T 1 . For the case just discussed where Δt equals 13 seconds, a convenient delay time would be 17 seconds, thereby allowing the operational cycle to be 30 seconds, an ideal time in which to measure the patients pulse as discussed earlier.
Referring now to FIG. 2, a preferred embodiment of the invention is shown in block diagram form. The thermistor probe 20 is inserted into the patient's body orally or rectally or otherwise, and produces a signal on line 22 which is fed to an analog-to-digital converter 24. This analog to digital converter 24, converts the signal to a frequency varying signal. This converter 24 will be shown in more detail hereinafter. This signal of varying frequency is fed on line 26 to an up/down decade converter 28. This up/down decade counter 28 is of the conventional type and will be used to perform the operation required by equation (5). The signal on line 26 from the converter 24 has a frequency which is equal to, or represents, ten times the temperature as measured by the probe 20, where the numerical value of the frequency in HZ is 10 times the numerical value of the temperature in degrees. Because of this the up/down decade counter 28 can be used to solve equation (5). When the counter 28 is cleared by a signal on line 30, to either all zeroes or all ones, and the counter is selected to be a down counter by a signal on line 32, upon the first temperature measurement being clocked into counter 28, the counter will count down the exact number of pulse which appear on line 26. The counter 28 and the analog to digital converter 24 are enabled for a preselected period of time, 1 sec, by an enable signal appearing on line 34. The enable signal is produced by a logic unit 36 which will be explained in further detail later. In order to solve equation (5) the first measurement T 1 must be subtracted from twice the value of T 2 , upon this first use of the down counter the required subtraction has already been performed. A count-up signal now appears on line 32 from the logic unit 36, and a second temperature measurement T 2 on line 26 is counted up into counter 28. In order to accomplish the doubling of this measurement the signal on line 26 is allowed to enter the up-counter 28 for a time, 2 sec, defined by the enable signal on line 34, which is exactly two times the previously mentioned preselected time allowed for the down-counting function of the counter 28. In this way equation (5) is solved and the desired T F information is contained in the counter 28. This information is then fed by multi-channel lines 38 to a multiplayer 40, which in a simple embodiment may comprise merely digital switches The information is fed through the multiplexer 40 to a conventional decoder 42 which is used to decode the signal for display by well known light emitting diodes digital display 44. The light emitting diode decoder 42 is driven by a conventional driver unit 46, which also produces a signal on 48 which is fed to a over one-hundred indicator 50. The over one-hundred indicator 50 may be a simple flip-flop and is used to produce a signal, fed to the light emitting diodes digital display 44 on line 52, which inhibits or blanks an indication of any numeral other than a "one" in the hundreds column. Since in this embodiment of the invention the measurement period is 30 seconds and it is desired to display this time for use in another clinical function, i.e. pulse taking, an oscillator 54 is required having a frequency of oscillation given by 10Hz. The oscillator 54 signal is clocked into a conventional decade counter 56 on line 58. The counter 56 has already been cleared by the clear signal on line 30 which was also used to clear the up/down counter 28. The oscillator 54 also provides the general timing signals for the required operations of the subject invention, and so the contents of the decade counter 56 are fed by multi-channel lines 60 to the logic unit 36. In order to obtain the thirty-second display on the light emitting diodes digital display 44 the oscillator 54 clock pulses are fed through the decade counter and into the multiplexer 40 on multi-channel lines.
The logic unit 36 may be of a conventional design and would consist of standard gating and logic circuits arranged so as to provide the timing function, blanking pulses, enable signals at the appropriate times and for the appropriate durations. The logic unit also controls the multiplex unit 40 by a signal on line 62 so that first the thirty-second timing count is displayed, then the temperature information as contained in the decade counter 28 is displayed. A one-second blanking pulse on line 64 is also provided to supply a brief interval between the display of the two types of information.
In addition another function of the logic unit 36 is to provide a power off signal on line 66, which is fed to the power switch 68. This signal is produced at the end of a preselected time period during which the display device 44 is displaying the temperature information. A momentary contact start switch 70 is used to trigger the power switch 68, which then produces the counter clear signal on line 30 and serves to start the temperature measuring cycle.
Referring now to FIG. 3, the analog-to-digital converter, 24 of FIG. 2, is shown in more detail. This converter is actually an oscillator whose frequency of oscillation, dependent on R and C, is varied by varying R. In this case, a conventional operational amplifier 80 is connected in the conventional manner to form a free running multivibrator, with the exception that the thermistor probe 20 is included in the feedback connection. The variable resistance presented by the thermistor probe 20 when it resonates with the capacitor 82 determines the frequency of oscillation. Additional resistors 84 and 86 are included in the thermistor 20 input circuit in order to balance the input impedance to allow different probes, say rectal and oral, to be used interchangeably. The converter 24 is enabled as was stated by an enable signal on line 34 from the logic unit 36. This unit 36 turns on the converter 24 for one second for the first temperature measurement T 1 and for 2 seconds for the second temperature measurement T 2 .
It should be understood that the details of the foregoing embodiment are set forth by way of example only. Any type of thermistor probe may be utilized and the logic may comprise many well known forms. Accordingly, it is contemplated that this invention not be limited by the particular details of the embodiment as shown except as defined in the appended claims.
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An electronic apparatus to measure temperature which provides an accurate final temperature reading prior to the actual stabilization of the temperature sensor. An algorithm is provided which allows taking only two sensor temperature measurements at preselected times yet accurately predicts the sensor final or stabilization temperature. Temperature resistance varying signals are converted to temperature-frequency varying signals, clocked into an up/down counter, to compute final temperature which is displayed digitally. A thirty-second timing sequence is also digitally displayed for use when the invention is utilized for medical applications.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention relates generally to an apparatus and method for selectively applying grouting material directly to a targeted location.
[0003] 2. Description of Related Art
[0004] Grout is widely used to fill the gaps and seal the joints between floor and wall tiles, etc. Grout is known to come in a wide variety of types and colors to fit the specific requirements of the grouting job to be performed. Grout is typically prepared at or near the time and location of the project to be performed. Generally enough grout is prepared to complete the grouting of an entire target surface or group of surfaces. Applying grout from the same batch assures that the appearance of the grout on such target surface or surfaces will appear uniform. Grout is typically applied by spreading a grout material on the surface of a tiled surface and working the grout into the joints. After the filling of the joints are complete, the excess grout is scrapped off the tile. Next, the tiles are wiped off using a damp sponge, cloth or other suitable item. In performing such cleaning, operators must be careful not to remove the grout that has been worked into the joints; otherwise the operator must repeat the grouting steps to repair the damage to the previously grouted joint.
[0005] Applicators have been developed to reduce the time needed to apply grout to a tiled area. Such applicators attempt to reduce clean up time by attempting to apply the grout directly to the joint itself while avoiding contact with the tile surfaces. For example, an applicator has been developed which uses plunger for forcing grout out of a nozzle under pressure into the gap between tiles to ensure a proper amount of grout is within the gap. This device includes a tube assembly having a piston passageway with a smooth cylinder bore wall and a threaded tip end and an open handle end with a detachable unshaped hand grip assembly removably attached to the outside. Further, the tube assembly has a separate injector tube, nose piece and nozzle tip. Grout is forced out of the tube from the nozzle end, where, an operator, using two hands, grabs the u-shaped handle with one hand, and with the other hand, grabs the plunger handle and pushes on the plunger handle while pulling on the u-shaped handle end. The u-shaped hand grip assembly is removably attached to the outside of the tube assembly via a hose-type clamp. The hose-type clam has a screw and worm drive where the u-shape handle is slid over the tube assembly and the worm screw is tightened until the corresponding circular band is tightened sufficiently about the tube assembly such that it will remain static during the push-pull operation of the applicator. To remove the u-shaped handle, the same worm screw is loosened until the circular band is sufficiently loose to slide off the tube assembly.
[0006] Although such device provides the advantage of providing a tool that allows for the directed and controlled release of grout to a desired gap between tiles, many drawbacks still remain. One area of concern is the difficulty in using this design. Here, an operator must use two hands to create the pressure for extruding the grout from the device. Further, the push-pull design of the device requires that an operator position themselves behind the length of the device at the end of the plunger handle, thus creating a corresponding distance between the operator's eye, and the gap being filled. Further, each operator must go through a learning process as to how to operate such a unique mechanism.
[0007] Another area of concern is the time and effort needed to replace an empty tube. If an operator has assembled a series of pre-filled tube assemblies and wishes to sequentially switch from each used up tube assembly to a waiting pre-filled assembly, the operator must take the time and effort to set-aside the device, retrieve a separate tool (a screwdriver) to assist in removing the u-shaped handle, use the tool to loosen the u-shaped handle from the tube assembly, remove the handle from the tube, slide the handle around the new filled tube assembly, use the screwdriver to tighten the u-shaped handle about the tube, and reposition themselves behind the device to continue the grouting process.
[0008] Another area of concern is the cost of the tube assembly itself. The cost of an assembly tube includes the following: the material cost to provide sufficient structural integrity such that the tightening of the u-shaped device thereabout does not cause such a constriction which impedes the stroke of the plunger through the chamber located inside, the material cost to provide sufficient applicator tube integrity such that the push-pull motion about the device does not deform the applicator tube and otherwise negatively impede the use of the device, the material cost to include a platform-type component at the plunger end of the tube for providing structural support for the opening of the tube, and the manufacture and material costs associated with the production and design of a applicator tube having separate sections. In addition, this design includes an angled nose piece that does not provide for the extrusion of the grout therein resulting in the loss of such grout if discarded, or requires the time and energy to retrieve the remaining grout. Further, all the above costs are multiplied when it is desired to use multiple applicator tubes to complete a grouting operation.
[0009] Another area of concern is the reliability of the device. Because the tube is constructed of multiple parts, and the operation of the piston crosses a seam of such multiple parts, there is inherent reliability issues and wear-and-tear issues regarding the repeated crossing of such boundary by the internal plunger. Further, the lack of a centering mechanism for the shaft leading to the plunger, and the general instability of the overall push-pull design, each contribute to a torquing of the shaft and a resulting torquing of the plunger. Such torquing of the plunger raises issue of jeopardizing the seal upon such movements as well as the longer term wear-and-tear on the inner walls of the assembly tube and the plunger.
[0010] Other application devices, although not generally known to be used in conjunction with grouting operations, but generally known to be used with caulking operations, are caulking guns. Such caulking guns are hand-held devices using a griping-trigger assembly to control the movement of piston-plate mechanism to cause the extrusion of caulking material stored in an interchangeable caulking tube. Here, the caulking gun is a tool used to act upon a disposable caulking tube. Pre-filled caulking tubes are purchased for use and discarded after the pre-filled caulking material has been dispensed. The limited types and colors of caulks used allows manufacturers to easily and economically produce and sell such pre-filled caulking tubes. The caulking tube designs are typified by their use of a cardboard or plastic tube to form its outer/inner shell. At one end of the tube is an applicator tip. At the other end is an opening that exposes the full width of the inner shell. Inside the inner shell, although obscured by a push-plate, is the caulking material. The push-plate is a circular plate with a perpendicular boarder around its edge where the perpendicular boarder or sides extend down towards the open end of the tube. The push-plate is used to urge the caulking material down the inner shaft and out the applicator tip. The push-plate also provides an atmospheric seal between the caulking material and the empty portion of the inner shaft, allowing the caulking material inside to be stored for an indefinite time before its use.
[0011] Force is applied against the push-plate by a piston-plate mechanism, which forces the caulking material out of the application tip. The piston-plate mechanism is characterized by a shaft extending down the inner shaft of the caulking tube with a plate that contacts and pushes the push-plate. The push-plate provides the necessary wall-to-wall coverage to displace the caulk material down the inner shaft. It is not necessary that the piston-plate plate extend to the wall surfaces. The push-plate has its perpendicular sides extending down the open end of the tube. The piston-plate's plate is in contact with the surface of push-plate's circular plate beyond the edges of such perpendicular sides. The width of the piston-plate plate cannot extend from wall-to-wall, as the sides of the push-plate, having a certain thickness, are located there between. As such, any piston-plate plate must be smaller in diameter than the diameter of the inner tube and no greater than the diameter between the two perpendicular sides of the push-plate. In fact, the reason for the use of the push plate generally, is as a footing to prevent the piston-plate's piston from breaching, or breaking through, the push-plate barrier and contacting the caulking material itself.
[0012] One of the preferred caulking gun design includes the use of a gasket that is of a diameter larger than the diameter of the inner tube and which extends about the edges of the piston-plate plate. Further, this circular gasket is held in place by the use of two piston-plates sandwiched on either side of such gasket. The gasket is designed to extend from the edges of the piston-plate plates and extend partially along the perpendicular sides of the push-plate, so as not to exceed the ends of such perpendicular sides. This design provides a vacuum between the piston-plates and the push-plate such that a moving back of the piston-plate pulls the push-plate, via a vacuum therebetween, in a backward motion. Therefore, this design requires that the gasket does not extend to the walls of the tube, as this would interfere with both the vacuum attempted to be created between the two plates, and with the backward movement of the push-plate along the walls of the tube.
[0013] Another preferred caulking gun design does not alter the diameter of the plunger-plate, but adds a spring-like mechanism used in the retraction of the associated piston rod. Here again, this design uses a plunger plate that fits within the diameter of the perpendicular sides of the push-plate and does not use a gasket. This caulking gun design is concerned with retaining the caulking tube or cartridge within the caulking gun until it is intentionally released by the operator. One embodiment here introduces a spring-like plate behind the plunger plate that resists movement in the backward direction, when the plunger-plate is approaching the exit point of the caulking tube.
[0014] Yet another design proposes a interchangeable plunger-plate design where the caulking gun accepts either of two sized cartridges, namely a ¼ gallon or {fraction (1/10)} gallon cartridge. Here, depending on the size of the caulking cartridge, either a smaller or larger plunger-plate is used. In both cases, the plunger-plates are standard size for their corresponding caulking cartridges. As such, they are designed to fit between the perpendicular walls of the corresponding push-plates, and do not contain a flexible gasket.
[0015] As demonstrated above, a need exists for a refillable, hand-squeezed driven grouting applicator. Desirably, the new apparatus is capable of dispensing grouting material without the use of a push-plate. Further it would be desirable if the new apparatus was capable of extruding the grout without the need for an operator to use two hands.
BRIEF SUMMARY OF THE INVENTION
[0016] A method and apparatus for applying sealing material is disclosed utilizing a plunger with a flexible outer surface and with an extended position and a compressed position. A cartridge for receiving grout has a chamber of substantially equal size to the plunger in its compressed position and a hand-squeezed driving mechanism for moving the plunger along the chamber of the cartridge.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0017] [0017]FIG. 1 is a cut-away side elevation view of a prior art caulking gun system;
[0018] [0018]FIG. 2 is a cut-away side elevation view of one embodiment of a grouting gun;
[0019] [0019]FIG. 3 is a front perspective view of a portion of the grout cartridge of one embodiment of the invention;
[0020] [0020]FIG. 4 is a side view of an application cap of one embodiment of the invention;
[0021] [0021]FIG. 5 is a perspective view of a portion of a grout cartridge of one embodiment of the invention;
[0022] [0022]FIG. 6 is a side view of an application cap of one embodiment of the invention;
[0023] [0023]FIG. 7 is a perspective view of a plunger and a piston-end portion of a grout cartridge of one embodiment of the invention; and
[0024] [0024]FIG. 8 is a side view and a front view of a plunger of one embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0025] The embodiment shown in FIG. 2 includes the grouting gun 200 , the grout cartridge 210 , and the piston 212 . In this embodiment, the grouting gun 200 contains similar components as found in typical caulking guns. One skilled in the art is generally familiar with the components of a typical caulking guns. Grouting gun 200 further comprises grouting gun housing 214 , grout cartridge chamber 216 , handle 218 , trigger 220 and barrel 222 . However, some embodiments (not shown) do not include a typical barrel 222 where the grout cartridge itself acts as the barrel 222 where the end of the grout cartridge 210 is screwed into, or otherwise secured to, the grouting gun housing 214 .
[0026] Grout cartridge chamber 216 includes a grout cartridge access opening (not shown), and a applicator tip opening or aperture 224 . Again, referring to the above described embodiment that is absent barrel 222 , here cartridge chamber 216 is also absent, and such embodiment is therefore also absent such grout cartridge access opening and applicator tip opening 224 . The embodiment shown in FIG. 2, like typical caulking guns, has a trigger 220 connected to a piston 212 such that repeated squeezing of the trigger 220 causes forward movement of piston 212 down barrel 222 and through grout cartridge chamber 216 . This ability to generate the necessary force to move a piston by the hand-squeezing motion of one hand alone, hand-squeezing being the opposing forces generated from within the hand itself, allows for the other hand to perform other tasks at the same time that the other hand is generating this force. Other embodiments use other means to manually move piston 212 and include the transferring of a squeezing motion of the hand into the movement of such piston. For example, one embodiment, not shown, uses a dual trigger-type arrangement where handles and triggers on either side of a barrel are squeezed to produce the desired movement of the piston. As shown in FIG. 2, the barrel 222 has a grout cartridge chamber 216 . Again, as discussed above, some embodiments are absent barrel 222 altogether.
[0027] Grout cartridge 210 is located in grout cartridge chamber 216 inside barrel 222 and includes nozzle 226 , inner cartridge wall 228 , outer cartridge wall 230 and piston opening 232 . In this embodiment, the grout cartridge 210 is different than caulk cartridges found in typical caulking guns at least because there is no push-plate between the piston 212 and the sealing material. In addition, grout cartridge also contains grout 234 (sealing material). Also, in this embodiment, and unlike typical caulking guns, the grout cartridge 210 is designed to receive sealing material through its piston opening 232 . Here, the grout cartridge 210 is made out of plastic so that it is easily cleaned. However, other embodiments include a grout cartridge 210 made of other materials such as of cardboard or metal. Further, in this embodiment, the grout cartridge 210 is designed to handle the structural demands of operating within a grout cartridge chamber, but is not designed to withstand those structural demands of grouting guns which simply attach to the open end of a grouting cartridge. Other embodiments with grout cartridges with thicker sidewalls and with greater structural integrity are used to withstand the inherent additional forces present in such grouting gun designs. The grout cartridge 210 has dimensions of approximately 10 inches long (not including a nozzle or applicator tip) and with an inside diameter of 2⅜ inches.
[0028] In addition, the grout cartridge 210 of this embodiment is also different than the typical caulk cartridges where the grout cartridge contains a nozzle 226 rather than a permanently attached applicator tip. As shown in FIG. 2, nozzle 226 protrudes from the front of barrel 222 within the applicator tip opening or aperture 224 and extends beyond the front of barrel 222 such that its threads 236 are exposed, (See FIG. 5), and such that applicator tip 238 , (See FIG. 4), approximately 2½ inches long, may be attached thereto as shown. FIG. 2 shows the applicator tip 238 disengaged from and in front of nozzle 226 . As shown in FIG. 5, other embodiments locate threads 236 inside nozzle 226 such that the applicator tip 238 , (See FIG. 6), is subsequently screwed into, rather than onto, nozzle 226 . Further, in other embodiments, (not shown), a lip is used instead of threads 236 such that the applicator tip is snapped on rather than screwed on.
[0029] As shown in FIG. 4, this embodiment uses one of a multiple of interchangeable applicator tips 238 depending on the grouting job to be performed. Applicator tips are shown in FIGS. 4 and 6 as having openings of {fraction (1/4)} inch and ⅛ of an inch. Another embodiment, (not shown), which uses a permanently attached applicator tip, provides such a tip having an internal space that is increasingly larger towards the base of the applicator tip such that the applicator tip may be cut off at an appropriate position resulting in an opening of a desired width, for example, ¼ or ⅛ of an inch. Further, in the current embodiment, the amount of grout 234 that is available for use in grout cartridge 210 is, depending on which applicator tip 238 is used, {fraction (1/4)} inch or {fraction (1/8)} inch, is 85 linear feet or 160 linear feet, respectively.
[0030] The inner cartridge wall 228 , as shown in FIGS. 2 and 7, has a uniform and smooth surface such that piston 212 is capable of achieving and maintaining an airtight seal along the usable portion of the grout cartridge 210 . Here, the term ‘usable portion’ is used to refer to that portion of the grout cartridge 210 that piston 212 is to both travel and be required to keep a seal with inner cartridge wall 228 . Other embodiments, (not shown), do not require that the seal be airtight, but rather that the seal be sufficient to preclude an unreasonable amount of grout to pass to the non-grout side of the piston 210 .
[0031] As shown in FIG. 2, piston 212 is comprised of shaft 240 and plunger 242 . In this embodiment shaft 240 is the same shaft as found in typical caulking guns. As such, the shaft 240 is operatively connected to trigger 220 such that the shaft 240 extends down the barrel 222 of the grouting gun 200 as the trigger 220 is repeatedly pulled. However, the plunger 242 is not typical of those found in caulking guns. The plunger 242 includes a gasket 243 which forms a flexible outer surface of plunger 242 and extends outward and contacts inner cartridge wall 228 . Further, the plunger 242 is intended to directly contact the grout material. In contrast, and as shown in FIG. 1 plungers from typical caulking guns are intended to contact a push-plate 10 only, and it is the push-plate 10 that is in contact with the sealing material 12 . Again referring to FIG. 2, the design of the plunger 242 , includes a gasket 243 being sandwiched between two piston-plates 244 and 248 such that gasket 243 extends about the edges of such piston-plates and forms an airtight seal with inner cartridge wall 228 .
[0032] Further, as shown in FIGS. 2 and 7, piston opening 232 is large enough to accept the entry of piston 212 . As shown in FIG. 2, when the piston 212 is in position A rather than position B, or is otherwise outside of grout cartridge 210 as also shown in FIG. 7, the gasket 243 is not in contact with the inner cartridge wall 228 , and as such is in an expanded state, or a relaxed position, such that its outer boundary extends beyond the inner cartridge wall 228 (e.g., d 1 is greater than d 2 ). The gasket 243 in its expanded position is approximately 2{fraction (13/32)} inches in diameter. And when gasket 243 is in position B, within grout cartridge 210 , e.g., within the inner void therein, the gasket 243 is in its compressed position where it conforms to the diameter equal to that defined by the inner walls 228 of grout cartridge 210 . The gasket 243 in its compressed position is substantially the same diameter as that of the inner cartridge wall 228 . It is this compressed nature, or the close tolerance associated therewith, where the plunger 242 is sized to produce an airtight seal with the inner cartridge wall 228 that allows for the efficient displacement of the grout down the grouting cartridge chamber 216 in the direction of the opening of nozzle 226 . Other embodiments, (not shown), include a fluted end to assist in the compressed deformation of gasket 243 . Although not shown, gasket 243 may experience deformation in an additional direction than in and inward radial direction, for example, in either direction along the inner cartridge wall 228 .
[0033] Therefore, other embodiments exist that utilize a plunger 242 with the properties associated with this close tolerance, or otherwise provide the above described compressed and relaxed positions. For example, one embodiment uses a plunger 242 that is substantially made of rubber, and is of sufficient thickness as to provide the pushing force down grouting cartridge chamber 216 without deforming to a point which allows the grouting material to pass by the edges of plunger 242 . Another embodiment is where a single metal piston plate is used that contains front and rear lips on its outside edge, where an o-ring is placed there between, and provides the airtight seal with inner cartridge wall 228 when inserted into grout cartridge 210 .
[0034] As best shown in FIG. 8, the piston-plates 244 and 248 of this embodiment are made of a rigid material metal such as steel. The diameter of each piston plate 244 and 248 in this embodiment is approximately 2{fraction (5/16)} inches. What is essential is that the diameter of any such rigid piston-plate, 244 or 248 , associated with the plunger be no larger than the piston opening 232 . Other embodiments utilize other metals than steel, while yet other embodiments use rigid materials other than metal. What is less important than the rigidity of the inner portion of the plunger 242 , is the overall capability of the plunger 242 to both force the grout material down the grout cartridge 210 and to maintain a significant seal with the inner cartridge wall 228 .
[0035] In operation, the operator selects an applicator tip 238 to attach to grout cartridge 210 . The selected applicator tip 238 is then twisted onto the nozzle 226 via threads 236 until it is sufficiently tightened. If grout cartridge 210 has not yet been filed with grout 234 , the operator then fills it with grout 234 . Because of the nature of grout, including, for example, that in comes in many types and colors, its tendency to harden, and that grout is often specifically mixed for a particular project, that it is generally expected that grout cartridges 210 would not be sold with a grout already pre-mixed and stored therein. Rather, it is generally expected that empty grout cartridges will be sold that will be subsequently filled at the project location by an operator. Next, the operator grabs the grouting gun 200 , an embodiment thereof shown in FIG. 2, by handle 218 . To avoid inadvertently spilling grout from the piston opening 232 of grout cartridge 210 , and to otherwise take advantage of gravity in the preparation of grouting gun 200 , the operator may point the barrel 222 of gun 200 towards the ground. With the hand not on the handle 218 , the operator slides in grout cartridge 210 into the grout cartridge chamber 216 through the grout cartridge access opening in barrel 222 of the grouting gun 200 . In doing so, the operator aligns the applicator tip 238 so that it enters applicator tip opening 224 . Once the grout cartridge 210 has been inserted with applicator tip 238 protruding through applicator tip opening 224 , then the operator may engage plunger 242 with grout cartridge 210 .
[0036] Operator uses trigger 220 to move shaft 240 down the barrel 222 until the plunger 242 engages the outside edge of piston opening 232 of grout cartridge 210 . As best shown in FIG. 7, the piston opening 232 in this embodiment provides the means for compressing the plunger portion of piston 212 as the piston enters grout cartridge 210 . Here, although the diameter d 1 for the relaxed or expanded plunger 242 is larger than the diameter d 2 for the piston opening 232 in the back of grout cartridge 210 , a force applied along piston 212 towards piston opening 232 causes an initial contact between gasket 243 and the grout cartridge 210 , as the operator continues to squeeze the trigger 220 and the force down shaft 240 continues the gasket 243 is deformed in an inward radial direction until the plunger 242 is within grout cartridge 210 . Once inside the grout cartridge 210 the gasket 243 assumes its compressed size. The trigger 220 is continued to be squeezed until the plunger engages the grout 234 and the grout 234 begins to emerge from opening in applicator tip 238 .
[0037] Now that the grouting gun 200 has been readied for use, the operator then, by placing one hand on the barrel 222 and the keeping the other on the trigger 220 , places the applicator tip 238 within the joint that is intended to be filled and squeezes trigger 220 while directing the applicator tip 238 along the length of the joint such that a desired amount of grout 234 is applied to the area within the joint. This ability to direct the precise amount of grout 234 to be applied to a targeted joint without otherwise depositing such grout 234 on the surrounding tile surfaces, provides the advantage of eliminating the need for a floater and the otherwise significant clean up time otherwise associated with cleaning up the grout 234 that remains on the tile rather than in the joints. The clean up time will be reduced to that of cleaning just the grouting gun 200 itself.
[0038] Once the process of filling the joints has been complete, or the operator wishes to temporarily end the current joint filling process, the operator need only apply a cap to the end of the applicator tip 238 and set aside the grouting gun 200 for later use. The seals at the applicator tip 238 and at the plunger 242 allow for the indefinite storage of the remaining grouting mixture which allows for the immediate initiation of a new grouting process without any preparation of the grouting gun as well as saving the cost of having to dispose of the grout 234 remaining at the time that the process is aborted.
[0039] Many of the embodiments discussed above are based on changes or improvements to existing designs for caulking guns. A number of such embodiments can be achieved by modifying the piston-plate portion associated with existing caulking guns. For example, one may remove the piston plate portion from the piston leaving just the shaft 240 . The removed piston plate is generally characterized by its diameter which is smaller than the diameter of the piston opening d 2 , and which otherwise lacks the ability to provide an airtight seal with the inner cartridge wall 228 . Then, a plunger, such as the plunger 242 as shown in FIG. 8, is added to the end of shaft 240 . Here, the plunger is capable of generating an airtight seal with inner cartridge wall 228 when inserted into grout cartridge 210 . Finally, rather than inserting a caulk cartridge into the gun, a grout cartridge 210 , having the properties discussed above, is instead inserted or loaded into the gun. The operation of such an apparatus is generally described above.
[0040] It should be noted that the insertion of a caulk cartridge into such a modified system using a plunger is not recommended for a number of reasons, including, but not limited to the following: the push-plates 10 found in most caulk cartridges are designed for use in conjunction with piston plates of the caulking gun design where contact between the two is designed to occur at a diameter significantly less that the diameter of the corresponding caulk cartridge opening; also the gasket 243 of plunger 242 is not designed to withstand the pressure that the perpendicular boarder of the push plate would cause; slippage may occur such that a portion of a gasket may remain in contact with a far edge of the perpendicular boarder of the push-plate, while an another edge may slip towards the contact side of the push-plate causing a torquing force about the push-plate potentially resulting in greater slippage resistance or potentially a total twisting of the push-plate resulting in a variety of complicating factors; and also in addition to the original internal design friction forces inherent between the push-plate and the inner sidewalls of the caulk cartridge, additional external design frictional forces are added between the contact of the new non-standard plunger 242 and the inner sidewalls.
[0041] While only a few embodiments and aspects of the invention have been described above, including the preferred embodiment, those of ordinary skill in the art will recognize that these embodiments and aspects may be modified and altered without departing from the central spirit and scope of the invention. Thus, the embodiments and aspects described above are to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims, rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are intended to be embraced herein.
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A method and apparatus for applying sealing material having a plunger with a flexible outer surface and with an expanded size and a compressed size and a cartridge for receiving grout having an inner void of substantially equal size to the plunger compressed size and a hand-squeezed driving mechanism for moving plunger along the inner void of the cartridge.
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BACKGROUND
The invention relates to a process and a device for manufacturing a composite strand formed by combining a multiplicity of continuous glass filaments with continuous high-shrinkage organic thermoplastic filaments.
The manufacture of composite strands is disclosed especially in EP-A-0 367 661 which describes a process employing a first installation comprising a bushing that contains molten glass, from which continuous glass filaments are drawn, and a second installation comprising a spinning head, supplied under pressure with an organic thermoplastic that delivers continuous filaments.
The two types of filaments are assembled into at least one composite strand and during the assembly the filaments may be in the form of webs, or in web and strand form. In the composite strand, the glass filaments or strand are surrounded by thermoplastic filaments that protect the glass from rubbing on the solid surfaces with which the strand is in contact.
Although the incorporation of thermoplastic filaments enables the abrasion resistance of the strand to be improved, it also introduces tensions in the strand due to a shrinkage phenomenon of said filaments, which causes waviness of the glass filaments. The presence of waviness is particularly visible when the composite strand is wound in the form of a bobbin as this is deformed over its entire periphery.
The shrinkage phenomenon has several drawbacks: it requires resorting to thick spools for producing the bobbins so that they can withstand the shrinking exerted by the composite strand and it disrupts the unwinding of the strand from the bobbin due to the fact that it does not have the ideal geometric characteristics that are required for the desired application. Furthermore, such a strand is not advantageous for producing a fabric that can be used as a reinforcing material for large-size flat parts since, because of the waviness, the filaments are not perfectly aligned in the final composite. The reinforceability of the strands in a given direction is found to be reduced.
To solve the problem of shrinkage of the thermoplastic filaments, various solutions have been proposed.
In EP-A-0 505 275, a process for manufacturing a composite strand similar to that described previously in EP-A-0 367 661 is proposed, which plans to form the thermoplastic filaments using a spinning head that is normally used in the field of the synthetic fibre industry. In this way, it is possible to obtain a composite strand formed from one or more glass strands surrounded by organic filaments, which is independent of the configuration of the spinning head used for extruding the organic filaments.
In EP-A-0 599 695, it is proposed to mingle the thermoplastic filaments with glass filaments at a speed during the commingling that is greater than the drawing speed of the glass filaments. The speed difference is determined so that the shrinkage phenomenon compensates for the excess initial length of the thermoplastic filaments relative to the glass filaments.
In one embodiment, the thermoplastic filaments pass onto a variable speed drawing unit of the type comprising drums, which accentuates the excess length, which makes it possible to obtain a composite strand of which the glass filaments are linear and the thermoplastic filaments are wavy.
In EP-A-0 616 055, a process for producing a glass/thermoplastic composite strand is also proposed, which consists in mingling a web of thermoplastic filaments with a bundle or a web of glass filaments, the thermoplastic filaments being, upstream of the point of convergence, heated to a temperature above their relaxation temperature, drawn then cooled. The composite strand obtained has no waviness and is stable over time.
The direct manufacture of rovings, without passing through an intermediate step of unwinding the tape and winding the strand, is carried out continuously by drawing the composite strand under the bushing at a speed compatible with the drawing of the glass filaments. This already high speed (of the order of a few meters to about ten meters per second) is associated with a drawing speed of the thermoplastic filaments upstream of the convergence points that is even higher.
The production of a composite strand without waviness under such conditions occurs via a precise synchronization of the relative speeds of the rotating elements of the drawing unit and by maintaining the initial difference between the drawing speeds of the glass filaments and the thermoplastic filaments.
These conditions are limited to thermoplastic materials that undergo a limited shrinkage. When the shrinkage is larger, the drawing unit becomes inoperable due to the fact that its speed can no longer be increased so as to sufficiently increase the length of the thermoplastic filaments so that the composite strand does not have any waviness.
SUMMARY
The object of the present invention is to provide a process enabling the manufacture of a composite strand comprising commingled continuous high-shrinkage thermoplastic filaments and continuous glass filaments that does not have any waviness during its manufacture and that remains stable over time.
This object is achieved via a process for manufacturing a composite strand formed by commingling continuous glass filaments mechanically drawn from the holes in a bushing filled with molten glass and continuous organic thermoplastic filaments emanating from a spinning head, said thermoplastic filaments being mingled in the form of a web with a bundle or a web of glass filaments, in which, before their commingling with the glass filaments, the thermoplastic filaments are drawn, heated then projected onto a moving support with a speed during their projection onto the support that is greater than the running speed of said support. The combined effect of the drawing and the projection of the heated thermoplastic filaments gives them a high level of crimping that consequently makes it possible to compensate for the shrinkage of the thermoplastic in the composite strand.
Advantageously, the heating and protection of the thermoplastic filaments are carried out simultaneously.
According to a first embodiment of the invention, the thermoplastic filaments are guided in the form of a web up to the glass filaments, also in the form of a web, and are combined with the latter at identical speeds between the coating roll and the point of gathering all the filaments into a composite strand.
According to another embodiment, the thermoplastic filaments are projected onto the glass filaments deposited onto the moving support, in the running direction of said support. Thus a web formed by the entanglement of the crimped thermoplastic filaments with the linear glass filaments is obtained, this web consequently being assembled to form the composite strand.
The process according to the invention makes it possible to obtain a composite strand without any waviness: the glass filaments that are incorporated into the composition of the composite strand are linear immediately after their assembly with the thermoplastic filaments, and they retain their linearity after the collection in the form of a package. In the end, the thermoplastic filaments in the composite strand may be linear or wavy depending on the level of crimping that has been conferred on them at the beginning.
Thanks to the invention, it is possible to form bobbins under the normal conditions for producing glass strands, especially using spools of conventional thickness given the absence of shrinkage of the composite strand, these spools possibly being removed in order to obtain balls and reused if necessary. This has the advantage of being able to extract the composite strand according to the method of unwinding (from the outside) or unravelling (from the inside).
Besides the fact that it makes it possible to obtain a composite strand without waviness using a high-shrinkage thermoplastic, the process according to the invention ensures a homogeneous distribution and a high commingling of the filaments within the composite strand.
The invention also provides a device for carrying out this process.
According to the invention, in order to enable the manufacture of a composite strand formed from continuous glass filaments and from continuous high-shrinkage thermoplastic filaments, this device comprises, on the one hand, an installation comprising at least one bushing supplied with molten glass, the lower face of which has a very large number of holes, this bushing being associated with a coating device, and on the other hand, an installation comprising at least one spinning head supplied under pressure with molten organic thermoplastic, the lower face of which is equipped with a very large number of holes, this spinning head being associated with a drawing unit of the type comprising drums, with a device for projecting thermoplastic filaments that is provided with heating means, with a drum-type moving support and with a means enabling the thermoplastic filaments to be mingled with the glass filaments, finally means common to the two installations enabling the assembly and winding of the composite strand.
The drum drawing unit has at least two rolls operating at variable speeds, preferably ensuring an increasing linear speed of the thermoplastic filaments. When the drawing unit comprises more than two rolls, the latter advantageously operate in pairs. The drawing unit may be provided with heating means, for example electric or infrared heating means, preferably placed in the first drum encountered by the thermoplastic filaments with the objective of preheating them and thus promoting their drawing.
Preferably, the means enabling the thermoplastic filaments to be projected onto the moving support is a device using the properties of fluids that may be liquids or gases, such as pulsed or compressed air. Advantageously, it is a Venturi system, the role of which is solely to project the thermoplastic filaments by giving them an adequate spatial distribution and orientation, without giving them any additional speed.
According to a preferred embodiment of the invention, the heating means, especially electrical, are associated with the device ensuring the projection of the thermoplastic filaments. In this way, the heating of the thermoplastic filaments at a temperature close to their softening point is carried out homogeneously and rapidly, which makes it possible to obtain a satisfactory crimping state during the projection onto the moving support.
The moving support may be made from a drum, the surface of which consists of perforations, comprising an element for separating the internal volume into at least two compartments, one connected to means enabling it to be maintained under vacuum, the other associated with means enabling it to be put under excess pressure. The size and placement of the compartments are chosen so as to maintain the thermoplastic filaments in their initial crimping state, in the form of a web at the surface of the drum situated above the first compartment, and to obtain the separation of the web when it passes above the second compartment.
The means enabling the two types of filaments to be mingled may be constituted by a Venturi system as described previously that enables the thermoplastic filaments to be projected into a web or a bundle of glass filaments. Preferably, this system projects the thermoplastic filaments at an identical speed to the drawing speed of the glass filaments.
The means ensuring the commingling of the filaments may also be constituted by the drum-moving support. In this case, the drum is used to support the web of glass filaments, which winds around it, and the crimped thermoplastic filaments in web form are mingled with the glass filaments along a generatrix of the drum.
The devices described previously enable the production of composite strands, from precrimped high-shrinkage thermoplastic filaments and from glass filaments, which do not have any subsequent deformation, that is to say that remain stable over time.
Such devices can be applied to any type of known glass, for example E-glass, R-glass, S-glass, AR-glass or C-glass, E-glass being preferred.
In the same way, it is possible to use any thermoplastic capable of having a high shrinkage, for example a polymer belonging to the group of polyurethanes, polyesters such as polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), and polyamides such as nylon-6, nylon-6,6, nylon-11 and nylon-12.
BRIEF DESCRIPTION OF THE DRAWINGS
Other details and advantageous features of the invention will become apparent on reading the description of the examples of devices for carrying out the invention described with reference to the appended figures that represent:
FIG. 1 : a schematic representation of an installation according to the invention; and
FIG. 2 : a schematic representation of a second embodiment of the invention.
DESCRIPTION
Represented in FIG. 1 is a schematic view of a complete installation according to the invention. It comprises a bushing 1 supplied with molten glass either via a hopper containing cold glass, for example in the form of beads that drop simply by gravity, or from the forehearth of a furnace that feeds glass directly to its top.
Whatever the type of feed, the bushing 1 is usually made of a platinum-rhodium alloy and it is heated by resistance heating so as to remelt the glass or keep it at a high temperature. A multitude of streams of molten glass flow from the bushing 1 , these streams are drawn in the form of a bundle 2 of filaments by a device, not shown, also allowing the bobbin 3 to be formed. Placed in the path of the bundle 2 is a coating roll 4 , for example made of graphite, which deposits a size onto the glass filaments that is intended to prevent or limit the rubbing of the filaments on the members with which they come into contact. The size may be aqueous or anhydrous (that is to say comprising less than 5% by weight of water) and contain compounds, or derivatives of these compounds, which are incorporated into the composition of the thermoplastic filaments 5 that will combine with the glass filaments to form the composite strand 6 .
Also represented schematically in FIG. 1 is a spinning head 7 from which the thermoplastic filaments 5 are extruded. The spinning head 7 is supplied with a molten, high-shrinkage thermoplastic, for example coming from an extruder, not shown, supplied with granules which flows under pressure through a large number of holes positioned under the spinning head 7 , to form the filaments 5 by drawing and cooling. Cooling of the filaments is carried out by forced convention, by means of a conditioning device 8 having a suitable shape for the spinning head 7 and that generates a laminar air flow perpendicular to the filaments. The cooling air has a flow rate, a temperature and a humidity that are kept constant. The filaments 5 then pass over a roll 9 that makes it possible to assemble them in the form of a web 10 , on the one hand, and to deflect their path, on the other hand.
After passing over the roll 9 , the web 10 of thermoplastic filaments passes over a drawing unit 11 formed, for example, from rolls 12 , 13 that may turn at the same speed or have different speeds so that the acceleration is carried out in the run direction of the thermoplastic filaments. The drawing unit 11 has the role of drawing the filaments 5 and of giving a set speed to the web 10 . It is possible to vary the rotational speed of rolls 12 and 13 so as to precisely adjust the projection speed of the thermoplastic filaments onto the drum 17 . Rolls 12 and 13 may be associated, where appropriate, with a heating system, for example an electric heating system, which makes it possible to ensure a homogeneous and rapid preheating of the thermoplastic filaments by contact with the surface of the rolls. The drawing unit 11 may be formed from a higher number of rolls, preferably functioning in pairs, for example four or six rolls.
The web 10 of thermoplastic filaments, optionally preheated, is then directed towards the deflecting roll 14 , which may be heated and optionally be motor-driven, then it passes into a crimping device 15 formed, for example from a Venturi system 16 and a drum 17 .
The Venturi system 16 makes it possible to keep the thermoplastic filaments separate and to project them as a regular web of suitable size onto the drum 17 . The Venturi system 16 operates by an injection of compressed air and imparts no additional speed to the web 10 . This system is associated with a heating device (not shown), for example using a fluid such as hot air or steam, and has the role of bringing the thermoplastic filaments to a temperature close to the softening point of the thermoplastic in order to improve their crimpability.
At the outlet of the Venturi system 16 , the web 10 of thermoplastic filaments is projected onto the drum 17 . The rotational speed of the drum 17 is lower than the speed of the web 10 during its projection so that the filaments crimp when they come into contact with the surface of said drum.
The drum 17 is equipped with a central groove 18 , having a width slightly less than that of the drum, which is pierced by multiple holes (not shown). It also comprises an element 19 , that is coaxial and immobile relative to the drum, which is used to separate the interior of the drum into two compartments 20 , 21 . Compartment 20 is connected to a device, not shown, which enables it to be put under vacuum, for example a suction pump, and compartment 21 is connected to a device, not shown, enabling it to be put under an excess pressure, for example an air injection device.
After its projection onto the drum 17 , the web 10 of crimped filaments is held in the groove 18 level with the compartment 20 under vacuum and it is cooled, by simple contact with the perforated surface or via a fluid, for example water or a sizing composition sprayed onto the filaments. Next, the web 10 is separated from the surface of the drum 17 level with the compartment 21 under the effect of the pressurized air passing through the perforations.
The web 10 then passes onto a deflecting roll 22 , then into a Venturi device 23 that keeps the crimped thermoplastic filaments in individual form until they are mingled with the glass filaments of the web 24 .
Joining of the web 10 of thermoplastic filaments and the web 24 of glass filaments takes place between the coating roll 4 and the element 25 being used to assemble the filaments into a composite strand. During the commingling of the filaments, the thermoplastic filaments arrive with a speed equal to that of the glass filaments.
A deflector 26 equipped with a notch keeps all the filaments in place, in particular along the edges, and helps to reduce the disturbance undergone by the web 24 of glass filaments at the moment when the web 10 of crimped thermoplastic filaments is projected onto it.
The web 27 of intermingled crimped thermoplastic filaments and glass filaments then passes onto the device 25 that enables assembly of the filaments into a composite strand 6 , which is immediately wound in the form of a bobbin 3 thanks to a drawing device, not shown, that operates at a given linear speed kept constant to guarantee the desired linear density.
This linear speed that enables the drawing of the glass filaments is in general equal to that imparted by the drum 17 to the web 10 of crimped thermoplastic filaments. Nevertheless, it is possible to mingle the thermoplastic filaments with the glass filaments at a speed, during their projection, which may be lower in order to given an extra tension to the thermoplastic filaments to improve the ability to keep them in web form until the point of commingling with the glass filaments. Under these conditions, the difference between the projection speed of the thermoplastic filaments and the drawing speed of the glass filaments does not exceed 10%.
FIG. 2 represents an installation according to a second embodiment of the invention. In this figure, the common devices and means bear the same numbers as in FIG. 1 .
The bundle 2 of glass filaments flowing from the bushing is drawn by a device (not shown) that forms the bobbin 3 . The bundle 2 passes over the coating roll 4 that deposits a size on the glass filaments and the web 24 formed is wound over the drum 17 .
The thermoplastic filaments 5 extruded from the spinning head 7 , cooled by the conditioning device 8 are assembled into a web 10 level with the roll 9 . The web 10 then passes onto the drawing unit 11 having rolls 12 , 13 and is drawn under the same conditions as in FIG. 1 . After roll 13 , the web 10 is directed towards the roll 14 , that is optionally heated and/or motor-driven, and into the crimping device 15 formed from the Venturi system 16 and the drum 17 .
In the Venturi system, the thermoplastic filaments of the web 10 are kept in their individual state and are heated at a temperature close to the softening point in order to help to obtain a high level of crimping.
The heated web 10 is projected onto the drum 17 that rotates at a lower speed than the projection speed of the filaments, which crimps them. Joining of the web 10 of crimped thermoplastic filaments and the web 24 of glass filaments is carried out along a generatrix of the drum 17 . The projection of the web 10 takes place while the filaments of the web 24 are contained within the groove 18 of the drum 17 ; this way of proceeding avoids disturbing the web of glass filaments and thus makes it possible to reduce the risk of said filaments breaking.
Immediately after their joining with the web 24 , the crimped thermoplastic filaments intermingle with the glass filaments and are flattened to the bottom of the groove 18 level with the compartment 20 under vacuum. When the web of thermoplastic filaments and glass filaments wound up onto the drum 17 arrives level with the compartment 21 that is under the action of pressurized air, it is detached from the surface under the effect of the air pressure coming from the inside of said compartment.
The web 27 passes onto the roll 22 and onto the device 25 for gathering the filaments into a composite strand 6 , which is wound in the form of the bobbin 3 . A second device 25 may be placed between the exit of the drum 17 and the roll 22 in order to help to obtain a better assembly of the composite strand.
The bobbins obtained using the process according to the invention are composed of a composite strand, of which the glass filaments are linear and the thermoplastic filaments are crimped (or wavy) in a way that is permanent and stable over time. The level of crimping or waviness of the thermoplastic filaments in the composite strand depends on the size of the crimping that was given to them during projection onto the moving support.
Moreover, the distribution of the glass filaments and the thermoplastic filaments within the composite strand is homogeneous, which translates into good commingling of the filaments.
It is possible to apply some modifications to the process and device that have just been described. Firstly, it is possible to use a size made up of several solutions, whether aqueous or not, comprising compounds that are capable of copolymerizing over a relatively short time when they are brought into contact with each other. In this case, the coating device comprises separate rolls, each of them depositing one of the sizing solutions on the glass filaments. It is also possible to anticipate a drying device that enables water to be removed from the glass filaments, or at least for the water content to be substantially reduced, before winding.
It is also possible to combine the invention with the production of complex composite strands, that is to say composite strands comprising organic thermoplastics that have different shrinkages. For this, it is possible to form different types of filaments, for example from one or more spinning heads, and to project them, in individual form or after having been assembled, onto the glass filaments.
EXAMPLE 1
A composite strand was manufactured in the installation described in FIG. 1 under the following conditions:
thermoplastic filaments:
thermoplastic: polyethylene terephthalate (PET); number of filaments: 1200 filaments; linear density: 359 tex; flow rate of the device 8 : 500 m 3 /h; speed of the drawing unit: 1500 m/min; temperature of rolls 12 and 13 : 240° C.; draw ratio in the melt phase: 1560; air temperature in the Venturi device 16 : 260° C.; rotational speed of the drum 17 : 990 m/min; cooling by water-spraying; and degree of crimping: 8%.
The degree of crimping was measured according to the formula 100×(L−L o )/L o , in which L o is the length of a crimped filament and L is the length of the same filament after a sufficient drawing to make it linear.
glass filaments:
number of filaments: 1600;
composite strand:
glass/thermoplastic weight ratio: 75/25; linear density: 1491 tex; and linear speed (winding): 1000 m/min.
The bobbin 3 was dried in an oven at 118° C. for 32 hours. The shrinkage of the thermoplastic filaments was around 6%. The geometry of the bobbin was not changed after drying.
EXAMPLE 2
A composite strand was manufactured in the installation described in FIG. 2 under the following conditions:
thermoplastic filaments:
thermoplastic: polyamide (PA); number of filaments: 1200 filaments; linear density: 466 tex; flow rate of the device 8 : 400 m 3 /h; speed of the drawing unit: 1800 m/min; temperature of rolls 12 and 13 : 180° C.; draw ratio in the melt phase: 3640; air temperature in the Venturi device 16 : 200° C.; rotational speed of the drum 17 : 1008 m/min; cooling by water-spraying; and degree of crimping: 10%.
The degree of crimping was measured according to the formula 100×(L−L o )/L o , in which L o is the length of a crimped filament and L is the length of the same filament after a sufficient drawing to make it linear.
glass filaments:
number of filaments: 1600;
composite strand:
glass/thermoplastic weight ratio: 70/30; linear density: 1597 tex; and linear speed (winding): 1008 m/min.
The bobbin 3 was dried in an oven at 118° C. for 32 hours. The shrinkage of the thermoplastic filaments was around 7%. The geometry of the bobbin was not changed after drying.
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The invention relates to a process and a device for manufacturing a composite strand formed by combining continuous glass filaments with continuous high-shrinkage organic thermoplastic filaments.
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TECHNICAL FIELD
[0001] The invention relates to a secure wireless communication system. More specifically, the present invention relates to a system for an improved system and method for wireless communication between two locations, and the wireless monitoring of one location from a second location.
BACKGROUND OF THE INVENTION
[0002] Wireless communication in the abstract has been known and popular for some time. In recent years, various improvements in radio transmission bandwidth and signal strength have enhanced the number and type of wireless communication systems available to consumers. An exemplary wireless monitoring system is disclosed in U.S. Pat. No. 6,759,961 to Fitzgerald et al. Various other exemplary wireless monitoring systems are currently offered for sale by Fisher-Price, among others.
[0003] Wireless monitoring systems can be used for a variety of purposes, such as home security, intercom devices, and law enforcement. Another application particularly suited for wireless monitoring systems is a baby monitor, in which a transmitting device is positioned at the location of an infant, for example, a baby crib, and captures noises made by the infant. A receiving device is positioned elsewhere, such that a parent can attend to other duties while listening to the sounds transmitted from the infant's location.
[0004] One shortcoming of present wireless monitoring systems is that the sound data transmitted from the transmitting device to the receiving device is typically in analog form. For example, the sound is in the standard analog waveform, and is therefore subject to standard waveform degradation. In such systems, owing to analog signal degradation, the quality of the sound received by the receiver will be inherently less than the quality of the sound sent by the transmitter. Across a substantial distance, the reduction in sound quality can be so substantial as to render the received sounds indistinguishable from background noise.
[0005] Another shortcoming of present wireless monitor systems is that they are susceptible to eavesdropping. The audio transmission between the transmitting and receiving devices is a standard radio transmission, which can be received by a standard radio reception device listening at the correct frequency. Such devices are notoriously insecure, and for the same reason can interfere with other radio transmissions such as a wireless phone or stereo system. Conversely, such wireless monitor devices receive interference from the other radio devices as well, sometimes requiring the user to place the devices in awkward places to avoid interference.
[0006] The present invention is provided to solve the problems discussed above and other problems, and to provide advantages and aspects not provided by prior systems and/or methods of this type. A full discussion of the features and advantages of the present invention is deferred to the detailed description, which proceeds with reference to the accompanying drawings.
SUMMARY OF THE INVENTION
[0007] A secure wireless communication system is provided comprising a transmitter and a receiver. The transmitter has an input for receiving audio information and a filter for modifying the audio information. The transmitter further comprises a selector for selecting a radio frequency, and an antenna for transmitting the modulated audio information on the selected radio frequency carrier. The receiver has an antenna for receiving the modulated audio information from the transmitter, and a filter for modifying the audio information. The receiver further comprises an output for communicating the audio information.
[0008] It is an object of the present invention to provide a wireless communication system that will both transmit and receive audio information having a higher sound quality than systems known in the art. To that end, the transmitter of the present system is, in one embodiment, provided with a converter to convert captured analog sound to a digital equivalent prior to transmission. Conversely, the receiver in that embodiment is provided with a converter for converting the received digital audio information into an analog form prior to communicating the information to the sound output.
[0009] It is a further object of the present invention to provide for a wireless communication system for the secure transmission of audio information. In an embodiment, the transmitter of the present system is provided with a translator for translating the audio information into an encrypted audio information prior to transmission. Likewise, in that embodiment, the receiver is provided with a translator for translating received encrypted audio information into non-encrypted audio information, prior to communicating the information to the sound output.
[0010] In an embodiment, the transmitter of the present invention is provided with an amplifier to amplify the audio information captured by the input, thereby increasing the sound quality and dynamic range of the captured audio information. Preferably, the receiver is also provided with an amplifier for further improving the sound quality and volume level of the audio information.
[0011] It is a further object of the present invention to provide a wireless communication system that will have a greater range of transmission capability from the transmitter to the receiver. In an embodiment, the transmitter is provided with a radio frequency (“RF”) power amplifier for increasing the distance over which the transmitter can transmit the audio information. Preferably, the receiver also comprises a low noise amplifier (“LNA”) for further increasing the operable distance at which the receiver can receive transmissions from the transmitter.
[0012] It is a further object of the present invention to provide a wireless communication system that will be less susceptible to interference from neighboring radio frequency devices, and will be less likely to provide interference for those neighboring devices. In an embodiment, the transmitter is provided with a radio frequency filter for determining a radio frequency at which to transmit the audio information. Preferably, the receiver likewise comprises a radio frequency filter for receiving the audio information transmitted at the radio frequency selected by the transmitter.
[0013] Other features and advantages of the invention will be apparent from the following specification taken in conjunction with the following drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] To understand the present invention, it will now be described by way of example, with reference to the accompanying drawings in which:
[0015] FIG. 1 is a flowchart illustration of a transmitter and the components thereof configured for transmitting audio information in accordance with the principles of the present invention;
[0016] FIG. 2 is a software flowchart illustrating operations performed by a microcontroller installed within a transmitter configured in accordance with the principles of the present invention;
[0017] FIG. 3 is a flowchart illustration of a receiver and the components thereof configured for receiving audio information in accordance with the principles of the present invention; and,
[0018] FIG. 4 is a software flowchart illustrating operations performed by a microcontroller installed within a receiver configured in accordance with the principles of the present invention.
DETAILED DESCRIPTION
[0019] While this invention is susceptible of embodiments in many different forms, there is shown in the drawings and will herein be described in detail preferred embodiments of the invention with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention and is not intended to limit the broad aspect of the invention to the embodiments illustrated.
[0020] Referring initially to FIG. 1 , there is illustrated a block diagram for a wireless transmitter 100 configured in accordance with the principles of the present invention. The wireless transmitter 100 includes an input 101 . In a preferred embodiment and as illustrated in FIG. 1 , input 101 is a microphone. It will be understood that input 101 is any input capable of receiving audio information, including an eighth- or quarter-inch stereo input port, and an RCA input port. A microphone for the present invention is either directional or omni-directional, for receiving sound in a frequency range of at least 50 Hz to 20 kHz.
[0021] The transmitter 100 includes a filter 103 , 106 , 108 , 110 for modifying the audio information and radio signal. As illustrated in FIG. 1 , a variety of different types of filters may be used in the present invention without departing from the principles thereof. In one embodiment, the filter is a low pass audio filter 103 . The low pass audio filter 103 allows lower frequency signals to pass through the filter 103 , while blocking undesirable high frequency signals. Those high frequency signals are highly attenuated by the filter 103 , thereby eliminating the static “squeal” common with short-wave radio transmission and improving the quality of the audio information. In that embodiment, the low pass audio filter 103 can be constructed of either passive or active electronic components.
[0022] In another embodiment, the filter for modifying the audio information is a Gaussian low pass filter 106 . A Gaussian low pass filter 106 in the present system is advantageous for use in an embodiment involving an analog-to-digital (“A/D”) converter 104 . When analog audio information is converted to digital form, the resulting audio signal is a square waveform. A Gaussian low pass filter 106 can be used to “smooth” the edges of that digitized audio waveform, resulting in a waveform suitable for frequency modulation (“FM”). As will be understood by one of skill in the art, a Gaussian low pass filter 106 is essentially an equation applied upon the input audio information signal to approximate a Gaussian curve. The Gaussian low pass filter 106 is also useful for achieving radio transmission compliance with Part 15 of the rules of the Federal Communications Commission. While it is particularly advantageous to use the Gaussian low pass filter 106 in an embodiment with the A/D converter 104 , it is to be understood that the Gaussian low pass filter 106 can also be used in the present invention without the A/D converter 104 .
[0023] In another embodiment, the filter for modifying the radio frequency signal is a surface acoustic wave (“SAW”) filter 108 . The purpose of the SAW filter 108 is to accept radio waves within a desired frequency range, while rejecting radio waves outside of the designed range. In any RF transmission, captured audio information will necessarily include information at undesirable frequencies, usefully heard by the user as a background static “hiss”. Furthermore, audio information transmitted at frequencies relatively close to each other, such as a cordless phone and a standard home radio receiver, can be more effectively isolated from each other by using the SAW filter 108 , whereby interference from other radio frequency devices can be reduced.
[0024] As illustrated in FIG. 1 , the filters 103 , 106 , 108 , 110 are not mutually exclusive. All of them can be used as filters with the present invention. In the combination illustrated, the filters 103 , 106 , 108 , 110 are positioned so as to create the highest quality audio information to be transmitted by the transmitter 100 . As further illustrated in FIG. 1 , the filters 103 , 106 , 108 , 110 may be used repetitively. In a preferred embodiment, for example, two SAW filters 108 , 110 are used to enhance the quality of the RF signal prior to transmission.
[0025] The transmitter 100 further comprises a selector for selecting a radio frequency at which to transmit the modulated audio information. The selected radio frequency can be pre-programmed into the transmitter 100 , such that by default, the audio information will be transmitted at the selected radio frequency. In another embodiment, a selector switch is provided for the user to select a radio frequency, to which the frequency modulator 107 is tuned to frequency modulate and transmit the digitized audio information.
[0026] The transmitter 100 further comprises an antenna 111 , which is used to radiate electromagnetic waves at the selected frequency. Antenna 111 converts radio frequency electrical energy to radiated electromagnetic energy. The size of antenna 111 is determined by the frequency of the signal to be transmitted. In a preferred embodiment, a wire cut to one-half wavelength is sufficient for the purposes of the present invention.
[0027] In one embodiment, the transmitter 100 further comprises an A/D converter 104 , which converts the captured analog audio information to a digital signal representing equivalent information. As will be understood by one of skill in the art, A/D converter 104 samples and stores a plurality of data points of the amplitude of the captured input analog audio information, and based on those stored sample points, creates a digitally equivalent signal. It will be further understood by those of skill in the art that in the present invention, a variety of A/D conversion algorithms can be used without departing from the principles of the invention, including Delta-Sigma, CVSD, ADPCM, PCM, uLaw, aLaw and the like.
[0028] In one embodiment, the transmitter 100 further comprises a microcontroller 105 , which is used to control the routing of data through the various electrical components of the transmitter 100 . As illustrated in FIG. 1 , microcontroller 105 further allows the trafficking of the digital data stream from the A/D converter 104 to a radio frequency modulator 107 . In one embodiment of the present invention, microcontroller 104 can add packet information, error correction and/or encryption security to the audio information that is to be transmitted by the transmitter 100 . Microcontrollers capable of use in the present invention for those tasks are currently available from Motorola, Texas Instruments, Cypress, Microchip and Amtel, among others.
[0029] As illustrated in FIG. 2 , a software diagram is illustrated for use with a microcontroller 105 installed in the transmitter 100 . At initial step 200 , digital audio information is received by the microcontroller 105 from the A/D converter 104 , and stores that information in a memory, as illustrated in step 201 . It will be understood that the received audio information is stored in memory essentially as it is received; that is, steps 200 and 201 are performed nearly simultaneously. Next, at step 202 , the microcontroller 105 creates a data packet to accompany the transmission of the audio information. It will be understood by one of skill in the art that a data packet is a method of transmitting information so as to include meta-data, i.e., information about the transmitted information. In the present invention, the meta-data in the data packet can include error control information and encryption information. In one embodiment, and as illustrated at step 203 , the audio information is encrypted. Information necessary to decrypt the encrypted audio information may be stored as meta-data in the data packet awaiting transmission, or can be stored in a microcontroller 317 installed within the receiver 300 .
[0030] In one embodiment, and as illustrated at step 204 , error checking information can be added as meta-data to the data packet awaiting transmission. It will be appreciated by one of skill in the art that a variety of encryption and error-checking algorithms can be used with the present invention without departing from the principles thereof. Encryption is useful in the present invention, so as to avoid surreptitious eavesdropping upon the transmissions from the transmitter 100 . Error checking is useful in the present invention, so as to provide a way for the receiver 300 to ensure that all of the data transmitted by the transmitter 100 was actually received.
[0031] Referring again to FIG. 1 , in one embodiment, the transmitter 100 further comprises an audio amplifier 102 , 109 . The amplifier may be an automatic gain control amplifier 102 , which amplifies the strength of the audio information captured by the microphone 101 . The amplifier 102 includes a variable gain element that dynamically adjusts the voltage level from the microphone, and essentially increases the amount of audio information that can be effectively captured by the microphone 101 . The amplifier 102 provides dynamic amplification, such that when a low-level signal is received from the microphone 101 , the amplifier 102 amplifies the gain strength from that signal, whereas when a high-level signal is received from the microphone 101 , the amplifier 102 provides less gain strength to that signal. Electronic components for constructing an exemplary automatic gain control amplifier 102 for use in the present system are available from Analog Devices, part no. SSM2167.
[0032] Another amplifier for use in the transmitter 100 is a radio frequency power amplifier 109 , which boosts the voltage level or power level of a signal, thereby creating a linear replica of the input signal, but with enhanced power level prior to transmission. The purpose of the power amplifier 109 is to increase the signal strength of the transmitter 100 , and thus enhance both the distance at which transmitter 100 and receiver 300 may effectively communicate, and increase the clarity of the audio information received by receiver 300 . The output signal from the power amplifier 109 may also be a non-linear analog function of the input signal. As illustrated in FIG. 1 , the automatic gain control amplifier 102 and the radio frequency power amplifier 109 are not mutually exclusive of each other, and indeed are preferably used simultaneously in the transmitter 100 assembly.
[0033] In one embodiment, transmitter 100 further comprises a voltage control oscillator 107 , which changes its frequency according to a control input, thereby creating a radio frequency carrier signal. The voltage control oscillator 107 optionally includes a radio frequency modulator, which in turn modulates the frequency of the voltage control oscillator 107 output, thereby creating a frequency-modulated signal for FM transmission. Voltage control oscillator 107 and radio frequency modulator are preferably, and as illustrated, contained in the same discrete electronic component, but may be separated without departing from the principles of the present invention.
[0034] Referring to FIG. 3 , a component diagram is provided of the components of a receiver 300 configured in accordance with the present invention. The receiver comprises an antenna 312 for receiving the audio information transmitted from the antenna 111 of the transmitter 100 . Opposite the transmitter antenna 111 , the antenna 312 converts radiated electromagnetic energy to radio frequency electrical energy. Similar to the transmitter antenna 111 , the size of the receiver antenna 312 is determined by the frequency of the signal to be received; in the preferred embodiment, a one-half wavelength wire is sufficient.
[0035] The receiver 300 further comprises a filter 313 , 315 , 301 . In one embodiment, the filter 313 is a radio frequency SAW filter 313 , 315 , discussed previously in the context of the transmitter 100 . As in the transmitter 100 , the SAW filter 313 , 315 in the receiver 300 is for isolating a desired range of radio signal information from background noise, thereby increasing the clarify and range of the audio information. As illustrated in FIG. 3 , a plurality of SAW filters 313 , 315 may be included in the receiver 300 assembly; in particular, it is useful to provide a first SAW filter 313 prior to routing the audio information to a low noise amplifier 314 , as will be herein discussed, and also a second SAW filter 315 to filter information output from the low noise amplifier 314 .
[0036] The low noise amplifier 314 is provided in one embodiment, to enhance the strength of signals received from the transmitter 100 , thereby increasing the operative distance at which transmitter 100 and receiver 300 may communicate. Amplifier 314 can be constructed of a discrete radio frequency transistor, or of MMIC amplifiers. In another embodiment, the receiver 300 further comprises an audio amplifier 320 , for increasing the amplitude of the audio information before it is transmitted to the audio output 321 . To adjust the sound level of the audio output 321 , the audio amplifier 320 may be operably driven by a volume control operable by the user. Audio amplifier 320 is preferably, as will be understood by one of skill in the art, an integrated circuit device optimized for high audio voltage gain, with the ability to drive the low impedance of a standard speaker coil.
[0037] In a preferred embodiment, the receiver 300 further comprises a radio frequency receiver circuit 316 , which detects, demodulates and amplifies received radio frequency signals. The radio frequency receiver circuit in turn comprises a voltage control oscillator 301 , a radio frequency mixer 302 , a filter 303 and a signal detector 304 . As will be understood by one of skill the art, the radio frequency receiver circuit 316 is for selecting from among the electromagnetic information received by the antenna 312 the audio information transmitted at the selected frequency by the transmitter 100 . Exemplary radio frequency receiver circuits for use in the present invention are available as model no. ML2722 from Micro Linear and model no. BH4127 from ROHM.
[0038] In one embodiment, the receiver further comprises a microcontroller 317 , for routing information between the various electrical components of the receiver 300 , and for performing various data operations upon the received audio information. Referring now to FIG. 4 , there is illustrated a software flowchart for use in the microcontroller 317 of the receiver 300 . At initial step 401 , the audio information is received from the antenna 312 (or from another device such as the receiver circuit 316 , which received the audio information from the antenna 312 ). As the audio information is received, it is in step 402 stored in a random access memory. In the preferred event that the audio information has been encoded into a data packet, the data packet is unpacked by the microcontroller 317 , as will be understood by one of skill in the art, at step 403 ; i.e., the data packet is separated into its information and meta-data components as previously described with reference to the microcontroller 105 of the transmitter 100 .
[0039] In the preferred event that the audio information transmitted from the transmitter 100 was encrypted, the microcontroller 317 next, at step 404 , decrypts the encrypted audio information. Information necessary for decrypting the encrypted audio information may be pre-programmed into the microcontroller 317 , or may be included in the meta-data of the transmitted audio information packet. In the preferred event that the meta-data associated with the audio information packet includes error checking information, the microcontroller 317 next, at step 405 , uses that error checking information to verify that the audio information received from the transmitter 100 is received from error. The algorithms necessary for performing the decryption and error checking have been discussed in referenced to the transmitter 100 , and will be understood by one of skill in the art. Lastly, at step 406 , the microcontroller transmits the decrypted audio information to the next element in the electrical assembly of the receiver 300 .
[0040] In one embodiment, the receiver 300 further comprises a digital-to-analog (“D/A”) converter 316 , for translating received digital audio information into analog audio information so that it may be communicated to the audio output 321 . Preferably and as previously discussed and as illustrated in FIG. 1 , the audio information transmitted by the transmitter 100 is digital audio information. Before the received digital audio information may be communicated to the audio output 321 , it must be translated into analog audio information. Therefore, in the preferred embodiment, the receiver 300 includes a D/A converter 318 for that purpose.
[0041] The receiver 300 further comprises an output 321 . In a preferred embodiment, the audio output 321 is a standard speaker, an electro-acoustic transducer for converting electrical signals into sound audible by the user. In the preferred embodiment, the speaker 321 has an impedance between 8 and 32 ohms at up to 1 watt of voltage. Audio output 321 can also be an audio output port, such as a quarter-inch or eighth-inch stereo output port, or RCA output port.
[0042] As illustrated in FIG. 1 and FIG. 2 and described herein, it will be understood that the precise illustrated assemblies of the transmitter 100 and the receiver 300 , i.e. the order and arrangement of the components, is not required to fulfill the objectives of the present invention. Other arrangements and orders of the various components are possible to achieve those objectives, without departing from the principles of the present invention.
[0043] While the specific embodiments have been illustrated and described, numerous modifications come to mind without significantly departing from the spirit of the invention, and the scope of protection is only limited by the scope of the accompanying Claims.
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A wireless audio communication system and monitor is disclosed, comprising a transmitter and a receiver. The transmitter comprises an input for receiving audio information, and a filter for modifying the audio information. The transmitter further comprises a converter for converting the audio information into a digital audio information, and an antenna for wirelessly transmitting the digital audio information at a selected radio frequency. The receiver comprises an antenna for receiving the transmitted digital audio information, and a filter for modifying the digital audio information. The receiver further comprises a converter for converting the digital audio information into the audio information, and an output for communicating the audio information.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to co-pending U.S. Provisional Patent Application No. 62/259,859, filed on Nov. 25, 2015, the entire contents of which is hereby incorporated by reference.
FIELD
[0002] The present invention relates to mobile (e.g., wheeled) devices and, more particularly, to a handle assembly for such devices.
SUMMARY
[0003] Tool storage devices are often used to transport tools and accessories between and around worksites. As such, the devices may include wheels and a telescoping handle assembly to allow for convenient transportation of the tool storage devices. However, durability is a factor because the devices may be used in various terrain and weather conditions on the worksite. Due to these conditions and the generally rugged use, the devices sustain various shocks and impacts that are transmitted from the device (e.g., the wheels) through the telescoping handle assembly. These impacts and shocks can lead to early failure of the mechanism that secures the telescoping handle assembly in an extended position.
[0004] In one independent aspect, a telescoping handle assembly for a mobile device, such as a wheeled device, a storage device, etc. may be provided. The handle assembly may generally include a first handle section; a second handle section telescopingly arranged relative to the first handle section; and a latch assembly fixed to one of the first handle section and the second handle section and selectively engageable with the other of the first handle section and the second handle section. The latch assembly may include a latch body positioned between the first handle section and the second handle section, and a shock-absorbing mount positioned between the latch body and the one of the first handle section and the second handle section.
[0005] In another independent aspect, a wheeled mobile device may generally include a frame; a wheel assembly supporting the frame; and a telescoping handle assembly including a first handle section, a second handle section telescopingly arranged relative to the first handle section, and a latch assembly fixed to one of the first handle section and the second handle section and selectively engageable with the other of the first handle section and the second handle section. The latch assembly may include a latch body positioned between the first handle section and the second handle section, and a shock-absorbing mount positioned between the latch body and the one of the first handle section and the second handle section.
[0006] In yet another independent aspect, a method of assembling a telescoping handle assembly for a mobile device may be provided. The method may generally include fixing a latch body of a latch assembly to one of a first handle section and a second handle section; positioning a shock-absorbing mount between the latch body and the one of the first handle section and the second handle section; and inserting the one of the first handle section and the second handle section into the other of the first handle section and the second handle section in a telescoping arrangement with the latch assembly positioned in the other of the first handle section and the second handle section.
[0007] Other independent features and independent aspects of the invention will become apparent by consideration of the following detailed description, claims and accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a perspective view of a mobile device, such as a wheeled storage device (e.g., a portable rolling tool bag).
[0009] FIG. 2 is an enlarged exploded view of a handle assembly for the device shown in FIG. 1 .
[0010] FIG. 3 is a perspective view of a latch assembly for the handle assembly shown in FIG. 2 .
[0011] FIG. 3A is a perspective view of a bushing of the latch assembly shown in FIG. 3
[0012] FIG. 4 is an enlarged cross-sectional view of the handle assembly of FIG. 2 taken generally along line 4 - 4 in FIG. 1 .
[0013] FIG. 5 is an enlarged cross-sectional view of the handle assembly of FIG. 2 taken generally along line 5 - 5 in FIG. 1 .
[0014] FIG. 6 is a perspective view of a prior art latch assembly.
DETAILED DESCRIPTION
[0015] Before any independent embodiments of the invention are explained in detail, it is to be understood that the invention is not limited in its application to the details of construction and the arrangement of components set forth in the following description or illustrated in the following drawings. The invention is capable of other independent embodiments and of being practiced or of being carried out in various ways. Also, it is to be understood that the phraseology and terminology used herein is for the purpose of description and should not be regarded as limiting.
[0016] Use of “including” and “comprising” and variations thereof as used herein is meant to encompass the items listed thereafter and equivalents thereof as well as additional items. Use of “consisting of” and variations thereof as used herein is meant to encompass only the items listed thereafter and equivalents thereof.
[0017] FIG. 1 illustrates a mobile device 10 , such as a portable rolling tool bag, movable between and around various locations (e.g., work sites, construction sites, garages, etc.). Exemplary devices are shown and described in U.S. Patent Application Publication No. 2016/0023349, filed Jul. 17, 2015, the entire contents of which is hereby incorporated by reference. In other constructions (not shown), the device 10 may include a tool box, a storage device, a suitcase, a trolley, a dolly, a hand truck, a cart, a wheel barrow, a stroller, a wheel chair, a bed, a table, etc.
[0018] The device 10 generally includes a frame 14 supported by one or more wheels 18 . As a tool bag, the illustrated device 10 also includes a body 22 defining a storage compartment (not shown), capable of supporting and storing tools, accessories, materials, etc., in an organized manner. A handle assembly 26 is connected to the frame 14 and facilitates maneuvering of the device 10 .
[0019] The handle assembly 26 includes a handle member 30 connected to an end of one or more support arms 34 (two in the illustrated construction) adjustably supported by the frame 14 . Each support arm 34 includes a number of telescoping arm sections 38 a , 38 b . . . 38 n (three in the illustrated construction). The arm sections 38 a - 38 c are adjustable between an extended position (see FIGS. 1-2 ) and a retracted position (not shown) to adjust the position of the handle member 30 relative to the frame 14 and the body 22 .
[0020] Each arm section 38 is an elongated hollow member with a substantially uniform cross-section extending along its length. Each outer arm section (e.g., the arm section 38 b ) has a cross-section sized to slidingly receive an associated inner arm section (e.g., the arm section 38 a ) having a relatively smaller concentric cross-section. In the illustrated embodiment, each arm section 38 has a generally rectangular cross-section defined by a pair of short walls 47 and a pair of long walls 48 . In other embodiments (not shown), the arm sections 38 may have any shape cross-section with corresponding walls.
[0021] With reference to FIGS. 1-2 , a latch assembly 42 is provided between adjacent arm sections 38 to selectively and releasably hold the arm sections 38 in the extended position. In the illustrated construction, each outer arm section (e.g., the arm section 38 b ) defines a recess (e.g., an opening 46 ) proximate its upper end 39 , and each inner arm section (e.g., the arm section 38 a ) supports a projection 50 proximate its lower end 40 . Each projection 50 is selectively engageable in an associated opening 46 to hold the adjacent arm sections (e.g., the arm sections 38 a , 38 b ) in a selected relative position. In the illustrated embodiment, the opening 46 arranged to receive the projection 50 is defined in one of the short walls 47 .
[0022] Each projection 50 (see FIG. 3 ) is movably supported on a lower portion 55 of a latch body 54 . The lower portion 55 of the latch body 54 is sized to be slidingly received in the outer arm section 38 (e.g., the arm section 38 b ) and is too large to be received in the inner arm section 38 (e.g., the arm section 38 a ). An actuating member 58 is operable to move the projection 50 relative to the body 54 between a projected, latching position (see FIG. 3 ) and a retracted, release position (see FIG. 5 ). An actuator (not shown) is operable by the user to retract and disengage each projection 50 from its associated recess 46 so that the arm sections 38 can be retracted and the handle member 30 lowered.
[0023] The body 54 is fixed to the arm section (e.g., the arm section 38 a ), for example, by a rivet 62 ( FIGS. 2 and 4 ), or a similar fastener, such as a pin, etc. In the illustrated construction, the rivet 62 extends through a pair of openings 64 defined in the long walls 48 of the arm section 38 adjacent the lower end 40 of the arm section 38 and an opening 66 in an upper portion 56 of the body 54 aligned with the openings 64 (as shown in FIG. 4 ). In the illustrated embodiment, one end of the rivet 62 has a pre-formed head and the other end of the rivet 62 is deformed to secure the rivet 62 from being axially removed from the opening 66 in the body 54 .
[0024] The upper portion 56 of the body 54 is sized to be received in the lower end 40 of the inner arm section 38 (e.g., the arm section 38 a ), as shown in FIGS. 4-5 . The lower portion 55 of the body 54 inhibits insertion of the upper portion 56 of the body 54 into the arm section 38 to a position in which the openings 64 in the long walls 48 do not align with the opening 66 in the body 54 .
[0025] A similar handle assembly including a latch assembly is illustrated and described in U.S. Pat. No. 6,339,863, issued Jan. 22, 2002, and in U.S. Pat. No. 6,619,448, issued Sep. 16, 2003, the entire contents of both of which are hereby incorporated by reference.
[0026] In existing handle assemblies, a failure mode is a fracture around the rivet which causes the handle assembly to fail at 17 to 22 miles in a fatigue cyclic loading “life test”. Such failure is likely to occur even with improved materials, geometry of an existing latch assembly (see FIG. 6 ).
[0027] As shown in FIGS. 2-5 , the illustrated latch assembly 42 incorporates a shock-absorbing mount 70 ( FIG. 3A ) operable to absorb, dampen, limit, reduce, etc. a shock or impact between the frame 14 and the handle member 30 (e.g., between the body 54 and the walls 47 , 48 of the adjacent arm section 38 ). The mount 70 may increase or contribute to an increase in the life, strength, durability, etc. of the handle assembly 26 to, for example, at least 30 miles or more in the fatigue cyclic loading “life test”.
[0028] In the illustrated construction, the mount 70 includes a bushing 74 received in the opening 66 and is positioned between the body 54 and the rivet 62 . The bushing 74 is formed of shock-absorbing material, such as, for example, urethane (e.g., thermoplastic polyurethane (TPU)), soft plastic, rubber, etc. The material, material characteristics, structure, etc. of the bushing 74 can be adjusted based on, for example, the desired shock-absorbing characteristics.
[0029] As illustrated, the bushing 74 is formed as a discrete or separate part and is inserted into the opening 66 . In other constructions (not shown), the bushing 74 may be formed with the body 54 , for example, in a multi-shot molding process for the body 54 . After the bushing 74 is assembled with the body 54 , the rivet 62 is inserted.
[0030] In operation with the illustrated mount 70 , an impact or shock on the device 10 (e.g., on the wheels 18 as the device 10 is rolled across an uneven surface) is transmitted through the frame 14 to the outer arm section (e.g., the arm section 38 b ), through the walls 47 , 48 of the arm section 38 b to the body 54 . The shock is absorbed or dampened by the bushing 74 before reaching the rivet 62 and, through the rivet 62 , the inner arm section (e.g., the arm section 38 a ) and the handle member 30 . An impact or shock on the handle member 30 is likewise absorbed or dampened by the bushing 74 before reaching the walls 47 , 48 of the outer arm section 38 b . Providing a mount 70 between each of the adjacent arm sections 38 sequentially reduces the magnitude of the impact or shock as it passes through each of the mounts 70 .
[0031] In other constructions (not shown), in addition to or as an alternative to the illustrated mount 70 , a shock-absorbing mount may be provided at one or more other locations between components in the force-transmitting path between the frame 14 and the handle member 30 . For example, a shock-absorbing bushing, plate, other structure, etc., may be provided between the long walls 48 of the outer arm section 38 b and the end of the rivet 62 . In another example, a shock-absorbing mount may be provided between the frame 14 and the adjacent arm section 38 c.
[0032] In the illustrated construction, the mount 70 has the form of the hollow cylindrical (e.g., tubular) bushing 74 received in the circular opening 66 and receiving the cylindrical rivet 62 . In other constructions, the mount 70 may have a different form factor. For example, with a square or rectangular pin (not shown), the mount 70 may include a pad (e.g., a flat isolation pad) engaging between the pin and the associated support structure (e.g., the opening in the latch body, the opening in the wall of the arm section, etc.).
[0033] In the illustrated construction, a shock-absorbing mount 70 is provided between each adjacent arm section 38 of each support arm 34 of the handle assembly 26 . Accordingly, each additional connection and corresponding mount 70 increases the impact or shock reduction capability. In other constructions (not shown), a shock-absorbing mount 70 may be provided between only selected adjacent arm sections (e.g., between only the arm sections 38 b , 38 c closest to the frame 14 ).
[0034] One or more independent features and/or independent advantages of the invention may be set forth in the claims.
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A telescoping handle assembly, a mobile device, and a method of assembling a telescoping handle assembly for a mobile device. The handle assembly may include a first handle section, and a second handle section telescopingly arranged relative to the first handle section. The handle assembly may further include a latch assembly fixed to one of the first handle section and the second handle section and selectively engageable with the other of the first handle section and the second handle section. The latch assembly may include a latch body positioned between the first handle section and the second handle section and a shock-absorbing mount positioned between the latch body and the one of the first handle section and the second handle section.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a fibrous web impregnated with a lotion for household cleaning purposes. More particularly it relates to a fibrous web bonded with a rubber latex and wherein the lotion contains a metal salt as an anti-fogging ingredient.
2. Description of the Prior Art
Fibrous cleaning materials comprising an impregnated fibrous web bonded with a latex material is known to be useful for household cleaning. In particular, a fibrous web impregnated with a rubber latex is known to have exceptional utility for this purpose. Such a product is described in U.S. Pat. No. 3,981,741 granted Sept. 21, 1976 to lino. One of the main technical problems with the use of such a wiper has been the formation of a "fog" on the surface of articles cleaned with such a product. The fog is especially noticeable on surfaces such as glass and chrome. This fog is believed to consist of residues extracted from binder material on the web. The inventor in the aforementioned U.S. Pat. No. 3,981,741 apparently deals with this problem by including a polar high molecular weight substance such as polyvinyl acetate or acrylonitrile-butadiene copolymer. According to said patent disclosure the particles of the rubber and those of the polar high molecular weight substance presumably prevent each other from forming films, with the result that the particles adhere to the fibrous material individually.
SUMMARY OF THE INVENTION
In accordance with the present invention, a fibrous web adapted for wiping purposes is bonded with a rubber latex selected from the group consisting of natural rubber latex, butadiene rubber latex and styrene-butadiene rubber latex and impregnated with a cleaning lotion containing zinc chloride. Without wishing to be bound by theory, the present inventor believes that the zinc chloride insolubilizes the low molecular weight molecules present on the web that are not cross linked so that they do not dissolve into the lotion and form an unsightly residue when applied to glass, chrome, and like surfaces.
Since zinc chloride is a deliquescent crystal, when it is left behind on a mirror or like object, it will absorb moisture from the air, remain transparent and serve as an extremely effective anti-fogging device. Zinc chloride also has an insolublizing effect which serves to increase the wet strength of the web.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The rubber used in the present invention is selected from the group consisting of natural rubber, polybutadiene rubber, and styrene butadiene rubber. Of these, styrene butadiene is preferred and most particularly a styrene butadiene latex of high styrene content. The latex may be carboxylated and may contain N-methylolacrylamide groups, or other means of highly crosslinking the polymer.
The fibrous web to be bonded with the rubber latex in accordance with this invention may be comprised of natural or synthetic fibers and may consist of any nonwoven fabric woven, knitted or netted fabric, paper and the like. A nonwoven fabric predominately of short (paper length) fibers is preferred for its low cost and disposability.
The cleaning property of the fibrous web is enhanced by impregnation with a lotion which contains, for example, water, a glycol, surfactant, film former, preservative and fragrance. In accordance with the present discovery, if the lotion further includes 0.2 to 1% by weight zinc chloride the problem of fogging is eliminated. The exact mechanism for this improvement is not understood. Other metal salts tried by the present inventor have not been found to have the suitability of the zinc chloride. Aluminum chloride, while it appeared to insolubilize the low molecular weight molecules of the rubber latex, left behind crystals on the surface which was wiped. Other metal chlorides, namely cobalt, strontium and manganese yielded only a slight improvement on the fogging problem. Nitrates of magnesium, aluminum, nickel and cadmium gave good improvement but are not suitable for use on the human skin.
The composition of the cleaning lotion is adjusted to suit the particular cleaning object or purpose. In general it comprises the following ingredients:
Surface active agents are added to increase the effect of removing dirt, especially grease, from the surface to be cleaned. The surfactant should be non-ionic so as not to interfere with the action of the zinc chloride.
Wetting agents, such as polyvinyl alcohol and carboxymethyl cellulose may also be included for enhancing the cleaning effect of the wiper.
Water soluble, non-volatile solvents which act to dissolve oily dirt are included for an improved cleaning effect. Examples include polyethylene glycol, glycerin, polypropylene glycol, ethylene glycol monobutyl ether and like polyhydricalcohols. Such solvents should, of course, not be a solvent for the rubber latex.
Fragrances may be included for their esthetic value and a preservative to stabilize and increase the shelf life of the lotion.
In accordance with the present invention, a rubber latex is applied to a fibrous web by conventional methods, for example, by dipping, by roller coating or by spraying. As will be understood by one of ordinary skill in the art to which the present invention pertains the amount of latex applied to the fibrous web is sufficient to provide the strength required by the cleaning purpose. Thereafter the web containing the rubber latex is dried in order to achieve the bonding effect.
Subsequently the bonded web is impregnated with the cleaning lotion again by conventional means to provide the desired level of addition of the cleaning lotion.
The principles, features and advantages of the present invention will be further understood upon consideration of the following specific example; wherein percentages are all by weight:
EXAMPLE
An air laid web consisting of 90% Northern Pine pulp and 10% polyester fibers of 15/8" length was impregnated by dipping it in a binder emulsion comprising a high styrene butadiene latex containing an urea formaldehyde cross linking resin. The binder was implied at the rate of 9% solids by weight of the web. Thereafter a lotion was applied at the rate of 300% by weight of the fibrous web. The cleaning lotion comprised ethylene glycol monobutyl ether 7%, propylene glycol 7%, surfactants 0.7%, fragrance 0.035%, preservative 0.08%, zinc chloride 0.5% and distilled water 84.685%.
In order to evaluate the antifogging effect of the zinc chloride, optical reflectance tests were carred out to measure the amount of haze and visual contamination on the test surface which consisted of a mirror. The optical reflectance tests were conducted as follows:
A mirror (one foot square) was cleaned with soap and water, then rinsed and wiped dry with a clean towel with good wipe dry properties and no latex additives or soluble materials. The wipers were lotionized with 300% by weight of lotion. The mirror was wiped evenly by one pass at a time until the whole mirror had been wiped. Then the procedure was repeated in the cross-direction. The mirror was allowed to dry at 75° F. and 50% relative humidity for one hour. After the drying step, the light which was transmitted back to an incident light source was measured by an optical densicron attached to a motorized traverse rail which passed across the mirror. The signal was connected to a recorder and the change (compared to measurements on the clean mirror) in transmitted or reflected light was observed. This yielded a measure of light scattered by a residue film or haze.
The results were as follows:
______________________________________Sample Description Percent Reflectance______________________________________Clean Mirror 93.6Control Sample Wipe 84.9Sample with 0.5% Zinc chloride 93.9______________________________________
The control sample wipe was identical to the wipe described in the Example except for the omission of zinc chloride. The reduction in transmittance represented by the control sample wipe containing no zinc chloride in the lotion would be a commercially unacceptable result. As may be seen from the above, the inclusion of zinc chloride improves the performance of the wiper to the point where the mirror is wiped clean and restored to the original or better transmittance.
Although the invention has been described with reference to a preferred embodiment thereof, it is to be understood that various changes may be resorted to by one skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
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Fibrous web adapted for wiping purposes bonded with a rubber latex and impregnated with a cleaning lotion containing zinc chloride.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method for hydrocracking heavy fraction oils, particularly those containing asphaltene, i.e., 10 wt. % or more of pentane-insoluble ingredients.
2. Prior Art
Recently, hydrogenolysis of heavy fraction oils has increasingly been of importance. There have been proposed many methods for thermal cracking, catalytic cracking, and hydrogenolysis, etc.
The heavy fraction oils referred to herein are hydrocarbon oils containing 50 wt. % or more of a fraction boiling above 350° C., particularly those containing 1.0 wt. % or more of pentane-insoluble ingredients. For example, they include residual oils yielded by atmospheric or vacuum distillation of crude oils, or oils produced from coal, oil sand, oil shale, bitumen or the like. The term "cracking" herein is intended to obtain light fraction oils including naphtha and gasoline fractions, and, kerosene and light oil fractions.
In the general hydrogenation treatment of heavy fraction oils, the reduction of catalytic activity is the most serious problem technically or economically. Namely, the heavy fraction oil contains an asphaltene fraction which contains heavy metals such as vanadium and nickel. These metals severely deteriorate catalysts and hinder economical and continuous long-term uses of the catalysts. Many efforts for improving catalysts have been exerted to solve such a problem, and many improved catalysts have been proposed but they are not completely satisfactory. In addition, there have been proposed many elaborate contributions to improve a reaction apparatus, however, there have been left many problems to be solved.
Moreover, the cost of hydrogen is an important factor economically and technically. In the hydrotreatment of heavy fraction oils, the amount of consumption of hydrogen may be increased as a starting oil is heavier, thus costing a great deal.
As one of methods which solve the problem of such hydrogen cost, there is known a method in which a hydrogen donor compound yielded by hydrogenating a polycyclic aromatic compound is used (for example, U.S. Pat. No. 4,430,197). When the hydrocracking of a heavy fraction oil is effected with use of such a hydrogen donor compound, it is also well known that a catalyst is not necessarily needed and the hydrocracking reaction proceeds in an atmosphere of hydrogen gas at a relatively low pressure (for example, U.S. Pat. No. 4,294,686 and Oil & Gas Journal, Nov. 22, 1982, Pages 111 through 116).
The hydrogen donor solvent described above is a compound yielded by hydrogenating a hydrocarbon compound having polycyclic aromatic rings such as naphthalene and anthracene. It is well known that such a hydrogen donor liberates a hydrogen atom at high temperatures (for example, above 380° C.). There have also been accordingly proposed many trials to take advantages of said liberation nature industrially (for example, U.S. Pat. No. 2,953,513). It is also well known that such a hydrogen donor material is included in a thermally cracked oil, catalytically cracked oil, and hydrogenated oil from a heavy fraction oil, serving as an effective hydrogen donor in itself (for example, U.S. Pat. No. 3,970,545).
However, the cracking reaction in these methods is effectively performed only at relatively high temperatures, resulting in deposition of carbonaceous materials to cause a problem of what is called coking.
SUMMARY OF THE INVENTION
In view of the drawbacks of the conventional methods for hydrogenating heavy fraction oils, it is an object of the present invention to provide a more effective method for cracking heavy fraction oils in which is solved the problem as to an increased pressure loss caused by coking in a cracking tower (reaction tower) when treating the heavy fraction oils containing 1.0 wt. % or more of asphaltene.
It is another object of the present invention to provide a method for cracking heavy fraction oils containing 1.0 wt. % or more of asphaltene with little reduction of catalyst activity, reduced consumption of hydrogen and high cracking efficiency.
According to the present invention, the interior of a cracking tower is vertically divided into at least two portions with a partition for housing a solid catalyst having a hydrogenation function, and the divided portions are communicated with each other at the upper and lower parts thereof. The starting heavy fraction oil, a hydrogen donor solvent, and a hydrogen-containing gas are introduced into at least one of the divided portions at the lower part of said at least one portion, and further the fluid so introduced is circulated between the divided portions.
The method described above serves to relieve the problem of coking, and to effectively crack heavy fraction oils.
It should be noted here that cracking with use of a hydrogen donor does not require a catalyst and it can be effected without a catalyst in many cases. The present inventor has found the following facts experimentally:
(1) Upon cracking heavy oils with use of a hydrogen donor, cracking can be effectively achieved due to the presence of a slight catalytic action.
(2) At this point, the presence of the slight catalytic action greatly inhibits the formation of carbonaceous materials.
(3) The "slight catalytic action" described above can be effected not only by the presence of a catalyst having relatively high activity, for example a commercially available one, in a small quantity relative to the amount of starting oil used, but also by the presence of a catalyst having relatively low activity.
(4) As a countermeasure against troubles such as an increase in pressure loss due to production of carbonaceous materials, and blockade or clogging, it is effective to increase the flow rate of the fluid.
Namely, when cracking heavy fraction oils with the aid of a hydrogen donor, the presence of a slight catalytic action is effective, for which a solid catalyst can be the most conveniently used. Although the solid catalyst may be used in a fixed bed form, its use is likely to cause blocking or clogging. With such form, the flow rate of a fluid is insufficient, and the fluid and gas are prevented from flowing due to carbonaceous materials produced, resulting in accumulation of the carbonaceous materials followed by causing blocking. To avoid this, it is considered to fluidize the catalyst for use. However, when heavy fraction oils are generally cracked using a hydrogen donor solvent, the catalyst in the form of very fine particles should be employed to produce a uniform flow of the catalyst with use of the starting oil, the hydrogen donor and the gas. With the use of such fine particles, it is difficult to separate these particles from the resulting reaction products. When there are used relatively large particles (for example, more than 0.1 mm) which may be separated from the reaction products, a high fluid flow rate is required to fluidize these particles. However, it is impossible to obtain such a high flow rate only by the use of the starting oil and the hydrogen donor. Accordingly, for this purpose, it is necessary to recycle the reaction products. The recycling will be the cause for complication of an apparatus to be installed and for an increase in construction cost.
According to the present invention, a required flow velocity can be obtained by causing a natural circulating flow in a cracking tower and thereby avoiding any clogging with carbonaceous materials, while an effective cracking reaction may be carried out by placing a catalyst having a hydrogenating function in the cracking tower thereby causing the cracking reaction effectively and enabling the production of carbonaceous materials to be greatly reduced.
Another method for hydrocracking heavy hydrocarbon oils containing 1.0 wt. % or more of asphaltene, comprises the two steps (1) and (2):
(1) a starting heavy fraction oil is cracked in the presence of at least one kind of a solid material selected from the group consisting of solid catalysts and porous solids, and a hydrogen donor solvent; and at least 50 wt. % of heavy metals contained in the starting oil is caused to adhere to the solid material, and
(2) the reaction product mixture from the aforesaid stage (1) which is separated from the solid material to which the heavy metals have adhered at the cracking tower, and then hydrogenated in the presence of hydrogen gas and a hydrogenation catalyst; after which
(3) the reaction product mixture from the second step is sorted into a fraction including the hydrogen donor solvent, and other desired fractions, and the fraction including the hydrogen donor is recycled to the first step.
One characteristic of the cracking method just described above according to the present invention, is to treat heavy fraction oils in the two steps by the use of the hydrocracked oil functioning itself as a hydrogen donor since the hydrocracked oil contains the original hydrogen donor compound. The present inventor has revealed that when heavy fraction oils were cracked with use of a hydrogen donor solvent, metals such as vanadium and nickel are in a state in which they are apt to be removed. Consequently, by cracking heavy fraction oils with use the hydrogen donor solvent and removing metals in the first step, there are obtained oils which have been cracked to some extent while the metals have been almost removed therefrom. Thus, in the second step, the reduction of catalytic activity may be remarkably lessened and the operational conditions are enabled to be remarkably mild.
The methods according to the present invention will be described below with reference to the accompanying drawings in which:
FIGS. 1 through 3 are respectively longitudinal and cross-sectional views of a cracking tower used in the present invention. Numeral 1 is an introduction tube for introducing a starting oil, a hydrogen donative solvent and a hydrogen-containing gas, and 2 a partition for housing a solid catalyst with a hydrogenating function. The partition 2 in FIG. 1 is cylindrically shaped around the tube 1. The partition 2 in FIG. 2 comprises two plates around the introduction tube 1. The partition 2 in FIG. 3 is plate-shaped, on one side of which is provided the introduction tube 1. Numeral 3 is a foamy hydrogen-containing gas rising in a cracking tower, 4 an outlet pipe for discharging cracked fluid (produced by cracking) and the hydrogen-containing gas, and 5 a cracking tower.
In FIG. 1(a), H indicates the height of the cracking tower 5, h the height of the cylindrical partition 2, Di the inside diameter of the cracking tower 5, do the outside diameter of the cylindrical partition 2, di the inside diameter of the cylindrical partition 2, and 1 the distance between the lower end part of the cylindrical partition 2 and an air space in the cracking tower 5.
In FIG. 2, two of the plate-shaped partitions 2 are provided around the introduction pipe 1 and the outlet pipe 4. Both side ends of each of the partition are substantially brought into contact with the side surface of the cracking tower 5, and the upper and lower side ends thereof are communicated with each other on the upper and lower parts.
In FIG. 3, one sheet of the plate-shaped partition 2 is employed to provide the introduction pipe 1 and the outlet pipe 4 on one side. Both of the side ends of the partition 2 are brought into contact with the wall surface of the cracking tower 5, and the upper and lower side ends are communicated with each other at the upper and lower parts thereof. FIGS. 4(a) and (b) exemplarily show partitions 2 usable in the present invention, (a) a cylindrical one 2 and (b) a plate-shaped one 2.
Next, the method according to the present invention will be described below with reference to FIG. 1.
A starting oil, a hydrogen donative solvent and a hydrogen-containing gas are introduced through the introduction pipe 1 provided on the lower part of the cracking tower 5. The interior of the cracking tower 5 is vertically divided into two parts by the cylindrical partition 2 including a solid catalyst housed therein, and the aforesaid two parts are communicated with each other on the upper and lower parts of the partition 2. It is preferable for the introduced hydrogen-containing gas 3 to be introduced toward the inner part of the cylindrical partition 2 so as not to flow into the outside portion of the partition 2. The same is also applied to the heavy fraction oil and the hydrogen donor solvent. The foamy hydrogen-containing gas 3 ascends the interior of the partition 2.
With such construction, the fluid in the cracking tower 5 is circulated in the direction of an arrow shown in the figure due to the intra-tower pressure unbalance caused by the small specific gravity of the region in which the hydrogen-containing gas 3 is present exists.
A part of the above-described circulating fluid is capable of passing through the solid catalyst-housed partition 2 from the outside of the partition 2 (the side on which the hydrogen-containing gas 3 is not present) to the interior thereof (the side on which the gas is present, in the direction shown by an arrow (dotted line). The amount of passage of the fluid changes depending on the pressure balance between the outside and inside of the partition 2. The void ratio of the partition 2 preferably ranges from 5 to 95% in general. The void ratio used herein is the proportion of a portion existing as a space in a unit volume.
With such arrangement where a cylinder as the partition 2 is inserted in the cracking tower 5, it is possible to yieId a circulating flow inside the tower, assure a required flow velocity, and avoid any blocking in the cracking tower 5 caused by carbonaceous materials therein.
The hydrogen-containing gas 3 rises in the cylindrical partition 2 and is exhausted from the outlet pipe 4, while the fluid circulates in the cracking tower 5 and, after a prescribed residence time, is discharged from the outlet pipe 4. Accordingly, the fluid which resides for a prescribed period of time under conditions of a prescribed temperature and pressure can be cracked to produce lighter fractions. At this point, the fluid contacts with the catalyst in the cylindrical partition 2 while circulating in the cracking tower 5, so that the cracking may be more effectively effected with the attendant remarkable reduction of production of carbonaceous materials as compared with a case in which no catalyst is used.
To obtain a satisfactory circulating flow with the structures of the cracking tower 5 and cylindrical partition 2, the symbols indicated in FIG. 1 should preferably be in the following relationships:
e<di
1.01≦Di/di≦3.0
0.05≦(do-di)/2di≦3.0
The partition for housing a solid catalyst according to the present invention is porous as a whole, one part or the whole of which being composed of the solid catalyst having a hydrogenation function, while it is generally porous plain plate- or curved plate-shaped as a whole. A part or the whole of the plate is formed by an assembly of solid catalyst particles having a hydrogenation function. The partition may be illustrated by those prepared by housing at least one kind of particulate catalyst selected from extrusion molded catalyst, spherical catalyst and compression molded catalyst, in a metal mesh, punching metal or the like, and may also be illustrated by an assembly of catalyst particles bonded to each other with a binder.
The thickness of the partition for housing a solid catalyst is 1/200 to 1/5, preferably 1/100 to 1/10, of the inside diameter of the reaction tower.
The sizes of openings of the metal mesh and punching metal for housing a solid catalyst are such that solid catalyst particles do not pass through the openings and the fluid may sufficiently contact with the catalyst particles.
The amount of catalyst used in the present invention ranges from 1/100 to 1/1.5, preferably 1/50 to 1/2, of the internal volume of the cracking tower.
The solid catalyst is not particularly limited only if it is one having a hydrogenation function such for example as hydrocracking, hydrodemetallization, hydrodesulfurization or hydrodenitrification. But, from the viewpoint of long-term operation, the preferable catalyst is one which will not remarkably decrease in activity due to vanadium, nickel and the like contained in starting oils even if it has originally low activity.
For example, there can be used the same catalysts as employed in a heavy fraction oil treating process such as hydrocracking, hydrodesulfurization or hydrodenitrification for heavy fraction oils, or there can also be employed such catalysts already used.
In addition, it is possible to add a small quantity of a new catalyst to the above-described catalysts or to also use catalysts having relatively low activity instead of the above-described used catalysts. The solid catalysts include oxides or sulfides of a Group VIII metal such as nickel or cobalt or of a Group VI B metal such as molybdenum or tungsten, the metal oxides or sulfides being carried on an inorganic substance such as alumina, silica, silica-alumina, alumina-boria, silica-alumina-magnesia, silica-alumina-titania, or natural or synthetic zeolite.
Although the solid catalyst is not particularly limited in shape, for example an extrusion molded catalyst, a spherical catalyst or a compression molded catalyst may be used.
The diameter of the catalyst particle ranges from 0.01 to 10 mm, preferably 0.1 to 5 mm.
Operating conditions used in the present invention are as follows: reaction temperature, 380° to 470° C.; reaction pressure, 30 to 150 kg/cm 2 .G varying depending on the kind of hydrogen-containing gas; residence time of starting heavy fraction oil in the cracking tower, preferably 0.2 to 10 hours; circulating flow speed of the fluid in the cracking tower, at least 1 cm/sec., preferably 5 to 100 cm/sec.
According to the present invention, 30 wt. % or more of heavy metals such as vanadium and nickel, etc., contained in a starting heavy fraction oil can be adhered to the catalyst in the cracking tower.
The starting oils used in the present invention include heavy fraction oils containing at least 1.0 wt. %, preferably 5 to 30 wt. %, of asphalten (pentane-insoluble ingredients), preferably 5 to 30 wt. % and comprising at least 50 wt. % of a fraction boiling above 350° C.; atmospheric or reduced pressure distillation residual oils; and oils obtained from coal, oil sand, oil shale, bitumen and the like.
One of preferable hydrogen donor solvents used in the present invention is a hydride of a polycyclic aromatic hydrocarbon. The polycyclic aromatic hydrocarbons are illustrated by those having 2 to 6 rings, preferably 2 to 4 rings and the derivatives thereof. The polycyclic aromatic hydrocarbons can be used singly or in combination. There can be listed, as examples of the polycyclic aromatic hydrocarbons, naphthalene, anthracene, phenanthrene, pyrene, naphthacene, chrysene, benzopyrene, perylene, picene and the derivatives thereof.
In addition, the hydrogen donor solvents according to the present invention further include the hydrides of hydrocarbon oils containing at least 30 wt. % of polycyclic aromatic hydrocarbons and boiling in the range of 150° to 1500° C. As examples of the hydrocarbon oils, there can be listed various products obtained from petroleum such as a cycle oil from a cat cracker (FCC), a bottom oil from a catalytic reformer or a thermally cracked oil of naphtha, or various products such as tar oil, anthracene oil, creosote oil and coal liquefied oil, each being produced from coal.
The hydrogen-containing gases used in the present invention are preferably those containing at least 70 wt. % of hydrogen gas and include hydrogen-containing gases from a reformer.
Another method for cracking heavy fraction oils according to the present invention will be further detailed below with reference to FIGS. 5 and 6.
FIG. 5 is an example of a flow chart illustrating execution of the method according to the present invention.
In FIG. 5, numeral 1 is a cracking tower, 2 hydrogenation tower, 3 a separation device, 4 an introduction passage for a starting heavy fraction oil, 5 an introduction passage for hydrogen gas, 6 and 7 effluent passages for reaction product mixtures in the cracking and hydrogenation towers, respectively, 8 a recycling flow passage for a hydrogen donor solvent from the separation device 3 to the cracking tower, and 9 and 10 product effluent passages from the separation device.
The starting heavy fraction oil is passed, together with a recycled hydrogen donor solvent from the recycle flow passage 8, to the cracking tower 1 where the cracking is effected using the hydrogen donor W solvent. The reaction in the cracking tower is carried out at preferably 380°-470° C. The supply of hydrogen to the cracking tower is effected by the hydrogen donor solvent and, therefore, it is not necessarily required to supply hydrogen gas, particularly high pressure one, from other sources. However, in order to prevent coking and make conveniently the hydrogen pressure in the cracking tower equal to that in the hydrogenation tower which is required to be high, it is preferable to introduce hydrogen gas usually from the hydrogen gas introduction passage 5 to the cracking tower and effect the reaction under a hydrogen gas pressure of 30-150 kg/cm 2 .G.
In conventional cracking with use of a hydrogen donor solvent, it is a common practice to effect a reaction in a cracking tower in the blank state. Namely, a hydrogen donor solvent and starting oil each at a high temperature are introduced into a tower or a vessel in the blank state (without fillers and the like charged) where the cracking of the oil is effected in the presence of hydrogen liberated by the hydrogen donor solvent. In contrast, one of the characteristics of the method according to the present invention is that the solid catalyst, porous solid or both are placed in the cracking region employing the hydrogen donor solvent and then vanadium and nickel which are made apt to be removed due to cracking are allowed to adhere to the solid materials. Further, the method according to the present invention is characterized in that cracked products from the cracking tower and the hydrogen donor solvent liberating hydrogen in the cracking tower are both directly introduced into the hydrogenation tower. But, the catalyst and/or the porous material existing in the cracking tower is not introduced into the hydrogenation tower.
Namely, the whole contents (called a reaction product mixture) in the cracking tower after the reaction except the solid catalyst and porous solid are introduced into the hydrogenation tower.
As described above, in the present invention, unlike in conventional methods, the cracked products from the cracking tower are not separated by distillation and the used hydrogen donor solvent is not hydrogenated separately, but these cracked products and solvent are passed through the passage 6 from the cracking tower 1 to the hydrogenation tower 2 where the hydrogen donor solvent and the cracked products are hydrogenated in the presence of a hydrogenation catalyst. The hydrogenation in the hydrogenation tower is quite the same as that effected by the conventional fixed floor system. The hydrogenation tower effects hydrogenation at a reaction temperature of 300° to 450° C. and a hydrogen pressure of 30 to 150 kg/cm 2 .G in the downstream flow in the presence of a hydrogenation catalyst. Since the starting heavy fraction oil has been hydrocracked in the cracking tower, an operating condition may be mild in the hydrogenation tower. In addition, since the metals have been removed in the cracking tower, the catalystic activity will little decrease in the hydrogenation tower.
The hydrogen donative solvent is regenerated or hydrogenated due to hydrogenation in the hydrogenation tower to recover its hydrogen donative nature, while the cracked products are hydrogenated are refined to remove the impurities such as sulfur-containing and nitrogen-containing ingredients.
The reaction product mixture in the hydrogenation tower, i.e., the whole contents in this hydrogenation tower except the solid catalyst, is fed via the fluid passage 7 to the separation device 3 and then separated into desired respective fractions by a separation treatment such as distillation. The desired fractions are passed through the product effluent passage 9 to recover them as gas, a gasoline naphtha fraction, a kerosine fraction, a light oil fraction, a heavy oil fraction and the like; and the hydrogen donor solvent is recycled through the recycling passage 8 to the cracking tower. Then, make-up 11 is preferable to compensate for a loss of the hydrogen donative solvent.
The hydrogen donative solvent described above is not required to be previously hydrogenated before being introduced into the apparatus. Namely, it is hydrogenated in the hydrogenation tower to provide a new hydrogen donative solvent.
The solid catalyst and/or porous solid used in the cracking tower of the present invention is intended not only to crack heavy fraction oils, but also to collect metals, which are made apt to be removed due to cracking, by allowing them to adhere to the solid materials. In addition, it is preferable that the solid catalyst and the porous solid have high capability of attaching such metals thereto.
As the porous materials, there can be listed alumina, silica-alumina, ceramics, carbonaceous materials, clay and the like, which are inexpensive.
There is set no particular limitation on a catalyst used for in the hydrogenation tower of the present invention. Namely, catalysts generally used in hydrogenation treatment can be used for respective desired purposes. What types of catalysts may be used is dependent on the composition and properties of a starting oil to be used and desired products to be obtained.
Such reactions as effected in the first and hydrogenation towers in the present invention, although they may be executed in two separate towers, they may also be effected in one tower by dividing it into two areas for reaction, one area being for the first step reaction (cracking) and the other for the second step reaction (hydrogenation).
The above and other objects, features and advantages of the present invention will become more apparent from the following description when taken in conjunction with the accompanying drawings in which a preferred embodiment of the present invention is shown by way of illustrative examples.
BREIF DESCRIPTION OF THE DRAWINGS
FIGS. 1 to 3 are schematic views illustrating respectively cracking towers aocording to the present invention, in which (a) is a longitudinal section of the cracking tower and (b) is a cross-sectional view of the same;
FIGS. 4(a) and (b) are perspective views of a partition provided in the cracking tower, (a) cylindrical one and (b) plate-shaped one;
FIG. 5 is a block diagram illustrating a method for hydrocracking heavy fraction oils according to the present invention; and
FIG. 6 is a graph illustrating variation in degree of cracking with the lapse of time in Example 2 and Comparative Example 2.
DESCRIPTION OF THE PREFERRED EMBODIMENT
EXAMPLE 1
The first hydrocracking method for heavy fraction oils according to the present invention will be described below experimentally for Arabian reduced pressure residual oil with reference to the cracking tower in FIG. 1. There are shown the properties of starting oils in Table 1, the operating conditions in Table 2, and the dimensions of the cracking towers in Table 3. A cylindrical partition is provided by housing an 1/32 inch extrusion molded catalyst composed of cobalt (3.6 wt. %) and molybdenum (10.7 wt. %) carried on a silica-alumina carrier (pore volume 0.55 cc/g), surface area (93 m 2 /g), average pore radius 62 Å) in a cylindrical metal mesh. The starting oil listed in Table 1 and a hydrogen donor solvent (tetralin) are introduced in a weight ratio of 1:1 into a cracking tower at the lower part thereof, while hydrogen gas is introduced into the cracking tower at the lower part. They are permitted to ascend only in the cylindrical partition along it. The resulting reaction products are recovered, and the tetralin is separated, and thereafter the properties of the products are measured. Although the operation of the apparatus is successively executed for 1300 hours, there is found no increase of pressure loss. The properties of the resultant products are listed in Table 1, and the mass balance and consumption of hydrogen in Table 4.
COMPARATIVE EXAMPLE 1
The cylindrical partition was removed from the apparatus shown in the Example 1, and the same starting oil was treated under the same conditions. The operation was interrupted after 420 hours because of a great increase in pressure loss. The properties of a product obtained during the operating time were shown in Table 1, and the mass balance and consumption of hydrogen shown in Table 4.
TABLE 1______________________________________ STARTING HEAVY COMPARA- FRACTION TIVEITEM OIL EXAMPLE 1 EXAMPLE 1______________________________________Specific 1.030 0.932 0.940Gravity (d.sub.4.sup.15)Viscosity (cSt) 142.9 29.52 34.71 (at 160° C.) (at 50° C.) (at 50° C.)Carbon 22.31 8.78 10.62Residue (wt %)Softening 43.5 -- --Point (°C.)Asphaltene 13.1 2.7 10.3(Pentane-Insolubles) (wt %)Elementary Analysis (wt %)S 4.80 0.70 0.81N 0.4 0.15 0.2C 84.3 86.8 87.4H 10.2 11.9 11.6H/C 1.45 1.65 1.58(Atomic Ratio)Metal (ppm)V 140 13 114Ni 47 8 41Cracking Rate -- 83.5 79.6(wt %)Demetallization -- 88.8 17.1(wt %)______________________________________
TABLE 2______________________________________ COMPARATIVEITEM EXAMPLE 1 EXAMPLE 1______________________________________Reaction Temperature (°C.) 450 450Reaction Pressure 70 70(kg/cm.sup.2 · g)Residence Time (hr) 1.0 1.0Solvent tetralin tetralinSolvent Ratio 1.0 1.0(wt ratio)Tetralin/Starting HeavyFraction OilHydrogen Supply 1200 1200(Nm.sup.3 /Kl)Starting HeavyFraction OilPressure Loss (kg/cm.sup.2 · g)after Operation Initiation100 hrs 0.85 0.85200 hrs 0.90 1.13400 hrs 0.90 2.54Flow Velocity of 20 --circulation fluid (cm/sec)______________________________________
TABLE 3______________________________________ COMPARATIVEITEM EXAMPLE 1 EXAMPLE 1______________________________________Di 50 50do 36 --di 22 --l 20 --H 3000 3000h 2000 2000______________________________________ (unit: mm)
TABLE 4______________________________________ COMPARATIVEITEM EXAMPLE 1 EXAMPLE 1______________________________________H.sub.2 S 3.51 3.23NH.sub.3 0.07 0.07C.sub.1 -C.sub.3 5.03 4.59Below 343° C. 31.21 27.83343/565° C. 45.68 43.37Above 565° C. 16.50 22.70Total 102.0 101.80Chemical Consumption 262 237of Hydrogen (Nm.sup.3 Kl)______________________________________ (unit: wt % to starting heavy fraction oil)
The following results were obtained from Tables 1 to 4.
(1) A long-term operation is possible for the hydrocracking method according to the present invention:
In Comparative Example 1, the pressure loss in the system was gradually increased and, therefore, the operation had to be suspended 420 hours later. This was because carbonaceous materials were produced by the cracking reaction and accumulated in the cracking tower as well as in pipings located downstream of the cracking tower to prevent fluids and gases from flowing therethrough, finally blocking or clogging the tower and pipings. In contrast, in Example 1, the production of carbonaceous materials were reduced because of larger effect of the catalyst and higher flow speed of the fluid in the cracking tower, thus enabling long-term operation to be effected.
(2) The rate of cracking was higher in the method according to the present invention:
A cracking method with use of a hydrogen donor solvent generally exhibits a high cracking rate as compared with other methods. Further, the additional use of a suitable catalyst in the cracking method enables hydrogen in vapor phase to be effectively utilized. Accordingly, higher cracking rates (refer to Table 1) are obtained even under the same conditions. Namely, hydrocracking can be promoted (Table 4), while operating conditions may be made milder when the same cracking rate is desired to be obtained.
(3) Products having excellent properties can be obtained:
As shown in Table 1, in Example 1, hydrocracking can be much promoted as compared with Comparative Example 1, and the content of asphaltene above 565° C. (pentene-insolubles) is conspicuously reduced. A higher H/C ratio (atomic ratio) was found. This shows that transfer of the hydrogen to the oil is frequently effected, thereby promoting hydrogenation of products and enabling more satisfactory products to be produced.
(4) Demetallization is effected:
When a heavy fraction oil is cracked with use of a hydrogen donor solvent, metals such as vanadium and nickel, contained in the heavy fraction oil are become facilitated to be removed. At this time, demetallization may be effected owing to the presence of a catalyst. Almost all the metals remain in the products in Comparative Example 1, whereas about 90% of the metals is removed and adhered to the catalyst present there in Example 1 as is apparent from Table 1. This is very advantageous in view of the succeeding process. Namely, since these metals cause catalytic activity to be reduced, previous removal thereof benefits the successive processes in view of catalytic activity. In addition, it is preferable that the catalyst used in the cracking tower have high capability of adhering metals thereto.
EXAMPLE 2
Khafuji reduced pressure residual oil was experimentally cracked by the method of the present invention. In the cracking tower, a direct desulfurization catalyst for atmospheric pressure residual oil which had been industrially already employed for about 8,000 hours was used as a downstream fixed bed. In the hydrogenation tower, there was used an 1/16 inch extrusion molded catalyst composed of cobalt (3.5 wt. %) and molybdenum (12.0 wt. %) carried on a silica-alumina carrier (pore volume 0.6 cc/g, surface area 190 m 2 /g, average pore radius 65 Å). As a reaction apparatus, there were used the cracking and hydrogenation towers which were each 40 mm in inside diameter and 1,300 mm in length. Each tower was filled with said catalyst so as to provide 1,000 mm of filling length. The starting oils and hydrogen gas as indicated in Table 5 were heated with a heater, and fed to the cracking tower in a downstream flow. As the hydrogen donor solvent, the bottom oil from a reforming device having the properties shown in Table 8 was employed, and make-up was used in amounts of 20 wt. % of the starting oil. The gas and liquid effluent from the hydrogenation tower were passed to a vapor-liquid separator where they were separated from each other, and thereafter the liquid was passed to a rectifying tower to recover fractions boiling in the range of from 25° to 350° C. for recycled use as a hydrogen donative solvent. The amount of solvent recycled was 1.5 times as large as that of the oil. The hydrogen gas was, after separated through the vapor-liquid separator, partly recycled and the remainder was mixed with make-up hydrogen and thereafter fed, together with the starting oil and the circulating solvent, through a heater into the cracking tower. The operation was conducted for 2,500 hours in succession.
The properties of the treated starting oil and those of the products were shown in Table 5. The operating conditions were shown in Table 6. The mass balance in the present experiment was shown in Table 7. Variation in cracking rates with the lapse of time was shown in FIG. 6. The rate of cracking was defined as follows:
(a-b/a)
a: proportion (wt. %) of fraction boiling above 565° C. in the starting oil
b: proportion (wt. %) of fraction boiling above 565° C. in the product
In addition, in order to estimate a rate of demetallization in the cracking tower, a liquid sample was collected and amounts of metals were measured. The result was listed in Table 9.
COMPARATIVE EXAMPLE 2
The same starting oil, apparatus, and catalyst as used in Example 2 were employed in this comparison test to conduct a hydrogenation experiment by making use of a prior fixed bed reaction device. But, the same cracking and hydrogenation towers were each charged with the same catalyst as charged in the hydrogenation tower in Example 2. There were not conducted addition of any hydrogen donor solvent to the reaction system and recycling thereof. Namely, a prior hydrocracking method using hydrogen and a proper catalyst was employed. The operation was continuously conducted for 2,500 hours, and the results were compared with those obtained in Example 2. The operating time was listed in Table 6 as well as the product properties and mass balance in Tables 5 and 7. The cracking rates varying with the lapse of time were shown in FIG. 6.
In addition, the starting oil and hydrogen gas were charged downstream as in Example 2.
Further, the cracking rate and demetallization rate at the outlet of the cracking tower were shown in Table 9.
TABLE 5______________________________________Properties of fractions above 350° C.in starting heavy fraction oils and products STARTING HEAVY COMPARA- FRACTION TIVE OIL EXAMPLE 2 EXAMPLE 2______________________________________Specific 1,028 0.920 0.931Gravity (d.sub.4.sup.15)Viscosity 2,030 14.15 35.20(cSt at 100° C.)Carbon Residue 21.9 3.51 6.11(wt %)Fluid Point (°C.) +45 -- --Pentane-Insolubles 9.9 2.3 7.8(wt %)Elementary Analysis (wt %)S 5.30 1.19 0.91N 0.40 0.22 0.17C 84.3 88.3 88.0H 10.5 9.5 10.2Metal (ppm)V 131 20 49Ni 39 11 25Compositionanalysis offractionsbelow 250° C.Saturated -- 80.5 83.1fractionsOlefin fraction -- 0.2 0.1Aromatic fraction -- 19.3 16.8______________________________________
TABLE 6______________________________________Operating Conditions COMPARATIVE EXAMPLE 2 EXAMPLE 2______________________________________Reaction Temperature (°C.)Cracking tower 440 400Hydrogenation tower 340 400Reaction Pressure 60 167(kg/cm.sup.2 g)LHSV (Charged starting 0.3 0.2amount/amount ofcatalysis) (hr.sup.-1)Hydrogen Supply 500 1,000Nm.sup.3 /m.sup.3 starting heavyfraction oil)Hydrogenative Solvent Bottom oil in none a reforming tower (See Table 9)Circulation fluid 1.5 noneamount(m.sup.3 /m.sup.3 starting heavyfraction oil)______________________________________
TABLE 7______________________________________Mass Balance and Consumption of Hydrogen COMPARATIVE EXAMPLE 2 EXAMPLE 2______________________________________ wt %/starting wt %/starting oil oilH.sub.2 S 4.3 4.5NH.sub.3 0.2 0.3C.sub.1 -C.sub.4 4.9 7.1343° C..sup.- 38.1 26.1343° C./565° C. 38.4 29.8565° C..sup.+ 16.1 37.0Total 102.0 104.8Chemical Consumption 121 150of Hydrogen(m.sup.3 /Kl-starting oil)______________________________________
TABLE 8______________________________________ Properties of Solvent______________________________________Specific Gravity (d.sub.4.sup.15) 1,010Refractive Index (-) 1,603Bromination Value (-) 3.0Viscosity at 37.8° C. 3.15(cSt) at 98.9° 1.14Structural Analysis% CA (Aromatic compound) 73.5% CN (Naphthene compound) 13.6% Cp (Paraffin compound) 12.7Fractionation Properties (°C.)IBP 235 5 24610 25120 25630 26140 26750 27460 28270 29180 30690 337EP 378______________________________________
TABLE 9______________________________________Cracking Rate and Demetallization Ratein Cracking Tower COMPARATIVE EXAMPLE 2 EXAMPLE 2______________________________________Cracking Rate (%)Outlet of cracking 76 32towerOutlet of hydrogena- 81 51tion towerDemetallizationrateMetal Amount inStarting OilV (ppm) 131 131Ni (ppm) 39 39Outlet of crackingtowerMetal (ppm) andDemetallizationrate (%)V (ppm) 22 (83.2%) 65 (50.4%)Ni (ppm) 12 (69.2%) 30 (23.1%)______________________________________ (driving hrs. 2,000 hr)
Advantages of the method for cracking heavy fraction oils with use of a hydrogen donor solvent according to the present invention are as follows:
(1) The cracking is effective:
Cracking can be effectively conducted in the presence of any suitable catalyst. Namely, compared with the absence of any catalyst (only a starting oil, hydrogen donative solvent and hydrogen gas are present), the presence of such a catalyst can improve a cracking rate under the same conditions except the catalyst, permitting high quality products to be yeilded.
(2) Inhibition of production of carbonaceous materials:
Production of carbonaceous materials causes some problems as to the cracking of heavy fraction oils with use of a hydrogen donor solvent. The presence of even slight catalytic action greatly suppresses the production of carbonaceous materials. Thus, blocking due to carbonaceous materials produced is conspicuously reduced.
(3) Increase of pressure loss in the cracking tower can be eliminated:
When cracking of a heavy fraction oil is intended using a hydrogen donor solvent, they are required to reside in the cracking tower for a certain time (generally over 30 minutes). Accordingly, a fluid velocity in the cracking tower is not high in general methods, resulting in the production of carbonaceous materials which will cause blocking. In the method according to the present invention, there is formed a natural circulating flow in the cracking tower, so that a fluid velocity is made high to eliminate the problem described above. In addition, in the method of the present invention, a main stream of fluid does not pass through the catalyst layer. Consequently, there is no direct relationship between the increase of pressure loss in the catalyst layer and flows of the starting oil and hydrogen donor solvent. Thus, the cracking of the heavy fraction oil in the reaction tower will not be hindered due to an increase in pressure loss in the catalyst layer.
(4) Demetallization is effected simultaneously with cracking of a heavy fraction oil:
The present inventor has found experimentally as described before that upon cracking a heavy fraction oil using a hydrogen donor solvent, metals, such as vanadium and nickel, contained in the heavy fraction oil are facilitated to be removed. There exists a suitable catalyst in the cracking tower in the present method. Accordingly, metals facilitated to be removed due to cracking of the heavy fraction oil can be eliminated by the catalyst, thereby to achieve demetallization. Namely, a cracked product obtained by the method of the present invention has a low metal content, this being very advantageous for the succeeding processes.
(5) The cracking tower can be simplified in structure:
Cracking of a heavy fraction oil using a hydrogen donor solvent is conducted under a pressure of hydrogen. Accordingly, the cracking tower is at high pressure. It may also be possible to execute cracking in the presence of a catalyst fluidized in order to avoid an increase of pressure loss in the cracking tower. There are raised, however, various problems because the apparatus is complicated and is a high-pressure apparatus. The method of the present invention can be executed without applying any processing to the high-pressure apparatus and only with insertion of a molded solid catalyst into the cracking tower. Consequently, the apparatus can be much simplified in structure and also economized.
Likewise, advantages of the second method for cracking a heavy fraction oil according to the present invention by making use of a solid catalyst and porous solid are as follows:
(1) Reduction of catalytic activity in the method according to the present invention is slight:
As shown in FIG. 6, there is found slight reduction of cracking rate in Example 2, but found remarkable reduction in Comparative Example 2. It is clear that this will be caused by activity reduction of a catalyst. The cracking tower in Example 2 forms a cracking region using a hydrogen donative solvent, in which region the cracking can be promoted without any catalyst with the result that a cracking rate of 76% is reached and removal of 80% of metals is achieved. Accordingly, there is very little adhesion of the metals, such as vanadium and nickel to the catalyst in the hydrogenation tower, resulting in very slight activity reduction of the catalyst. In addition, the temperature in the hydrogenation tower is 340° C. in Example 2 and low as compared with 400° C. in Comparative Example 2. Consequently, the reduction of activity due to carbonaceous materials produced from asphaltene is also low. For these reasons, there is little reduction of cracking rate with the lapse of operation time in Example 2; but the reduction in Comparative Example 2 is remarkable.
(2) The cracking rate obtained by the present method is high:
The present method allows a large supply of oils as compared with Comparative Example 2 (in Table 6, LHSV=0, but 0.2 in Comparative Example 2) and, nevertheless, exhibits a high cracking rate (Table 9 and FIG. 6). This indicates that the cracking in the cracking tower is remarkable and the effect of a hydrogen donative solvent on the cracking is large.
(3) The present method can be executed at a low reaction pressure:
As shown in Table 6, the reaction pressure is 60 kg/cm 2 .G in Example 2 (167 kg/cm 2 .G in Comparative Example 2). Since, basically, transfer of hydrogen can be performed in liquid phase when a hydrogen donative solvent is used, the cracking can be sufficiently effected at such a low pressure as to keep the hydrogen donor solvent in the liquid phase without requiring such a high pressure as to use hydrogen in vapor phase. In addition, since, in the hydrogenation tower according to the present method, an oil already cracked is, as shown in Table 9, subjected to hydrogenation treatment and a used hydrogen donor solvent is hydrogenated, no high pressure is required and thus a pressure as used in Example 2 is sufficient for the present purposes.
(4) The consumption of hydrogen is lessened:
As shown in Table 7, the consumption of hydrogen is lessened in spite of achieving a high cracking rate. The reasons for this are as follows: In the first step reaction tower, hydrogen is transferred in liquid phase whereby the cracking can be effectively effected and there is a lessened consumption of hydrogen regardless of the high cracking rate. In addition, in the hydrogenation tower, hydrogenation of the already cracked oil is effected whereby the cracking reaction is conducted at a relatively low temperature with the attendant reduced consumption of hydrogen, and further hydrogenation of the used hydrogen donative solvent can be conducted with high efficiency, resulting in economizing hydrogen. Thus, it is possible to crack heavy fraction oils effectively even if the total consumption of hydrogen in the cracking and hydrogenation towers is reduced.
Although certain embodiments have been shown and described, it should be understood that many changes and modifications may be made therein without departing from the scope of the appended claims.
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A method for cracking a heavy fraction oil is provided in which is solved a problem as to an increase in pressure loss due to coking in a cracking tower during the treatment of heavy fraction oils containing at least 1.0 wt. % of asphaltene. The cracking tower is vertically divided into at least two portions with a partition for housing a solid catalyst having a hydrogenation function, and the divided portions are communicated with each other at the upper and lower parts of the tower. A starting heavy fraction oil, a hydrogen donative solvent, and a hydrogen-containing gas are introduced into at least one of the divided portions at the lower part thereof, and further the fluid is circulated between the divided portions. Another method for cracking heavy fraction oils is provided in which a heavy hydrocarbon oil containing at least 1.0 wt. % of asphaltene is hydrogenated, a starting heavy fraction oil is cracked in the presence of at least one kind of a solid material selected from solid catalysts and porous solids and of a hydrogen donor, and at least 50 wt. % of heavy metals contained in the starting heavy fraction oil is ahdered to the solid material, and a reaction product mixture from the first step is separated from the solid material and then hydrogenated in the presence of hydrogen gas and a hydrogenating catalyst.
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RELATED APPLICATIONS
[0001] This application is a continuation in part of co-pending U.S. application Ser. No. 14/827,445 entitled “Umbilical Cord Transplant Product” filed on Aug. 17, 2015.
TECHNICAL FIELD
[0002] This invention relates to a transplant product derived from human umbilical cord and shaped for use as a soft tissue barrier or wound covering or other internal or external healing attachment and the products method of manufacture.
BACKGROUND OF THE INVENTION
[0003] The use of placental tissue to harvest thin membranes of amnion or chorion is well known. The use of umbilical cords to harvest stem cells is also well documented. However, the use of the umbilical cord tissue as a source for wound covering has been avoided because of the very thick nature of the tubular umbilical cord tissue and the fact that it is such a thick material it is not considered readily absorbable during a normal soft tissue healing. All of these adverse preconceived notions in the medical community may be unwarranted, if not wrong, in many applications wherein the healing time is long or the thickness of the material can be an advantage. The inventors of the present invention have discovered a remarkable way to process the harvested umbilical cord that not only benefits from the otherwise perceived drawbacks, but in fact provides embodiments with heretofore unachievable attachment features that make suture tissue tears issue completely disappear while at the same time making the material easier to pass sutures compared to using thin amniotic membranes. All of this is accomplished without requiring an additional structural layers to prevent tissue suture tearouts.
SUMMARY OF THE INVENTION
[0004] A shaped transplant product derived from human umbilical cord has a collagenous tissue membrane derived from an umbilical cord made essentially of thick collagenous tissue which is shaped to form a soft tissue barrier or wound covering or other internal or external wound healing attachment. The shaped transplant product has a defined memory shape that can be configured to pass through a hollow cylindrical trocar or arthroscopy device for implantation. The defined memory shape can be a hollow elongated split tube. The split tube along the split can have abutting edges. The split tube can have an open split forming a gap between edges adjacent the open slit. The split tube can have overlapping edges. The split tube can have an elongated body having a center portion tapering toward opposing smaller ends to form a pre-set shape. The shaped transplant can have a shape imparted by a mandrel or core during manufacture, the mandrel or core, when removed, leaving the shaped transplant product with a pre-set shape.
[0005] The structural, chemical and biochemical properties are retained, the collagenous tissue membrane is cleaned removing the veins, arteries and Wharton's jelly without exposure to harsh chemicals. The collagenous tissue membrane is soaked in normal saline solution under mild agitation for a predetermined time to structurally increase tear resistance of the membrane. The collagenous tissue membrane is free of meconium. The collagenous tissue membrane has a general transparent or translucent appearance of a clear or slightly pink color.
[0006] The collagenous tissue membrane is subjected to a vacuum drying process under vacuum at a prescribed vacuum over a predetermined time at room temperature sufficient to dry without altering the structural and chemical properties of the tissue, preferably being placed in a freeze dryer which is set to run for 19 hours at 1100 mT and 25 degrees C. The collagenous tissue membrane, after drying, has a thickness between 100 microns to 1000 microns, typically averaging a thickness between 250 and 800 microns. The collagenous tissue membrane is cut into round, oval, square or rectangular shapes. After drying, the cut collagenous tissue membrane has at least one suture entry site formed integrally as a structurally enhanced peripheral wall that acts and performs like a grommet but without any additional parts. The suture entry site is formed by a heated tip that forms a toughened tissue membrane wall encircling each of the at least one sites. The suture entry site is heat formed having a reduced thickness puncture center or an opening either of which are surrounded by the toughened tissue membrane wall. The toughened tissue membrane wall is rigid, wherein the grommet-like feature is thickened relative to exterior surfaces of the adjacent collagenous tissue membrane. The cut collagenous tissue membrane can have two or more suture entry sites. The cut collagenous tissue membrane can be cut into a small size formed as a pledget for suturing through and attachment to a thin tissue.
[0007] In one embodiment, the cut collagenous tissue membrane has the at least one suture entry site positioned in a corner of the square or rectangular cut membrane. Each corner of the cut collagenous tissue membrane can be folded over to make a double thickness cut collagenous tissue membrane at the suture entry site. In another embodiment, the cut collagenous tissue membrane has two opposite edges, adjacent each edge is a plurality of suture entry sites. The number of the plurality of suture entry sites adjacent one edge is equal to the number of suture entry sites of the opposite edge. Preferably, the suture entry sites of one edge are offset relative to the suture entry sites of the opposite edge wherein the offset is arranged and positioned so the suture entry sites on one edge are interposed between the suture entry sites of the other edge when the cut collagenous tissue membrane is rolled or folded such that the two opposing edges are aligned. In this embodiment, the suture entry sites are configured to pass a suture helically wrapped to form a cylindrical cut collagenous tissue membrane for wrapping about a nerve, vein, artery or any other tubular or round tissue vessel.
DEFINITIONS
[0008] Meconium—is the earliest stool of a mammalian infant. Unlike later feces, meconium is composed of materials ingested during the time the infant spends in the uterus: intestinal epithelial cells, lanugo, mucus, amniotic fluid, bile, and water.
[0009] Pledget—compress or small flat mass usually of gauze or absorbent cotton that is laid over a wound or into a cavity to apply medication, exclude air, retain dressings, or absorb the matter discharged, as used herein, the pledget is made from the cut umbilical cord tissue.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The invention will be described by way of example and with reference to the accompanying drawings in which:
[0011] FIG. 1 is a photograph of a technician holding a cut lengthwise umbilical cord exposing the veins, arteries and Wharton's jelly.
[0012] FIG. 2 is a photograph of a technician holding a length of umbilical cord during recovery.
[0013] FIG. 3 is a photograph of the longitudinal dissection of the umbilical cord tissue.
[0014] FIG. 4 is a photograph showing the umbilical cord after cleaning and soaking in normal saline.
[0015] FIG. 5 is an example of the transplant product after cutting.
[0016] FIG. 6 is a microscoped photograph at × magnification showing the epithelial layer no longer intact.
[0017] FIG. 7 is a photograph of the transplant product showing a suture passing through a folded over end.
[0018] FIG. 8 is a schematic diagram of the cleaning steps.
[0019] FIG. 9 is a schematic diagram of the drying steps.
[0020] FIG. 10 is a schematic diagram of the cutting steps.
[0021] FIG. 11 is a schematic diagram of the packaging steps.
[0022] FIG. 12 is an embodiment of the transplant product derived from umbilical cord having folded over corners with suture entry sites.
[0023] FIG. 13 is an embodiment of the transplant product having suture entry sites in a single layer.
[0024] FIG. 14 is another embodiment having a plurality of suture entry sites adjacent along each side.
[0025] FIG. 15 is the embodiment shown in FIG. 14 rolled into a cylinder or tubular shape with a suture woven through the circumferentially offset suture entry sites.
[0026] FIG. 16 shows a plurality of mandrels or cores for imparting a pre-set shape to the collagenous tissue membrane of the present invention.
[0027] FIG. 17 is an exploded view of the membrane, an exemplary mandrel and a drying chamber for shaping the transplant product of the present invention.
[0028] FIG. 18A is a schematic view showing the core or mandrel assembly.
[0029] FIG. 18B is a schematic showing the membrane initially a flat rectangle later being shown shaped into a split tube.
[0030] FIG. 19 is an end view of a first shaped transplant product.
[0031] FIG. 20 is a perspective view of the embodiment of FIG. 19 .
[0032] FIG. 21 is an end view of a second embodiment shaped transplant product formed as a split tube with overlapping edges.
[0033] FIG. 22 is a partial perspective view of the embodiment of FIG. 21 .
[0034] FIG. 23 is a third embodiment of the shaped transplant product formed as a split tube have gapped edges.
[0035] FIG. 24 shows a fourth embodiment wherein the membrane when cut into elongated strips can be shaped into a spiral wrapped tube.
[0036] FIGS. 25-25C show the shaped transplant products corresponding to the mandrels shown in FIG. 16 .
DETAILED DESCRIPTION OF THE INVENTION
[0037] The present invention encompasses both the manufacturing of various embodiments of final transplant products 10 and the transplant products derived from human umbilical cords (UC) 2 . The final umbilical cord product 10 is categorized as a thick layer of a collagenous membrane 20 of dried umbilical cord 2 . The transplant product 10 is a semi-transparent collagenous membrane. All donated umbilical cords, preferably, are derived from cesarean section delivered placentas recovered from young, healthy consenting mothers according to established procedures from a recovering facility. Application of final processed transplant products is for homologous use as a soft tissue barrier or wound covering or for other internal wound healing applications. The tissue is for single patient use and is to only be handled by a licensed physician.
[0038] Processing of the transplant products, as shown in the photographs of FIGS. 1-7 , was conducted at approved biomedical facilities. During the processing of the final transplant product, the structural, chemical, and biochemical components of the tissue remained intact. The only solution the umbilical cord was exposed to during processing was a physiological grade normal saline solution (0.9% Sodium Chloride). This solution was used to aid in the cleaning of the tissue to remove all traces of blood and extraneous umbilical membrane tissue. The umbilical cord segments then underwent a gentle vacuum cycle shaping if desired to obtain a final product that was dried. The dried tissue 20 makes the final transplant product 10 by cutting and packaging in final packaging that is to be delivered to the end user. The final product can be to be stored at room temperature. The current shelf life of the final processed transplant product is expected to be 5 years based on the validation of the final packaging material used for storage.
[0039] As with all manufacturing processes, cleaning and further processing of the umbilical cord is performed using aseptic technique. Pre-cleaning microbiology cultures are taken of the umbilical cord prior to initiating the cleaning process. Once the cultures are taken, the umbilical cord is cut lengthwise and flattened exposing the inner lining. Removal of the vein, arteries and Wharton's Jelly are accomplished manually with the aid of forceps and/or razors. The umbilical cord is then exposed to a normal saline solution (0.9% Sodium Chloride) and soaked for 4-8 hours with slight agitation during this period. Acceptable cleaned umbilical cord segments of the collagenous tissue membrane 20 must be transparent in color, free of meconium, not fragile, and exhibit normal tissue integrity.
[0040] The cleaning process of the umbilical cord is performed inside an ISO Class 5, Class II biological safety cabinet (BSC) that is located inside an ISO Class 5 suite in a cleanroom. The process of cleaning the umbilical cord is performed as such to leave the structural and chemical properties of the membrane 20 intact.
[0041] Once the umbilical cord segments of the collagenous tissue membrane 20 are cleaned and meet the aforementioned acceptable criteria, they are then prepared to undergo the vacuum drying process. The cleaned umbilical cord membranes 20 are placed on a sterile plastic tray with the inner lining of the umbilical cord facing upwards and the epithelial side facing downward. A layer of medical grade foam is then gently placed on top surface or side 22 of the tissue membrane 20 and lightly pressed to ensure the membrane 20 has completely adhered to the foam. The foam is gently lifted off the plastic tray and turned over exposing the epithelial side 21 of the umbilical cord. Another layer of medical grade foam is placed over the umbilical cord membrane 20 sandwiching the tissue membrane 20 in place. The sandwiched tissues are placed into sterile drying trays with the epithelial layer side 21 facing upwards. The drying trays are then placed inside of a freeze dryer which is set to run for 19 hours at 1100 mT and 25° C. This cycle has shown to sufficiently dry the tissue without affecting the structural and chemical properties of the tissue.
[0042] The cutting of the tissue membrane 20 is performed once the vacuum drying process is complete. The dried tissue membrane 20 is removed from the freeze dryer and subsequently carefully removed from the medical grade foams. The dried umbilical cord segments are then placed on a sterile plastic cutting board. The collagenous tissue membrane 20 , after drying, has a thickness between 100 microns to 1000 microns, typically averaging a thickness between 250 and 800 microns. Table 1 below exhibits the final product sizes for flat membranes. Once the umbilical cord segments are cut into their designated sizes using a scalpel and ruler, an orientation notch is made for the end user to denote the sidedness of the allograft. Using a sterile 5 mm skin gauge, a notch can be placed in the upper left hand corner of the membrane denoting that the epithelial side is facing upward.
[0043] Final umbilical cord product 10 sizes are provided as an exemplary list: 1 cm×1 cm, 1 cm×2 cm, 2 cm×2 cm, 2 cm×3 cm, 3 cm×3 cm, 3 cm×4 cm, 3 cm×6 cm, 3 cm×8 cm.
[0044] Final processed umbilical cord membrane 20 tissues when cut form the transplant product 10 which are packaged in validated final packaging. The membrane 20 is aseptically double pouched; each pouch sealed using an impulse heat sealer. The outer packaging used is a chevron type pouch allowing the end user to easily present the sterile inner pouch containing the product to a sterile field. The packaged final product 10 is stored at room temperature until it is distributed to the end user.
[0045] In one embodiment, the collagenous tissue membrane 20 is subjected to a vacuum drying process under vacuum at a prescribed vacuum over a predetermined time at room temperature sufficient to dry without altering the structural and chemical properties of the tissue, preferably being placed in a freeze dryer which is set to run for 19 hours at 1100 mT and 25 degrees C. Due to the thickness of the collagenous tissue membrane 20 , which is typically much thicker than the thickness of tissue membranes derived from a placenta, make the umbilical cord derived membrane ideal for suturing. The collagenous tissue membrane 20 is cut into round, oval, square or rectangular shapes. After drying, the cut collagenous tissue membrane 20 can be made structurally enhanced for suturing by having at least one suture entry site 30 formed integrally as a structurally enhanced peripheral wall 32 that acts and performs like a grommet but without any additional parts. The suture entry site 30 is formed by a heated tip that forms a toughened tissue membrane wall 32 encircling each of the at least one sites 30 . The suture entry site 30 is heat formed having a reduced thickness puncture center or an opening 31 either of which are surrounded by the toughened tissue membrane wall 32 . The toughened tissue membrane wall 32 is rigid or generally tear resistant, wherein the grommet-like feature is thickened relative to exterior surfaces of the adjacent collagenous tissue membrane 20 . The cut collagenous tissue membrane 20 can have two or more suture entry sites 30 . The cut product 10 of collagenous tissue membrane 20 can be cut into a small size formed as a pledget for suturing through and attachment to a thin tissue.
[0046] In one embodiment illustrated in FIG. 13 , the cut collagenous tissue membrane 20 has the at least one suture entry site 30 positioned in a corner 12 of the square or rectangular cut membrane 20 . Each corner 12 of the cut collagenous tissue membrane 20 can be folded over to make a double thickness cut collagenous tissue membrane 20 at the suture entry site 30 wherein the top surface or side 22 is covered at the corners 12 by the epithelial side 21 , as shown in FIG. 12 . In another embodiment, the cut collagenous tissue membrane 20 has two opposite edges 26 , 27 , adjacent each edge 26 , 27 is a plurality of suture entry sites. The number of the plurality of suture entry sites adjacent one edge 26 either one less, equal to or one more than the number of suture entry sites 30 of the opposite edge 27 , as shown 8 and 9 suture entry sites 30 on the respective edges 26 , 27 in FIG. 14 . Preferably, the suture entry sites 30 of one edge 27 are offset relative to the suture entry sites 30 of the opposite edge 26 wherein the offset is arranged and positioned so the suture entry sites on one edge are interposed between the suture entry sites 30 of the other edge when the cut collagenous tissue membrane 20 is rolled or folded such that the two opposing edges 26 , 27 are aligned. In this embodiment, the suture entry sites 30 are configured to pass a suture 40 helically wrapped to form a cylindrical cut collagenous tissue membrane 20 for wrapping about a nerve, vein, artery or any other tubular or round tissue vessel.
[0047] With reference to FIGS. 16-24 , an important variation from the flat, round, rectangular or square transplant product 10 is described and shown hereinafter. The flat shaped product 10 , while ideal for wound bandaging and covering is not necessarily the best for wrapping blood vessels or peripheral nerves. As was mentioned in reference to FIG. 15 , the flat tissue product 10 could be sutured to form a tube.
[0048] In FIG. 16 , there are shown a variety of mandrels or cores that allow the collagenous tissue membrane to be pre-shaped during the manufacturing process.
[0049] As shown in FIGS. 19-24 , various split tube shapes can be made that have been dried to have the tubular shape formed during manufacturing. This shape has a memory so that when implanted, the split tube 10 S will revert back to the pre-set shape.
[0050] Preferably, this is achieved by wrapping the collagenous tissue membrane 10 prior to drying about a mandrel or core 100 A, 100 B, 100 C, 100 D or 100 E. As shown in FIG. 16 , the mandrel or core 100 A has a center portion diameter 101 that steps down at ends 102 . When the membrane is placed on this mandrel, that shape is imparted to it during drying, see FIG. 25A .
[0051] The mandrel or core 100 B is generally cylindrical, the mandrel or core 100 C has slightly tapered ends 102 and mandrel or core 100 D has a greater slope to create even smaller tapered ends 102 . This results in the shaped product 10 S as shown in FIGS. 25B, 25C and 25 respectively.
[0052] With reference to FIGS. 17, 18A and 18B , the inventors that in drying the grafts, and dehydrating the materials seeking a flat membrane for placement, real value is being missed for deployment via trocar and arthroscopic implementation. They realized that an umbilical sheet when wrapped on a mandrel, compressed with a clam shell sleeve, can be formed within a clam shell that can have a surface roughness that is either random or defined, and that the dried graft retains its shape following removal. This graft is intended to be formed by clamping a clam-shell like fixture for repeat use as a tool, with the option of being vacuum desiccated from the inside which provides conduit and varying thicknesses for delivery and remoistening.
[0053] As shown schematically in FIG. 18A , the mandrel 100 E, or any of the mandrels 100 A- 100 D as well, can be placed inside a sleeve 200 , the sleeve 200 can be a clam shell construct that is compressed against the mandrel 100 A- 100 E during drying. A vacuum can be pulled on the assembly, preferably through the mandrel to draw the membrane tightly on the mandrel to impart the desired shape.
[0054] The sleeve 100 can have heating rods 203 for drying, or the entire assembly placed in a heated drying oven, or simply room temperature dried. In any event, the goal is to make a pre-set shape, preferably of a split tube or a wrapped tube, to allow easing the covering on blood vessels or nerves. Once shaped, as shown in FIG. 18B , the transplant product 10 is transformed into a shaped transplant product 10 S.
[0055] With reference to FIGS. 19 and 20 , the split tube shaped transplant product 10 S can have abutting edges. Alternatively, as shown in FIGS. 21 and 22 , the membrane 20 can have overlapping edges 26 , 27 . The term “overlapping” implies the membrane, when placed on a mandrel 100 A- 100 E is wrapped greater than 360 degrees or greater than once. “Abutting” means the wrap is 360 degrees or close to it, and as shown in FIG. 23 , is wrapped less than once and a gap is formed as the edges 26 and 27 did not fully encircle the mandrel on shaping. Each style has distinct advantages depending on the procedure.
[0056] With reference back to FIG. 15 , the pre-set shaped product can be used without the suture holes, or when desired, can be provided with this feature as shown.
[0057] With reference to FIGS. 25A, 25B, 25C and 25 , the shaped products 10 S are shown corresponding to the mandrels 100 A- 100 D respectively.
[0058] 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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A shaped transplant product 10 derived from human umbilical cord 2 has a collagenous tissue membrane 20 derived from an umbilical cord 2 made essentially of thick collagenous tissue which is shaped to form a soft tissue barrier or wound covering or other internal or external wound healing attachment. The shaped transplant product 10 S has a defined memory shape that can be configured to pass through a hollow cylindrical trocar or arthroscopy device for implantation. The defined memory shape can be a hollow elongated split tube. The split tube along the split can have abutting edges. The split tube can have an open split forming a gap between edges adjacent the open slit. The split tube can have overlapping edges. The split tube can have an elongated body having a center portion tapering toward opposing smaller ends to form a pre-set shape.
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BACKGROUND OF THE INVENTION
[0001] The invention relates to wall construction and, in particular, to a system utilizing factory built panels and associated hardware for constructing curved walls.
PRIOR ART
[0002] Architects and/or building owners may specify curved interior walls to give rooms, partitions, corridors and the like a unique look, to create a focal point in the interior of the building, or otherwise depart from ordinary planar walls. Where the walls are to be finished with a hard finish other than plaster or drywall, it has often been the practice to construct a curved wall with custom millwork. This custom work, under most circumstances, is costly, because of the skilled labor and custom made panels or planks which, typically, are employed to create the curved surfaces. Consequently, architects and builders are restrained, due to the costs, from freely using their creativity in designing non-planar walls. Moreover, because each custom installation is just that, the final fit and finish of a custom built curved wall may be less than what is originally specified by the architect, thereby leading to further difficulties and controversies.
SUMMARY OF THE INVENTION
[0003] The present invention provides a system of pre-manufactured panels and integrated hardware that produces concave or convex walls with a consistent high-quality appearance. The system utilizes specially fabricated rectangular panels of a height and width suitable for the customer's application. The panels are uniquely cut with dado slots on their rear faces to obtain horizontal flexibility and vertical stiffness. The panels have two opposed edges, normally the horizontal edges, kerfed to accept a spline and wall attachment clip while the other edges, typically the vertical edges, are square cut. The outer decorative face of a panel can take a variety of forms such as wood veneer, high-pressure laminate, metal veneer, or other known finishes.
[0004] In accordance with the invention, the panels are interlocked to one another and retained against a subwall by special clips situated at the perimeter of each panel. Preferably, the spline used to join horizontal edges of adjacent panels is a flexible material such as extruded PVC so that it is readily manually bent on site into the radius of the wall. The vertical edges of adjacent panels are interconnected by joining them to vertical main rails with the use of panel clips secured to the rear faces of the panels. The main rails are attached to the sub-wall or framework and the panels, in turn, are fixed to the main rails by the panel clips. Advantageously, the slotted design of the panels as well as the character of the main rails, panel clips, retainer clips, and splines, enable the panel system to be used with any desired radius of curvature, both convex or concave above a certain minimum specified radius. Thus, the wall can have a changing radius and/or a serpentine configuration, as desired. As used herein, the term “cylindrical” is meant to describe a plane curved about one or more parallel axes.
[0005] The disclosed panel system affords the look of custom millwork with high quality fit and finish, but at substantially lower cost than custom millwork. Additionally, the system enables a wall to be installed with less time and less skill than required by custom millwork. The unique hardware assures consistent alignment between adjacent panels without exposed fasteners or clips to achieve a handsome, quality appearance.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] [0006]FIG. 1 is an exploded fragmentary perspective view of the curved wall panel assembly of the invention;
[0007] [0007]FIG. 2 is a fragmentary elevational view of the curved wall panel assembly of the invention;
[0008] [0008]FIG. 3 is a cross-sectional fragmentary view of the curved wall panel assembly taken in the plane 3 - 3 shown both in FIG. 1 and FIG. 2;
[0009] [0009]FIG. 4 is a fragmentary cross-sectional view of the curved wall assembly taken in the plane 4 - 4 shown in FIGS. 1 and 2; and
[0010] [0010]FIG. 5 is a schematic representation of a curved wall constructed in accordance with the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0011] Referring now to the drawings, a curved wall panel system 10 in accordance with the invention includes a plurality of rectangular panels 11 . In the following description, the panels and related hardware are indicated to have certain orientations which will produce a wall that is curved in a vertical column. The same parts can be turned 90° to produce a wall, arch, or ceiling that is curved in a horizontal column or turned in some other angle to produce a wall that is curved in an inclined column. Opposite vertical edges 12 of the panels 11 are joined or coupled to adjacent panel edges with main rails 13 and panel clips 14 . Opposite horizontal panel edges 16 have kerfs or slots 17 to receive a spline 18 and retainer clips 19 .
[0012] The panels 11 are ordinarily rectangular in shape, it being understood that this description includes the condition of being square. The panels 11 , for the most part, will have the same shape and size but this need not be the case. Typically, the size of the panels both vertically and horizontally can be selected to compliment the application. The long dimension of a panel 11 typically would run in the horizontal direction but, if desired, can be arranged to run in the vertical direction; that is to say, the long dimension of a panel can run in a direction parallel to the axis of the cylindrical plane of the wall, or can run circumferentially along the cylindrical surface of the wall. Preferably, the panel 11 is fabricated of ¾″ thick wood composite material forming a core 15 . An outer decorative panel face 21 can be laminated to this composite core 15 at the factory to satisfy a customer's specifications. The decorative panel face may comprise, for example, wood veneer, high pressure laminate, sheet metal or other known finish materials. The edges 12 , 16 can be stained, painted, laminated or the like with a color or finish to coordinate with the decorative outer face 21 . As shown, the vertical edges 12 are square cut. A rear face 22 of a panel 11 is machined with dado cuts in a direction parallel to the axis of the cylindrical section in which a panel is to be formed by bending or flexing action. The dado cuts or slots 22 are generally evenly spaced across the panel 11 and run the full distance between the kerfed edges 16 . As shown, the dado cuts 22 are in the shape of a dovetail such that the greatest width of a slot exists adjacent the finish face 21 . This configuration of the slots 22 achieves a high degree of flexibility in the horizontal direction while retaining stiffness in the perpendicular or vertical direction since the section modulus of the panel material between the slots is greater than that which would exist if the slots were rectangular in shape and had a width the same as the maximum width of the dado slot 22 . The dado cuts 22 are spaced a sufficient distance from the edges 12 to permit convenient, reliable attachment of the panel clips 14 .
[0013] The panel clips 14 are preferably roll-form galvanized 24 gauge steel strips that are somewhat shorter, e.g. 4″ shorter than the vertical height of a panel 11 and are attached to the panel such that they are centered in the vertical dimension. As indicated in FIG. 3, the cross-section of the panel clips takes a form similar to a narrow Z-shape. More particularly, the clip includes a base flange 30 , a short web 31 , a main flange 32 , and a minor flange 33 . The base flange 30 is provided with spaced holes to receive fastening screws 34 screwed into the panel core 15 to attach the base flange firmly on the panel 11 . In its free configuration, a panel clip 14 with its base flange 30 abutted to a rear face 24 of the panel core 15 , can have a bend line or corner 36 between the main and minor flanges 32 , 33 touching or nearly touching the core so that, as described later, it can firmly grip a part of a main rail 13 . As shown in FIG. 3, the web 31 holds the main flange 32 away from the core 15 to permit a part of a main rail 13 to be received between it and the adjacent area of the core or panel 11 . The panel clips 14 are assembled on the rear faces 24 of the core 15 in parallel alignment with the adjacent edges 12 .
[0014] A main rail 13 is disposed between vertical edges 12 of adjacent panels 11 . The main rails 13 are rigid elements preferably made of extruded aluminum. A cross-section of a main rail 13 is illustrated in FIG. 3. The main rail 13 includes a generally centralized rib 40 adapted to separate the vertical edges 12 of adjacent panels 11 and a pair of oppositely extending flanges 41 , 42 . A channel 43 , formed by a portion of the rib 40 , a web 44 and a flange 45 , exists between the rib and flange 42 . The channel or formation 43 receives hex head screws or like fasteners 46 and thereby ensures that there is no interference between such fasteners and the adjacent panel 11 . The channel 43 and, particularly the flange 45 and corresponding portion of the rib 40 allow the flanges 42 , 41 , respectively, to stand off a sub-wall structure or sub-framework indicated by the numeral 47 to which the main rail 13 is attached by the screws 46 . This standoff or spaced relation between the flanges 41 , 42 and subwall structure 47 allows the panel clips 14 to be received in the space between these flanges 41 , 42 and the sub-wall 47 . With reference to FIG. 3, it will be seen that the central rib 40 , having oppositely extending beads 48 or equivalent structure, is adapted to properly space and vertically align the panels 11 .
[0015] With reference to FIG. 4, a retainer clip 19 is shown in cross-section or profile. The retainer clip is conveniently made of extruded aluminum or other suitable material and is relatively short being, for example, about 2″ long. The profile of the retainer clip 19 is similar to a lower case “h”. A vertical part of the retainer clip section includes a web 50 having upper and lower horizontally extending flanges 51 , 52 . Near the mid-section of the web 50 , the clip 19 includes a wall 53 extending horizontally from the web 50 . Integral with a free edge of the wall 53 , is a depending flange 54 . An integral rectangular bar 55 exists at the intersection of a lower face of the wall 53 and the web 50 . Vertical edges 56 , 57 , of the flanges 51 , 52 and a vertical face 58 of the bar 55 , lie in a common vertical plane and are adapted to operate to standoff or hold the panels 11 a predetermined distance away from the sub-wall or sub-framework 47 , this distance being the same as the predetermined standoff distance developed by the flanges 41 , 42 of the main rails 13 . The depending flange 54 is spaced from the plane of the edges 56 , 57 , and surface 58 so that it fits in the kerf 17 on the upper horizontal edge 16 of a panel 11 and so that it captures a section 59 of the panel edge 16 formed when the kerf is cut into this edge, preferably with a snug or push fit. A channel-like area 61 formed between the flange 51 and wall 53 receives a hex head screw or like fastener to secure the retainer clip 19 and, therefore, the associated panels 11 to the sub-wall 47 . The retainer clips 19 are located at spaced intervals along the upper horizontal edges 16 of the panels at an appropriate spacing of, for example, 8″. The spline 18 , preferably, is extruded of flexible polyvinylchloride. Other bendable or pliable materials are contemplated, such as rubber or other elastomeric material, or malleable material such as soft extruded aluminum. The spline 18 is precut to a length that matches the horizontal dimension of the panels 11 . The spline 18 has the general shape of a “T”. An upper part 63 of the spline fits snugly in the kerf 17 of the lower horizontal edge 16 of the superjacent panel 11 while a lower part 64 of the spline has a reduced thickness to enable it to fit in a kerf 17 on the upper edge 16 of the subjacent panel 11 along with the retainer clip flange 54 . It will be understood that the width of the kerfs 17 on the upper and lower horizontal edges 16 is the same for the sake of simplicity in manufacture of the panels 11 . At the vertical mid-section of the spline cross-section, the spline 18 includes an integral bar-like formation 66 having upper and lower horizontal surfaces 67 , 68 . The lower horizontal surface 68 is adapted to bear against the upper horizontal edge 16 of the subjacent panel while the upper surface 67 is adapted to support the superjacent panel 11 by engagement with the lower horizontal surface of such panel. A decorative formation 69 can be integrated with the bar formation 66 of the splice to provide a finish for a vertical gap 71 between the upper and lower horizontal edges 16 of adjacent panels 11 . It will be understood that the splice 18 vertically and horizontally (in and out of the plane of the wall) aligns the panel edges 16 with which it is engaged.
[0016] From the foregoing description of the system 10 , its assembly is self-evident. ordinarily, panels 11 are stacked one over the other for the full height of a wall. Suitable base trim blocking, not shown, can be utilized to support the bottom row of panels or, the bottom row of panels can simply rest on the floor. A main rail is attached to the sub-wall 47 ; the main rail may be modified as needed, where a curved wall starts so that it can be concealed by suitable trim, if desired. With the first main rail 13 or its equivalent installed in a vertical orientation, the panel clip 14 of the first panel 11 is slid over the flange 42 of the main rail 13 . The upper edge of this panel is attached to the sub-wall 47 with retainer clips 19 by positioning their depending flanges 54 into the kerf 17 on the upper horizontal edge 16 of the panel. The retainer clips 19 can be positioned with regular spacing along this edge such as on 8″ centers. It will be understood that the retaining function of the clips 19 will cause the panel to assume a radius of curvature corresponding to that of the sub-wall 47 , either convex or concave by flexing or bending the panel. The spline 18 is likewise manually bent on site into the curvature of the panel and forced into the kerf 17 on the upper horizontal edge 16 , the thinner flange or lower part 64 being oriented downwardly. Thereafter, the next vertical panel 11 is installed by sliding its panel clip 14 over the flange 42 of the main rail and fitting its kerf 17 on its lower horizontal edge 16 over the upper part or flange 63 of the underlying spline 18 . Successive panels 11 are installed one over the other in the same manner as described above.
[0017] Next, another main rail 13 is installed by fitting its flange 41 into the space between the panel clips 14 and rear faces 24 of the first column of installed panels 11 . The main rail 13 is installed so that the channel 43 remains temporarily exposed to receive the mounting screws 46 . After this rail is secured by the screws 46 , another column of panels 11 is assembled on the sub-wall 47 and this process is repeated column by column until a wall is completed. The last column of panels 11 can be fitted with suitable trim as desired; similarly, top and bottom horizontal trim can be used at the floor and ceiling.
[0018] From the foregoing disclosure, it will be seen that a curved wall can be constructed with essentially any desired radius greater than a minimum of, for example, 7′. The wall installation requires relatively little labor and skill to afford a custom quality look. The connection between the panel clips 14 and main rails 13 is somewhat self-adjusting due to the ability of the panel clips 14 to flex slightly so as to allow the cantilevered bend line 36 to be displaced away from the rear face 24 of a panel and, thereby allow the vertical edge area of a panel to conform or be somewhat tangent to the curvature imposed on the panel 11 by the sub-wall 47 .
[0019] It should be evident that this disclosure is by way of example and that various changes may be made by adding, modifying or eliminating details without departing from the fair scope of the teaching contained in this disclosure. The invention is therefore not limited to particular details of this disclosure except to the extent that the following claims are necessarily so limited.
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The invention comprises a system for constructing a finished convex or concave curved wall of any desired radius beyond a specified minimum. The wall is constructed of pre-finished rectangular panels retained on a sub-wall structure in horizontal rows and vertical columns. The panels are retained on the sub-wall structure with vertical rails at their vertical edges and retainer clips spaced along their horizontal edges. The panels are slotted at their rear face to provide rigidity in the vertical direction and flexibility in the horizontal direction. The horizontal edges of the panels are kerfed to receive the retainer clips and flexible splice strips that conform to the curvature of the wall and align and space a panel with the panel immediately above it. Clips attaching vertical edges of the panels to the rails allow the associated areas of the panels to align tangentially with the curvature of the wall.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a process for working up hydrolysis residues obtained in the hydrolysis of solids-containing polysilane sludges from the synthesis of organochlorosilanes by the direct process. More particularly, the invention relates to the working up of hydrolysis reisdues from the synthesis of methylchlorosilanes.
2. Background Information
Organochlorosilanes and, in particular, methylchlorosilanes are used as starting materials for the production of silicones which are widely used, for example, as rubbers, jointing compounds, oils, structural sealants, etc. Dimethyldichlorosilane is required in particular for the production of methylchlorosilanes, being obtained in high yields when the direct reaction of silicon with methyl chloride is catalyzed by copper or copper compounds. The process is described in principle in U.S. Pat. No. 2,380,995. The industrial production of methylchlorosilanes by this process is carried out worldwide, the reaction normally being carried out in continuous fluidized-bed reactors.
Where the direct process is carried out in fluidized-bed reactors, the very fine fractions of silicon, catalyst and unreacted contact material are continuously discharged together with the reaction products, the crude silane mixture, and unreacted methyl chloride.
These dust-like fines are often collected together with the highest-boiling reaction products (Bp 760 >160° C.) in a so-called sludge vessel followed by a washing tower. The temperature of the vessle, which is under the usual excess pressure of 1.5-10 bar, is generally adjusted so that the mixture of solids and condensed fractions is kept sufficiently thinly liquid to facilitate discharge from the vessel.
According to DE-PS No. 2 362 494, the contents of the vessel may be expanded in a stirred container, preferably kept at normal pressure and the distillable components are removed from the mixture by heating. The contents of the vessel are then generally hydrolyzed.
The hydrolysis itself may be carried out in a downpipe, as described in DE-PS No. 2 362 494. The disadvantage is that, in view of the short contact times, hydrolysis is often incomplete and large quantities of water are consumed.
U.S. Pat. No. 4,221,691 describes a hydrolysis process in which the unpleasant property that the hydrolyzates have of sticking is prevented by the addition of mineral oil. However, since the hydrolyzates are regarded as worthless and are dumped, the additional organic pollution they cause is a disadvantage.
It is known from U.S. Pat. No. 4,408,030 that the problem of sticking can also be overcome by maintaining a minimum chlorine content, although technically this is difficult to do.
In all the processes mentioned above, a hydrochloric acid suspension is formed in which the more or less solid hydrolyzate is regarded as worthless and has to be dumped. However, the hydrolyzates are not without problems because they generally contain 2 to 10% predominantly metallic copper which can be partly eluted from the dumped hydrolyzate, thus endangering the ground water. In addition, most of the hydrolyzates obtained are vulnerable to oxidation and, in some cases, even show a tendency to ignite spontaneously so that they cannot be safely dumped.
Now, U.S. Pat. No. 4,758,352 describes a process in which the hydrolysis is carried out in water or a heavily diluted hydrochloric acid in a stirred container which is equipped with a high-speed disk stirrer, but not with baffles so that a vortex into which the material to be hydrolyzed is introduced can form. The preferred temperature is between 60° and 90° C. A suspension of finely divided solid hydrolyzates, in which more than 90% of the solid particles are smaller than 5 mm in diameter, is thus obtained.
The suspensions thus obtained are then oxidized with oxygen-containing gases which, according to the invention cited above, is preferably done with technically pure oxygen under a pressure above atmospheric pressure.
On completion of oxidation, solids and copper-containing liquid are separated from one another.
The process according to U.S. Pat. No. 4,758,352 gives a disposable, compact, non-gasing solid with no elutable heavy metals which is thermally inert in the context of the invention and may thus be safely dumped.
SUMMARY OF THE INVENTION
Now, the present invention relates to a process for working up high-boiling, solids-containing residues obtained in the synthesis of organoclorosilanes which are hydrolyzed and then oxidized, characterized in that a surface-active agent which hydrophilicizes the surface of the solids is added during hydrolysis and/or oxidation.
The addition of a surface-active agent in accordance with the invention is not confined to the combination of hydrolysis and oxidation and may also be applied where hydrolysis is carried out without subsequent oxidation. In general, the better wetting reduces the tendency of the hydrolyzate to stick, thus reducing contamination of the product-carrying parts of the plant.
Hydrolysis preferably comprises adding the surface-active agent to the water or the heavily diluted hydrochloric acid, which is fed to the stirred container comprising a high-speed disk stirrer for hydrolyzing the high-boiling solids-containing residue from the synthesis of organochlorosilanes, and thus hydrophilicizing the surface.
Oxidation preferably comprises adding the surface-active agent hydrophilicizing the surface to the suspension to be oxidized during filling of the oxidation reactor. It is also possible to add part of the surface-active agent during hydrolysis and another part during oxidation.
The surprising advantage of the working-up process according to the invention is that it provides for better wetting of the high-boiling, solids-containing residue to be hydrolyzed and hence for more effective hydrolysis and that oxidation, which according to the invention is preferably carried out by exposing the suspension obtained during hydrolysis to technically pure oxygen under a pressure above atmospheric pressure at temperatures of 80°±10° C., is not accompanied by any flotation and foaming effects, which could adversely affect the conduct of the reaction.
The type of substances which influence the surface can be very different. They are generally recruited from the class of surfactants and are therefore mainly organic in character. In the present cases, alkyl and alkylbenzene sulfonates have proved to be particularly suitable, although the invention is not confined to the use of surface-active agents from this group. On the contrary, it is possible to use any surface-active agents, which effectively wet the hydrolyzate and which are sufficiently stable in the hydrochloric acid medium, or mixtures thereof.
Alkyl sulfonates which may be successfully used are known, for example, under the trade names of "Mersolat H" and "Mersolat W" (Bayer AG). Alkylbenzene sulfonates, which are equally effective, are known, for example, under the trade name of "Marlon A 357" (Chemische Werke Huls).
Mixtures are also understood to include formulations of the type used, for example, as foam inhibitors for surfactant-containing solutions. The foam inhibitor DNE (Bayer AG), a mixture of fatty acid esters and higher hydrocarbons with carboxylic acid salts, may be successfully used in accordance with the invention. In this case, the surface-active agents are not from the class of alkyl and alkylbenzene sulfonates.
The expert knows that a number of compounds and formulations of different compounds may be used and that success generally requires close adaptation to the particular medium to be wetted. It is important that the surface is rendered hydrophilic and that the addition does not itself lead to problems such as foaming for example.
The quantity of surface-active agent required depends on the quantity of solids present in the suspension and their fineness.
In most cases, suspensions of 20 to 30% by weight solid hydrolyzate, determined as moist filter cake, are required for hydrolysis. Experience has shown that between 100 and 10,000 ppm, expressed as parts by weight of the active substance based on the suspension as a whole, have to be used for suspensions such as these. Additions of 200 to 5000 ppm active substance, based on the suspension as a whole, are preferred.
BRIEF DESCRIPTION OF THE DRAWING
The preferred embodiment of the process according to the invention is described in detail in the following with reference to the accompanying drawing and the Examples which are purely illustrative and are not intended to limit the invention in any way. FIG. 1 schematically depicts the invention process.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows the standard procedure. Gaseous reaction products, unreacted methyl chloride and fines enter the slude vessel 12 from the "direct synthesis reactors" 10. The non-volatile constituents are collected in the sludge vessel 12. The volatile constituents leave the vessel 12 for the product distillation stage 14. By means of a cycle valve, the non-volatile contents are expanded and introduced into a concentrator 16 to recover compounds which are volatile at atmospheric pressure.
Hydrolysis is carried out with water or dilute HCl in a stirrer-equipped reaction vessel 19.
Now, surface-active substances may be added in accordance with the invention to the water required for hydrolysis through the water inlet or, if desired, not until the next step, i.e., during filling of the oxidation reactor 20, in which the liquid is exposed to the gas containing the elemental oxygen; partial quantities may optionally be added at both places. After oxidation, the solid is separated from the aqueous liquid in a suitable filtration unit 22, the aqueous liquid is fed to a suitable wastewater treatment plant 24 and the solid is washed and then dumped. The washing water may optionally be reused for hydrolysis.
The invention will now be described with reference to the following non-limiting examples.
EXAMPLE 1
Example 1 demonstrates the effect which the addition of detergent constituents from the group of alkyl and alkylbenzene sulfonates has on the foaming of a hydrolyzed suspension gassed with air.
3 kg of a hydrolysis suspension containing 20% by weight moist solids, which had come from industrial direct synthesis, were gassed in a gassing apparatus with three baffles and a gassing stirrer (gassing stirrer diameter 4.6 cm, stirring speed 1585±30 r.p.m., vessel diameter=15 cm, vessel height=60 cm, filling level approx. 17.5 cm). In another test under the above-mentioned conditions, 2 g of a 30% solution of Mersolat® (Bayer AG) were added to the suspension before gassing. 4 g Marlon A 375® (Chemische Werke Marl Huls) were added to a third suspension. The behavior is shown in Table 1.
TABLE 1______________________________________Quantity Foam height Settling behavior of solidsadded: 3 ml during gassing after gassing______________________________________Comparison 11 cm approx. 50% of the solidstest with no floataddition2 g "Mersolat H" 1 cm more than 90% of the solids(30%) sediment4 g "Marlon 1 cm more than 90% of the solidsA 375" (30%) sediment______________________________________ "Mersolat H": sodium alkyl sulfonate "Marlon A 375": sodium alkylbenzene sulfonate
EXAMPLE 2
In the apparatus described in Example 1, quantities of 5000 ppm (based on suspension) of the organic foam inhibitors DNE on OC 6003 were added to a suspension, which forms an 18 cm tall layer of foam under gassing conditions without the addition of a surface-active agent.
Where the foam inhibitor DNE was added, the foam height was reduced to 3 cm. Where the foam inhibitor OC 6003 was added, the foam height was again reduced to 3 cm.
Whereas, after the termination of gassing in the untreated suspension, approximately 80% of the solids floated on the surface, approximately 50% of the solids sedimented where DNE was added and approximately 100% where OC 6003 was added.
Foam inhibitor DNE (Bayer AG):
A mixture of fatty acid esters and higher hydrocarbons with carboxylic acid salts.
Foam inhibitor VPOC 6003 (Bayer AG):
Alkyl polypropylene polyethylene glycol ether.
It will be appreciated that the instant specification and claims are set forth by way of illustration and not limitation, and that various modifications and changes may be made without departing from the spirit and scope of the present invention.
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A process is disclosed for working up the high-boiling, solids-containing residues obtained in the synthesis of organochlorosilanes which are hydrolyzed and then optionally oxidized, comprising adding during hydrolysis and/or oxidation a surface-active agent which hydrophilicizes the surface of the solids.
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CROSS-REFERENCE
[0001] This application claims the benefit of U.S. Provisional Application No. 61/157,777, filed Mar. 3, 2009, which application is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] Current electricity installations for residences or commercial locations are measured for their power consumption using standardized meters (watt-hour meters) which are inserted in standardized meter sockets. These sockets are comprised of standardized pins and sockets through which the various electrical interconnections from the electricity provided by a local electricity utility is passed through a meter and then delivered to the consumer. There are often multiple meters serving a single physical location.
[0003] In a standard meter, there is one side that serves as a conduit to an electricity provider (the “provider side”) and another side that is the conduit to supplying electricity to the premise or location that it services (the “consumer side”). The consumer side of the meters is usually wired to a panel box where the power flowing through the meter is distributed to the physical interior of the premise or consumer for use by the various loads and equipment of the consumer.
[0004] If a local generation system is to be used, currently, it may be connected to the panel box via a new conduit to the panel box. This new conduit source may be from the output of a grid compatible inverter, where it is connected to a new breaker on the premise's distribution panel. The new breaker must be sized according to the capacity of the panel box rating and the other loads present at the location or premise.
[0005] Current generations of systems for energy management, power management and performance measurement typically require an ability to measure the load (current, watts, KVAR, etc.) coming into a premise and usually this is difficult to access due to the limitations and security limits of existing electrical meters. The current practice requires current sensing coils to be somehow located and installed around existing wire and for voltage taps to be securely placed. Problems with physical access, variety of sizes and access issues typically arise.
[0006] This current practice has numerous flaws which results in longer than needed labor times and greater complexity of installation. For example, systems often may not be connected to local or renewable generators, advanced electrical storage or high current applications such as electric cars, because they have no physical space for an extra breaker or panel. In addition, there is often a need to reduce the size or cost of systems because of inadequate current capacity in existing panel boxes. Further, extra labor and design time is required up front to analyze and minimize costs and old systems often have to be completely replaced due to inability to locate available spare parts. Therefore, the present invention addresses these needs for simpler and faster interconnect means that allow for lower cost installation to more locations with less pre-planning and shorter lead times to accomplish the interconnect that can handle potentially more locally generated power.
[0007] Therefore, there exists a need for a simpler and faster interconnect means that allows for lower cost installation to more locations with less pre-planning and shorter lead times to accomplish the interconnect that can handle potentially more locally generated power.
SUMMARY OF THE INVENTION
[0008] The invention provides for meter socket connection methods and systems for use of local generators or monitoring of the connection. Various aspects of the invention described herein may be applied to any of the particular applications set forth below. The invention may be applied as a standalone system or as a component of an integrated solution. It shall be understood that different aspects of the invention can be appreciated individually, collectively or in combination with each other.
[0009] One aspect of the invention provides a system for interconnecting a watt-hour power meter to a local generator inverter. The system includes a watt-hour power meter for measuring power consumption and a meter socket positioned between a conduit to an electrical power provider and a conduit to an electrical power consumer. In addition, the system also includes a meter socket insert between the power meter and the meter socket. The meter socket insert may be formed with ports and connected to a local generator inverter.
[0010] In one aspect of the invention, the system further includes a powerline based communication network for measuring power consumption of a plurality of devices within reach of a powerline.
[0011] Other goals and advantages of the invention will be further appreciated and understood when considered in conjunction with the following description and accompanying drawings. While the following description may contain specific details describing particular embodiments of the invention, this should not be construed as limitations to the scope of the invention but rather as an exemplification of preferable embodiments. For each aspect of the invention, many variations are possible as suggested herein that are known to those of ordinary skill in the art. A variety of changes and modifications can be made within the scope of the invention without departing from the spirit thereof.
INCORPORATION BY REFERENCE
[0012] All publications, patents, and patent applications mentioned in this specification 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.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The novel features of the invention are set forth with particularity in the appended claims. A better understanding of the features and advantages of the present invention will be obtained by reference to the following detailed description that sets forth illustrative embodiments, in which the principles of the invention are utilized, and the accompanying drawings of which:
[0014] FIG. 1A illustrates a side view of a current watt-hour power meter and meter socket.
[0015] FIG. 1B illustrates a view of a current watt-hour power meter socket receptacles and pins.
[0016] FIG. 2 illustrates the architecture of a current configuration of a watt-hour meter and meter socket.
[0017] FIG. 3A illustrates one example of an architecture of a watt-hour power meter and meter socket with an adapter, in accordance with embodiments of the present invention.
[0018] FIG. 3B illustrates one example of an architecture of a watt-hour power meter and meter socket with an adapter using powerline communications to deliver data, commands, and configuration controls, in accordance with embodiments of the present invention.
[0019] FIG. 4A illustrates an adapter to be positioned between a watt-hour power meter and meter socket, in accordance with embodiments of the present invention.
[0020] FIG. 4B illustrates an example of an adapter positioned between a watt-hour power meter and meter socket and connected to powerline and measurement electronics, in accordance with embodiments of the present invention.
[0021] FIG. 5A illustrates an embodiment of the adapter as positioned between a watt-hour power meter and meter socket, in accordance with embodiments of the present invention.
[0022] FIG. 5B illustrates the meter-side of the adapter, in accordance with embodiments of the present invention.
[0023] FIG. 6 illustrates an embodiment of the adapter as positioned between a watt-hour power meter and meter socket, in accordance with embodiments of the present invention.
[0024] FIG. 7 illustrates the socket-side of the adapter, in accordance with embodiments of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0025] In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the invention. However it will be understood by those of ordinary skill in the art that the invention may be practiced without these specific details. In other instances, well-known methods, procedures, components and circuits have not been described in detail so as not to obscure the invention. Various modifications to the described embodiments will be apparent to those with skill in the art, and the general principles defined herein may be applied to other embodiments. The invention is not intended to be limited to the particular embodiments shown and described.
[0026] Embodiments of the present invention relate to the process of interconnecting local renewable energy generation and ‘smart monitoring’ systems to a local utility power grid. Embodiments of the present invention may lower the cost of interconnection and speed up the process of installation for local generation systems such as solar, wind or fuel cells to existing standardized power meters. For example, a local generator may be a solar, wind or any kind of generator, and the inverter of the local generator may be connected to a power meter, as described in embodiments of the present invention. Embodiments of the present invention may also allow for interconnection of locally monitored power demand management systems to such existing standardized power meters, whether a smart meter or a legacy meter.
[0027] Referring to FIG. 1A , a power meter, built and configured according to existing standards, is illustrated. An existing standardized meter generally has one conduit to a local electricity utility company (provider) 101 and another conduit to a residence or commercial location (premise) 102 . The meter then functions to measure the amount of power provided by the provider and consumed by the premise. Referring to FIG. 1B , the meter socket, built and configured according to existing standards, is illustrated. The interior of the meter socket contains, generally three rows of sockets: one for the provider side 103 , one for neutral sockets, and one for the consumer side 104 . The various phases for each are handled by one receptacle within each row and are matched to one pin built into the meter. These receptacle and pins are standardized and various meter manufacturers and receptacle manufacturer's product interoperate today with certification from Underwriters Laboratories.
[0028] Typically, a power source may provide electrical power service to a residential or commercial building site over two to three incoming line conductors. The line conductors are connected to a standard electric meter socket. In addition, a neutral line conductor extends from the power source to the meter socket. Typically, the meter socket is mounted to a wall of the building site. In order to measure the electrical power consumed by the building site, a watt-hour meter is removably attached to the meter socket.
[0029] A standard power (or watt-hour) meter includes a first pair of line contacts (line jaw contacts) and a second pair of load contacts (load jaw contacts). The line jaw contacts are positioned above the load jaw contacts, and a neutral jaw contact is located in the housing between the upper and lower line jaw contacts. The ends of the line conductors terminate at the line jaw contacts, and the load jaw contacts are attached to the electrical distribution wiring system of the building site. Thus, the meter includes a pair on line contacts and a pair of load contacts, and also a neutral blade contact. Each of these blade contacts are configured for being removably engaged to the jaw contacts of the meter socket. Therefore, each blade contact may resemble an elongated thin blade. When the watt-hour meter and the meter socket are connected together, an electrical circuit is completed so that electrical energy can pass from the line contacts to the load contacts for distribution to the building site. Energy consumption may also be measured as the energy passes through the meter.
[0030] Referring to FIG. 2 , an architectural overview of how a utility or power meter is configured in a typical home or building (or premise) is illustrated. Generally, in current configurations, when configuring a local or renewable generator grid, a compatible inverter 201 must be connected through the premise's distribution panel box 202 . Thus, a new conduit 207 to the panel box from the output of a grid compatible inverter must be formed. This is normally accomplished by connecting a new breaker (within 202 ), sized according to the capacity of the panel box rating and other loads present within the premise. The local generator grid compatible inverter 201 output is fed into a new breaker (within 202 ) on the premise's distribution panel 202 , which is then connected to a meter socket 203 on the consumer side.
[0031] The incoming AC power line 204 then passes through the utility company meter 206 on its way to one or more breaker boxes before being generally distributed throughout the home or building through conventional power wiring 205 . Output from a local generator grid compatible inverter 201 must also pass through the breaker box (within 202 ). This current practice has numerous flaws which result in longer than needed labor times and greater complexity of installation, as discussed above.
[0032] In contrast, referring to FIG. 3A , the local (renewable) generator grid compatible inverter 301 may bypass the breaker box on the premise's distribution panel 302 , and may be run to a socket adapter (or shim) 303 as illustrated in embodiments of the present invention. Thus, a new breaker on the premise's distribution panel 302 is no longer necessary. The socket adapter (or shim) 303 may be a meter socket insert. On the consumer side, the same housing and existing approved breakers 302 may be incorporated, so there is no need to expand, replace or install a new breaker panel box. The existing conduit 304 from the distribution panel to the consumer side of the meter may also be utilized so there is no need to make any alterations to such conduit. Thus, instead of requiring a new breaker, the local (renewable) generator grid compatible inverter 301 may be run directly to a socket adapter (or shim) 303 .
[0033] In contrast, referring to FIG. 3B , a local (renewable) generator grid compatible inverter 301 b may be connected to a breaker box on the premise's distribution panel 302 b, and communications between a unit (such as a storage unit or intelligent power management system) may run to a socket adapter (or shim) 303 b as illustrated in embodiments of the present invention, via powerline communications. Thus, there is no longer a need for separate wiring to each device with a premise. The socket adapter (or shim) 303 b may be a meter socket insert, and, for example, an intelligent power management unit may be embedded within the meter socket insert 303 b as described below. Each meter socket insert 303 b may include microprocessors that measure power, and the local renewable generator, storage unit or other device on the consumer's premise utilize such measurements for obtaining timely information on the power load of the consumer's premise. On the consumer side, the same housing and existing approved breakers may be incorporated, so there may be no need to expand, replace or install a new breaker panel box. The existing conduit 304 b from the distribution panel 302 b to the consumer side of the meter may also be utilized so there is no need to make any alterations to such conduit.
[0034] Referring to FIG. 4A , a shim or adapter that may be placed between the current meter and the current socket is shown. The adapter (or shim) has a meter side 401 , which is the side connected to the meter, and a socket side 403 , which is the side connected to the socket. The adapter (or shim) also has a consumer side 402 , which is the side of the conduit to the premise. An alternate consumer side 404 may provide an additional breaker connection or conduit to the premise for physical access in case of any obstructions to 402 .
[0035] Referring to FIG. 4B , a shim or adapter that may be placed between the current meter and the current socket is shown. The adapter (or shim) may have integrated measurement coils or sensors 405 , which are connected to built-in power measurement electronics, control computer and powerline communications module 407 . Voltage taps 406 located on the customer side of the meter power measurement may be used for at least three purposes including voltage measurement, providing power to a built-in power measurement electronics, control computer and/or powerline communications module 407 , as well as to provide a connection for the powerline communications electronics to a powerline.
[0036] Thus, to elaborate further, another aspect of the invention is the inclusion of a form of powerline based communication network. The network may conform to a standard such as the HomePlug standard (IEEE 1901 draft standard for powerline communications or other equivalent) to communicate with an integrated power measurement and data logging capability. For example, the network may be able to measure power consumed or required by certain devices or appliances that are plugged into the network (or within reach of a certain power line or network of power lines) or other data relating to devices or appliances on the network. The data and information that is measured and collected may be communicated to other devices within the premise or within the reach of the power line for various purposes including control, measurement and configuration.
[0037] Referring to FIG. 5A , a shim or adapter 501 may be placed between the current meter 502 and the current socket 503 . The “meter side” 505 has a series of compatible receptacles to the meter, and the “socket side” 504 has a series of compatible pins to plug into the current socket. The adapter 501 may be safely and easily employed to bridge the meter 502 and the socket 503 . The adapter 501 positioned between the meter 502 and the socket 503 may include a line conductor and a pair of load conductors. The line conductor may have a first end configured for being connected to one of the line jaw contacts of the watt-hour meter socket and a second end for being connected to one of the blade contact of the watt-hour meter. Each load conductor may have a first end configured for being engaged by jaw load contacts of the watt-hour meter socket and a second end for being connected to blade contacts of the watt-hour meter. In addition, the neutral conductor may have a first end configured for being engaged by jaw neutral contact and a second end for being connected to blade contact of the watt-hour meter. A means for securing, e.g., a cotter pin, may also be employed to secure the line conductor or load conductor. It can be appreciated that any type of contact configuration may be employed herein so long as electrical contact sufficient to handle the load can be made between the elements.
[0038] In FIG. 5B , the “meter side” of the shim or adapter is shown. As shown in FIG. 5B , the pins 506 on the consumer side of the shim or adapter are wired such that they feed to an electric breaker or fuse suitable for interconnection to the provider's grid. The supply side of the breaker (line conductor) 507 may be connected to the receptacles 508 of the shim or adapter, and the load side of the breaker (pair of load conductors) 507 may be connected to the wires coming from one or more of the conduit ports at the top or bottom of the shim or adapter, and which run to the outputs of the local generation facility (local generator conduit port) 509 .
[0039] Referring to FIG. 6 , the breaker 601 may be connected to either side of the shim or adapter 602 . Further, as shown, local generator conduit ports 603 may be at the top or bottom of the shim or adapter, and may run to the outputs of a local generation facility. Thus, the local generation resource may be connected to the meter 604 , without having to connect to a new breaker on the existing breaker panel.
[0040] Referring to FIG. 7 , the “socket side” of the shim or adapter is shown. As shown in FIG. 7 , the conduit 701 , which is preferably a flexible conduit, on the consumer side, runs from the local generator conduit port to the output of a local grid compatible inverter (or local inverter). While a flexible wire may be preferably employed as the connector, any known mechanical means may be used in lieu thereof. For example, the adapter 702 may be manufactured with a non-flexible shunt, e.g., a solid copper bar, to bridge the connection. Further, any mechanical or other known means may be employed to attach the terminal ends of flexible wire from the local generator conduit port to the local grid compatible inverter (or local inverter). For example, chemical bonding may be employed in lieu of the mechanical means described. The conduit to the provider remains the same as it is in standardized meter configurations, thus ensuring the billing accuracy of the utility meter.
[0041] Each of the meter sockets discussed above may serve a variety of voltages and single, dual or three phase power. The shim or adapter may be inserted at the same time as the current net metering is swapped out, or alternatively it may be installed in advance of a utility swap. Thus, the provider's meter may remain in the same physical location and operate without change to its accuracy or completeness of data collection. In addition, the advantages of utilizing the shim or adapter as described in embodiments of the present invention would allow for a very quick connection to the full rate power potential for a premise or consumer location by a local generator or other applications such as an electric vehicle charger. Most importantly, embodiments of the present invention utilize existing approved breakers and conduits to reach and connect to the consumer side of standardized power meters, without avoiding having to expand, replace or install a new breaker panel box. A utility worker may easily remove the electric watt-hour meter from the meter socket, and arrange the adapter. Thus, an interconnection may be made where physical requirements for a particular installation may not allow a new panel box to be installed. Where a new panel box would otherwise prevent the ability for a local generator to be interconnected in a cost effective manner, embodiments of the present invention make that interconnection possible, in an efficient, cost-effective way.
[0042] In addition, an advantage of embodiments of the present invention is that local premise current and voltage measurement circuitry could be incorporated in the same housing so as to enable a feedback to any local generation or power control or storage equipment to have data on the total usage of the premise even in the absence of an accessible “smart meter” and so expand the locations where the generation, storage or power control system can be installed by eliminating the requirement for an accessible local utility smart meter.
[0043] All concepts of the invention may incorporate or integrate concepts utilized by other types of watt-hour meter adapters and inserts including but not limited to those described in U.S. Pat. No. 6,015,314 (Benfante) issued on Jan. 18, 2000, which is hereby incorporated by reference in its entirety.
[0044] While preferred embodiments of the present invention have been shown and described herein, it will be obvious to those skilled in the art that such embodiments are provided by way of example only. Numerous variations, changes, and substitutions will now occur to those skilled in the art without departing from the invention. It should be understood that various alternatives to the embodiments of the invention described herein may be employed in practicing the invention. It is intended that the following claims define the scope of the invention and that methods and structures within the scope of these claims and their equivalents be covered thereby.
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Systems and methods for faster, safer and lower cost means of interconnecting local generation or power monitoring systems to a residential or commercial electric power system so that the connection is made via a direct connection to the power meter socket on the consumer side of the meter. The breaker for the system is collocated with the interconnection. Further modern energy management system typically require measurement of an entire premise's power and energy load, requiring additional power measurement probes and communications wiring. Instead of being connected to a new, upgraded breaker in the main service panel on the consumer side of the meter which often requires extensive and time consuming work to do as well as additional potential complications, embodiments of the invention may allow for a quick interconnection by inserting an attachment underneath the existing standardized meter for simplified power connection, measurement and communications.
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RELATED APPLICATION
This application claims the benefit of U.S. Provisional Application Ser. No. 61/419,362, filed Dec. 3, 2010, the disclosure of which is hereby incorporated in its entirety herein by reference
FIELD OF THE INVENTION
The present invention relates to novel oxime derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals, as modulators of sphingosine-1-phosphate receptors. The invention relates specifically to the use of these compounds and their pharmaceutical compositions to treat disorders associated with sphingosine-1-phosphate (S1P) receptor modulation.
BACKGROUND OF THE INVENTION
Sphingosine-1 phosphate is stored in relatively high concentrations in human platelets, which lack the enzymes responsible for its catabolism, and it is released into the blood stream upon activation of physiological stimuli, such as growth factors, cytokines, and receptor agonists and antigens. It may also have a critical role in platelet aggregation and thrombosis and could aggravate cardiovascular diseases. On the other hand the relatively high concentration of the metabolite in high-density lipoproteins (HDL) may have beneficial implications for atherogenesis. For example, there are recent suggestions that sphingosine-1-phosphate, together with other lysolipids such as sphingosylphosphorylcholine and lysosulfatide, are responsible for the beneficial clinical effects of HDL by stimulating the production of the potent antiatherogenic signaling molecule nitric oxide by the vascular endothelium. In addition, like lysophosphatidic acid, it is a marker for certain types of cancer, and there is evidence that its role in cell division or proliferation may have an influence on the development of cancers. These are currently topics that are attracting great interest amongst medical researchers, and the potential for therapeutic intervention in sphingosine-1-phosphate metabolism is under active investigation.
SUMMARY OF THE INVENTION
A group of novel oxime derivatives, which are potent and selective sphingosine-1-phosphate modulators has been discovered. As such, the compounds described herein are useful in treating a wide variety of disorders associated with modulation of sphingosine-1-phosphate receptors. The term “modulator” as used herein, includes but is not limited to: receptor agonist, antagonist, inverse agonist, inverse antagonist, partial agonist, partial antagonist.
This invention describes compounds of Formula I, which have sphingosine-1-phosphate receptor biological activity. The compounds in accordance with the present invention are thus of use in medicine, for example in the treatment of humans with diseases and conditions that are alleviated by S1P modulation.
In one aspect, the invention provides a compound having Formula I or a pharmaceutically acceptable salt thereof or stereoisomeric forms thereof, or the geometrical isomers, enantiomers, diastereoisomers, tautomers, zwitterions and pharmaceutically acceptable salts thereof:
wherein:
A is C 6-10 aryl, heterocycle, C 3-8 cycloalkyl or C 3-8 cycloalkenyl;
B is C 6-10 aryl, heterocycle, C 3-8 cycloalkyl or C 3-8 cycloalkenyl;
R 1 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-8 alkyl, C 1-8 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is O, C(O), S, NH or CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-8 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-8 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-8 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-8 alkyl;
R 14 is H or C 1-8 alkyl; and
R 15 is H or C 1-8 alkyl;
R 16 is H, OH or C 1-8 alkyl; and
R 17 is H or C 1-8 alkyl.
In another aspect, the invention provides a compound having Formula I wherein L 1 is O, C(O), S or NH.
In another aspect, the invention provides a compound having Formula I wherein L 1 is O.
In another aspect, the invention provides a compound having Formula I wherein L 1 is S.
In another aspect, the invention provides a compound having Formula I wherein L 1 is CH 2 .
In another aspect, the invention provides a compound having Formula I wherein
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
In another aspect, the invention provides a compound having Formula I wherein
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
In another aspect, the invention provides a compound having Formula I wherein
In another aspect, the invention provides a compound having Formula I wherein
In another aspect, the invention provides a compound having Formula I wherein
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is O, C(O), S, NH or CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is O, S or CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
a is 0;
L 1 is O, S or CH 2 ;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is CH 2 ;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 2 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 3 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 4 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 5 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 6 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 7 is H, halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
R 8 is halogen, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)R 13 , NR 14 R 15 or hydroxyl;
L 1 is O, C(O), S or NH;
R 9 is O, S or CH 2 ;
R 10 is H or C 1-6 alkyl;
L 2 is CHR 16 , O, S, NR 17 or —C(O)—;
D is a group of formula
“*” indicating the point of attachment to the rest of the molecule;
R 11 is H, OPO 3 H 2 , carboxylic acid, PO 3 H 2 , C 1-6 alkyl, —S(O) 2 H, —P(O)MeOH, —P(O)(H)OH or OR 12 ;
R 12 is H or C 1-6 alkyl;
a is 0, 1 or 2;
b is 0 or 1;
c is 0, 1, 2 or 3;
R 13 is H, C 1-6 alkyl;
R 14 is H or C 1-6 alkyl; and
R 15 is H or C 1-6 alkyl;
R 16 is H, OH or C 1-6 alkyl; and
R 17 is H or C 1-6 alkyl.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is O, CH 2 , S or NH;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
a is 0;
L 1 is O, S or NH;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is CH 2 ;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is CH 2 ;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is CH 2 ;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is O or S;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is O;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is O;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is O;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is S;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, C 1-6 alkyl or halogen;
R 2 is H, C 1-6 alkyl or halogen;
R 3 is H, C 1-6 alkyl or halogen;
R 4 is H or C 1-6 alkyl,
R 5 is H or C 1-6 alkyl;
R 6 is H or C 1-6 alkyl;
R 7 is H;
L 1 is S;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule;
a is 0;
b is 1;
c is 0 or 1;
R 11 is carboxylic acid or PO 3 H 2 ; and
R 16 is H.
In another aspect, the invention provides a compound having Formula I wherein
R 1 is H, chloro, methyl or fluoro;
R 2 is H, chloro, methyl or fluoro;
R 3 is H, chloro, methyl or fluoro;
R 4 is H or methyl;
R 5 is H or methyl;
R 6 is H or methyl;
R 7 is H;
L 1 is S;
R 9 is CH 2 ;
R 10 is H;
L 2 is CHR 16 ;
a is 0;
b is 1;
c is 0 or 1; and
R 16 is H; and
R 11 is carboxylic acid or PO 3 H 2 ; and
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is chloro, methyl or fluoro;
R 2 is H;
R 3 is H or fluoro;
R 4 is methyl;
R 5 is methyl;
R 6 is H;
R 7 is H;
a is 0;
R 9 is CH 2 ;
R 10 is H;
L 1 is CH 2 ;
L 2 is CHR 16 ;
a is 0;
b is 1;
c is 0 or 1; and
R 16 is H; and
R 11 is carboxylic acid or PO 3 H 2 ; and
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is chloro or methyl;
R 2 is H ;
R 3 is H;
R 4 is methyl;
R 5 is methyl;
R 6 is H;
R 7 is H;
a is 0;
R 9 is CH 2 ;
R 10 is H;
L 1 is CH 2 ;
L 2 is CHR 16 ;
a is 0;
b is 1;
c is 0 or 1; and
R 16 is H; and
R 11 is carboxylic acid or PO 3 H 2 ; and
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
In another embodiment, the invention provides a compound having Formula I wherein:
R 1 is chloro or fluoro;
R 2 is H ;
R 3 is H or fluoro;
R 4 is methyl;
R 5 is methyl;
R 6 is H;
R 7 is H;
R 9 is CH 2 ;
R 10 is H;
L 1 is CH 2 ;
L 2 is CHR 16 ;
a is 0;
b is 1;
c is 0 or 1; and
R 16 is H; and
R 11 is carboxylic acid or PO 3 H 2 ; and
D is a group of formula
“*” indicates the point of attachment to the rest of the molecule.
The term “alkyl”, as used herein, refers to saturated, monovalent or divalent hydrocarbon moieties having linear or branched moieties or combinations thereof and containing 1 to 8 carbon atoms. One methylene (—CH 2 —) group, of the alkyl can be replaced by oxygen, sulfur, sulfoxide, nitrogen, carbonyl, carboxyl, sulfonyl, or by a divalent C 3-8 cycloalkyl. Alkyl groups can be substituted by halogen, hydroxyl, cycloalkyl, amino, non-aromatic heterocycles, carboxylic acid, phosphonic acid groups, sulphonic acid groups, phosphoric acid.
The term “cycloalkyl”, as used herein, refers to a monovalent or divalent group of 3 to 8 carbon atoms, derived from a saturated cyclic hydrocarbon. Cycloalkyl groups can be monocyclic or polycyclic. Cycloalkyl can be substituted by alkyl groups or halogen atoms.
The term “cycloalkenyl”, as used herein, refers to a monovalent or divalent group of 3 to 8 carbon atoms, derived from a saturated cycloalkyl having one double bond. Cycloalkenyl groups can be monocyclic or polycyclic. Cycloalkenyl groups can be substituted by alkyl groups or halogen atoms.
The term “halogen”, as used herein, refers to an atom of chlorine, bromine, fluorine, iodine.
The term “alkenyl”, as used herein, refers to a monovalent or divalent hydrocarbon radical having 2 to 6 carbon atoms, derived from a saturated alkyl, having at least one double bond. C 2-6 alkenyl can be in the E or Z configuration. Alkenyl groups can be substituted by alkyl groups.
The term “alkynyl”, as used herein, refers to a monovalent or divalent hydrocarbon radical having 2 to 6 carbon atoms, derived from a saturated alkyl, having at least one triple bond.
The term “heterocycle” as used herein, refers to a 3 to 10 membered ring, which can be aromatic or non-aromatic, saturated or non-saturated, containing at least one heteroatom selected form O or N or S or combinations of at least two thereof, interrupting the carbocyclic ring structure. The heterocyclic ring can be interrupted by a C═O; the S heteroatom can be oxidized. Heterocycles can be monocyclic or polycyclic. Heterocyclic ring moieties can be substituted by hydroxyl, alkyl groups or halogen atoms.
The term “aryl” as used herein, refers to an organic moiety derived from an aromatic hydrocarbon consisting of a ring containing 6 to 10 carbon atoms by removal of one hydrogen. Aryl can be monocyclic or polycyclic. Aryl can be substituted by halogen atoms, —OC 1-6 alkyl, C 1-6 alkyl, CN, C(O)(C 1-6 alkyl), N(C 1-6 alkyl) (C 1-6 alkyl) or NH 2 or NH(C 1-6 alkyl) or hydroxyl groups. Usually aryl is phenyl. Preferred substitution site on aryl are meta and para positions.
The term “hydroxyl” as used herein, represents a group of formula “—OH”.
The term “carbonyl” as used herein, represents a group of formula “—C(O)”.
The term “carboxyl” as used herein, represents a group of formula “—C(O)O—”.
The term “sulfonyl” as used herein, represents a group of formula “—SO 2 ”.
The term “sulfate” as used herein, represents a group of formula “—O—S(O) 2 —O—”.
The term “carboxylic acid” as used herein, represents a group of formula “—C(O)OH”.
The term “sulfoxide” as used herein, represents a group of formula “—S═O”.
The term “phosphonic acid” as used herein, represents a group of formula “—P(O)(OH) 2 ”.
The term “phosphoric acid” as used herein, represents a group of formula “—(O)P(O)(OH) 2 ”.
The term “sulphonic acid” as used herein, represents a group of formula “—S(O) 2 OH”.
The formula “H”, as used herein, represents a hydrogen atom.
The formula “O”, as used herein, represents an oxygen atom.
The formula “N”, as used herein, represents a nitrogen atom.
The formula “S”, as used herein, represents a sulfur atom.
Some compounds of the invention are:
3-({4-[({[(1E)-2-(3,5-difluorophenyl)-3-(3,4-dimethylphenyl)-1-methylpropylidene]amino}oxy)methyl]benzyl}amino)propanoic acid; [3-({4-[({[(1E)-2-(3,5-difluorophenyl)-3-(3,4-dimethylphenyl)-1-methylpropylidene]amino}oxy)methyl]benzyl}amino)propyl]phosphonic acid; [3-({4-[({[(1E)-2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)-1-methylpropylidene]amino}oxy)methyl]benzyl}amino)propyl]phosphonic acid; 3-[(4-{(1E)-N-[3-(3,4-dimethylphenyl)-2-(3-methylphenyl)propoxy]ethanimidoyl}benzyl)amino]propanoic acid; 3-[(4-{(1E)-N-[2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)propoxy]ethanimidoyl}benzyl)amino]propanoic acid; {3-[(4-{(1E)-N-[2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)propoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid; {3-[(4-{(1E)-N-[3-(3,4-dimethylphenyl)-2-(3-methylphenyl)propoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid; [3-({4-[(1E)-N-{2-[(3,4-dimethylphenyl)sulfonyl]-2-(3-fluorophenyl)ethoxy}ethanimidoyl]benzyl}amino)propyl]phosphonic acid; 3-({4-[(1E)-N-{2-[(3,4-dimethylphenyl)thio]-2-(3-fluorophenyl)ethoxy}ethanimidoyl]benzyl}amino)propanoic acid; {3-[(4-{[({(1E)-2-(3-chlorophenyl)-2-[(3,4-dimethylphenyl)thio]-1-methylethylidene}amino)oxy]methyl}benzyl)amino]propyl}phosphonic acid; 3-[(4-{[({(1E)-2-(3-chlorophenyl)-2-[(3,4-dimethylphenyl)thio]-1-methylethylidene}amino)oxy]methyl}benzyl)amino]propanoic acid; 3-({4-[({[(1E)-2-(3-chlorophenyl)-2-(3,4-dimethylphenoxy)-1-methylethylidene]amino}oxy)methyl]benzyl}amino)propanoic acid; [3-({4-[({[(1E)-2-(3-chlorophenyl)-2-(3,4-dimethylphenoxy)-1-methylethylidene]amino}oxy)methyl]benzyl}amino)propyl]phosphonic acid; 3-[(4-{(1E)-N-[2-(3-chlorophenyl)-2-(3,4-dimethylphenoxy)ethoxy]ethanimidoyl}benzyl)amino]propanoic acid; {3-[(4-{(1E)-N-[2-(3-chlorophenyl)-2-(3,4-dimethylphenoxy)ethoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid.
Some compounds of Formula I and some of their intermediates have at least one stereogenic center in their structure. This stereogenic center may be present in an R or S configuration, said R and S notation is used in correspondence with the rules described in Pure Appli. Chem. (1976), 45, 11-13.
The term “pharmaceutically acceptable salts” refers to salts or complexes that retain the desired biological activity of the above identified compounds and exhibit minimal or no undesired toxicological effects. The “pharmaceutically acceptable salts” according to the invention include therapeutically active, non-toxic base or acid salt forms, which the compounds of Formula I are able to form.
The acid addition salt form of a compound of Formula I that occurs in its free form as a base can be obtained by treating the free base with an appropriate acid such as an inorganic acid, for example, a hydrohalic acid, such as hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, nitric acid and the like; or an organic acid such as for example, acetic, hydroxyacetic, propanoic, lactic, pyruvic, malonic, fumaric acid, maleic acid, oxalic acid, tartaric acid, succinic acid, malic acid, ascorbic acid, benzoic acid, tannic acid, pamoic acid, citric, methylsulfonic, ethanesulfonic, benzenesulfonic, formic and the like (Handbook of Pharmaceutical Salts, P. Heinrich Stahal& Camille G. Wermuth (Eds), Verlag Helvetica Chemica Acta—Zürich, 2002, 329-345).
Compounds of Formula I and their salts can be in the form of a solvate, which is included within the scope of the present invention. Such solvates include for example hydrates, alcoholates and the like.
With respect to the present invention reference to a compound or compounds, is intended to encompass that compound in each of its possible isomeric forms and mixtures thereof unless the particular isomeric form is referred to specifically.
Compounds according to the present invention may exist in different polymorphic forms. Although not explicitly indicated in the above formula, such forms are intended to be included within the scope of the present invention.
The compounds of the invention are indicated for use in treating or preventing conditions in which there is likely to be a component involving the sphingosine-1-phosphate receptors.
In another embodiment, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier.
In a further embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one compound of the invention.
These compounds are useful for the treatment of mammals, including humans, with a range of conditions and diseases that are alleviated by S1P modulation.
Therapeutic utilities of S1P modulators are Ocular Diseases: wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis;
Systemic vascular barrier related diseases: various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury;
Autoimmune diseases and immunosuppression: rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, antoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermatitis, and organ transplantation;
Allergies and other inflammatory diseases: urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases;
Cardiac functions: bradycardia, congestional heart failure, cardiac arrhythmia, prevention and treatment of atherosclerosis, and ischemia/reperfusion injury;
Wound Healing: scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries;
Bone formation: treatment of osteoporosis and various bone fractures including hip and ankles;
Anti-nociceptive activity: visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains;
Anti-fibrosis: ocular, cardiac, hepatic and pulmonary fibrosis, proliferative vitreoretinopathy, cicatricial pemphigoid, surgically induced fibrosis in cornea, conjunctiva and tenon;
Pains and anti-inflammation: acute pain, flare-up of chronic pain, musculo-skeletal pains, visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, bursitis, neuropathic pains;
CNS neuronal injuries: Alzheimer's disease, age-related neuronal injuries;
Organ transplants: renal, corneal, cardiac and adipose tissue transplants.
In still another embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a therapeutically effective amount of at least one compound of the invention, or any combination thereof, or pharmaceutically acceptable salts, hydrates, solvates, crystal forms and individual isomers, enantiomers, and diastereomers thereof.
The present invention concerns the use of a compound of Formula I or a pharmaceutically acceptable salt thereof, for the manufacture of a medicament for the treatment of Ocular Diseases: wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis;
Systemic vascular barrier related diseases: various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury;
Autoimmune diseases and immunosuppression: rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, antoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermatitis, and organ transplantation;
Allergies and other inflammatory diseases: urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases;
Cardiac functions: bradycardia, congestional heart failure, cardiac arrhythmia, prevention and treatment of atherosclerosis, and ischemia/reperfusion injury;
Wound Healing: scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries;
Bone formation: treatment of osteoporosis and various bone fractures including hip and ankles;
Anti-nociceptive activity: visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains;
Anti-fibrosis: ocular, cardiac, hepatic and pulmonary fibrosis, proliferative vitreoretinopathy, cicatricial pemphigoid, surgically induced fibrosis in cornea, conjunctiva and tenon;
Pains and anti-inflammation: acute pain, flare-up of chronic pain, musculo-skeletal pains, visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, bursitis, neuropathic pains;
CNS neuronal injuries: Alzheimer's disease, age-related neuronal injuries;
Organ transplants: renal, corneal, cardiac and adipose tissue transplants.
The actual amount of the compound to be administered in any given case will be determined by a physician taking into account the relevant circumstances, such as the severity of the condition, the age and weight of the patient, the patient's general physical condition, the cause of the condition, and the route of administration.
The patient will be administered the compound orally in any acceptable form, such as a tablet, liquid, capsule, powder and the like, or other routes may be desirable or necessary, particularly if the patient suffers from nausea. Such other routes may include, without exception, transdermal, parenteral, subcutaneous, intranasal, via an implant stent, intrathecal, intravitreal, topical to the eye, back to the eye, intramuscular, intravenous, and intrarectal modes of delivery. Additionally, the formulations may be designed to delay release of the active compound over a given period of time, or to carefully control the amount of drug released at a given time during the course of therapy.
In another embodiment of the invention, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier thereof. The phrase “pharmaceutically acceptable” means the carrier, diluent or excipient must be compatible with the other ingredients of the formulation and not deleterious to the recipient thereof.
Pharmaceutical compositions of the present invention can be used in the form of a solid, a solution, an emulsion, a dispersion, a patch, a micelle, a liposome, and the like, wherein the resulting composition contains one or more compounds of the present invention, as an active ingredient, in admixture with an organic or inorganic carrier or excipient suitable for enteral or parenteral applications. Invention compounds may be combined, for example, with the usual non-toxic, pharmaceutically acceptable carriers for tablets, pellets, capsules, suppositories, solutions, emulsions, suspensions, and any other form suitable for use. The carriers which can be used include glucose, lactose, gum acacia, gelatin, mannitol, starch paste, magnesium trisilicate, talc, corn starch, keratin, colloidal silica, potato starch, urea, medium chain length triglycerides, dextrans, and other carriers suitable for use in manufacturing preparations, in solid, semisolid, or liquid form. In addition auxiliary, stabilizing, thickening and coloring agents and perfumes may be used. Invention compounds are included in the pharmaceutical composition in an amount sufficient to produce the desired effect upon the process or disease condition.
Pharmaceutical compositions containing invention compounds may be in a form suitable for oral use, for example, as tablets, troches, lozenges, aqueous or oily suspensions, dispersible powders or granules, emulsions, hard or soft capsules, or syrups or elixirs. Compositions intended for oral use may be prepared according to any method known in the art for the manufacture of pharmaceutical compositions and such compositions may contain one or more agents selected from the group consisting of a sweetening agent such as sucrose, lactose, or saccharin, flavoring agents such as peppermint, oil of wintergreen or cherry, coloring agents and preserving agents in order to provide pharmaceutically elegant and palatable preparations. Tablets containing invention compounds in admixture with non-toxic pharmaceutically acceptable excipients may also be manufactured by known methods. The excipients used may be, for example, (1) inert diluents such as calcium carbonate, lactose, calcium phosphate or sodium phosphate; (2) granulating and disintegrating agents such as corn starch, potato starch or alginic acid; (3) binding agents such as gum tragacanth, corn starch, gelatin or acacia, and (4) lubricating agents such as magnesium stearate, stearic acid or talc. The tablets may be uncoated or they may be coated by known techniques to delay disintegration and absorption in the gastrointestinal tract and thereby provide a sustained action over a longer period. For example, a time delay material such as glyceryl monostearate or glyceryl distearate may be employed.
In some cases, formulations for oral use may be in the form of hard gelatin capsules wherein the invention compounds are mixed with an inert solid diluent, for example, calcium carbonate, calcium phosphate or kaolin. They may also be in the form of soft gelatin capsules wherein the invention compounds are mixed with water or an oil medium, for example, peanut oil, liquid paraffin or olive oil.
The pharmaceutical compositions may be in the form of a sterile injectable suspension. This suspension may be formulated according to known methods using suitable dispersing or wetting agents and suspending agents. The sterile injectable preparation may also be a sterile injectable solution or suspension in a non-toxic parenterally-acceptable diluent or solvent, for example, as a solution in 1,3-butanediol. Sterile, fixed oils are conventionally employed as a solvent or suspending medium. For this purpose any bland fixed oil may be employed including synthetic mono- or diglycerides, fatty acids (including oleic acid), naturally occurring vegetable oils like sesame oil, coconut oil, peanut oil, cottonseed oil, etc., or synthetic fatty vehicles like ethyl oleate or the like. Buffers, preservatives, antioxidants, and the like can be incorporated as required.
Invention compounds may also be administered in the form of suppositories for rectal administration of the drug. These compositions may be prepared by mixing the invention compounds with a suitable non-irritating excipient, such as cocoa butter, synthetic glyceride esters of polyethylene glycols, which are solid at ordinary temperatures, but liquefy and/or dissolve in the rectal cavity to release the drug.
Since individual subjects may present a wide variation in severity of symptoms and each drug has its unique therapeutic characteristics, the precise mode of administration and dosage employed for each subject is left to the discretion of the practitioner.
The compounds and pharmaceutical compositions described herein are useful as medicaments in mammals, including humans, for treatment of diseases and/or alleviations of conditions which are responsive to treatment by agonists or functional antagonists of sphingosine-1-phosphate receptors. Thus, in further embodiments of the invention, there are provided methods for treating a disorder associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one invention compound. As used herein, the term “therapeutically effective amount” means the amount of the pharmaceutical composition that will elicit the biological or medical response of a subject in need thereof that is being sought by the researcher, veterinarian, medical doctor or other clinician. In some embodiments, the subject in need thereof is a mammal. In some embodiments, the mammal is human.
The present invention concerns also processes for preparing the compounds of Formula I. The compounds of formula I according to the invention can be prepared analogously to conventional methods as understood by the person skilled in the art of synthetic organic chemistry. The synthetic schemes set forth below, illustrate how compounds according to the invention can be made.
The following abbreviations are used in the general schemes and in the specific examples:
THF tetrahydrofuran
MPLC medium pressure liquid chromatography
NMO 4-Methylmorpholine N-oxide
CH 3 CN acetonitrile
CH 2 Cl 2 dichloromethane
TPAP Tetrapropylammonium perruthenate
MeOH methanol
NaCNBH 3 sodium cyanoborohydride
CD 3 OD deuterated methanol
DMSO-d6 deuterated dimethyl sulfoxide
NaOMe sodium methoxyde
EtOH ethanol
NaBH 4 sodium borohydride
MgSO 4 magnesium sulfate
NH 4 Cl ammonium chloride
HCl hydrochloric acid
DIBAL-H Diisobutylaluminium hydride
Et 2 O ether
MeOH methanol
K 2 CO 3 potassium carbonate
DMF N,N-dimethylformamide
Et 3 N triethylamine
CuI cooper iodide
PdCl 2 (PPh 3 ) 2 Bis(triphenylphosphine)palladium(II) chloride
NaH sodium hydride
EtOAc ethylacetate
AcOH acetic acid
TFA trifluoroacetic acid
NH 3 ammonia
CDCl 3 deuterated chloroform
n-Bu 4 NOH Tetrabutylammonium hydroxide
NH 2 NH 2 hydrazine
LAH or LiAlH 4 Lithium aluminium hydride
DEAD diethyl azodicarboxylate
Ph 3 P triphenylphosphine
Synthetic Scheme for Obtained Compound of Formula I Wherein D is
General Procedure A for Obtaining Intermediate 1
The starting material, a carboxylic acid (7.82 mmol) prepared according to, Marvin J. et al, Journal of Medicinal Chemistry, 44, 4230-4251, 2001 was dissolved in anhydrous ether (100 mL) at −10° C. A solution of LiAlH 4 (3.9 mL, 2.0M in hexane, 7.82 mmol) was added slowly and the reaction mixture was stirred at room temperature for 4 hours. The reaction was then quenched with aqueous NH 4 Cl and extracted with ether. The combined organic layers were washed with H 2 O and brine, then dried over Na 2 SO 4 . The solvent was removed under reduced pressure. The corresponding alcohol was obtained and isolated by MPLC using 10 to 20% ethyl acetate in hexane.
Diethyl azodicarboxylate (2.58 ml, 40% in toluene, 5.94 mmol) was added dropwise at 0° C. to this alcohol derivative (1.16 g, 4.57 mmol) with triphenylphosphine (1.44 g, 5.48 mmol), and N-hydroxyphthalimide (896 mg, 5.48 mmol) in THF (50 mL). The mixture was stirred at room temperature for 16 h and evaporated to dryness. The residue was purified by MPLC using 20-40% ethyl acetate in hexane to afford the corresponding N-alkoxyphthalimide.
A mixture of the above N-alkoxyphthalimide (2.0 g, 5 mmol) and hydrazine monohydrate (0.25 mL, 5 mmol) in MeOH (30 mL) was heated under reflux for 4 h. After cooling, the resulting suspension was filtered, and the filtrate was evaporated. The residue was triturated with Et 2 O and filtered, and the filtrate was evaporated to dryness. The residue was purified by MPLC using 10-20% ethyl acetate in hexane to give the corresponding hydroxyl amine of Intermediate 1 type.
General Procedure B for Obtaining Intermediate 2
To the mixture of Intermediate 1 (1.15 g, 4.27 mmol) and 1-(4-hydroxylmethyl)phenyl)ethanone (641 mg, 4.27 mmol) prepared according to Zhengqiang et al, Journal of Medicinal Chemistry, 50(15), 3416-3419; 2007, in methanol (20 mL) were added 3 drops of HOAc. The reaction solution was stirred at room temperature for 16 hours and then evaporated to dryness. The corresponding alcohol compound was obtained and purified by MPLC using 0-40% ethyl acetate in hexane.
The above alcohol (4.24 mmol) was mixed with NMO (1.24 g, 10.6 mmol), molecular sieve (600 mg) in AcCN (5 mL) and DCM (25 mL). A catalytic amount of TPAP (40 mg) was added. The resulting reaction mixture was stirred at RT for 1 hour and evaporated to dryness. The aldehyde Intermediate 2 type, was purified by MPLC using 0-10% ethyl acetate in hexane.
General Procedure C for Obtaining a Compound of Formula I wherein
from Intermediate 2
An intermediate 2 (250 mg, 0.62 mmol), β-alanine (52 mg, 0.59 mmol) and TEA (0.1 ml, 0.7 mmol) were stirred in MeOH (10 ml). Upon stirring at 60° C. for 90 min, the reaction solution was cooled to RT. NaBH 4 (50 mg, 1.35 mmol) was added and stirred at RT for 2 hour. The reaction was quenched with 0.5 mL of water and concentrated to minimal amount. The compound of Formula I was isolated by reverse phase MPLC using 10 to 90% H 2 O in AcCN.
General Procedure D for Obtaining a Compound of Formula I wherein
from Intermediate 2
Intermediate 2 (130 mg, 0.88 mmol), 3-aminopropylphosphonic acid (122 mg, 0.88 mmol) and tetra-n-butylammonium hydroxide (0.88 ml, 1.0M/MeOH, 0.88 mmol) were stirred in MeOH (10 ml). Upon stirring at 50° C. for 30 min, NaBH 3 CN (55 mg, 0.88 mmol) was added and stirred at 50° C. for 3 hour. The reaction was quenched with 0.5 mL of water and concentrated to a minimal amount. The compound of Formula I was isolated by MPLC using 10 to 90% MeOH in EtOAc.
Synthetic Scheme for Obtained Compound of Formula I Wherein D is
The compounds of Formula I wherein D is
are prepared according to procedures B and C as described above. The carboxylic acid staring material is replaced with a methyl ketone prepared according to Marvin J. et al, Journal of Medicinal Chemistry, 44, 4230-4251, 2001. The methyl ketone reacted with {4-[(aminooxy)methyl]phenyl}methanol, prepared according to Fensholdt, Jef et al, WO 200505417 according to the B procedure to afford the aldehyde Intermediate 3. Intermediate 3 is used in procedures C or D, as described above, to afford the compounds of Formula I.
Those skilled in the art will be able to routinely modify and/or adapt the following scheme to synthesize any compounds of the invention covered by Formula I.
DETAILED DESCRIPTION OF THE INVENTION
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention claimed. As used herein, the use of the singular includes the plural unless specifically stated otherwise.
It will be readily apparent to those skilled in the art that some of the compounds of the invention may contain one or more asymmetric centers, such that the compounds may exist in enantiomeric as well as in diastereomeric forms. Unless it is specifically noted otherwise, the scope of the present invention includes all enantiomers, diastereomers and racemic mixtures. Some of the compounds of the invention may form salts with pharmaceutically acceptable acids or bases, and such pharmaceutically acceptable salts of the compounds described herein are also within the scope of the invention.
The present invention includes all pharmaceutically acceptable isotopically enriched compounds. Any compound of the invention may contain one or more isotopic atoms enriched or different than the natural ratio such as deuterium 2 H (or D) in place of protium 1 H (or H) or use of 13 C enriched material in place of 12 C and the like. Similar substitutions can be employed for N, O and S. The use of isotopes may assist in analytical as well as therapeutic aspects of the invention. For example, use of deuterium may increase the in vivo half-life by altering the metabolism (rate) of the compounds of the invention. These compounds can be prepared in accord with the preparations described by use of isotopically enriched reagents.
The following examples are for illustrative purposes only and are not intended, nor should they be construed as limiting the invention in any manner. Those skilled in the art will appreciate that variations and modifications of the following examples can be made without exceeding the spirit or scope of the invention.
As will be evident to those skilled in the art, individual isomeric forms can be obtained by separation of mixtures thereof in conventional manner. For example, in the case of diasteroisomeric isomers, chromatographic separation may be employed.
Compound names were generated with ACD version 8; intermediates and reagent names used in the examples were generated with software such as Chem Bio Draw Ultra version 12.0 or Auto Nom 2000 from MDL ISIS Draw 2.5 SP1.
In general, characterization of the compounds is performed according to the following methods: Proton nuclear magnetic resonance ( 1 H NMR) and carbon nuclear magnetic resonance ( 13 C NMR) spectra were recorded on a Varian 300 or 600 MHz spectrometer in deuterated solvent. Chemical shifts were reported as δ (delta) values in parts per million (ppm) relative to tetramethylsilane (TMS) as an internal standard (0.00 ppm) and multiplicities were reported as s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad. Data were reported in the following format: chemical shift (multiplicity, coupling constant(s) J in hertz (Hz), integrated intensity).
All the reagents, solvents, catalysts for which the synthesis is not described are purchased from chemical vendors such as Sigma Aldrich, Fluka, Bio-Blocks, Combi-blocks, TCI, VWR, Lancaster, Oakwood, Trans World Chemical, Alfa, Fisher, Maybridge, Frontier, Matrix, Ukrorgsynth, Toronto, Ryan Scientific, SiliCycle, Anaspec, Syn Chem, Chem-Impex, MIC-scientific, Ltd; however some known intermediates, were prepared according to published procedures.
Usually the compounds of the invention were purified by column chromatography (Auto-column) on an Teledyne-ISCO CombiFlash with a silica column, unless noted otherwise.
Compounds I to 15 were prepared according to the general procedures A, B, C and D. The starting materials, intermediates and the results are tabulated below in Table 1 for each case. Compounds 1, 2, 3 and 4 were generated from Intermediates type 1 and 2. Compounds 5, 6 and 7 were generated from Intermediates type 3.
TABLE 1
Compound
Starting
material
Intermediate
IUPAC name
1 H NMR (Solvent; δ ppm)
Compound 1
1 H NMR (300 MHz, CD 3 OD) δ ppm 2.09 (s, 3 H) 2.14 (s, 3 H) 2.16 (s, 3 H) 2.28 (s, 3 H) 2.44 (t, J = 6.74 Hz, 2 H) 2.79- 2.93 (m, 3 H) 2.98-3.08 (m, 1 H) 3.27 (s, 1 H) 3.86 (s, 2 H) 4.30 (dd, J = 6.74, 2.05 Hz, 2 H) 6.76 (d, J = 7.62 Hz, 1 H) 6.82 (s, 1 H) 6.91 (d, J = 7.62 Hz, 1 H) 6.94-7.02 (m, 3 H) 7.08- 7.16 (m, 1 H) 7.38 (d, J = 8.20 Hz, 2 H) 7.60 (d, J = 8.20 Hz, 2 H).
Compound 2
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.58-1.76 (m, 2 H) 1.87- 2.06 (m, 2 H) 2.11 (s, 3 H) 2.14 (s, 3 H) 2.16 (s, 3 H) 2.28 (s, 3 H) 2.79-2.90 (m, 1 H) 2.96-3.14 (m, 3 H) 3.23- 3.28 (m, 1 H) 4.13 (s, 2 H) 4.27-4.35 (m, 2 H) 6.76 (d, J = 7.60 Hz, 1 H) 6.84 (s, 1 H) 6.90 (d, J = 7.60 Hz, 1 H) 6.90- 6.99 (m, 3 H) 7.09-7.17 (m, 1 H) 7.49 (d, J = 8.50 Hz, 2 H) 7.69 (d, J = 8.50 Hz, 2 H).
Starting
2-(3-methylphenyl)-3-(3,4-dimethylphenyl)propanoic
material
Intermediate
4-[3-(aminooxy)-2-(3-methylphenyl)propyl]-1,2-dimethylbenzene
1 H NMR (300 MHz, CD 3 OD) δ
1
ppm 2.13 (s, 3H) 2.14 (s,
3H) 2.25 (s, 3H) 2.64-2.82
(m, 1H) 2.90-2.99 (m, 1 H)
3.12 (m, 1 H) 3.79 (d, J = 6.74
Hz, 2 H) 6.74 (d, J = 6.88-6.95
(m, H) 6.80 (s, 1 H) 6.88-6.95
(m, 4H) 7.06-7.13 (m, 1 H).
Intermediate
4-{(1E)-N-[2-(3-methylphenyl)-3-(3,4-dimethylphenyl)
1 H NMR (300 MHz, CD 3 OD) δ
2
propoxy]ethanimidoyl}benzaldehyde
ppm 2.12-2.19 (m, 9 H) 2.29
(s, 3 H) 2.81-2.92 (m, 1 H)
2.98-3.08 (m, 1 H) 3.32-3.34
(m, 1 H) 4.36 (dd, J = 6.89,
1.61 Hz, 2 H) 6.75-6.86 (m, 2
H) 6.89-7.05 (m, 4 H) 7.10-
7.17 (m, 1 H) 7.90 (d, J = 8.20
Hz, 2 H) 7.81 (d, J = 8.20 Hz,
2H) 10.00 (s, 1 H).
Compound 3
1 NMR (300 MHz, CD 3 OD) δ ppm 2.09 (s, 3 H) 2.15 (s, 3 H) 2.16 (br. s., 3 H) 2.44 (t, J = 6.74 Hz, 2 H) 2.78-2.92 (m, 3 H) 2.98-3.07 (m, 1 H) 3.33-3.38 (m, 1 H) 3.84 (s, 2 H) 4.32 (m, 2 H) 6.75-6.79 (d, J = 7.62 Hz, 1 H) 6.84 (s, 1 H) 6.91 (d, J = 6.72, 1 H) 7.09- 7.23 (m, 4 H) 7.37 (d, J = 8.20 Hz, 2 H) 7.59 (d, J = 8.20 Hz, 2 H)
Compound 4
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.60-1.72 (m, 2 H) 1.91- 2.04 (m, 2 H) 2.09 (s, 3 H) 2.15 (s, 3 H) 2.16 (s, 3 H) 2.79- 2.88 (m, 1 H) 2.95-3.08 (m, 3 H) 3.33-3.38 (m, 1 H) 4.11 (s, 2 H) 4.25-4.35 (m, 2 H) 6.78 (d, J = 7.5 Hz, 1 H) 6.83 (m, 1 H) 6.93 (d, J = 7.50 Hz, 1 H) 7.09-7.25 (m, 4 H) 7.50 (d, J = 8.20 Hz, 2 H) 7.67 (d, J = 8.20 Hz, 2 H)
Starting
2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)propanoic acid
material
Intermediate
4-[3-(aminooxy)-2-(3-chlorophenyl)propyl]-1,2-dimethylbenzene
1 H NMR (300 MHz, CD 3 OD) δ
1
ppm 2.16 (s, 6 H) 2.61-2.84
(m, 1 H) 2.89-3.03 (m, 1 H)
3.19 (m, 1 H) 3.81 (d, J = 6.45
Hz, 2 H) 6.75 (d, J = 7.91 Hz, 1
H) 6.81 (s, 1 H) 6.92 (d,
J = 7.91 Hz, 1 H) 7.04-7.26
(m, 4 H)
Intermediate
4-{(1E)-N-[2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)
1 H NMR (300 MHz, CD 3 OD) δ
2
propoxy]ethanimidoyl}benzaldehyde
ppm 2.13 (s, 3 H) 2.15 (br. s.,
3 H) 2.16 (br. s., 3 H) 2.80-
2.90 (m, 1 H) 2.97-3.07 (m, 1
H) 3.33-3.42 (m, 1 H) 4.37
(m, 2 H) 6.79 (d, J = 7.62 Hz, 1
H) 6.84 (s, 1 H) 6.93 (d,
J = 7.62 Hz, 1 H) 7.09-7.26
(m, 4 H) 7.79 (d, J = 8.5 Hz, 2
H) 7.87 (d, J = 8.5 Hz, 2 H)
9.98 (s, 1 H)
Compound 5
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.66-1.71 (m, 2 H) 1.68 (s, 3 H) 1.88-2.06 (m, 2 H) 2.14 (s, 3 H) 2.16 (s, 3 H) 2.81- 2.92 (m, 1 H) 3.05 (t, J = 6.40 Hz, 2 H) 3.13-3.20 (m, 1 H) 3.71 (t, J = 7.91 Hz, 1 H) 4.11 (s, 2 H) 5.11 (s, 2 H) 6.68- 6.75 (d, J = 7.62 Hz, 1 H) 6.78 (s, 1 H) 6.88 (t, J = 7.62 Hz, 1 H) 7.01-7.28 (m, 4 H) 7.38 (d, J = 8.20 Hz, 2 H) 7.48 (t, J = 8.20 Hz, 2 H).
Starting
3-(3-chlorophenyl)-4-(3,4-dimethylphenyl)butan-2-one
material
Intermediate
4-[({[(1E)-2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)-1-
1 H NMR (300 MHz, CD 3 OD) δ
3
methylpropylidene]amino}oxy)ethyl]benzaldehyde
ppm 1.75 (s, 3 H) 2.13 (s, 3
H) 2.18 (s, 3 H) 2.83-2.93 (m,
1 H) 3.14-3.23 (m, 1 H) 3.76 (t,
J = 7.90 Hz, 1 H) 5.19 (s, 2 H)
6.703 (d, J = 7.62 Hz, 1 H) 6.81
(s, 1 H) 6.88 (d, J = 7.62 Hz, 1
H) 7.05-7.11 (m, 1 H) 7.14 (s,
1 H) 7.19-7.23 (m, 2 H) 7.44
(d, J = 8.50 Hz, 2 H) 7.85 (d,
J = 8.50 Hz, 2 H) 9.99 (s, 1 H).
Compound 6
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.57-1.68 (m, 2 H) 1.71 (s, 3 H) 1.87-2.06 (m, 2 H) 2.15 (s, 3 H) 2.17 (s, 3 H) 2.79- 2.93 (m, 1 H) 3.03 (t, J = 6.30 Hz, 2 H) 3.12-3.19 (m, 1 H) 3.75 (t, J = 7.91 Hz, 1 H) 4.12 (s, 2 H) 5.12 (s, 2 H) 6.64-6.76 (m, 4 H) 6.80-6.84 (m, 1 H) 6.88-6.96 (d, J = 7.62 Hz, 1 H) 7.40 (d, J = 8.30 Hz, 2 H) 7.47 (d, J = 8.30 Hz, 2 H).
Compound 7
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.71 (s, 3 H) 2.16 (s, 3 H) 2.18 (s, 3 H) 2.44 (t, J = 6.74 Hz, 2 H) 2.83-2.95 (m, 3 H) 3.18 (dd, J = 13.77, 7.62 Hz, 1 H) 3.76 (t, J = 7.90 Hz, 1 H) 3.87 (s, 2 H) 5.10 (s, 2 H) 6.67-6.80 (m, 4 H) 6.82 (s, 1 H) 6.92 (d, J = 7.62 Hz, 1 H) 7.33 (m, 4 H).
Starting
3-(3,5-difluorophenyl)-4-(3,4-dimethylphenyl)butan-2-one
material
Intermediate
4-[({[(1E)-2-(3,5-difluorophenyl)-3-(3,4-dimethylphenyl)-1-
1 H NMR (300 MHz, CD 3 OD) δ
3
methylpropylidene]amino}oxy)methyl]benzaldehyde
ppm 1.75 (s, 3 H) 2.13 (s, 3 H)
2.17 (s, 3 H) 2.83-2.93 (m, 1
H) 3.12-3.22 (m, 1 H) 3.79 (t,
J = 7.9 Hz, 1 H) 5.19 (s, 2 H)
6.69-6.84 (m, 5 H) 6.90 (d,
J = 7.62 Hz, 1 H) 7.44 (d,
J = 8.20 Hz, 2 H) 7.84 (d,
J = 8.20 Hz, 2 H) 9.98 (s, 1 H).
Compound 8
1 H NMR (600 MHz, CD 3 OD) δ ppm 1.57-1.70 (m, 2 H) 1.90- 1.99 (m, 2 H) 2.14-2.20 (m, 9 H) 2.98 (t, J = 6.31 Hz, 2 H) 3.27-3.32 (m, 1 H) 3.49 (dd, J = 14.06, 6.45 Hz, 1 H) 4.04 (s, 2 H) 5.30 (t, J = 6.31 Hz, 2 H) 6.94-7.02 (m, 2 H) 7.03- 7.16 (m, 4 H) 7.27-7.34 (m, 1 H) 7.47 (d, J = 8.22 Hz, 2 H) 7.61 (d, J = 8.22 Hz, 2 H)
Compound 9
1 H NMR (300 MHz, CD 3 OD) δ ppm 2.18 (s, 6 H) 2.20 (s, 3 H) 2.40 (t, J = 6.74 Hz, 2 H) 2.84 (t, J = 6.74 Hz, 2 H) 3.30 (m, 1 H) 3.51 (dd, J = 14.06, 6.45 Hz, 1 H) 3.80 (s, 2 H) 5.31 (t, J = 6.74 Hz, 1 H) 6.92-7.21 (m, 6 H) 7.32 (m, 1 H) 7.34 (d, J = 8.50 Hz, 2 H) 7.56 (d, J = 8.50 Hz, 2 H)
Compound 10
1 H NMR (600 MHz, CD 3 OD) δ ppm 1.62-1.73 (m, 2 H) 1.83-1.88 (m, 3 H) 1.90-1.99 (m., 2 H) 2.17-2.22 (m, 3 H) 2.25-2.29 (m, 3 H) 3.08 (t, J = 6.31 Hz, 2 H) 4.15 (s, 2 H) 4.90-5.08 (m, 3 H) 6.98-7.07 (m, 2 H) 7.10 (s, 1 H) 7.21- 7.40 (m, 6 H) 7.43-7.49 (m, 2 H)
Compound 11
1 H NMR (300 MHz, CD 3 OD) δ ppm 1.81-1.84 (m, 3 H) 2.15 (s, 3 H) 2.19 (s, 3 H) 2.43 (t, J = 6.74 Hz, 2 H) 2.87 (t, J = 6.74 Hz, 2 H) 3.81 (s, 2 H) 4.92-5.02 (m, 3 H) 6.93-7.12 (m, 3 H) 7.13-7.42 (m, 8 H)
Compound 12
1 H NMR (300 MHz, DMSO-d 6 ) δ ppm 1.67 (s, 3 H) 2.11 (d, J = 4.10 Hz, 6 H) 2.20-2.36 (m, 2 H) 2.59-2.83 (m, 2 H) 3.77 (br. s., 2 H) 5.08 (s, 2 H) 5.88 (s, 1 H) 6.62-6.78 (m, 1 H) 6.84 (d, J = 2.64 Hz, 1 H) 6.96 (d, J = 8.20 Hz, 1 H) 7.22- 7.35 (m, 5 H) 7.36-7.43 (m, 3 H).
Compound 13
1 H NMR (300 MHz, CDCl 3 ) δ ppm 1.56-1.77 (m, 5 H) 1.94- 2.09 (m, 2 H) 2.14 (d, J = 4.98 Hz, 6 H) 2.73 (br. s., 2 H) 3.97 (br. s., 2 H) 5.02 (s, 2 H) 5.67 (s, 1 H) 6.65 (dd, J = 8.20, 2.64 Hz, 1 H) 6.71-6.81 (m, 1 H) 6.93 (d, J = 8.20 Hz, 1 H) 7.12- 7.33 (m, 6 H) 7.36-7.53 (m, 3 H).
Compound 14
1 H NMR (300 MHz, DMSO-d 6 ) δ ppm 2.05 (s, 3 H) 2.06-2.11 (m, 6 H) 2.29 (t, J = 6.74 Hz, 2 H) 2.71 (t, J = 6.74 Hz, 2 H) 3.77 (br. s., 2 H) 4.34 (dd, J = 4.40 Hz, 1 H) 4.44 (dd, J = 7.00 Hz, 1 H) 5.57-5.68 (m, 1 H) 6.55-6.67 (m, 1 H) 6.76 (d, J = 2.64 Hz, 1 H) 6.91 (d, J = 8.20 Hz, 1 H) 7.28-7.46 (m, 6 H) 7.50 (br. s., 1 H) 7.55- 7.65 (m, 2 H)
Compound 15
1 H NMR (300 MHz, DMSO-d 6 ) δ ppm 1.66-1.87 (m, 2 H) 1.95-2.12 (m, 9 H) 2.71 (br. s., 2 H) 3.06-3.23 (m, 2 H) 3.85 (br. s., 2 H) 4.20-4.36 (m, 1 H) 4.39-4.53 (m, 1 H) 5.56-5.67 (m, 1 H) 6.51- 6.66 (m, 1 H) 6.74 (d, J = 2.05 Hz, 1 H) 6.88 (d, J = 8.20 Hz, 1 H) 7.22-7.44 (m, 4 H) 7.49 (d, J = 4.10 Hz, 3 H) 7.52-7.66 (m, 2 H).
Biological Data
Compounds were synthesized and tested for S1P1 activity using the GTP γ 35 S binding assay. These compounds may be assessed for their ability to activate or block activation of the human S1P1 receptor in cells stably expressing the S1P1 receptor.
GTP γ 35 S binding was measured in the medium containing (mM) HEPES 25, pH 7.4, MgCl 2 10, NaCl 100, dithitothreitol 0.5, digitonin 0.003%, 0.2 nM GTP γ 35 S, and 5 μg membrane protein in a volume of 150 μl. Test compounds were included in the concentration range from 0.08 to 5,000 nM unless indicated otherwise. Membranes were incubated with 100 μM 5′-adenylylimmidodiphosphate for 30 min, and subsequently with 10 μM GDP for 10 min on ice. Drug solutions and membrane were mixed, and then reactions were initiated by adding GTP γ 35 S and continued for 30 min at 25° C. Reaction mixtures were filtered over Whatman GF/B filters under vacuum, and washed three times with 3 mL of ice-cold buffer (HEPES 25, pH7.4, MgCl 2 10 and NaCl 100). Filters were dried and mixed with scintillant, and counted for 35 S activity using a β-counter. Agonist-induced GTP γ 35 S binding was obtained by subtracting that in the absence of agonist. Binding data were analyzed using a non-linear regression method. In case of antagonist assay, the reaction mixture contained 10 nM S1P in the presence of test antagonist at concentrations ranging from 0.08 to 5000 nM.
Table 2 shows activity potency: S1P1 receptor from GTP γ 35 S: nM, (EC 50 ).
Activity Potency:
S1P1 receptor from GTP γ 35 S: nM, (EC 50 ),
TABLE 2
S1P1
IUPAC name
EC 50 (nM)
3-({4-[({[(1E)-2-(3,5-difluorophenyl)-3-(3,4-dimethylphenyl)-
6.8
1-methylpropylidene]amino}oxy)methyl]ben-
zyl}amino)propanoic acid
[3-({4-[({[(1E)-2-(3,5-difluorophenyl)-3-(3,4-dimethylphenyl)-
0.88
1-methylpropylidene]amino}oxy)methyl]ben-
zyl}amino)propyl]phosphonic acid
[3-({4-[({[(1E)-2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)-1-
2.2
methylpropylidene]amino}oxy)methyl]ben-
zyl}amino)propyl]phosphonic acid
3-[(4-{(1E)-N-[3-(3,4-dimethylphenyl)-2-(3-methyl-
43.2
phenyl)propoxy]ethanimidoyl}benzyl)amino]propanoic acid
3-[(4-{(1E)-N-[2-(3-chlorophenyl)-3-(3,4-dimethyl-
15.6
phenyl)propoxy]ethanimidoyl}benzyl)amino]propanoic acid
{3-[(4-{(1E)-N-[2-(3-chlorophenyl)-3-(3,4-dimethylphenyl)
3.51
propoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid
{3-[(4-{(1E)-N-[3-(3,4-dimethylphenyl)-2-(3-methylphenyl)
23.4
propoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid
{3-[(4-{[({(1E)-2-(3-chlorophenyl)-2-[(3,4-dimethyl-
8.34
phenyl)thio]-1-methylethylidene}amino)oxy]methyl}ben-
zyl)amino]propyl}phosphonic acid
{3-[(4-{(1E)-N-[2-(3-chlorophenyl)-2-(3,4-dimethylphenoxy)
11.42
ethoxy]ethanimidoyl}benzyl)amino]propyl}phosphonic acid
3-[(4-{(1E)-N-[2-(3-chlorophenyl)-2-(3,4-dimethyl-
215.56
phenoxy)ethoxy]ethanimidoyl}benzyl)amino]propanoic acid
[3-({4-[(1E)-N-{2-[(3,4-dimethylphenyl)sulfonyl]-2-(3-fluoro-
51.81
phenyl)ethoxy}ethanimidoyl]benzyl}amino)propyl]phosphonic
acid
|
The present invention relates to novel oxime derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals as modulators of sphingosine-1-phosphate receptors.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to electromechanical timers used in appliance functions and in particular to a dryer timer that incorporates a voltage dropping resistor that enables the timer motor to be operated at two widely differing voltages.
2. Description of the Prior Art
Since automatic clothes dryers were first made, electromechanical timers have been used to time their cycles. These timers are in general similar to the timers used in other appliances, such as clothes washers, and operate on standard 120 VAC. For many years now it has been state-of-the-art in electric clothes dryers to power the motor through the heater during the permanent press cycle. Since the heater operates on 240 VAC, it is necessary to insert a voltage dropping resistor in the circuit between the heater and the motor; otherwise the motor would quickly burn out. Clearly, such a voltage dropping resistor must be able to dissipate large amounts of heat if it is to drop the voltage 120 volts. For this reason, up to now such voltage dropping resistors have been mounted on the interior wall of the dryer cabinet, which acts as a heat sink. The resistor is then connected by a wiring harness to the timer which is mounted elsewhere in the cabinet.
SUMMARY OF THE INVENTION
It is the object of the invention to provide a dryer timer in which the motor voltage dropping resistor is carried on the timer.
It is a further object of the invention to provide a dryer timer that provides the above object and that overcomes one or more disadvantages of the prior art and at the same time is less expensive to manufacture than previous timers and voltage dropping resistors for dryers.
The invention provides a dryer timer comprising: a housing; a motor; cam means driven by said motor and carried in the housing; heat dissipating means carried on the housing; a leadless resistor in thermal contact with the heat dissipating means; electrical switch means carried in the housing and responsive to the cam means for causing electrical current passing through the motor to pass through the resistor when in a first position and to pass through another circuit, not including said resistor, when in a second position; an electrical feed-through connected to the switch, passing through the housing, and electrically connected to the resistor; and an electrical terminal means carried on the housing for connecting the resistor to the heater circuit of a dryer. Preferably at least a portion of the heat dissipating means is integrally formed with the terminal. Preferably, the heat dissipating means further includes a means for clasping the resistor between the portion integrally formed with the terminal and the feed-through. Preferably, the resistor comprises a slug having a pair of parallel, substantially flat sides. Preferably the feed-through comprises a means for attaching a portion of the heat dissipating means to the housing. Preferably the feed-through comprises a rivet. Preferably the resistor comprises an organic resistor or inorganic/ceramic resistor.
The dryer timer according to the invention has been found to eliminate many errors in assembly in prior art dryers. For example, there are many terminals to be connected by wiring harnesses in dryers, and often the wrong terminals are connected. Or since inserting the voltage dropping resistor is a separate dryer assembly step, it is sometimes missed. Both the above errors often result in the timer motor burning up quickly which results in warranty repair calls and customer ill will. The timer according to the invention not only solves these serious problems but also provides a less expensive dryer. In addition, the resistor-dissipator system according to the invention lends itself to an automated assembly procedure which is much more reliable and accurate than the assembly methods associated with the prior art resistors. Numerous other features, objects, and advantages of the invention will become apparent from the following detailed description when read in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block circuit diagram showing a clothes dryer electrical circuit including a preferred embodiment of the circuit of the timer according to the invention;
FIG. 2 is a plan view of a portion of the back of a timer housing showing a preferred embodiment of the mounting of the voltage dropping resistor according to the invention;
FIG. 3 is a side view of the portion of the timer of FIG. 2.
FIG. 4 is an alternative preferred embodiment of the clothes dryer circuit, including an alternative preferred timer circuit according to the invention;
FIG. 5 is an alternative embodiment of the mounting of the voltage dropping resistor on the back of a timer according to the invention;
FIG. 6 is a side view of a portion of the timer housing of FIG. 5;
FIG. 7 is a side view of a portion of a timer showing another preferred embodiment of the mounting of the voltage dropping resistor on the back of the timer;
FIG. 8 is a view looking down on the mounting of FIG. 7 with the contact plate over the resistor removed to show the interior structure of the mounting;
FIGS. 9A and 9B show side and top views respectively of the combination terminal and lower portion of the heat dissipating means of the timer of FIG. 7;
FIG. 10A and 10B show side and top views respectively of the heat-dissipation plate connecting the feed-through and the resistor of FIG. 7; and
FIGS. 11A and 11B show side and top views respectively of the voltage dropping resistor of the embodiment of FIG. 7.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The timer according to the invention will be more easily understood when its use is understood, and thus we shall begin by first describing a typical use, making reference to FIG. 1, which shows a block circuit diagram of a preferred embodiment of the invention within the circuit of a conventional automatic electric clothes dryer having a permanent press cycle. It is understood that the use in a dryer and the embodiments of the inventions disclosed are exemplary and are not intended to be limiting of the invention. The conventional dryer shown in FIG. 1 is operated by placing wet clothes in an airtight drum that is made to rotate about a horizontal plane by motor 10. The speed of the drum is sufficient to lift the clothes 3/4 the way up the side, and then the clothes fall back to the bottom. A blower pulls room air into the dryer and a heater 11 heats it. This heated air is forced through the tumbling clothes and out the exhaust stack. A thermostat 12 is installed in the exhaust stack that senses the temperature of the exhaust air leaving the drum and controls the power to the heater to dry the clothes according to a programmed drying cycle determined by the timer cam means 14 which is mechanically driven by the timer motor 16 and mechanically drives the timer switches 18, 19, 20, 21 and 22. In a timed cycle switch 20 is closed downward and switch 22 is closed for the entire cycle so that the drum and timer cam rotate throughout the cycle, and switch 18 is closed for nearly the entire cycle, opening near the end to allow the clothes to cool down. In the permanent press cycle switch 22 is open and the drum rotates the entire cycle while the thermostat 12 turns the heater on and off; the time required to dry a load is determined by the size and wetness of the load. To properly dry any size load and any moisture content, it is desirable to connect the timer motor 16 in parallel with the control thermostat 12 and in series with the heater 11. This results in the timer motor 16 being off whenever the thermostat 12 is closed and the heater 11 is on, and the timer motor 16 being on whenever the thermostat 12 is off. Thus, the amount of drying time required to dry the clothes is determined by the thermostat 12. When the clothes are dry, the thermostat 12 opens and the timer motor 16 runs to the end of cycle and shuts off the dryer. To assure a proper cool down, switch 22 closes for the last 15 minutes of the cycle. As a result, the timer motor 16 in such a dryer must operate off of 120 V power sometimes and sometimes off of 240 volt power. This is accomplished by inserting a voltage dropping resistor 25 between the heater 11 and the timer motor 16.
In FIGS. 2 and 3, the mounting of the resistor 25 on the back 29 of timer housing 30 and its connection to electrical switch means 33 is shown. These FIGS. can best be oriented with FIG. 1 by tracing the connections of FIG. 1 on FIG. 4. The blade 34 of timer 22 is connected via feed-through 36 to terminal 39 and to resistor 25. Terminal 39 is connected to motor 16 via a standard electrical connector and wire (not shown in FIG. 4). The resistor 25 is leadless and is connected via terminal strap 41 to terminal 42 which is connected to the heater circuit in the dryer by a conventional electrical connector and wiring harness (not shown in FIG. 4). Turning now to a more detailed description of FIGS. 2 and 3, a terminal means 40, a heat dissipating means 50, a feed-through 36 and a portion of a switch means 33 are shown. Terminal means 40 is preferably a single piece of metal bent at 43A, 43B and 43C, lanced at 44, and having openings 46 and 47. One side is bent up at 48 to form a flange 49 which fits over a small strap 51 in the conventional housing 30. Opening 46 is generally circular with a notch 52. Shoulders 53 and 54 on terminal 42 act as a stop for a conventional electrical connector. The end 45 of terminal 42 is tapered to make connection easier. All corners, such as 56, are trimmed to prevent sharp edges to reduce the chance of arcing. Heat dissipation means 50 includes a member 55 having a plate 56 with four turned up flanges 57, 58, 59 and 61, a turned up terminal 39, and an opening 62. The end 64 of terminal 39 is tapered. Dissipation means 50 also includes at least end portion 65 of terminal means 40. This embodiment of the timer also includes another terminal 67 which is mounted on an insulating post 68 formed in housing 30. Post 68 is generally circular to fit into opening 46 and includes a key which fits into notch 52. The assembly is manufactured as follows: Member 55 and blade 34 are attached to the housing and electrically connected by feed-through 36, which is a conventional conductive rivet and which passes through bore 71 in housing body 30. Resistor 25 is placed in a locating pen formed by the four posts 57, 58, 59 and 60 of member 55. Terminal means 40 is then placed on housing 30 with opening 46 fitting over post 68 with key 69 fitting into notch 52. Rivet 74 is passed through opening 47 in terminal means 40 and bore 75 in housing body 30 and swagged to fasten the terminal means 40 to the housing. Resistor 25 is clasped between the end 65 of terminal means 40 and the head 72 of feed-through 36. Terminal 67 is then fastened to the housing and another timer switch 77 by rivet 79.
Preferably resistor 25 is about 3/8 inches in diameter by 1/8 inches thick and its contact surfaces are coated with brass. Flanges 57, 58, 59 and 61 are about 0.110 inches high by 0.09 inches wide and are spaced about 0.210 inches from the center of plate 56. Strap 41 is about 1.5 inches long and is about 5/16 inches wide near the terminal end and over the resistor 25 and about 1/4 inches wide near the area of bends 43A and 43B, while about 0.5 inches wide in the area of flange 49. Post 68 is about 5/16 inches in diameter by 1/8 inches high. Other dimensions are derivable from those above and the drawings, or are conventional.
FIG. 4 shows an alternative preferred embodiment of a clothes dryer circuit including an alternative timer circuit. In this embodiment the connection 67 of FIG. 4 is made to the terminal corresponding to 67 of FIG. 3 and the switch 22 is replaced with a single-pole-double-throw switch 80. The motor connection is made on the "T" terminal 81 (not shown in FIGS. 3 and 4 but shown in FIG. 5) which connects to the blade of timer 80, a common timer circuit. This embodiment is presented to indicate that the invention is not limited to any particular dryer or timer circuit.
Turning to FIGS. 5 and 6, another preferred embodiment of a timer according to the invention is shown, in which the voltage dropping resistor 125 is connected to what is known as the "fifth circuit" of a standard dryer timer. Again the voltage dropping resistor is leadless and is clasped between feed-through 132 and a portion 142 of terminal means 134. Terminal means 134 is preferably of one piece construction and includes a strap portion 136, a terminal portion 137, two flanges 139 and 140 and a dimple 142. Terminal 137 has shoulders 146 and 147 which act as a stop for the connector to the dryer, and its end 148 is tapered for ease of connection. The corners, such as 149, of strap 136 are trimmed to remove the sharp corners. Strap 136 also includes a hole 144. A heat dissipation means 130 includes a member 31 having a plate portion 151, dimples 153 and 155, and three turned up flanges 156, 158 and 159. Feed-through 132 comprises a rivet 132. Housing 133 is a conventional timer housing that includes a molded seat 163 that is raised above the timer back 129. A bore 165 is formed in the seat 163. Terminal member 134 sits on seat 163 and is held in place by rivet 166 which passes through bore 165 and hole 144. Flange 139 abuts the side 141 of housing 133 to locate terminal member 134. Resistor 125 is located and clasped by flange 140 of terminal member 134, flanges 156, 158 and 159 of heat dissipation member 131, dimples 142, 153, 155 and the head 168 of rivet 132. The two dimples 153 and 155 and the head of rivet 168 form a three-point seat for resistor 125 and, with dimple 142, ensure good electrical connections to resistor 125. Heat dissipation means 130 primarily includes flanges 156, 158, 159 of heat dissipation member 131, strap 136 and flange 140 of terminal means 134, but also includes the other surfaces of the member 131 and terminal means 134, which together form a relatively large area of good heat conducting material to dissipate the heat produced in resistor 125. Heat dissipation member 131 is held in place by rivet 132 which feeds through bore 170 in housing 133 to also fasten blade 172 of a timer switch to the housing. Preferably resistor 125 is about 3/8 inches in diameter and 1/8 inches thick and its contact surfaces are coated with brass. Flanges 156, 158 and 159 are preferably about 0.110 inches high and 0.09 inches wide and are spaced about 0.210 inches from the center of the plate 151. Strap 136 is about 0.850 inches long and about 0.340 inches wide. Dimple 142 is about 0.150 inches in diameter by 0.025 inches high and placed about 0.62 inches from terminal 137. Terminal 137 is about 0.45 inches high by a quarter inch wide. Flanges 139 and 140 are about 0.10 inches long by 0.08 inches wide. Other dimensions are derivable from those given above and the drawings, or are conventional. This embodiment may be used most easily in combination with the circuit of FIG. 4 but also may be used with other circuits as well.
Turning now to FIGS. 7 through 11B, another preferred embodiment of the mounting of the voltage dropping resistor 200 is shown. The mounting comprises a top plate 202, a bottom-plate-terminal combination 204, a rivet feed-through 207, and a post 208 integrally formed in housing body 209. The voltage dropping resistor 200 is leadless and is clasped between the head 210 of feed-through 207 and a portion of terminal means 204. Terminal means 204 is shown in FIGS. 9A and 9B. It includes a terminal portion 211, a plate portion 212 and a pair of turned-up flanges 214 and 215. Plate portion 212 has an opening 217 in it in the form of a circle with a pair of tabs 218 and 219 extending into the circle. The end 221 of plate 212 is in the form of an arc of a circle. Top plate 202 is shown in FIGS. 10A and 10B. It is generally rectangular in shape with sides 222 and 223 formed in an arc of a circle and having a pair of bent-down flanges 224 and 225. A circular opening 228 is formed in the plate nearer flange 225. Resistor 200 is a hollowed out cylinder with cylindrical bore 232 and flats 233 and 234 along opposing sides of the cylinder parallel to the cylindrical axis. The ends are covered with thin layers 237 and 238 of brass. Housing body 209 is integrally molded with a slightly raised seat 240 and a post 208 formed on the seat. Post 208 is circular with a pair of notches 243 and 244 and a cylindrical bore 246 passes through it. The resistor 200 is mounted as follows. Opening 217 in terminal means 204 is placed over post 208 with tabs 218 and 219 fitting into notches 243 and 244 respectively. Resistor 200 is placed over post 208 with bore 232 fitting snugly on the post and with the flat sides 233 and 234 fitting snugly between flanges 214 and 215 respectively on terminal means 204. Plate 202 is placed over the resistor 200 with flanges 224 and 225 fitting snugly over flat sides 233 and 234 respectively. Rivet 207 is placed through opening 228 in top plate 202 and passes through bore 246 in housing body 209. A switch part 249 is placed over the end of rivet and the end is clinched to hold the mounting assembly together and to housing body 209. In this embodiment dissipating means 255 comprises plate 202 and terminal means 204 as well as rivet 207 and the metal parts connected to them. Preferably resistor 200 is 0.450 inches high, 0.710 inches in diameter with a 0.360 diameter bore 232 and 0.638 inches between flats 233 and 234. Flanges 224 and 225 of plate 202 are about 0.150 inches high and 0.550 inches wide and opening 228 is about 0.130 inches in diameter. Opening 217 is about 0.355 inches in diameter with tabs 218 and 219 about 1/16 inches wide. Flanges 214 and 215 are about 0.150 inches high and 0.550 inches wide. Terminal 211 is about 0.425 inches long from the bend 258 and about 1/4 inches wide. Terminal means 204 and plate 202 are about 0.032 inches thick. Seat 240 is about 0.1 inches high or sufficient to provide clearance between terminal means 204 and its neighbor terminal 280. Other dimensions are obtainable from those given and the drawings, or are conventional.
The housing 30 is preferably molded in one piece from phenolic or other suitable plastic although seat 163 and post 68 could be formed of separate pieces of phenolic or other suitable plastic. The terminal means 40 and 134 and heat dissipation members 55 and 131 are preferably made of 0.032 inch thick Olin Corporation Alloy No. 260 brass or similar material. Terminal means 204 and plate 202 are preferably made of 0.032 inch thick Olin Corporation Alloy No. 110 copper. The resistors 25 and 125 are preferably carbonaceous organic resistors having a brass coating on the contact surfaces although other leadless resistors may be used.
It is a feature of the invention that the voltage dropping resistor is a leadless resistor. Further it is a feature of the invention that the heat dissipating means 50, 130, and 255 are formed from the feed-through, terminal straps and terminals which also perform other conventional functions in the timer. This combination permits the resistor and its connection to dissipate the relatively large heat associated with the voltage dropping function and still be price competitive with the prior art. The heat dissipation parts are raised 50° to 60° C. over ambient temperatures by the heat dissipated, and thus conventional resistors and resistor connections are not adequate.
Another feature of the invention is that the locations of the voltage dropping resistors 25, 125 and 200 are much closer to the terminals which are to be connected to the wiring harness. This makes it easier to view the terminals and resistor all at once and to make sure that the resistor is in place and the harness is connected to the proper terminal in the process of assembling the dryer. This eliminates many of the costly mistakes associated with the prior art.
A further feature of the invention is that the resistors 25, 125, and 200 are of the same order of size as the timer and the parts of which it is composed and thus the whole assembly lends itself to be automatically assembled with the usual automated assembly equipment available to assemble timers. This further ensures against error and lower costs.
There has been described a novel dryer timer that incorporates the voltage dropping resistor that allows a timer motor to be operated at two widely differing voltages into the timer and has numerous other features and advantages. It is evident that those skilled in the art may now make many uses and modifications of the specific embodiment described without departing from the inventive concepts. For example, the invention can be applied in any timer in which an exterior resistor is added for voltage dropping purposes although it is particularly useful when large energies need to be dissipated. Other types of materials or other timer circuits may be employed. Consequently, the invention is to be construed as embracing each and every novel feature and novel combination of features present in the timer described.
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A dryer timer includes a housing and a motor and a cam assembly carried in the housing. A switch in the housing is responsive to the cam to switch the motor between a 120 VAC standard timer circuit and a 240 VAC dryer heater circuit. A leadless voltage dropping resistor in the 240 VAC circuit is mounted on the exterior of the housing clasped between the feed-through to the switch and a terminal strap connected to the timer terminal which connects to the dryer heater circuit. A flanged member connected to the feed-through and the terminal strap engaged the flat surfaces of the disk-shaped leadless voltage dropping resistor to dissipate the heat it produces.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a radiation-sensitive resin composition containing an alkali-soluble resin, and more particularly to a radiation-sensitive resin composition which is sensitive to such radiations as ultraviolet rays, far ultraviolet rays, X-rays, electron beams, molecular beams, gamma-rays, synchrotron radiations, proton beams, etc. and suitable for use as a photoresist for fabrication of highly integrated circuits.
2. Description of the Prior Art
Positive type photoresists are widely used in the manufacture of integrated circuits, because they give photoresist patterns with high resolution. With the recent trend toward integrated circuits of higher integration, however, there has been a growing demand for a positive type photoresist from which a photoresist pattern with a further enhanced resolution can be formed. That is, in the formation of a fine photoresist pattern by use of a positive type photoresist, it is required that the development of a latent image, formed by exposure, with a developing solution consisting of an aqueous alkaline solution should proceed rapidly to the area where the exposed portion adjoin a wafer (namely, the base portion of the pattern).
However, the conventional positive type photoresists have a developability problem in that when the interval of pattern elements of the photoresist pattern to be formed is 0.8 μm or below, an undeveloped residue called "scum" is liable to be left upon development.
In response to the increasing integration of integrated circuits, furthermore, the etching method for wafers has been changing from the conventional wet etching, which involves heavier side etching, to the dry etching with less side etching. In the dry etching, the photoresist pattern should not change during etching; therefore, the photoresist should have good heat resistance.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a radiation-sensitive resin composition suitable for use as a positive type photoresist which has such excellent developability as to inhibit effectively the generation of scum in the formation of a photoresist pattern, has high sensitivity and which is excellent in heat resistance and remained thickness ratio upon development.
According to the present invention, there is provided a radiation-sensitive resin composition containing an alkali-soluble resin, comprising a compound having the following general formula [I]: ##STR2## wherein R 1 , R 2 , R 3 and R 4 may be the same or different and each of R 1 to R 4 may comprise two or more different groups, and R 1 to R 4 are each a substituted or unsubstituted alkyl group, a substituted or unsubstituted aryl group or an OD group, wherein D is a hydrogen atom or an organic group containing a 1,2-quinonediazide group, at least one of R 1 , R 2 and R 4 containing at least one OD group; R 5 and R 6 are each a hydrogen atom or a substituted or unsubstituted alkyl group; a, b and d are each an integer of from 0 to 5, provided at least one of a, b and d is a positive integer; and c is an integer of from 0 to 4.
The radiation-sensitive resin composition of the present invention can be used suitably as a positive type photoresist which has excellent developability such as to inhibit effectively the generation of scum in the formation of a photoresist pattern, has high sensitivity and is excellent in heat resistance and remained thickness ratio upon development.
DETAILED DESCRIPTION OF THE INVENTION
Alkali-soluble resin
The alkali-soluble resin for use in the present invention (the resin will be hereinafter referred to as "resin (A)") includes, for example, novolak resins, resol resins, polyvinylphenol and derivatives thereof, styrene-maleic anhydride copolymers, polyvinyl hydroxybenzoate, carboxyl group-containing methacrylic resins, etc., of which particularly preferred are novolak resins. Of the novolak resins, those obtained by polycondensation of a phenol having the following general formula [II]: ##STR3## wherein n is an integer of from 1 to 3, with an aldehyde, are especially preferable.
Preferred examples of the phenol for preparation of the novolak resin include o-cresol, m-cresol, p-cresol, 2,3-xylenol, 2,4-xylenol, 2,5-xylenol, 2,6-xylenol, 3,4-xylenol, 3,5-xylenol, 2,3,4-trimethylphenol, 2,3,5-trimethylphenol, 3,4,5-trimethylphenol, and so on, of which preferred are o-cresol, m-cresol, p-cresol, 2,5-xylenol, 3,5-xylenol and 2,3,5-trimethylphenol. The phenols may be used either singly or in combination of one or more.
The aldehydes for polycondensation with the above phenols include, for example, formaldehyde, trioxane, paraformaldehyde, benzaldehyde, acetaldehyde, propylaldehyde, phenylacetaldehyde, α-phenylpropylaldehyde, β-phenylpropylaldehyde, o-hydroxybenzaldehyde, m-hydroxybenzaldehyde, p-hydroxybenzaldehyde, o-chlorobenzaldehyde, m-chlorobenzaldehyde, p-chlorobenzaldehyde, o-nitrobenzaldehyde, m-nitrobenzaldehyde, p-nitrobenzaldehyde, o-methylbenzaldehyde, m-methylbenzaldehyde, p-methylbenzaldehyde, p-ethylbenzaldehyde, p-n-butylbenzaldehyde, furfural, etc., with formaldehyde being particularly preferable. These aldehydes may be used either singly or in combination of two or more.
The aldehyde is used preferably in an amount of from 0.7 to 3 moles, more preferably from 0.8 to 1.5 moles, per mole of the phenol.
In the polycondensation of the phenol and the aldehyde, generally, an acidic catalyst is used. The acidic catalysts usable include, for example, inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid, etc., and organic acids such as formic acid, oxalic acid, acetic acid, etc. The amount of the acidic catalysts used is ordinarily from 1×10 -5 to 5×10 -1 mole per mole of the phenol.
In the polycondensation, generally, water is used as a reaction medium. However, where the phenol used for the polycondensation is insoluble in the aqueous solution of the aldehyde and therefore the reactants form a heterogeneous system from the beginning of the reaction, a hydrophilic solvent may also be used as the reaction medium. The hydrophilic solvents usable in such a case include, for example, alcohols such as methanol, ethanol, propanol, butanol, etc., and cyclic ethers such as tetrahydrofuran, dioxane, etc. The amount of the reaction medium is ordinarily from 20 to 1000 parts by weight per 100 parts by weight of the reactants.
The polycondensation temperature can be controlled suitably according to the reactivity of the reactants, and is generally from 10° to 200° C., preferably from 70° to 130° C.
The polycondensation may be carried out, for example, by a method in which the phenol, aldehyde, acidic catalyst and so on are placed in a reaction vessel at a time, or a method in which the phenol, aldehyde and so on are added gradually as the reaction proceeds.
After the polycondensation is finished, the temperature of the reaction system is generally raised to a temperature of from 130° to 230° C., in order to remove the unreacted reactants, the acidic catalyst, the reaction medium, etc. from the reaction system. Then, volatile components are distilled off under a reduced pressure, for instance from about 20 to 50 mmHg, and the resin (A) formed is recovered.
The weight average molecular weight in terms of polystyrene (hereinafter referred to as "Mw") of the resin (A) used in the present invention is preferably from 2,000 to 20,000, a more preferable range being from 3,000 to 15,000. When Mw exceeds 20,000, uniform application of the composition of the invention to a wafer may become difficult and, further, the developability and sensitivity of the composition are apt to be lowered. When Mw is below 2,000, on the other hand, the composition tends to be poor in heat resistance of the resist pattern to be obtained.
The resin (A) with a high Mw value can be obtained by dissolving the resin obtained as above in a good solvent such as ethyl cellosolve acetate, dioxane, methanol, ethyl acetate, etc., then adding a poor solvent such as water, n-hexane, n-heptane, etc. thereto, separating a resin solution layer thus formed, and recovering the resin (A) having a high molecular weight.
Compound (A) of the general formula [I]
The composition according to the present invention contains at least one of the compounds having the aforementioned general formula [I], namely: ##STR4##
The compound of the general formula [I] includes a compound represented by the general formula [I] wherein all of the D's are hydrogen atoms (hereinafter referred to as "compound (A)" and derivatives of the Compound (A) represented by the general formula [I] wherein at least one of the D's is an organic group containing a 1,2-quinonediazide group (hereinafter referred to as "compound (B)").
In the general formula [I], the groups R 1 to R 4 are each a substituted or unsubstituted alkyl group, a substituted or unsubstituted aryl group or an OD group, wherein D is a hydrogen atom or an organic group containing a 1,2-quinonediazide group. The substituted or unsubstituted alkyl group includes, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, t-butyl, cyclohexyl, hydroxymethyl, chloromethyl, bromomethyl, 2-chloromethyl, trimethylsilylmethyl, benzyl and cumyl groups, etc., of which preferred are methyl, ethyl, hydroxymethyl and the like. The substituted or unsubstituted aryl group includes, for example, phenyl, 1-naphthyl, 2-naphthyl, 4-hydroxyphenyl, 4-trimethylsiloxyphenyl, 4-methoxyphenyl and 4-acetylphenyl groups, etc., of which preferred are phenyl, 4-hydroxylphenyl and the like.
The organic group containing a 1,2-quinonediazide group includes, for example, 1,2-benzoquinonediazide-4-sulfonyl group, 1,2-naphthoquinonediazide-5-sulfonyl group, 1,2-naphthoquinonediazide-4-sulfonyl group, 2,1-naphthoquinonediazide-5-sulfonyl group, 2,1-naphthoquinonediazide-4-sulfonyl group and so on, of which preferred are the 1,2-naphthoquinonediazide-4-sulfonyl and 1,2-naphthoquinonediazide-5-sulfonyl groups and the like.
The groups R 1 to R 4 bonded to respective benzene rings may be the same or different and each of R 1 to R 4 may comprise two or more different groups, and at least one of the groups R 1 , R 2 and R 4 contains at least one OD group.
The groups R 5 and R 6 are each a hydrogen atom or a substituted or unsubstituted alkyl group. Examples of the substituted or unsubstituted alkyl group include methyl, ethyl, n-propyl, isopropyl, n-butyl, t-butyl, cyclohexyl, hydroxymethyl, chloromethyl, bromomethyl, 2-chloromethyl, trimethylsilylmethyl, benzyl and cumyl groups, etc., of which preferred are methyl, ethyl and hydroxymethyl groups and the like.
Specific examples of the compound (A) having the general formula (I) (the compound (A) corresponds to the case where at least one of the aforementioned OD groups is the hydroxyl group) include the followings: ##STR5##
The aforementioned compound (A) can be obtained by condensation of a substituted or unsubstituted phenol with a substituted acetophenone in the presence of an acidic catalyst, as for instance disclosed in German Patent No. 1,930,333 (Federal Republic). The reaction product is obtained generally as an oily mixture, which may be purified by recrystallization, for instance.
The compound (B) is a compound obtained by substituting part or the whole of the hydroxyl groups contained in the compound (A) by an organic group containing a 1,2-quinonediazide group. The compound (B) can be obtained, for example, by esterification of the aforementioned compound (A) with a 1,2-naphthoquinonediazidesulfonyl halide such as 1,2-naphthoquinonediazide-4-sulfonyl chloride, 1,2-naphthoquinonediazide-5-sulfonyl chloride, etc.
In the present invention, in order that the developability-improving effect of the compound (B) may be attained satisfactorily, the average percentage of condensation upon the esterification, defined as [(the number of phenolic hydroxyl groups esterified)/(the number of phenolic hydroxyl groups before reaction)]×100 and hereinafter referred to as "average condensation degree", is generally 100% or below, preferably 50% or below, and more preferably 30% or below.
In the present invention, the compound (A) or compound (B) as mentioned above is used preferably in an amount of from 0.5 to 90 parts by weight, more preferably from 2 to 50 parts by weight, per 100 parts by weight of the resin (A).
1,2-Quinone diazide compound
In the present invention, where the compound (B) is not used, it is necessary to use a 1,2-quinone diazide compound other than the compound (B). Where the compound (B) is used, a 1,2-quinone diazide compound other than the compound (B) can be used in the composition of the invention. Such 1,2-quinone diazide compounds include, for example, 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-5-sulfonates, etc. More specific examples of the usable 1,2-quinone diazide compounds are 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of (poly)hydroxybenzenes such as p-cresol, resorcinol, pyrogallol, phloroglucinol, etc.; 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of (poly)hydroxyphenyl alkyl ketones or (poly)hydroxyphenyl aryl ketones such as 2,4-dihydroxyphenyl propyl ketone, 2,4-dihydroxyphenyl n-hexyl ketone, 2,4-dihydroxybenzophenone, 2,3,4-trihydroxyphenyl n-hexyl ketone, 2,3,4-trihydroxybenzophenone, 2,4,6-trihydroxybenzophenone, 2,3,4,4'-tetrahydroxybenzophenone, 2,2',3,4'-tetrahydroxybenzophenone, 3'-methoxy-2,3,4,4'-tetrahydroxybenzophenone, 2,2',4,4'-tetrahydroxybenzophenone, 2,2',3,4,6'-pentahydroxybenzophenone, 2,3,3',4,4',5'-hexahydroxybenzophenone, 2,3',4,4',5',6-hexahydroxybenzophenone, etc.; 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of bis[(poly)hydroxyphenyl]alkanes such as bis(4-hydroxyphenyl)methane, bis(2,4-dihydroxyphenyl)methane, bis(2,3,4-trihydroxyphenyl)methane, 2,2-bis(4-hydroxyphenyl)propane, 2,2-bis(2,4-dihydroxyphenyl)propane 2,2-bis(2,3,4-trihydroxyphenyl)propane, 1,1-bis(4-hydroxyl)-1-phenylethane, 1,1,1-tris(4-hydroxyphenyl)ethane, etc.; 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of alkyl (poly)hydroxybenzoates or aryl (poly)hydroxybenzoates such as lauryl 3,5-dihydroxybenzoate, phenyl 2,3,4-trihydroxybenzoate, lauryl 3,4,5-trihydroxybenzoate, propyl 3,4,5-trihydroxybenzoate, phenyl 3,4,5-trihydroxybenzoate, etc.; 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of bis(polyhydroxybenzoyl)alkanes such as bis(2,5-dihydroxybenzoyl)methane, bis(2,3,4-trihydroxybenzoyl)methane and bis(2,4,6-trihydroxybenzoyl)methane, or bis(polyhydroxybenzoyl)benzenes such as p-bis(2,5-dihydroxybenzoyl)benzene, p-bis(2,3,4-trihydroxybenzoyl)benzene, p-bis(2,4,6-trihydroxybenzoyl)benzene; and 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of polyethylene glycol di[(poly)hydroxybenzoates] such as ethylene glycol di(3,5-dihydroxybenzoate), polyethylene glycol di(3,5-dihydroxybenzoate), polyethylene glycol di(3,4,5-trihydroxybenzoate), etc.; and 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of phenol resins, and so on.
Of the aforementioned 1,2-quinone diazide compounds, particularly preferred are polyhydroxybenzophenone 1,2-naphthoquinonediazidesulfonates such as 2,3,4-trihydroxybenzophenone 1,2-naphthoquinonediazide-4-sulfonate, 2,3,4-trihydroxybenzophenone 1,2-naphthoquinonediazide-5-sulfonate, 2,3,4,4'-tetrahydroxybenzophenone 1,2-naphthoquinonediazide-4sulfonate, 2,3,4,4'-tetrahydroxybenzophenone 1,2-naphthoquinonediazide-5-sulfonate, 3'-methoxy-2,3,4,4'-tetrahydroxybenzophenone 1,2-naphthoquinonediazide-4-sulfonate, 3'-methoxy-2,3,4,4'-tetrahydroxybenzophenone 1,2-naphthoquinonediazide-5-sulfonate, 1,1,1-tris(4-hydroxyphenyl)ethane 1,2-naphthoquinonediazide-5-sulfonate, etc., and 1,2-quinonediazidesulfonates obtained by sustituting, for instance, from 20 to 100 mol %, preferably from 40 to 100 mol %, of the hydrogen atoms of the hydroxyl groups contained in a novlak resin or resol resin (hereinafter referred to simply as "resin (B)") by a 1,2-quinonediazidesulfonyl group such as 1,2-naphthoquinonediazide-4-sulfonate group, 1,2-naphthoquinonediazide-5-sulfonate group, etc.
The resin (B) can be obtained by condensation of a phenol and an aldehyde. The phenols usable for the condensation include phenol, 1-naphthol, 2-naphthol and the like, as well as those phenols mentioned above for use in synthesis of the resin (A). As the aldehyde for the condensation, also, those aldehydes usable in synthesis of the resin (A) can be used. Such an aldehyde is used preferably in an amount of from 0.1 to 3 moles, more preferably from 0.2 to 1.5 moles, per mole of the phenol used. In the condensation, further, alkaline catalysts as well as those acidic catalysts usable for synthesis of the resin (A) can be used.
Generally, the Mw of the resin (B) is preferably not more than 10,000, more preferably from 200 to 2,000 in view of easiness of esterification and solubility in solvents. An especially preferred Mw value ranges from 300 to 1,000. The 1,2-quninonediazidesulfonates of the resin (B) include, for example, 1,2-benzoquinonediazide-4-sulfonates, 1,2-naphthoquinonediazide-4-sulfonates and 1,2-naphthoquinonediazide-5-sulfonates of phenol/formaldehyde condensed novolak resins, m-cresol/formaldehyde condensed novolak resins, p-cresol/formaldehyde condensed novolak resins, o-cresol/formaldehyde condensed novolak resins, m-cresol/p-cresol/formaldehyde condensed novolak resins, etc.
In the composition of the present invention, the amount of the 1,2-quinone diazide compound is generally from 3 to 100 parts by weight, preferably from 5 to 50 parts by weight, per 100 parts by weight of the resin (A), with the total amount of the 1,2-quinonediazidesulfonyl groups in the composition being controlled to within the range of generally from 5 to 25% by weight, preferably from 10 to 20% by weight.
Other compounding agents
The composition according to the present invention can further comprise various compounding agents such as sensitizer, surface active agent, dissolution accelerator, etc.
Sensitizers can be incorporated in the composition, in order to enhance sensitivity of the composition. Such sensitizers include, for example, 2H-pyrido-(3,2-b)-1,4-oxazin-3(4H)-ones, 10H-pyrido-(3,2-b)-(1,4)-benzothiazines, urazols, hydantoins, barubituric acids, glycine anhydrides, 1-hydroxybenzotriazoles, alloxans, maleimides, etc. The amount of the sensitizers used is generally up to 50 parts by weight per 100 parts by weight of the resin (A).
Surface active agents can be incorporated in the composition, for improving the application properties or developing properties of the composition. The usable surface active agents include, for example, polyoxyethylene lauryl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether, polyoxyethylene octylphenyl ether, polyoxyethylene nonylphenyl ether, polyethylene glycol dilaurate, polyethylene glycol distearate, etc.; F-Top EF301, EF303 and EF352 (tradenames for products by Shin-Akita Kasei K.K.), Megafac F171, F172 and F173 (tradenames for products by Dainippon Ink & Chemicals, Inc.), Fluorad FC430 and FC431 (tradenames for products by Sumitomo 3M Co., Ltd.), Asahi Guard AG710, Surflon S-382, SC-101, SC-102, SC-103, SC-104, SC-105 and SC-106 (tradenames for products by Asahi Glass Co., Ltd.), etc.; organosiloxane polymer KP341 (tradename for a product by Shin-Etsu Chemical Co., Ltd.); acrylic or methacrylic (co)polymers Polyflow No. 75 and No. 95 (tradenames for products by Kyoeisha Chemical Co., Ltd.), etc.
The amount of the surface active agent used is generally 2 parts by weight or less per 100 parts by weight of solid components in the composition.
Dissolution accelerators can be incorporated in the composition, in order to accelerate dissolution of the composition in the developing solution and to improve the sensitivity and developing properties of the composition. Such dissolution accelerators include, for example, 1,1-bis(4-hydroxyphenyl)-1-phenylethane, 1,1,1-tris(4-hydroxyphenyl)ethane, 3,5-dimethyl-4,4'-dihydroxydiphenylmethane, bisphenol A, 3,5-dimethyl-2',4-dihydroxydiphenylmethane, 1,1-bis(4-hydroxyphenyl)cyclohexane, 1,1-bis(4-hydroxyphenyl)-4-methylcyclohexane, alkali-soluble novolak resins having a weight average molecular weight in terms of polystyrene of 2,000 or less, etc. The amount of the dissolution accelerators used is generally up to 50 parts by weight per 100 parts by weight of the resin (A).
In the composition of the present invention, furthermore, a dye or pigment may be incorporated in order to visualize a latent image in the area irradiated with radiations and to reduce the influence of halation upon the irradiation. Also, an adhesion aid can be incorporated in the composition in order to improve the adhesion of the composition. Moreover, stabilizer, defoaming agent, etc. may also be incorporated in the composition, as required.
Preparation of the composition and formation of pattern
The composition of the present invention is prepared, for example, by dissolving the resin (A) and the compound (A) or compound (B), optionally with 1,2-quinone diazide compounds and other compounding agents as required, in a solvent so as to obtain a solids content of, for example, from 20 to 40% by weight, and filtrating the resultant solution through a filter having a pore diameter of about 0.2 μm.
Examples of the solvent for use here include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, methyl cellosolve acetate, ethyl cellosolve acetate, etc.; diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol methyl ether acetate, propylene glycol propyl ether acetate, toluene, xylene, methyl ethyl ketone, cyclohexanone, ethyl 2-hydroxypropionate, ethyl 2-hydroxy-2-methylpropionate, ethyl ethoxyacetate, ethyl hydroxyacetate, methyl 2-hydroxy-3-methylbutanoate, ethyl acetate, butyl acetate, methyl 3-methoxypropionate, ethyl 3-methoxypropionate, ethyl 3-ethoxypropionate, methyl 3-ethoxypropionate, etc. These solvents may be used either singly or in combination of two or more. Furthermore, high boiling point solvents can also be added, such as N-methylformamide, N,N-dimethylformamide, N-methylformanilide, N-methylacetamide, N,N-dimethylacetamide, N-methylpyrrolidone, dimethyl sulfoxide, benzyl ethyl ether, dihexyl ether, acetonylacetone, isophorone, caproic acid, caprylic acid, 1-octanol, 1-nonanol, benzyl alcohol, benzyl acetate, ethyl benzoate, diethyl oxalate, diethyl maleate, gammabutyrolactone, ethylene carbonate, propylene carbonate, phenyl cellosolve acetate, etc.
The composition of the present invention is applied by spin coating, flow-coating, roll coating or the like to, for example, a silicon wafer or a wafer having a coating of aluminum or the like thereon, whereby a photosensitive layer is formed. The photosensitive layer is then irradiated with radiations through a predetermined mask pattern, followed by development with a developing solution to form a pattern.
Where the composition of the present invention is used as a positive type photoresist, the effect of the invention can be further enhanced by applying the composition to a wafer or the like, subjecting the applied composition to prebaking and exposure, and then heating the composition at a temperature of from 70° to 140° C., followed by development.
Developing solution
As the developing solution for the composition of the present invention, aqueous alkaline solutions are used which contain an alkaline compound such as sodium hydroxide, potassium hydroxide, sodium carbonate, sodium silicate, sodium metasilicate, aqueous ammonia, ethylamine, n-propylamine, diethylamine, di-n-propylamine, triethylamine, methyldiethylamine, dimethylethanolamine, triethanolamine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, choline, pyrrole, piperidine, 1,8-diazabicyclo-(5,4,0)-7-undecene, 1,5-diazabicyclo-(4,3,0)-5-nonane, etc., in a concentration of generally from 1 to 10% by weight, preferably from 2 to 5% by weight.
To the developing solution, furthermore, water-soluble organic solvents, for example, alcohols such as methanol, ethanol, etc., or surface active agents may also be added in appropriate amounts.
The development of a latent image with the developing solution consisting of the aqueous alkaline solution as above is, in general, followed by rinsing in water.
EXAMPLES
The present invention will now be explained more in detail by referring to the following examples, which are not to be construed as limitative of the invention.
In the examples, measurement of Mw and evaluation of photoresists were carried out as follows.
Mw
Mw was measured by gel permeation chromatography with monodisperse polystyrene as a standard, using GPC columns (two G2000H 6 columns, one G3000H 6 column and one G4000H 6 column, produced by Toyo Soda Mfg. Co., Ltd.) under the conditions of a flow rate of 1.5 ml/min, a column temperature of 40° C. and with tetrahydrofuran as eluent.
Sensitivity
Exposure was carried out on a Model NSR-1505G4D step and repeat reduction projection aligner (numerical aperture: 0.45, a product by Nikon Corp.) using g-line of a wavelength of 436 nm, with the exposure time varied, or on a Model NSR-1505i6A step and repeat reduction projection aligner (numerical aperture: 0.45, a product by Nikon Corp.) using i-line of a wavelength of 365 nm, with the exposure time varied. After the exposure, development was carried out using a 2.4 wt. % aqueous solution of tetramethylammonium hydroxide as a developing solution at 25° C. for 60 seconds, followed by rinsing with water and drying to form a photoresist pattern on a wafer. An exposure time suitable for forming a 0.6-μm line-and-space pattern (1L/1S pattern) in a width ratio of 1:1 was determined (this exposure time will be hereinafter referred to as "optimum exposure time").
Resolution
The minimum size of photoresist patterns resolved upon exposure for the optimum exposure time was measured.
Remained thickness ratio upon development
The thickness of a pattern developed after exposure for the optimum exposure time was divided by the photoresist film thickness before the development, then the resultant quotient was multiplied by 100, and the value thus obtained was presented with the percent symbol, %.
Developability
The extent of scumming or residue left upon development was examined.
Heat resistance
A wafer provided thereon with a photoresist pattern was placed in a clean oven to determine the temperature at which the pattern started being deformed.
Pattern shape
After development of a 0.6-μm photoresist pattern, the upper edge A and the lower edge B of the developed portion, generally rectangular in section, were measured under a scanning electron microscope. The pattern shape was judged as good when the A and B values of the pattern satisfied the relationship: 0.85≦B/A≦1. When the sectional contour of the pattern trailed at its foot or reversely tapered, the pattern shape was judged as bad, even if the value of B/A was in the above range.
SYNTHESIS OF RESIN (A)
Synthesis Example 1
A flask equipped with a stirrer, a cooling pipe and a thermometer was charged with 67.6 g (0.63 mol) of m-cresol, 10.0 g (0.073 mol) of 2,3,5-trimethylphenol, 31.8 g (0.29 mol) of p-cresol, 107.1 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 1.32 mol) and 1.33 g (1.06×10 -2 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out with stirring for 30 minutes. Then, 17.5 g (0.16 mol) of m-cresol and 40.0 g (0.29 mol) of 2,3,5-trimethylphenol were added to the flask, and polycondensation was further carried out for 40 minutes.
Next, the oil bath temperature was raised to 180° C. and, simultaneously, the pressure inside the flask was reduced to a value of from 30 to 50 mmHg, thereby removing water, oxalic acid and the unreacted formaldehyde, m-cresol, p-cresol and 2,3,5-trimethylphenol.
The molten resin thus obtained was recovered by cooling back to room temperature. The resin obtained will be referred to as "resin (A1)".
Synthesis Example 2
The resin (A1) was dissolved in ethyl cellosolve acetate so as to attain a solids content of 20% by weight. To one part by weight of the resin solution thus obtained, two parts by weight of methanol and one part by weight of water were added, followed by stirring, and the stirred admixture was left to stand. After the admixture separated into two layers by being left to stand, the resin solution layer (lower layer) was taken out, concentrated, dehydrated and dried, whereby the resin was recovered. The resin thus obtained will be referred to as "resin (A2)".
Synthesis Example 3
An autoclave was charged with 69.2 g (0.64 mol) of m-cresol, 21.8 g (0.16 mol) of 2,3,5-trimethylphenol, 61.0 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.75 mol), 6.3 g (0.05 mol) of oxalic acid dihydrate, 52.6 g of water and 182 g of dioxane. With the autoclave immersed in an oil bath to maintain the temperature inside the autoclave at 130° C., condensation was carried out with stirring for 6 hours. After the reaction, the temperature was returned to room temperature, and the reaction mixture of the autoclave was removed into a beaker. After the reaction mixture in the beaker separated into two layers, the lower layer was taken out, concentrated, dehydrated and dried, whereby a resin was recovered. The resin obtained will be referred to as "resin (A3)".
Synthesis Example 4
A flask similar to that used in Synthesis Example 1 was charged with 13.0 g (0.12 mol) of m-cresol, 32.4 g (0.3 mol) of p-cresol, 39.0 g (0.32 mol) of 3,5-xylenol, 56.9 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.70 mol) and 0.083 g (6.59×10 -4 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out with stirring for 30 minutes. Then, polycondensation was carried out further for 45 minutes, with continuous and gradual addition of 51.9 g (0.48 mol) of m-cresol and 9.77 g (0.08 mol) of 3,5-dimethylphenol to the flask according to the progress of the reaction.
Thereafter, the resin formed was recovered in the same manner as in Synthesis Example 1. The resin thus obtained will be referred to as "resin (A4)".
Synthesis Example 5
An autoclave was charged with 69.2 g (0.64 mol) of m-cresol, 19.5 g (0.16 mol) of 3,5-xylenol, 58.4 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.72 mol), 0.90 g (7.14×10 -3 mol) of oxalic acid dihydrate, 54.4 g of water and 228 g of dioxane. Polycondensation was carried out or 10 hours, and the resultant resin was recovered in the same manner as in Synthesis Example 3. The resin obtained will be referred to as "resin (A5)".
Synthesis Example 6
A flask similar to that used in Synthesis Example 1 was charged with 26.0 g (0.24 mol) of m-cresol, 78.2 g (0.64 mol) of 3,5-xylenol, 146 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 1.80 mol) and 0.164 g (1.30×10 -3 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out with stirring for 30 minutes. Then, 104 g (0.96 mol) of m-cresol and 20.0 g (0.16 mol) of 3,5-xylenol were further added to the flask, and the contents of the flask was reacted further for 70 minutes.
Next, the oil bath temperature was raised to 180° C. and, simultaneously, the pressure inside the flask was reduced to a value of from 30 to 40 mm Hg, thereby removing water, oxalic acid and the unreacted formaldehyde, m-cresol and 3,5-xylenol. Subsequently, the resin thus formed was recovered in the same manner as in Synthesis Example 1. The resin obtained will be referred to as "resin (A6)".
Synthesis Example 7
A flask similar to that used in Synthesis Example 1 was charged with 95.2 g (0.88 mol) of m-cresol, 24.4 g (0.18 mol) of 2,3,5-trimethylphenol, 154 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 1.90 mol) and 1.82 g (0.014 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out with stirring for 90 minutes. Then, 23.8 g (0.22 mol) of m-cresol and 97.6 g (0.72 mol) of 2,3,5-trimethylphenol were further added to the flask, and the contents of the flask was reacted further for 60 minutes.
Next, the oil bath temperature was raised to 180° C. and, simultaneously, the pressure inside the flask was reduced to a value of from 30 to 40 mm Hg, thereby removing water, oxalic acid and the unreacted formaldehyde, m-cresol and 2,3,5-trimthylphenol. Subsequently, the resin thus formed was recovered in the same manner as in Synthesis Example 1. The resin obtained will be referred to as "resin (A7)".
Synthesis Example 8
The resin (A7) was dissolved in ethyl cellosolve acetate so as to attain a solids content of 20% by weight. To one parts by weight of the resin solution thus formed, 1.8 parts by weight of methanol and one part by weight of water were added, followed by stirring, and the stirred admixture was left to stand. After the admixture separated into two layers by being left to stand, the resin solution layer (lower layer) was taken out, concentrated, dehydrated and dried, whereby a resin was recovered. The resin thus obtained will be referred to as "resin (A8)".
SYNTHESIS OF RESIN (B)
Synthesis Example 9
A flask similar to that used in Synthesis Example 1 was charged with 108.0 g (1.00 mol) of m-cresol, 24.3 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.30 mol) and 0.30 g (2.40×10 -3 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out for 40 minutes. Then, the resin thus formed was recovered in the same manner as in the synthesis of resin (A1). The resin thus recovered will be referred to as "resin (B1)".
Synthesis Example 10
A flask similar to that used in Synthesis Example 1 was charged with 64.9 g (0.60 mol) of m-cresol, 43.3 g (0.40 mol) of p-cresol, 20.3 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.25 mol) and 0.30 g (2.40×10 -3 mol) of oxalic acid dihydrate. With the flask immersed in an oil bath to maintain the temperature inside the flask at 100° C., polycondensation was carried out with stirring for 30 minutes. The resin thus formed was then recovered in the same manner as in Synthesis Example 1. The resin obtained will be referred to as "resin (B2)".
ABBREVIATION OF COMPOUND (A)
Abbreviations will be hereinafter used for the following compounds, which each are included in the aforementioned compound (A):
1,1-bis(4-hydroxyphenyl)-1-[4-{1-(4-hydroxyphenyl)-1methylethyl}phenyl]ethane will be referred to simply as "compound (A1)", and
1,1-bis(4-hydroxyphenyl)-1-[4-(4- hydroxybenzyl) phenyl]ethane as "compound (A2)".
SYNTHESIS OF COMPOUND (B)
Synthesis Example 11
A flask equipped with a stirrer, a dropping funnel and a thermometer was charged with 42.5 g (0.10 mol) of the compound (A1), 53.7 g (0.20 mol) of 1,2-naphthoquinonediazide-5-sulfonic acid chloride and 100 g of dioxane, under shielding from light, and the contents of the flask was stirred to effect dissolution.
Next, the flask was immersed in a water bath controlled to a temperature of 30° C. When the temperature inside the flask attained a steady value of 30° C., 22.3 g (0.22 mol) of triethylamine was slowly added dropwise to the solution in the flask through the dropping funnel in such a way that the temperature would not exceed 35° C.
Thereafter, precipitates of triethylamine hydrochloride were removed by filtration, and the filtrate was poured into a large amount of diluted hydrochloric acid, to permit precipitation. The precipitates thus formed were then collected by filtration, and dried a whole day and night in a heating vacuum dryer controlled to 40° C., to yield a compound. The compound obtained will be referred to as "compound (B1)".
Synthesis Example 12
A compound (B2) was obtained in the same manner as in Synthesis Example 11 except that 42.5 g (0.10 mol) of the compound (A1), 67.2 g (0.25 mol) of 1,2-naphthoquinonediazide-5-sulfonic acid chloride and 27.8 g (0.275 mol) of triethylamine were used.
Synthesis Example 13
A compound (B3) was obtained in the same manner as in Synthesis Example 11 except that 42.5 g (0.10 mol) of the compound (A1), 53.7 g (0.20 mol) of 1,2-naphthoquiononediazide-4-sulfonic acid chloride and 22.3 g (0.22 mol) of triethylamine were used.
Synthesis Example 14
A compound (B4) was obtained in the same manner as in Synthesis Example 11 except that 39.6 g (0.10 mol) of the compound (A2), 53.7 g (0.20 mol) of 1,2-naphthoquinonediazide-5-sulfonic acid chloride and 22.3 g (0.22 mol) of triethylamine were used.
SYNTHESIS OF 1,2-QUINONE DIAZIDE COMPOUND
Synthesis Example 15
A quinone diazide compound (I) was obtained in the same manner as in Synthesis Example 11 except that 10.0 g of the resin (B1), 13.9 g of 1,2-naphthoquinonediazide-4-sulfonic acid chloride and 5.75 g of triethylamine were used.
Synthesis Example 16
A quinone diazide compound (II) was obtained in the same manner as in Synthesis Example 11 except that 10.0 g of the resin (B2), 16.6 g of 1,2-naphthoquinonediazide-5-sulfonic acid chloride and 6.86 g of triethylamine were used.
Examples 1 to 15, and Comparative Examples 1 to 3
In each example, a resin (A), a quinone diazide compound, a compound (A) or compound (B), and a solvent were mixed together to form a uniform solution, which was filtered through a membrane filter with 0.2 μm pore diameter to prepare a solution of the composition according to the present invention.
The solution thus obtained was applied by a spin coater to a silicon wafer having a silicon oxide film thereon. The solution thus applied was prebaked on a hot plate at 90° C. for 2 minutes to form a photoresist film 1.2 μm thick. Then, as mentioned above, the photoresist film was subjected to exposure, by irradiation with radiations at a wavelength of 436 nm (g-line) or 365 nm (i-line) through a reticle, and then to development, rinsing and drying. Thereafter, the photoresist film was evaluated as to sensitivity, resolution, remained thickness ratio upon development, developability, heat resistance and pattern shape. The results are shown in Table 1, together with the resins and the like used.
In Examples 1 to 11 and Comparative Examples 1 and 2, the exposure was carried out by irradiating with g-line, whereas i-line was used for the same purpose in Examples 12 to 15 and Comparative Example 3.
TABLE 1__________________________________________________________________________ Quinonediazide.sup.2) Compound (A) or Dissolution.sup.3) Resin A compound Compound (B) accelerator Solvent.sup.4) Kind Mw Amount.sup.1) Kind Amount.sup.1) Kind Amount.sup.1) Kind Amount.sup.1) Kind Amount.sup.1)__________________________________________________________________________Examples 1 A1 4300 100 II/V 7.5/20 A1 5 -- -- α 320 2 A1 4300 100 IV 25 B2 5 -- -- β 320 3 A4 4500 100 III/V 12.5/12.5 A2 5 -- -- α 320 4 A6 3700 100 V 20 B3 7.5 -- -- α 320 5 A7 4000 100 V 25 A1 5 -- -- α 320 6 A2 9900 80 I/IV 5/20 A1 15 -- -- α 320 7 A3 9200 85 V 20 A1/B1 15/5 -- -- β 320 8 A5 9000 85 V 15 A2/B4 15/5 -- -- α 320 9 A8 8900 80 V 20 A1/B1 20/5 -- -- β 32010 A5 9000 85 V 15 A1/B2 15/10 -- -- α 32011 A8 8900 80 V 20 B2 5 S1 20 α 32012 A6 3700 100 II/IV 5/20 A1 5 -- -- α 32013 A8 8900 80 V 5 A2/B4 20/20 -- -- β 32014 A3 9200 80 -- -- B2 25 S2 20 α/β 256/6415 A3 9200 80 -- -- A1/B1 20/30 -- -- β 320ComparativeExamples 1 A1 4300 100 II/V 7.5/20 -- -- -- -- α 320 2 A4 4500 100 III/V 12.5/12.5 -- -- S3 5 α 320 3 A7 4000 100 IV 25 -- -- -- -- α/β 256/64__________________________________________________________________________ Properties of resist Sensitivity Resolution Pattern Remained thickness Heat resistance (msec) (μm) shape ratio (%) Deveropability (°C.)__________________________________________________________________________Examples 1 290 0.50 Good >99 Good 150 2 300 0.50 Good >99 Good 150 3 280 0.50 Good >99 Good 150 4 270 0.50 Good >99 Good 150 5 330 0.50 Good >99 Good 150 6 320 0.48 Good >99 Good 150 7 290 0.48 Good >99 Good 150 8 270 0.48 Good >99 Good 150 9 300 0.48 Good >99 Good 15010 270 0.48 Good >99 Good 15011 270 0.48 Good >99 Good 15012 290 0.40 Good >99 Good 15013 300 0.40 Good >99 Good 15014 240 0.40 Good >99 Good 15015 290 0.40 Good >99 Good 150ComparativeExamples 1 390 0.55 Good >99 Scum 150 exist at 0.50 μm 2 380 0.55 Reversely 96 Scum 145 tapered exist at 0.50 μm 3 290 0.45 Pattern >99 Scum 150 head exist at rounded 0.40 μm__________________________________________________________________________ Notes: .sup.1) Addition amounts are in parts by weight. .sup.2) The quinone diazide compounds (III) to (V) are as follows: III: Condensation product of 1 mol of 2,3,4trihydroxybenzophenone and 3.0 mol of 1,2naphthoquinonediazide-5-sulfonic acid chloride. IV: Condensation product of 1 mol of 2,3,4,4tetrahydroxybenzophenone and 3.6 mol of 1,2naphthoquinonediazide-5-sulfonic acid chloride. V: Condensation product of 1 mol of 2,3,4,4tetrahydroxybenzophenone and 4.0 mol of 1,2naphthoquinonediazide-5-sulfonic acid chloride. .sup.3) The dissolution accelerators are as follows: S1: 1,1,1tris(4-hydroxyphenyl)ethane S2: 1,1bis(4-hydroxyphenyl)-1-phenylethane S3: an alkalisoluble novolak resin (Mw = 520) synthesized in the same manner as in Synthesis Example 1 except that 108.0 g (1.00 mol) of mcresol, 20.3 g of a 37 wt. % aqueous solution of formaldehyde (formaldehyde: 0.25 mol) and 0.30 g (2.40 × 10.sup.-3 mol) of oxali acid dihydrate were placed in a flask, and subjected to condensation for 30 minutes, with the temperature inside the flask maintained at 100° C. .sup.4) The kinds of solvents are as follows: α: Ethyl cellosolve acetate. β: Ethyl 2hydroxypropionate.
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A radiation-sensitive resin composition containing an alkali-soluble resin, comprising a polyhydroxy compound having the following formula: ##STR1## or a quinonediazidesulfonate of the polyhydroxy compound. The radiation-sensitive resin composition is suitable for use as a positive type photoresist which has such excellent developability as to inhibit effectively the generation of scum in the formation of a photoresist pattern, has high sensitivity and is excellent in heat resistance and remained thickness ratio upon development.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This patent application claims the benefit of priority to German Patent Application Serial No. 102011010110.1, filed Feb. 2, 2011, which is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to an apparatus for removing a surface layer from food products having a product feed which feeds a product to be processed along a product conveying direction to a removal tool such that the product is pressed with a component perpendicular to the product conveying direction toward an operative surface of the removal tool.
BACKGROUND
[0003] Such apparatus are used in the food industry, for example, to separate the fat cover and/or the rind of a meat product from the quality meat. Depending on the purpose and on the kind of product, different tools such as rollers or knife blades are used for the removal, which are pressed toward the moving product transversely to the product conveying direction. It is necessary for a correct function of such a removal apparatus that the pressure of the removal tool onto the product surface is maintained during the total removal procedure.
[0004] Spring devices are therefore provided in conventional removal apparatus to pretension the removal tool toward the product surface. There is, however, the problem here that the spring force is dependent on the deflection of the spring device that is on the position of the removal tool relative to a base position, and the pressing force thus varies in the event of an irregular product thickness. This can have the result that the removal of the surface layer does not run ideally.
[0005] It is therefore a feature of the invention to ensure a uniform removal of the surface layer in an apparatus of the named kind also for products of irregular thickness.
[0006] The above referenced feature is provided by an apparatus for removing a surface layer from food products having a product feed which feeds a product to be processed along a product conveying direction to a removal tool. The product is pressed with a component perpendicular to the product conveying direction toward an operative surface of the removal tool.
[0007] In accordance with an embodiment of the invention, the position of the removal tool relative to the product feed is adjustable by means of an adjustment apparatus, with a control unit associated with the adjustment apparatus being designed to adjust the position of the removal tool relative to the product feed in dependence on the contour of the product. The pressing force can be varied as desired by the active adjustment of the relative position between the product feed—for example a product support surface—and the removal tool since said pressing force ultimately depends on the spacing between the operative surface of the removal tool and the corresponding counter-force which is associated with the product feed. In this respect, it does not play any role whether a spring device is additionally also provided for pressing on which is influenced in its deflection by the adjustment procedure or whether the relative position between the removal tool and the product feed is fixed, apart from the adjustment procedure, and the pressing force is ultimately based on the elasticity of the product. Depending on the application, the adjustment apparatus can move the removal tool itself or move a corresponding counter-surface of the product feed. The adjustment of the relative position can also take place in that both the removal tool and an associated counter-surface of the product feed are moved by the adjustment apparatus.
[0008] Provision is made in an embodiment that the relative position between a counter-surface of the product feed and the removal tool is adjustable.
[0009] Provision can furthermore be made that the counter-surface is formed at a pressing apparatus, with the pressing apparatus in particular including a pressing roller.
[0010] In accordance with a possible embodiment, the relative position is adjustable between a pressing apparatus and a product support surface of the product feed. In this respect, in particular the removal tool is arranged in a cut-out or recess of the product support surface.
[0011] Provision can furthermore be made that the product feed includes a pressing apparatus which is designed to press the product toward a product support surface of the product fed, with in particular the removal tool being arranged in a cut-out or recess of the product support surface.
[0012] In an embodiment, the removal tool may be arranged in a fixed position with respect to the adjustment direction relative to a product support surface of the product feed. This is, however, not compulsory. Alternatively, the removal tool can be adjustable with respect to the product support surface.
[0013] In an embodiment, the control unit may be designed to continuously adjust a counter-surface of the product feed and/or the operative surface of the removal tool to follow the contour of the product during the removal procedure. In other words, the adjustment apparatus guides the counter-surface or the removal tool continuously along the surface of the product during the removal procedure. The counter-surface or the removal tool therefore does not passively follow the product surface as with usual removal apparatus, but is rather actively guided along it. In this manner, an unchanging pressing force and thus an unchanging removal effect can be achieved during the total removal procedure. The counter-surface is in particular formed at a pressing apparatus, e.g. at a pressing roller, which can be driven and thus can also serve as a conveying roller or it can be not driven and can be freely rotatable.
[0014] In accordance with an embodiment, the spacing of a counter-surface of the product feed and/or of the operative surface of the removal tool from a product support surface of the product feed can be adjusted by means of the adjustment apparatus. The product support surface can e.g. be the surface of a belt conveyor which simultaneously also serves for the product advance. Alternatively, a static product support surface could also be provided.
[0015] Furthermore, a detection device for determining the contour of the product can be provided which is connected to the control unit and which in particular works in a contactless manner. The control unit is thus able to carry out the position adjustment with reference to the specifically measured contour of the product just to be processed, whereby a particularly exact following adjustment of a counter-surface and/or of the removal tool can be achieved.
[0016] The detection device can include at least one distance measuring sensor, in particular an ultrasound based sensor. A reliable determination of the product contour is hereby possible without piercing or cutting into the product or otherwise damaging it.
[0017] A contactless distance detection can take place in an optical manner in accordance with an embodiment of the invention. An optical detection device can be provided, for example which is based on the triangulation principle or on the light sectioning process. In particular, at least one line projector with a laser as a light source can be used in conjunction with at least one camera for observing the projected line on the product in order thus to determine the product contour by the line offset. A further possibility for contactless contour detection is the use of an X-ray scanner which is able to determine the inner structure of a product using density differences. The portion of the structure information related to the outer contour can be extracted from this exhaustive structure information. The use of an X-ray scanner is in particular suitable with applications in which the inner structure of the product anyway has to be determined—for example to observe an exact product portion weight.
[0018] It is generally also conceivable, in accordance with an independent aspect, to press the product toward a product support surface from above, e.g. by means of a pressing roller or a conveying roller, with a knife blade which is vertically adjustable in dependence on the contour removing a lower surface layer of the product while the product is conveyed in the direction of the knife blade.
[0019] In accordance with an embodiment, the removal tool comes into enragement with the product surface from below in order thus to remove a lower surface layer of the product. In this case, gravity can assist or even completely provide the pressing force. The removal tool can be positioned in a cut-out or recess of the corresponding product support surface for this purpose. Depending on the application, the lower removal tool can in this respect be vertically adjustable or an upper counter-surface, e.g. a top section of the product feed, can be adjusted in dependence on the product contour with a fixed-position removal tool. In principle in accordance with the invention, at least two removal tools can be provided which can be adjusted in dependence on the contour and which are operative at oppositely disposed product sides.
[0020] In accordance with an embodiment, the removal tool includes a tool for defatting, skinning and/or derinding. The invention allows a particularly effective cutting of the rind and/or of the fat cover of a meat product from the quality meat component lying thereunder by providing an unchanging pressing force.
[0021] In accordance with an embodiment, the removal tool includes at least one roller rotatable about an axis of rotation extending transversely to the product conveying direction. In such an embodiment, fat is removed, for example, in that it is led through a restriction between the rotatable roller and a support surface of a product conveyor. The pressing force with which the roller is pressed toward the product surface is in this respect predefined by the height of the restriction. The pressing force can be reduced as required by increasing this height by means of a positional adjustment of the roller. The roller can have a ribbing such as is known in the field of defatting machines. The roller can alternatively be a pressing roller which presses the product toward a product support surface in which the removal tool is arranged.
[0022] In accordance with an embodiment, the removal tool includes at least one knife or a blade, with a conveying device preferably formed as a roller in particular being disposed before the knife or the blade in the product conveying direction.
[0023] The knife or the blade may be arranged in a recess or cut-out of the product support surface, in particular together with the additional conveying device preferably formed as a feed roller. The knife or blade and the feed roller are consequently located beneath the product and the feed roller serves to feed the surface layer to be removed to the cutting edge of the knife or blade safely and reliably. The knife or the blade and optionally also the feed roller can be adjustable, with, however, this preferably only taking place in the sense of a one-time machine setting for the respective product and having nothing to do with the adjustment in dependence on the product contour in accordance with the invention.
[0024] The knife or the blade can be provided with an apparatus which serves to deflect the cut-off surface layer, e.g. a rind, downwardly, e.g. into a collection container.
[0025] The adjustment apparatus may include a motorized actuating drive. A sufficiently fast and reliable following adjustment of the removal tool and/or of a counter surface of the product feed can hereby be ensured.
[0026] The actuating drive can in particular include a controllable electric motor by means of which a fast and exact positional adjustment can be achieved.
[0027] In accordance with a further embodiment of the invention, a pressing apparatus of the product feed and/or the removal tool is attached to a pivot arm, with the pressing apparatus and/or the removal tool being able to be raised and lowered with respect to a product support surface of the product feed by means of the adjustment apparatus. The pivot arm can in this respect form a lever for amplifying the adjustment force.
[0028] The adjustment apparatus can be designed to adjust the relative position between the product feed and the removal tool furthermore in dependence on a quality of the product. It can, for example, be desirable to predefine different pressing forces for different types of product. The removal quality can thus be further optimized.
[0029] The removal tool can generally be adjusted relative to a support surface or support plane for the product or relative to a counter-surface located above the support surface, e.g. formed at a pressing apparatus, with it not playing any role whether the removal tool, the support surface or the counter-surface or both components are moved, i.e. it is, for example, also possible to adjust the support surface or the counter-surface in the vertical direction in dependence on the contour and so to press the product toward a removal tool fixed in the vertical direction by means of the adjustable support surface.
[0030] The invention furthermore relates to a method for removing a surface layer from food products, wherein a contour of a product to be processed is determined, the product is fed along a product conveying direction to a removal tool such that the product is pressed with a component perpendicular to the product conveying direction toward an operative surface of the removal tool and the relative position between the product feed and the removal tool is adjusted in dependence on the determined contour of the product by means of an adjustment apparatus.
[0031] The position of a pressing apparatus of the product feed can in particular be adjusted to follow the contour of the product during the removal procedure.
[0032] In accordance with an embodiment, the contour of the total product is determined before the start of the removal procedure. This can in particular be advantageous if the product contour anyway has to be determined for other purposes.
[0033] Alternatively, the contour of the product can also be determined point-wise or section-wise during the removal procedure. Such a contour detection “on the fly” can be advantageous for specific applications.
[0034] The invention will be described in the following by way of example with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0035] FIG. 1 shows a simplified side view of an apparatus for removing a surface layer from food products in accordance with one embodiment of the invention;
[0036] FIG. 1 a shows a simplified side view of an apparatus for removing a surface layer from food products in accordance with another embodiment of the invention;
[0037] FIG. 2 shows a simplified side view of an apparatus for removing a surface layer from food products in accordance with yet another embodiment of the invention.
DETAILED DESCRIPTION
[0038] In accordance with FIG. 1 , a derinding machine or defatting machine for meat products includes a removal roller 10 by means of which a surface layer 30 such as a fat cover can be removed from a meat product 11 . The removal roller 10 has a toothed arrangement 12 for this purpose. The removal roller 10 can e.g. include a plurality of disks which are arranged next to one another along an axis of rotation R of the removal roll 10 and at whose circumference teeth are respectively formed.
[0039] A product feed 13 serves to feed the meat product 11 along a product conveying direction P to the removal roller 10 . The product feed 13 includes two driven belt conveyors 15 which are arranged behind one another and on which the meat product 11 lies. Alternatively or in addition to the belt conveyors 15 , further mechanisms can be provided for effecting the product advance. The removal roller 10 is rotatable about the axis of rotation R extending at a right angle to the product feed direction P and is arranged in a recess 16 between the two belt conveyors 15 . The removal roller 10 can thereby come into engagement with the lower side of the meat product 11 . To be able to remove surface layers 30 of different thickness from the lower side of the meat product 11 , the removal roller 10 is vertically adjustable relative to the support surfaces 17 of the belt conveyors 15 located in a common plane, which is illustrated by a double arrow in FIG. 1 . This vertical setting preferably takes place before the actual removal procedure, i.e. with respect to the height the removal roller 10 is arranged in a fixed position relative to the support surfaces during the removal procedure. Provision can alternatively be made that the removal roller 10 is also vertically adjustable during the removal procedure and indeed with respect to or in dependence on the contour of the product 11 . In the embodiment described here, it is, however, a counter-surface of the product feed which will be described in more detail in the following and which is adjustable relative to the fixed removal roller 10 in dependence on the product contour.
[0040] The product feed 13 furthermore includes a pressing apparatus in the form of a pressing roller 31 which preferably has a ribbing not shown in FIG. 1 . The pressing roller 31 presses the meat product 11 downwardly with a counter-surface 18 on the product side toward the support surfaces 17 of the belt conveyors 15 and toward an operative surface 20 of the removal roller 10 at the product side. Since the pressing roller 31 is rotatably driven about an axis of rotation extending parallel to the axis of rotation R of the removal roller 10 , it also forms a conveying roller for assisting the product advance. Such a conveying function is, however, not compulsory for the pressing roller 31 , i.e. the pressing roller 31 also forms an element of the product feed 13 as a component not providing the advance of the product 11 .
[0041] In the course of the transport on the belt conveyors 15 , the meat product 11 moves between the pressing roller 31 and the removal roller 10 so that the meat product 11 is pressed with a component perpendicular to the product conveying direction P toward the removal roller 10 . The force with which the removal roller 10 presses toward the lower side of the meat product 11 or with which the product 11 is pressed toward the removal roller 10 by means of the pressing roller 31 depends on the ratio between the product height H and the clearance W between the removal roller 10 and the pressing roller 31 , i.e. between the operative surface 20 of the removal roller 10 and the counter surface 18 of the pressing roller 31 .
[0042] As can be seen from FIG. 1 , the meat product 11 has an irregular contour so that the product height H and consequently the pressing force of the removal roller 10 would vary during the removal procedure without further measures.
[0043] In order nevertheless to ensure an unchanging pressing force during the total removal procedure, an adjustment apparatus 19 is provided by means of which the pressing roller 31 can be actively raised and lowered in order thus actively to vary its spacing from the removal roller 10 in dependence on the product contour.
[0044] To determine the contour of the meat product 11 , an ultrasound sensor 21 is provided which continuously detects the distance from the product surface and transmits it to an electronic control unit 23 . The control unit 23 controls a motorized actuating drive 25 , which can be a servo motor for example, in dependence on the received distance signal. An actuating piston 27 which engages at an end of a pivot arm 29 at which the pressing roller 31 is supported can be moved out and in by means of the actuating drive 25 . The pivot arm 29 is pivotably supported at its other end at a fixed-position reference point of the product feed 13 , which is not shown in detail in FIG. 1 . The pivot arm 29 can be upwardly pivoted by a moving out of the actuating piston 27 , whereby the pressing roller 31 is raised with respect to the support surfaces 17 and the removal roller 10 . Conversely, the pivot arm 29 can be downwardly pivoted by moving in the actuating piston 27 , whereby the pressing roller 31 is lowered with respect to the support surfaces 17 .
[0045] The control unit 23 regulates the actuating drive 25 such that the pressing roller 31 is continuously adjusted to follow the contour of the meat product 11 during the total removal procedure, that is it is actively guided along the upper side of the meat product 11 . An unchanging pressing force and thus an unchanging quality of the removal taking place by means of the removal roller 10 can be maintained by this active following adjustment of the pressing roller 31 despite an irregular product contour. It results as a further advantage of the controlled following adjustment that apart from the following adjustment process the base value of the pressing force of the removal roller 10 can also be varied as required in order thus, for example, to take account of a different thickness or consistence of different meat products 11 .
[0046] Another embodiment of the invention shown in FIG. 1 a provides that instead of a rotating removal roller a knife or a blade 33 is used for derinding or defatting a meat product 11 . To drive the meat product 11 safely and reliably toward the blade 33 , in addition to the belt conveyors 15 —of which only one is shown in FIG. 1 a —a conveyor device 35 in the form of a feed roller can be provided which is situated directly in front of the blade 33 in the product conveying direction P.
[0047] The arrangement of blade 33 and feed roller 35 is, like the removal roller shown in FIG. 1 , arranged in a recess 16 between the two belt conveyors 15 so that the blade 33 and the feed roller 35 are therefore located beneath the meat product 11 . To be able to remove surface layers 30 of different thickness from the lower side of the meat product 11 , the blade 33 is vertically adjustable relative to the support surfaces 17 of the belt conveyors 15 , which is illustrated by a double arrow in FIG. 1 a. If the application should require, the feed roller 35 can also be vertically adjustable.
[0048] The blade 33 cuts the surface layer 30 from the meat product 11 . In this respect, the blade 33 remains substantially in a fixed position, i.e. no rotational movement takes place as in the removal roller 10 in accordance with FIG. 1 . If it should be necessary due to the application, however, a vertical adjustment of the blade 33 could take place during the operation of the defatting machine. Such a vertical adjustment of the blade 33 is, however, not decisive for the setting of the pressing force. The cut-off surface layer 30 moves downwardly into a suitable collection container, not shown, with an apparatus being able to be arranged in the region of the blade 33 which assists the downward deflection of the cut-off surface layer 30 .
[0049] A pressing roller 31 presses the meat product 11 downward toward the blade 33 and the feed roller 35 by a counter-surface 18 at the product side in an analogous manner to the embodiment in accordance with FIG. 1 . The pressing roller 31 is in turn continuously adjusted to follow the contour of the meat product 11 during the total removal procedure to ensure an unchanging pressing force during the total removal procedure. The adjustment of the pressing roller 31 takes place in this respect in the same manner as in the apparatus in accordance with FIG. 1 , with the adjustment apparatus being omitted in FIG. 1 a for simplification.
[0050] In accordance with the further embodiment shown in FIG. 2 a defatting machine for meat products includes a removal roller 10 which is arranged above the support surface 17 for the meat product 11 . The removal roller 10 can have a suitable ribbing, which is not shown in FIG. 2 . A product feed 13 serves to feed the meat product 11 along a product conveying direction P to the removal roller 10 . The product feed 13 for this purpose includes a driven belt conveyor 15 on which the meat product 11 lies. Alternatively or in addition to the belt conveyor 15 , further mechanisms can be provided for effecting the product advance. The removal roller 10 is rotatable about an axis of rotation R extending at a right angle to the product conveying direction P.
[0051] In the course of the transport on the belt conveyor 15 , the meat product 11 moves between the pressing surface 17 of the belt conveyor 15 and the removal roller 10 so that the meat product 11 is pressed with a component perpendicular to the product conveying direction toward the removal roller 10 . The force with which the removal roller 10 presses toward the upper side of the meat product 11 depends on the relationship between the product height H and the clearance W between the removal roller 10 and the support surface 17 . As can be seen from FIG. 2 , the meat product 11 has an irregular contour so that the product height H and consequently the pressing force of the removal roller 10 would vary during the removal procedure without further measures.
[0052] In order nevertheless to ensure an unchanging pressing force during the total removal procedure, an adjustment apparatus 19 is provided by means of which the removal roller 10 can be actively raised and lowered in order thus actively to vary the spacing between the operative surface 20 of the removal roller 10 at the product side and the support surface 17 of the belt conveyor 15 in dependence on the product contour. To determine the contour of the meat product 11 , an ultrasound sensor 21 is provided which continuously detects the distance from the product surface and transmits it to an electronic control unit 23 . The control unit 23 controls a motorized actuating drive 25 , which can be a servo motor for example, in dependence on the received distance signal. An actuating piston 27 which engages at an end of a pivot arm 29 at which the pressing roller 10 is supported can be moved out and in by means of the actuating drive 25 . The pivot arm 29 is pivotably supported at its other end at a fixed-position reference point of the product feed 13 , which is not shown in detail in FIG. 2 . The pivot arm 29 can be upwardly pivoted by a moving out of the actuating piston 27 , whereby the removal roller 10 is raised with respect to the support surface 17 . Conversely, the pivot arm 29 can be downwardly pivoted by moving in the actuating piston 27 , whereby the removal roller 10 is lowered with respect to the support surfaces 17 . The control unit 23 regulates the actuating drive 25 such that the removal roller 10 is continuously adjusted to follow the contour of the meat product 11 during the total removal procedure, that is it is actively guided along the upper side of the meat product 11 . An unchanging pressing force and thus an unchanging quality of the removal can be maintained by this active following adjustment of the removal roller 10 despite an irregular product contour. It results as a further advantage of the controlled following adjustment that apart from the following adjustment process the base value of the pressing force of the removal roller 10 can also be varied as required in order thus, for example, to take account of a different thickness or consistence of different meat products 11 .
[0053] In all embodiments shown, the ultrasound sensor 21 detects the contour of the meat product 11 in a point-wise or line-wise manner in front of the removal roller 10 viewed in the product conveying direction P. Alternatively, a contour detection device could also be provided which determines the contour of the total meat product 11 before the start of the removal procedure. Such a contour detection device could also be arranged at a different position of the defatting machine or the defatting machine could be part of a larger production line and can receive the contour data from another apparatus.
[0054] As already initially mentioned, the distance detection can alternatively take place in an optical manner. An optical detection device can be provided, for example which is based on the triangulation principle or on the light sectioning process. In particular at least one line projector—preferably with a laser as a light source—can be used in conjunction with at least one camera for observing the projected lines on the product in order thus to determine the product contour by the line offset. A further possibility for contactless contour detection is the use of an X-ray scanner which is able to determine the inner structure of a product using density differences. The portion of the structure information related to the outer contour can be extracted from this exhaustive structure information.
[0055] 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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An apparatus for removing a surface layer from food products includes a product feed which feeds a product to be processed along a product conveying direction to a removal tool. The product is pressed with a component perpendicular to the product conveying direction toward an operative surface of the removal tool. The relative position between the product feed and the removal tool is adjustable by means of an adjustment apparatus, with a control unit associated with the adjustment apparatus designed to adjust the position of the removal tool relative to the product feed in dependence on the contour of the product.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/908,933, filed Mar. 29, 2007.
TECHNICAL FIELD
[0002] The present invention relates to leaching chambers for receiving and dispersing water and wastewater when buried in the soil, and more particularly, to such pre-molded leaching chambers as are corrugated and arch-shaped in cross-section with contiguously molded end walls, and lateral interior chambers having fluid communication openings at the chamber base.
BACKGROUND ART
[0003] The use of above-ground watering systems, particularly in dry climates such as the southwestern regions of the United States and in the Mediterranean regions of Europe, the Middle East, and Africa, brings with it a list of known problems. In addition to water loss through evaporation during the watering process, if watering is provided too lightly, shallow plant rooting results. Additionally, repeated surface applications of water tend to produce the buildup of mineral salts, which are detrimental to healthy plant growth.
[0004] As increasing population pressures result in greater demands upon fresh water supplies, the benefits of underground irrigation have become increasingly attractive. Such systems place water almost directly into the plant root zone and eliminate evaporative water losses. Their protected location also minimizes the risk of damage from surface activities.
[0005] The subsurface fluid distribution system described in my previous patent, Sipaila, U.S. Pat. No. 5,921,711, provides such a subterranean system with reserve fluid storage capacity to maintain soil dampness as well as replace water taken up by plants. As used in a passive subsurface irrigation system, capillary physics and gravity are relied upon to deliver water and nutrients to plants through an interconnected series of chambers and pans. Such systems are capable of reducing the amount of irrigation water required by 50-80% over the more traditional above-ground systems.
[0006] As is typical for such systems, the leaching chamber has sloped sidewalls that extend to a curved, arched top. When installed, such extended-arch chambers must resist both top and side loadings. The slots in the sidewalls permit the transport of water from within, but act to weaken the sidewall structure.
[0007] While thickening the sidewall would provide additional strength, it also results in an increase in the amount of material required—which is a polyolefin, and is thus tied to the rising cost of petrochemicals. In addition, the added weight of the resulting product adds to the cost of transporting the chambers to the installation site. Also, while it is vital that such chambers are able to efficiently stack for transport, the stacking of such bulked-up chamber walls must not result in forcing the sidewalls out, resulting in the overall flattening and weakening of the arch-shaped chamber.
[0008] It thus is desirable to provide additional solutions that increase the structural integrity of the arched chamber in a manner that enhances the operational efficiency and is not negated by increased transportation costs or product damage during shipment.
DISCLOSURE OF THE INVENTION
[0009] These and other objects are achieved by providing a pre-molded leaching chamber of arch-shaped cross-section, having a pair of contiguously molded, opposing end walls, alternating peak and valley corrugations along its length, and interior chambers formed at the base of the chamber at each peak corrugation providing fluid communication between the exterior and interior of the leaching chamber. The interior chambers are formed by an inner wall attached to an interior surface of the leaching chamber and extending substantially within the peak corrugation, spaced from the outer wall, to the base of the chamber. Vertically off-set apertures are formed in the inner wall and in the opposing outer wall, enabling fluid flow within the inner chamber.
[0010] A leaching chamber comprising: a corrugated outer shell extending along a longitudinal axis in a manner defining alternating peak corrugations and valley corrugations, said corrugated outer shell having an arch-shaped cross-section with a pair of opposed lateral end walls formed therein and no floor; and a plurality of inner walls attached to an interior wall of said corrugated outer shell, each at a location within a separate interior valley formed in said interior wall, with each of said interior valleys corresponding to a peak corrugation formed in said outer shell, said plurality of inner walls extending from a location of attachment to said interior wall to a terminus of a respective one of said interior valleys, each of said plurality of inner walls extending in a manner inwardly spaced from said corrugated outer shell to define a plurality of interior chambers, wherein each of the plurality of interior chambers has an inner wall aperture formed in said respective inner wall and an outer shell aperture formed in the corrugated outer shell.
[0011] A leaching chamber having an arch-shaped cross-section and alternating peak corrugations and valley corrugations along its length comprising: a pair of opposed end walls attached to said leaching chamber at opposite ends thereof, each of said pair of opposed end walls having a connecting pipe aperture formed therein; and a plurality of inner walls attached to an inner surface of said leaching chamber and extending towards a base of said leaching chamber, each of said plurality of inner walls extending in a spaced-apart manner from a separate one of such adjacent lateral wall segment of said leaching chamber as defines one of said alternating peak corrugations, each of said plurality of inner walls and each of said respective adjacent lateral wall segments define an individual interior chamber formed therebetween, each of said inner walls and said adjacent lateral wall segments have an aperture formed therein, whereby fluid communication between an interior of said leaching chamber and an outer environment of said leaching chamber may occur through each of said plurality of interior chambers.
[0012] These and various other advantages and features of the present invention are pointed out with particularity in the claims. Reference should also be had to the drawings which form a further part hereof, as well as to the accompanying descriptive matter in which are illustrated and described in various examples of with the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a partial top perspective view of a leaching chamber in accordance with the present invention.
[0014] FIG. 2 is a partial bottom perspective view of the leach chamber of FIG. 1 .
[0015] FIG. 3 is a cross-sectional view, with portions shown in phantom, taken along line 3 - 3 of FIG. 1 .
[0016] FIG. 4 is a partial cross-sectional view taken along line 4 - 4 of FIG. 1 .
[0017] FIG. 5 is a partial cross-sectional view taken along line 5 - 5 of FIG. 1 .
[0018] FIG. 6 is a partially exploded cross-sectional view of a plurality of stacked leaching chambers, the cross-sectional views of each of the chambers taken along line 3 - 3 of FIG. 1 .
[0019] FIG. 7 is a partial cross-sectional view showing a connecting pipe enabling fluid communication between an adjacent pair of leaching chambers.
[0020] FIG. 8 is a cross-sectional view, similar to FIG. 3 , with portions shown in phantom, taken along line 3 - 3 of FIG. 1 showing an alternative embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] Reference is now made to the drawings wherein like numerals refer to like parts throughout. In FIG. 1 , a leaching chamber 10 includes a corrugated outer shell 14 and an end wall 18 . A connecting pipe aperture 22 is centrally located in the end wall 18 , and is appropriately sized to receive a connector pipe that extends between and is used to connect adjacent leaching chambers (not shown in the Figures).
[0022] The end wall 18 also includes a pair of outer fluting extrusions 26 that are centrally located and extend between the connecting pipe aperture 22 and a base 24 of the end wall 18 . Functioning as stiffeners, the outer fluting extrusions 26 , together with a single inner fluting extrusion 28 (see FIG. 3 ), provide three-dimensional structural support to the end wall 18 without compromising the extrusion process of fabricating the leaching chamber 10 .
[0023] Additional structural support is provided by a footing flange 32 that is attached to and extends from the base 24 of the end wall 18 . A plurality of triangular braces 34 are arranged in a spaced-apart manner along the footing flange 32 to provide lateral rigidity to the flat end wall 18 . Each of these end wall reinforcement features may be fabricated as part of the extrusion process used to form the end wall and corrugated outer shell of the leaching chamber 10 .
[0024] A support footing 42 extends along each lateral terminus of the corrugated outer shell 14 , providing a stable support base when the leaching chamber 10 is positioned for use in an irrigation system or drainage system as well as when it is stacked for transport. In regard to the latter function, a stacking nub 46 is formed on and projects at a lateral location on the corrugated outer shell 14 . The stacking nubs 46 are positioned in a manner that provides support to the support footing 42 when a plurality of leaching chambers 10 are vertically stacked (see FIGS. 3 and 6 ).
[0025] The corrugated outer shell 14 exhibits a repeating outer pattern of peak corrugations and valley corrugations (ridges and grooves), with these outer peaks and valleys inversely corresponding to peaks and valleys from a perspective within the leaching chamber 10 (see FIG. 2 ). An inner wall 52 is formed within each of the interior valleys, and extends from the support footing 42 to a fused attachment seam 54 formed in the corrugated outer shell 14 .
[0026] The inner wall is inwardly spaced from the corrugated outer shell 14 at its location of attachment to the support footing 42 , forming an interior chamber 58 (see FIG. 4 ). A plurality of such interior chambers 58 are formed in, and laterally extend along, in a spaced-apart manner, both longitudinal sides of the leaching chamber 10 . Each of the interior chambers 58 is provided an inner wall aperture 62 formed in the inner wall 52 and an outer shell aperture 64 that is formed in the corrugated outer shell 14 .
[0027] In a presently preferred embodiment, the inner wall aperture 62 and the outer shell aperture 64 are vertically off-set, with the outer shell aperture 64 at a vertical location that is lower than the inner wall aperture 62 when the leaching chamber 10 is in operation. As is best shown in FIG. 4 , this vertical off-set inhibits the reverse flow of particulate matter from the outer environment through the interior chamber 58 , which would otherwise result in the fouling of the primary chamber of the leaching chamber 10 .
[0028] As discussed previously, most applications require a series of leaching chambers 10 that are connected together using discrete connecting pipes, with each pipe extending between opposing connecting pipe apertures to connect together adjoining leaching chambers 10 . It is essential that each leaching chamber 10 remain in fluid communication with any adjoining leaching chamber 10 with which it shares a connecting pipe 70 (see FIG. 7 ).
[0029] As is depicted in both FIGS. 5 and 7 , a stop nub 68 is formed in an interior wall of the corrugated outer shell 14 and extends downwardly to provide a surface against which an end of the connecting pipe 70 can rest. The stop nub 68 resists any further inward migration of the connecting pipe 70 after installation. Such longitudinal movement—in either direction, could result in the dislodgement of the connecting pipe 70 from an adjoining leaching chamber 10 , which in turn would abruptly end or severely impair the fluid communication therebetween. The distance between the adjacent, connected leaching chambers 10 can be as short as a few inches or as long as ten feet, depending upon the particular application. Separation in typical athletic fields is about one foot between the end walls 18 .
[0030] In an alternative embodiment of the present invention shown in FIG. 8 , the connecting pipe aperture 22 has been repositioned close to the base 24 of the end wall 18 . Under this embodiment drainage occurs at the bottom of the leaching chamber 10 , and no or only a very slight amount of water remains within the leaching chamber 10 —unlike the reservoir of water created within the leaching chamber 10 when the connecting pipe aperture 22 is positioned at a higher location on the end wall 18 (see FIG. 3 ).
[0031] The embodiment of FIG. 8 is also provided a lower profile, having a preferred height A of 4 inches instead of 6.3 inches, and a width B of 8.25 inches instead of the previous 13.25 inches. These dimensions provide a reduced profile having less cost in material, the ability to be placed at a shallower depth and with less fill—both lowering installation costs. The remaining dimensions are preferably much the same as in the previously discussed embodiment, the connecting pipe aperture 22 having a diameter C of 2.375 inches, the inner wall aperture 62 having a height D of 0.875 inches, and the outer shell aperture 64 having a height E of 1 inch (preferably reduced by one-half inch as compared to the previously-discussed embodiment).
[0032] The embodiment shown in FIG. 8 is best suited for applications in which drainage is the primary and/or only intended function. However, in flat arrays of the system, water backup can be obtained by utilizing an up-turned elbow as a terminating connecting pipe (not shown in the Figures). Such a terminus would create a pressure head, resulting in the flooding of the connector pipe and all intermediate leaching chambers—making irrigation a possible, but not preferred function of the alternative embodiment shown in FIG. 8 .
[0033] In a presently preferred embodiment, and recognizing that other dimensions are possible—and considered within the scope of the present invention, the leaching chamber 10 is fabricated by extruding a plastic such as high density polyethylene, polypropylene or other suitable polymers. By positioning all of the offset and connecting apertures in an injection mold cavity, all of the improvements can be monolithically molded to produce a one-piece leaching chamber without any other machining. The inner wall apertures and the outer shell apertures are spaced approximately one-and-a-half inches apart, on center, and are vertically offset approximately 1 to 1½ inches. The ½ inch stacking nub 46 and ¼ diameter and ½ inch-long stop nub 68 ; the ¼ inch by 3 inch-long fluting extrusions, the 2 inch height of the inner wall 52 ; the 1 inch width of the footing flange 32 , the ½ inch triangular braces 34 , and the 1 inch wide support footing 42 can all be incorporated in the same injection mold process to produce a single piece integrated chamber.
[0034] The installation of the leaching chambers in accordance with the present invention is initiated by the excavation of a series of trenches, fourteen to eighteen inches deep and eighteen to forty-eight inches wide. The length and width of the trenches will vary, depending upon the design requirements for the particular leaching bed, irrigation field or drainage tile. At a minimum, an excavated section of length four feet is leveled, and if downward leaching of water is not desired, water impermeable liners or enclosing boxes are installed in the leveled trench. Thereafter a series of leaching chambers are placed within the trench, and laid end-to-end so that the lateral leaching chamber water discharge apertures are substantially aligned. The leaching chambers are then connected to one another utilizing the end panel connector pipes.
[0035] A layer of sand or suitable fine gravel for drainage applications is then back-filled over the leaching chambers. Since the upward capillary draw of most sands exceeds a ten-inch vertical above the waterline, a preferred depth of the fill sand over the leaching chambers is approximately twelve inches from the trench bed. The present invention can make use of sands of varying coarseness, with a sand coarseness of 0.3 mm to 0.6 mm grain size being viewed as particularly appropriate.
[0036] Finally, the sand layer may be optionally covered with top soil to a depth of between approximately zero to four inches. Because of the arched cross-section of the outer shell 24 , the leaching chambers 10 are sufficiently strong to withstand the weight of vehicles on top of the replaced soil. Additionally, the individual settling of the leaching chambers within the trenches will not cause a break in the sand seal of the system, since the connector pipes 70 are self-adjusting with the apertures 22 in the end wall 18 .
[0037] Depending upon the slope of the particular terrain, several different arrangements of the leaching chamber arrays are possible. Since the leaching chamber units act independently throughout their (preferred) four foot length, on sloping terrain the trenches are preferably excavated level along the slope contours. The “adjacent” leaching chambers can then be connected perpendicularly across the slope contours, with such adjacent leaching chambers located on different vertical levels, utilizing longer connector pipes where required.
[0038] My invention has been disclosed in terms of a preferred embodiment thereof, which provides an improved half-pipe leaching chambers for subterranean fluid distribution that is of great novelty and utility. Various changes, modifications, and alterations in the teachings of the present invention may be contemplated by those skilled in the art without departing from the intended spirit and scope thereof. It is intended that the present invention encompass such changes and modifications.
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A leaching chamber having an arch-shaped cross-section, a pair of contiguously molded, opposing end walls, and alternating peak and valley corrugations along its length, is provided interior chambers and fluid communication openings along the base on each extending side of the chamber. Formed within the chamber at locations corresponding to each peak corrugation, an inner wall is attached to an interior surface and extends substantially within the peak corrugation to the base of the chamber. An aperture is formed in both the inner wall and in the opposing outer wall of the chamber, enabling fluid communication through the interior chamber—and thus into and out from the interior of the leaching chamber itself.
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BACKGROUND OF THE INVENTION
[0001] This invention relates to a control unit assembly for use with a medical device and, particularly, a pneumatic medical device, such as a compression device for a limb. In particular, the invention relates to a control unit assembly for use with a mobile compression device suited for use in the treatment of venous leg ulcers, oedema, deep vein thrombosis and vascular disorders.
[0002] Various medical devices are known that require inflation of one or more cells with fluid to a desired pressure, for example, compression devices which are used to apply pressure or pressure offloading devices such as mattresses or cushions which are used to even out pressure points. Compression devices are known for applying compressive pressure to a patient's limb. These types of devices are used to assist mainly in the prevention of deep vein thrombosis (DVT), vascular disorders and the reduction of oedema. Prior art devices are adapted for use in a hospital setting in which they are used predominantly for the prevention of DVT in patients with a high risk for developing this condition. U.S. Pat. Nos. 5,117,812; 5,022,387; 5,263,473; 6,231,532; 6,440,093 and 6,463,934 disclose such devices.
[0003] Compression therapy is used in the treatment of venous leg ulcers. The treatment relies on the compression achieving a reduction in oedema and improved return of blood via the venous system. This in turn reduces the residence time for blood supplied to the lower limb and the severity of ischaemic episodes within the limb that can result in tissue breakdown.
[0004] Compression of the limb can be achieved by a pneumatic or hydraulic compression device.
[0005] WO 2004/084790 discloses one type of mobile compression device. By “mobile” it is meant that the user wearing the compression device has relative freedom to move about. The device of WO 2004/084790 comprises one or more fluid inflatable cuffs containing one or more cells arranged for fitting on to a leg or an arm. The device allows the adjustment of the pressure in the cells dependent on the pressure profile desired. The application of pressure by the cells in the sleeve or cuff is maintained by a pump and valves which are operated by an automatic control unit which detects the fall or rise in pressure in each cell throughout the device. Where excessive or deficient pressure is detected by a sensor located in the cell, the control unit activates the pump to restore the intended pressure.
[0006] In the compression devices of the prior art, the control unit is a separate component which is typically not integral to the compression device and remotely operated. This is often on the user's belt, placed in a pocket or carried around by hand which is inconvenient for the user.
[0007] As a control unit, generally, includes a pump, electronic circuitry, conduits for connecting the control unit to the compression device, valves, a source of power, etc., the control unit is usually quite large. Hence, the known control units are bulky and heavy. Therefore, positioning of the unit in the device has not been practical because attaching the known control units to an outer surface of the compression device would result in an excessive weight burden impairing the mobility of the user. Integral positioning is also unnecessary as most of the prior art devices are used in a hospital setting where mobility of the patient is not the main concern. Were the control unit to be positioned on the device, weight would be localized at the attachment point of the device resulting in a weight imbalance on the compression device. Also, a bulky control unit protruding from an outer surface of the compression device permits the unit to be knocked and possibly broken when the user is mobile and would not fit beneath clothing.
[0008] There are barriers to reducing the size of the control unit. The conduits between the pump and the inflatable cells have in the past been external and would thus present a trip or tangle hazard. The power consumption by the components in a typical hospital device would make the battery too large to be carried on the device itself and would make it too bulky to fit under clothing.
[0009] The above disadvantages may contribute to low patient compliance and limit use. A control unit which is an integral part of a device with a low profile and whose internal components are miniaturized sufficiently so as not to affect the performance of the control unit or the medical device has therefore been sought.
SUMMARY OF THE INVENTION
[0010] According to a first aspect of the present invention, there is provided a control unit for a medical device wherein the control unit comprises a pump, a conduit and control means for controlling the flow of fluid from the pump through the conduit characterized in that the conduit is a rigid internal passage located in the control unit.
[0011] The control unit of the invention has the advantage that, as the conduits are rigid it is possible to make a detachable connection between the control unit and a docking unit which is part of the medical device. This also makes it possible for there to be no external conduits between the control unit and the docking unit on the medical device. In this way, the control unit can be readily attached and detached from the medical device.
[0012] According to a second aspect of the present invention, there is provided a control unit assembly for a medical device wherein the assembly comprises a control unit and a docking unit, the docking unit located on the medical device wherein
a. the control unit comprises a pump, a conduit and control means for controlling the flow of fluid from the pump through the conduit; and b. the docking unit comprises a detachable fluid transfer connector which connects the conduit to an inflatable cell of the device.
[0015] Preferably, the docking unit also comprises a backing plate and the connector is a relatively inflexible connector of the plug and socket type. The connector, preferably, forms an air tight seal and allows the repeated attachment and removal of the control unit. The number and arrangement of the connectors will be adapted to suit the number of cells present in the device.
[0016] The provision of the backing plate with rigid connectors permits direct insertion of the control unit into the device and allows it to be removed and re-inserted. This overcomes the need for remote positioning of the control unit assembly. Instead, the pump draws air or fluid from an external source into the conduits and to the rigid fluid transfer connectors of the backing plate into the cells of the compression device.
[0017] The rigid connectors, where present, act to hold to the control unit assembly securely while permitting the control unit to be readily detached from the compression device. To assist in the securement of the control unit to the device, an additional press-fit retaining means which acts against a spring bias and can be released by the pressing of a button on the control unit may be provided.
[0018] The presence of the docking unit and the detachable fluid connectors gives the advantage that the control unit is removable and, therefore, reusable. This is because typically the control unit assembly is significantly more costly to produce. Designed as a separate unit, it can have a working life of many years and can be transferred between devices and between patients. For cost-effective treatment of patients, the recycling of the control unit, rather than its disposal after each patient, is desirable. In contrast, the medical device whose inner surfaces come into contact with the patient's skin are typically single use and disposed of once no longer required by a particular patient. In any case, compression devices will typically have a working life of no longer than six months. Hence, the easy removal of the control unit assembly from the medical device and replacement on another medical device is advantageous.
[0019] The invention further provides that the conduits in the control unit are preferably rigid internal passages wholly located within the control unit in the form of a manifold.
[0020] The term “manifold” means the fluid transfer conduits that form a labyrinth of passages in the rigid material of the control unit. Preferably, the conduits terminate in connectors suitable for making connections with other components of the control unit assembly and compression device. The manifold replaces the plurality of tubes between the pump and device and makes the control unit compact enough to be received in the docking unit. The docking unit is, preferably, a pouch within the outer contour of the device.
[0021] Preferably, the control unit further comprises a plurality of valves located between the pump and the conduits, the plurality of valves being arranged in a ranked or tiered hierarchical structure
[0022] The term “hierarchical or ranked valve tree structure” means the that valves are arranged in ranks according to their proximity in the direction of fluid flow from the pump. The valve closest to the pump directs fluid flow to a further rank or ranks of valves. In this manner, the number of valves needed in the control unit to control the plurality of inflatable cells is reduced.
[0023] The provision of the ranked valve arrangement permits size reduction of the control unit by reducing the number of valves and, therefore, the space that they occupy and their power consumption. This permits the proximal positioning of the control unit assembly on or within an outer sleeve of a compression device. When placed discretely within an outer sleeve of the compression device, there are no external edges of the control unit which can be knocked or damaged during use resulting in improved patient safety, quality of patient life and control unit life. Furthermore, improved patient compliance is expected with such a discretely concealed unit.
[0024] The ranked valve tree structure of the valve assembly where present, advantageously provides a means of selectively varying the air or fluid pressure of individual cells in the compression device without simultaneously activating all of the valves. Furthermore, the ranked valve tree structure reduces the number of valves required to achieve pressure variation. The tree structure thus permits size reduction in the control unit as fewer valves are needed. Hence, this arrangement is particularly amenable to portable power sources such as a battery. The valves are preferably latching valves as they further reduce the power consumption in the device.
[0025] Further, according to the invention, a compression device for use on a limb comprising a control unit assembly according to the first and second aspects of the present invention is provided.
[0026] Preferably, the one or more detachable fluid transfer connectors of one aspect of the invention is adapted for connection with the air or fluid transfer conduits in the control unit and in the compression device. More preferably, this is achieved by a male connector tube on the control unit assembly being engageable with a female connector slot on the compression device or a female connector slot on the control unit assembly being engageable with a male connector tube on the compression device.
[0027] A latch can be used to retain the male and female parts in place in order to secure the control unit. Preferably, the latch can be easily released so that the control unit assembly can be removed from the compression device, for example, by pushing a button on the exterior of the compression device.
[0028] Any number of rigid air or fluid transfer connectors can be employed. However, preferably, four or five connectors will be present and this will be dependent on the requirements of the compression device. Preferably, the air or fluid transfer connectors are made of a rigid plastics material which can be integrally formed as part of the backing plate. This may be achieved, for example, by means of injection molding techniques during the manufacture of the docking unit or backing plate.
[0029] The control unit assembly of the first and second aspects of the invention may comprise an additional (booster) portable battery as a power source. This may be a re-chargeable nickel cadmium, nickel metal hydride or lithium ion battery or any other lightweight battery that provides sufficient power.
[0030] Preferably, the control unit is attached to the backing plate in a sliding press-fit to engage the connectors and the latch.
[0031] The compression device, preferably, has an outer surface with a pouch for receiving and holding the control unit assembly. The docking unit is positioned in the pouch and can conveniently be in the form of a backing plate.
[0032] The compression device may contain many inflatable cells dependent on the individual needs of a patient and may be adapted for an arm or a leg. In a preferred embodiment, the device is adapted for use below the knee of a patient and comprises three inflatable cells located in the region between the knee and the ankle and two inflatable cells located in the heel and foot region.
[0033] In another embodiment, the invention provides a control unit assembly for a medical device wherein the assembly comprises a control unit and a docking unit, the docking unit located on the medical device wherein the control unit comprises a pump, a conduit and control means for controlling the flow of air through the conduit and the docking unit comprises a detachable air inlet connector which provides air to the pump, the connector being provided with a filter.
[0034] In this way, the air inlet to the pump is provided with a filter on the device side of the assembly. Thus, when the device has reached the end of its useful life and is replaced, the control unit is indirectly provided with a new filter. If the filter were placed in the control unit, it would not be replaced during the lifetime of the control unit without servicing of the unit. In addition, the provision of the filter on the device side of the assembly means that contamination of the control unit and its electrical circuitry is limited. If the filter were present in the control unit, during operation of the device unfiltered air would be drawn into the control unit at least as far as the filter. As the filter is external to the control unit, only filtered air is drawn into the control unit. This gives the advantage that reliability of the control unit may be improved.
BRIEF DESCRIPTION OF THE DRAWINGS
[0035] FIG. 1 is a perspective view of the control unit assembly of the invention integrated in a mobile compression device worn on the limb of a patient.
[0036] FIG. 2 is a perspective view of a backing plate for receiving a control unit to form the assembly of the invention.
[0037] FIG. 3 is a perspective view of one end of the control unit of the invention showing the connectors which engage the connectors of the backing plate in use.
[0038] FIG. 4 is a perspective view of the backing plate and control unit of the assembly removed from the compression device to show the coming together of the connectors and the springs which bias the assembly apart for detachment of the control unit.
[0039] FIG. 5 is a schematic air flow logic diagram of the assembly of the invention.
[0040] FIG. 6 is a schematic view of the interior of the control unit of the assembly of FIG. 1 showing the air manifold.
DETAILED DESCRIPTION OF THE INVENTION
[0041] In FIG. 1 a control unit assembly and compression device according to an embodiment of the invention is shown worn on the leg of a patient. The device comprises a sleeve 2 having a leg cuff 4 connected to a foot cuff 6 . The device also comprises a control unit assembly 8 comprising a control unit 10 . The control unit 10 is small and when removed from the sleeve 2 may be hand held. The control unit 10 is battery powered and rechargeable so that it can be recharged when attached to or detached from the sleeve 2 . FIG. 1 also shows the pouch 12 provided on sleeve 2 for receiving the control unit 10 and the low profile of the assembly. The control unit assembly follows the contour of the device and integrates the assembly into the device.
[0042] FIG. 2 is a perspective view taken from above the device with the control unit 10 removed showing the interior of the pouch 12 and the backing plate 14 . The control unit 10 may be slidably engaged in the pouch 12 and retained in position by a latching means. FIG. 1 shows a release button 22 positioned on the pouch 12 of the device which when depressed releases the control unit 10 from the pouch 12 .
[0043] FIG. 3 is a perspective view of the control unit 10 removed from the pouch 12 and viewed from the bottom, showing the connectors 16 for engagement with the rigid connectors 18 of the backing plate 14 .
[0044] FIG. 4 is a perspective view of the backing plate 14 , removed from the device for the purposes of illustration, showing the rigid connectors 18 for engagement with the connectors 16 of the control unit 10 . FIG. 4 shows the control unit 10 being slid into engagement with the backing plate 14 . As the control unit 10 is slid into the backing plate 14 , it begins to compress two springs 20 which act to bias the control unit 10 and backing plate 14 apart. Further sliding movement of the control unit 10 causes the connectors 16 , 18 to engage in a fluid tight seal and the control unit 10 to engage a latch (not shown) which retains the control unit 10 in the pouch 12 against the springs 20 . The control unit 10 is released from the pouch 12 by depressing button 22 ( FIG. 1 ), the outline of which is visible on the sleeve 2 . The springs 20 then cause the control unit 10 and backing plate 14 to spring apart and the control unit 10 can be removed from the device. The springs 20 can be in the form of a leaf spring located in the backing plate 14 which similarly biases the parts of the assembly apart.
[0045] FIG. 4 also shows air filter 24 provided on the air inlet/outlet connector of the backing plate 14 . As the air filter 24 is provided on the backing plate 14 , it is naturally replaced when the control unit 10 is used with a new device. This reduces the service requirements of the control unit 10 .
[0046] Referring to FIGS. 5 and 6 , the control unit 10 has fluid flow conduits 40 , 42 , 44 , 46 , 48 which terminate in connectors C 1 , C 2 , C 3 , C 4 and an air inlet/outlet C 5 . When a cell is required to be inflated, air is taken in via the conduit 48 by the operation of pump (labeled “PUMP”) and valves V 4 and V 5 under instruction from a processor (not shown). The processor instructs valves V 3 , V 1 and V 2 which are arranged between the air inlet/outlet C 5 and the conduits 40 , 42 , 44 , 46 such that only one of the conduits 40 , 42 , 44 , 46 is operational at any one time. From FIG. 5 it can be seen that valve V 3 directs fluid from/to the air inlet/outlet C 5 to/from either valve V 1 or V 2 which in turn selectively open or close fluid paths to connectors C 1 or C 2 , or C 3 or C 4 . The valves are preferably latching valves.
[0047] A sensor S 1 ( FIG. 6 ) is located in conduit 40 between connector C 1 and valve V 1 in the control unit 10 . Similarly, sensors S 2 , S 3 and S 4 are located in conduits 42 , 44 , 46 , respectively. Sensors S 1 to S 4 are all fluid pressure sensors controlled by a processor (not shown) and arranged to provide an indication of pressure exerted by the respective cells in the device. S 5 independently monitors the pressure in the fluid flow system of the device.
[0048] FIG. 6 also shows the air manifold 50 with its labyrinth of passages that supplies air from the pump to each of the connectors C 1 to C 5 . The air manifold 50 replaces the external tubes needed with prior art devices between a distal control unit and the connectors of the device.
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A control unit for a medical device wherein the control unit comprises a pump, a conduit and control means for controlling the flow of fluid from the pump through the conduit; and wherein the conduit is a rigid internal passage located in the control unit.
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BACKGROUND OF THE INVENTION
The present invention relates to a twin-cylinder circular knitting machine for manufacturing socks and stockings with knitted fabric tensioning device.
Twin-cylinder circular knitting machines are known which have a device for applying tension to the knitted fabric. The device comprises an element for retaining the initial portion of the fabric which is arranged inside the lower needle cylinder proximate to the region where the knitting is formed, and a fluid-activated piston provided with a hollow stem which is open at its ends and can slide inside a cylindrical chamber defined coaxially in the upper needle cylinder.
The retention element faces the lower end of the stem of the piston, and its dimensions are such as to allow the descent of the stem into the lower needle cylinder, passing around said retention element so as to apply tension to the fabric which extends from the retention region to the region of the machine where knitting is formed.
The upper end of the stem can be connected to an aspiration device which aspirates the fabric at the end of the knitting and turns it inside out.
The descent of the piston in order to apply tension to the fabric being formed is obtained by gravity by providing appropriate piston weighting elements, whereas the ascent of the piston is caused by a pressurized fluid which is fed into the cylindrical chamber.
These known types of twin-cylinder machines with device for applying tension to the fabric have some problems.
Due to the fact that the piston stem descends by gravity, damage to the fabric may occur due to excessive traction stresses, particularly in the initial portion of the fabric, when the lower end of the stem makes contact with the fabric and the weight of the piston, the stem and the weighting elements bears on a short length of fabric.
Furthermore, since the stem of the piston is rigidly associated with the upper needle cylinder in rotation about its axis, while the cylindrical chamber in which it slides is defined by a tubular body which is fixed to the supporting structure of the upper needle cylinder, there occurs rapid wear of the gaskets interposed between the piston and the tubular body in which it slides.
The tension application device is furthermore provided with an engagement device which is mounted on the supporting structure of the upper needle cylinder and can engage the piston in order to keep it in a raised position when the application of tension to the fabric is not required. The use of the engagement device which must engage the piston, which rotates together with the upper needle cylinder, complicates the connection between said two elements.
SUMMARY OF THE INVENTION
The aim of the present invention is to obviate the above described problems by providing a twin-cylinder circular knitting machine for manufacturing socks and stockings with a device for applying tension to the fabric which effectively avoids excessive stresses of the fabric so as to ensure its integrity even in the case of fabrics having scarce mechanical strength.
Within the scope of this aim, an object of the invention is to provide a machine with a device for applying tension to the fabric which in any case ensures the application of adequate tension to the fabric during its formation.
Another object of the invention is to provide a device for applying tension to the fabric which has reduced problems of wear of the sealing elements and has a relatively simple construction.
This aim, these objects and others which will become apparent hereinafter are achieved by a twin-cylinder circular knitting machine for manufacturing socks and stockings with a knitted fabric tensioning device, comprising a lower needle cylinder and an upper needle cylinder which are mutually coaxial and activatable with rotary motion about their common axis, a device for applying tension to the knitted fabric being accommodated inside said needle cylinders, said device comprising: means for retaining the fabric proximate to the knitting forming region; a first fluid-activated piston accommodated in said upper needle cylinder and provided with a hollow stem which is open at its ends, the lower end of said stem being engageable, by means of the sliding of said piston parallel to the axis of the needle cylinders, with the knitted fabric being formed in order to apply tension thereto; said retention means having dimensions for allowing said stem to slide outside said retention means, characterized in that it comprises auxiliary actuation means which act on said piston for its descent at a controlled rate at least until the lower end of said stem makes contact with the fabric in the region comprised between said retention means and the knitting forming region, said retention means and said stem being rigidly associated with said upper needle cylinder in rotation about its axis.
BRIEF DESCRIPTION OF THE DRAWINGS
Further characteristics and advantages of the invention will become apparent from the description of a preferred but not exclusive embodiment of the machine with device for applying tension to the fabric according to the invention, illustrated only by way of non-limitative example in the accompanying drawings, wherein:
FIG. 1 is an axial sectional view of the upper needle cylinder and of part of the lower needle cylinder of the machine according to the invention, with the fabric tension application device in an inactive condition; and
FIGS. 2 to 4 are sectional views of the machine, taken similarly to FIG. 1, illustrating the operation of the fabric tension application device.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the above figures, the machine according to the invention, generally designated by the reference numeral 1, comprises a lower needle cylinder 2 and an upper needle cylinder 3 which are mutually coaxial and activatable with rotary motion about their common axis 4.
In particular, the upper needle cylinder 3 is supported so as to be rotatable about the axis 4 by a supporting structure 5 by means of a main bearing 6. The rotary actuation of the upper needle cylinder is obtained, in a known manner, by means of a motor, not illustrated for the sake of simplicity, which is connected to a gearwheel 7 fixed coaxially to the upper needle cylinder 3.
A first tubular body 8 is arranged inside the upper needle cylinder 3 and coaxially thereto, is rigidly associated with said upper needle cylinder in rotating about the axis 4 and is connected, with its upper end, to a duct 9 which can be controllably connected to an aspiration device. The lower end of the first tubular body 8 faces the lower needle cylinder 2 and is arranged proximate to the knitting forming region 10.
The machine according to the invention is provided with a device for applying tension to the fabric comprising fabric retention means which are conveniently constituted by a plug-like element 11 which can slide, in a known manner, inside the lower needle cylinder 2 along the axis 4, in order to engage in the lower end of the first tubular body 8 so as to block the initial end of the fabric which is aspirated along the first tubular body 8.
The fabric tension application means also comprise a first piston 12 which is arranged around the first tubular body 8. The first piston 12 is provided with a hollow stem 15 which is open at its ends, surrounds said first tubular body 8 and extends toward the lower needle cylinder 2. The piston 12, with its stem 15, is arranged between the first tubular body 8 and a second tubular body 14 which is fixed inside the upper needle cylinder for a portion of its length. A first chamber 13 with an annular cross-section is defined between the piston 12-stem 15 assembly and the tubular body 14, on the inner surface of which the piston 12 slides; said chamber is delimited upwardly by a gasket of the piston 12 and downwardly by a gasket 13a which makes contact with the stem 15.
The piston 12 furthermore has an upper extension 12a with which weighting elements 16 are associated in order to facilitate its descent.
The chamber 13 with annular cross-section is connectable to a source of pressurized fluid in order to raise the piston 12. More particularly, a passage 17 is defined in the second tubular body 14, proximate to the lower end of the chamber 13, and connects the chamber 13 to an interspace 18 defined between the second tubular body 14 and the inner surface of the upper needle cylinder 3. The interspace 18 is connected, through a hole 19, to an annular groove 20, defined between the outer surface of the upper needle cylinder 3 and a portion of the supporting structure 5, which is in turn connected to a duct 21 on which a controllable electric valve 22 is arranged. Through the electric valve 22, the chamber with annular cross-section 13 is connectable either to a source of pressurized fluid, for example air, in order to raise the piston 12, or to a discharge to allow its descent.
According to the invention, auxiliary actuation means are provided which act on the piston 12 in order to make it descend at a controlled rate, at least until the lower end of the stem 15 makes contact with the fabric.
Said auxiliary actuation means are constituted by a second piston 23, which is arranged above the first piston 12 and can slide inside a second chamber 24 with annular cross-section defined between the first tubular body 8 and a third tubular body 25, rigidly associated with the first tubular body 8 in rotation about the axis 4.
The chamber 24 is connected, above the piston 23, to a duct 26 which partially extends inside the upper needle cylinder 3 and, similarly to the interspace 18, is connected to an annular recess 27 defined between the outer surface of the upper needle cylinder 3 and a portion of the supporting structure 5, which is in turn connected to a further duct 28 on which a flow regulator 29 and an electric valve 30 are arranged; said electric valve can be controllably connected to a source of pressurized fluid, for example air, or to a discharge.
Springs 31 for the return of the piston 23 are arranged in the chamber 24 below the piston 23.
The second piston 23 is provided with retention means 32 which can be controllably engaged with, or disengaged from, the extension 12a of the first piston 12. Said retention means are constituted by hook-like elements 33 which are associated with the second piston 23 and protrude downward from the second chamber 24.
Each hook-like element 33 is pivoted to the piston 23 with its upper end so that it can oscillate in a plane which is radial to the upper needle cylinder so that its lower end engages with, or disengages from, the extension 12a of the piston 12.
The oscillation of the hook-like elements 33 is obtained by means of cam-shaped abutments 34 and 35 which are applied respectively to the first tubular body 8 and to the inner surface of the third tubular body 25, so as to cause an oscillation of the hook-like elements toward the axis 4, when the piston 23 has completed its descent in order to disengage from the extension 12a of the piston 12, and in the opposite direction, when the piston 23 is completing its ascent in order to engage the extension 12a.
It should be noted that the assembly constituted by the first tubular body 8, by the second piston 2 with hook-like elements 33 and by the third tubular body 35, as well as the assembly constituted by the first piston 12 and by the second tubular body 14, is rigidly associated with the upper needle cylinder, and thus there is a reduced wear of the gaskets 36 and 37 arranged on the pistons 12 and 23 and the use of bearings for connection between the various elements is not required.
Conveniently, means are provided for detecting the axial position of the first piston 12; said means are constituted by a pair of sensors 38 and 39, for example of the electromagnetic type, which are spaced along the axis 4 and are applied to a housing 40 which is fixed to the supporting structure 5 and surrounds the upper portion of the first tubular body 8.
The operation of the fabric tension application device according to the invention is as follows.
When the knitting of the fabric begins, the plug-like element 11 is spaced downward from the first tubular body 8, which is connected to an aspiration device so as to draw inside it the initial portion of the formed knitted fabric. The first piston 12 is engaged by the hook-like elements 33, and the second piston 23 is in the maximum rise condition by virtue of the action of the springs 31, since the second chamber 24 is connected to the atmosphere by the electric valve 30 (FIG. 1).
After the initial portion of fabric has been drawn into the first tubular body 8, the plug-like element 11 is raised so as to enter the lower end of the first tubular body 8, locking the fabric. At this stage, the position of the electric valve 30 is switched so as to cause the progressive descent of the second piston 23 and of the first piston 12, which is still engaged with the hook-like elements 33. The descent rate of the first piston 23 can be adjusted by means of an appropriate setting of the flow regulator 29, so that the contact of the lower end of the stem 15 with the fabric in the region comprised between the first tubular body 8 and the knitting forming region 10 occurs without damaging the fabric, even in the case of fabrics having low mechanical strength (FIG. 2).
After the lower end of the stem 15 has made contact with the fabric and the application of tension thereto has thus begun, i.e. when the second piston 23 has almost completed its descent, the hook-like elements 33 are disengaged, by virtue of the action of the abutment 35, from the first piston 12, which continues its descent by gravity, continuing to apply tension to the fabric (figure 3).
At the end of the formation of the fabric, the first chamber 13, which has so far been connected to the atmosphere, is connected by means of the electric valve 22 to a source of compressed air so as to raise the first piston 12 (FIG. 4), while the plug-like element 11 is disengaged from the first tubular body 8 so that the fabric is drawn along said first tubular body 8 and unloaded, in a known manner, outside the machine.
At the end of the ascent of the piston 12, the position of the electric valve 30 is switched again; by connecting the second chamber 24 to the atmosphere, said electric valve raises the second piston 23, with consequent engagement of the hook-like elements 33 with the extension 12a by virtue of the presence of the abutment 34.
At this stage, the position of the electric valve 22 is switched again, and the cycle restarts as already described.
In practice it has been observed that the machine with the tension application device according to the invention fully achieves the intended aim, since by allowing to adjust the descent rate of the tension application piston so as to contain the stresses discharged onto the fabric at the moment of contact, it avoids ripping and tearing of the fabric when tensioning begins.
Furthermore, by virtue of the fact that the actuation elements which make contact with the tension application cylinder are rigidly associated with the upper needle cylinder in its rotation about its axis, reduced wear occurs and the entire arrangement of the fabric tensioning device is simplified.
The machine with the fabric tensioning device thus conceived is susceptible to numerous modifications and variations, all of which are within the scope of the inventive concept; all the details may furthermore be replaced with technically equivalent elements.
In practice, the materials employed, as well as the dimensions, may be any according to the requirements and the state of the art.
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The twin-cylinder circular knitting machine with knitted fabric tensioning device having members for retaining the fabric proximate to a knitting forming region. A first fluid-activated piston is accommodated in the upper needle cylinder and is provided with a hollow stem which is open at its ends. The lower end of the stem is engageable, by means of the sliding of the piston parallel to the axis of the needle cylinders, with the knitted fabric being formed in order to apply tension thereto. The retention members have dimensions for allowing the stem to slide outside of the retention members. The tensioning device also has an auxiliary actuation piston which acts on the piston to achieve its descent at a controlled rate at least until the lower end of the stem of the piston makes contact with the fabric in the region comprised between the retention members and the knitting forming region.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is directed to a sound signal generating apparatus and method for reducing pop noise in a class-D amplifier.
2. Discussion of the Related Art
Audio signal amplifiers used for amplifying audio signals are generally classified into classes A, AB, B, C, and D depending on their operating state during power amplifying stage.
Among the various classes of audio signal amplifiers, the class-D amplifiers are more popular because their efficiency is higher than that of class AB amplifiers and their linearity is also superior due to low cross-over.
Class-D amplifiers are also referred to as switch-mode amplifiers because they resemble switch-mode voltage regulators. A class-D amplifier uses Pulse Width Modulation (PWM) method on an input analog signal or digital PCM signal. This means an input analog signal is modulated by a higher frequency modulation or carrier signal, usually a saw-tooth triangular wave or an input digital PCM signal is converted to a related PWM signal. Upon pulse width modulation, the analog input signal or digital PCM signal becomes discreet or digital with pulse widths used to represent signal strengths of the input original.
The PWM signal presented to the amplifier is a high frequency digital signal with varying widths. A low band pass filter is used to filter the high frequency component to extract the input signal and reduce switching noise.
FIG. 1 shows a waveform of input signals PWMA and PWMB being applied to a conventional class-D amplifier, wherein pulse width modulating signals PWMA, PWMB have substantially the same pulse width but are opposite to each other in phase. FIG. 2 shows a waveform of a speaker voltage VC 1 when PWMA, PWMB and power DET 1 are applied (Here, DET 1 is transited from “Low” to “High” when voltage is turned on). It can be seen from FIG. 2 that a severe overshoot occurs at or near the time when power is applied. The overshoot is caused by the same pulse width of the pulse width modulating signals PWMA, PWMB. This overshoot voltage VC 1 at the speaker results in ‘click or pop’ noise.
Therefore, a need exists for an apparatus and a method for generating PWM signals which operate a class-D amplifier but without the pop noise upon application of power or when power is removed from the amplifier.
SUMMARY OF THE INVENTION
A circuit is provided for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same phase and an opposite phase relationship with the PWM second signal, the circuit comprising: a power detector for detecting power turn on to the amplifier and outputting a power on signal; and a pulse generator having: a duty cycle generator for generating a first pulse signal corresponding to the PWM first signal and a second pulse signal corresponding to the PWM second signal; and a pulse reducing generator for generating a reduced-width first pulse or a reduced-width second pulse for outputting to the amplifier upon receipt of the power on signal.
Preferably, the pulse generator further includes a controller for outputting the reduced-width first pulse or the reduced-width second pulse upon receipt of the power on signal and for outputting the first pulse signal and the second pulse signal to the amplifier thereafter.
According to this embodiment, the circuit further preferably includes a select circuit for generating a select signal for selecting between the PWM first and second signals during one selection mode and the signals from the pulse generator during another selection mode, and a counter for counting time upon receipt of the power on signal and to output the select signal in the another selection mode upon reaching a predetermined count for outputting the PWM first and second signals to the amplifier, wherein the reduced-width first pulse is about one-half the pulse width of the first pulse signal.
According to an aspect of the invention, the circuit further includes a delay for delaying by a predetermined time the first pulse signal to output a delayed first pulse signal that transitions with a delay by the predetermined time to provide a time gap between the transition of the delayed first pulse signal and the transition of the second pulse signal, wherein the amplifier includes a serially connected pair of transistors for receiving at their gates the first pulse signal and the second pulse signal.
According to another embodiment of the present invention, a circuit is provided for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same and an opposite phase relationship with the PWM second signal, the circuit comprising: a power detector for detecting power turn off to the amplifier and outputting a power off signal; and a counter for counting the duration of the pulse width of the PWM first signal, the counter being activated upon detection of the power off signal, and for outputting a select signal upon reaching a predetermined reduced-width time count to cause an output of a reduced pulse width PWM first signal or reduced pulse width PWM second signal prior to complete power turn off from the amplifier. Preferably, the circuit further includes a synchronizing circuit for synchronizing the power off signal using a system clock, wherein the amplifier includes a pair of transistors for receiving at their gates the PWM first signal and the PWM second signal.
The circuit further includes a mute circuit for outputting the select signal to cause an output of a reduced pulse width PWM first signal or reduced pulse width PWM second signal upon receipt of a mute signal, wherein the mute circuit is an AND gate, and wherein the reduced pulse width PWM first signal or reduced pulse width PWM second signal is the last pulse signal received by the amplifier prior to complete power turn off, and wherein the reduced-width is about one half of the width of the PWM first signal or the PWM second signal.
According to still another embodiment of the invention, a circuit is provided for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same phase and an opposite phase relationship with the PWM second signal, the circuit comprising: a power detector for detecting power turn on to the amplifier and outputting a power on signal and detecting a power turn off to the amplifier and outputting a power off signal; a pulse generator having: a duty cycle generator for generating a first pulse signal corresponding to the PWM first signal and a second pulse signal corresponding to the PWM second signal, and a reduced-width generator for generating at least one of a reduced-width first pulse and a reduced-width second pulse; a controller for selecting one of the reduced-width first pulse and the reduced-width second pulse for outputting to the amplifier upon receipt of the power on signal and for selecting the first pulse signal and the second pulse signal for outputting to the amplifier thereafter; and a counter for counting the duration of the pulse width of the PWM first signal, the counter being activated upon detection of the power off signal and a select circuit for outputting an off select signal upon reaching a predetermined reduced-width time count to cause an output of one of a reduced-width PWM first signal and a reduced-width PWM second signal, wherein the select circuit further includes a counter for counting time upon receipt of the power on signal and to output an on select signal for first outputting one of the reduced-width first pulse and the reduced-width second pulse and then the first pulse signal and the second pulse signal to the amplifier.
The circuit according to this embodiment further includes a mute circuit for outputting the on select signal for outputting one of the reduced-width first pulse and the reduced-width second pulse to the amplifier upon receipt of a mute signal, wherein the mute circuit is synchronized using a system clock and upon mute inactivation, to cause an output of one of the reduced-width PWM first signal and the reduced-width PWM second signal, wherein the reduced-width first pulse signal has a pulse width about one half of the pulse width of the first pulse signal, and wherein the predetermined reduced-width time count is about one half the duration of the pulse width of the PWM first signal.
The circuit according to this embodiment further includes a delay for delaying by a predetermined time the first pulse signal to output a delayed first pulse signal that transitions with a delay by the predetermined time to provide a time gap between the transition of the delayed first pulse signal and the transition of the second pulse signal, wherein the amplifier includes a pair of transistors for receiving at their gates the delayed first pulse signal and the second pulse signal, wherein the amplifier includes a pair of transistors for receiving at their gates the first pulse signal and the second pulse signal.
According to another aspect of the invention, a method is provided for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same phase and an opposite phase relationship with the PWM second signal, the method comprising: detecting power turn on to the amplifier and outputting a power on signal; and generating a first pulse signal corresponding to the PWM first signal and a second pulse signal corresponding to the PWM second signal; and generating a reduced-width first pulse or a reduced-width second pulse for outputting to the amplifier upon receipt of the power on signal.
Preferably, the method further includes outputting the reduced-width first pulse or the reduced-width second pulse to the amplifier upon receipt of the power on signal and outputting the first pulse signal and the second pulse signal to the amplifier thereafter, and generating a select signal for selecting between the PWM first and second signals during one selection mode and the first pulse signal and the second pulse signal during another selection mode for outputting to the amplifier, wherein the reduced-width first pulse is about one-half the pulse width of the first pulse signal.
According to still another aspect of this embodiment, the method further includes delaying by a predetermined time the first pulse signal to output a delayed first pulse signal that transitions with a delay by the predetermined time to provide a time gap between the transition of the delayed first pulse signal and the transition of the second pulse signal, and the steps of: detecting power turn off to the amplifier and outputting a power off signal; counting the duration of the pulse width of the PWM first signal upon detection of the power off signal; and outputting a select signal upon reaching a predetermined reduced-width time count to cause an output of a reduced pulse width PWM first signal or reduced pulse width PWM second signal prior to complete power turn off from the amplifier, wherein the reduced pulse width PWM first signal or reduced pulse width PWM second signal is the last pulse signal received by the amplifier prior to complete power turn off, and wherein the reduced-width is about one half of the width of the PWM first signal or the PWM second signal.
According to still another embodiment of the present invention, a circuit is provided for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same phase and an opposite phase relationship with the PWM second signal, the circuit comprising: means for detecting power turn on to the amplifier and outputting a power on signal and detecting a power turn off to the amplifier and outputting a power off signal; means for generating a first pulse signal corresponding to the PWM first signal and a second pulse signal corresponding to the PWM second signal, and a reduced-width generator for generating at least one of a reduced-width first pulse and a reduced-width second pulse; means for selecting one of the reduced-width first pulse and the reduced-width second pulse for outputting to the amplifier upon receipt of the power on signal and for selecting the first pulse signal and the second pulse signal for outputting to the amplifier thereafter; and a counter for counting the duration of the pulse width of the PWM first signal, the counter being activated upon detection of the power off signal and a select circuit for outputting an off select signal upon reaching a predetermined reduced-width time count to cause an output of one of a reduced-width PWM first signal and a reduced-width PWM second signal.
BRIEF DESCRIPTION OF THE DRAWINGS
The embodiments of the present invention will become more apparent when detailed description of embodiments are read with reference to the accompanying drawings in which:
FIG. 1A shows a waveform of a PWM switching signal and FIG. 1B shows a class-D amplifier;
FIG. 2 shows an overshoot response of a speaker voltage when used with the amplifier of FIG. 1 ;
FIG. 3 shows a block diagram of a switching signal generating apparatus according to an embodiment of the present invention;
FIG. 4 shows a circuit of a half-bridge typed class-D amplifier having one power source;
FIG. 5A shows a circuit of a half-bridge typed class-D amplifier having two power sources;
FIG. 5B is a circuit of a full-bridge typed class-D amplifier having one power source;
FIG. 6 shows a detail block diagram of a pulse signal generating circuit of FIG. 3 ;
FIG. 7 shows waveforms of a first detecting signal DET 1 and first and second pulse signals PUL 1 , PUL 2 from the pulse signal generating circuit according to an embodiment of the present invention.
FIG. 8 shows switching waveforms at a time of power-on for the switching signal generating apparatus;
FIG. 9 shows switching waveforms at a time of power-off for the switching signal generating apparatus;
FIG. 10 shows a block diagram of a switching signal generating apparatus according to another embodiment of the present invention;
FIG. 11 shows switching waveforms at a time of mute-on and mute-off for the switching signal generating apparatus;
FIG. 12 is a graph showing a response of speaker voltage in an audio sound regenerating apparatus according to an embodiment of the present invention;
FIG. 13 is a flowchart showing a method of generating a switching signal according to an embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. It should be noted that like reference numerals are used for designation of like or equivalent parts or portion for simplicity of illustration and explanation.
FIG. 3 is a switching signal generating apparatus 600 according to a preferred embodiment of the present invention.
Referring to FIG. 3 , the switching signal generating apparatus 600 includes a power detecting circuit 610 , a pulse signal generating circuit 620 , a first selection circuit 630 , an audio signal processor 640 , a second selection circuit 650 , and a dead time controlling circuit 660 .
The general operation of the switching signal apparatus 600 is herein described. The power detecting circuit 610 detects power turn-on and outputs a first detecting signal DET 1 to the pulse signal generating circuit 620 . The power detecting circuit 610 also detects a disconnection of the power supply or power off and outputs a second detecting signal DET 2 , which is output to the audio signal processor 640 . The power detecting circuit 610 receives a timing signal PPS for synchronizing timing signals of the device to a system clock. The period of the timing signal PPS corresponds to the period of the PWM signals generated from the audio signal processor 640 . Further, the power detecting circuit 610 generates and outputs a control signal SEL to the pulse signal generating circuit 620 , the first selection circuit 630 , and the second selection circuit 650 .
The pulse signal generating circuit 620 generates a first pulse signal PUL 1 and a second pulse signal PUL 2 in response to the first detecting signal DET 1 and control signal SEL. A system clock signal can be used to synchronize the pulse signals PUL 1 and PUL 2 . According to at least one preferred embodiment according to the present invention, the pulse signals PUL 1 and PUL 2 are shaped by the pulse signal generating circuit 620 to output at opposite phase and to have initial smaller pulse widths upon application of the first detecting signals DET 1 to prevent simultaneous turn-on of the transistors on the audio sound regeneration circuit.
The audio signal processor 640 receives an audio input signal AUDIO and modulates the audio input signal AUDIO with a pulse train to output a pulse width modulated audio signal APWM, wherein the width of the pulses represent the strengths of the input audio signal. The audio signal processor 640 outputs the pulse width modulation period PPS and is preferably inactivated when the second detecting signal DET 2 is active, signaling power off.
The first selection circuit 630 selects either the first pulse signal PUL 1 or the pulse width modulated audio signal APWM in response to the control signal SEL and outputs a first selected signal MUXA. The second selection circuit 650 selects either the second pulse signal PUL 2 or the pulse width modulated audio signal APWM in response to the control signal SEL and outputs a second selected signal MUXB. Thus, each output signal from the first and second selection circuits 630 , 650 is either the pulse signals PUL 1 , PUL 2 or the pulse width modulated audio signal APWM in opposite phase. The first and second selection circuits 630 , 650 are preferably multiplexers.
The dead time controlling circuit 660 receives the first and second selected signals MUXA, MUXB from the first and second selection circuits 630 , 650 , respectively. According to an embodiment of the present invention, the dead time controlling circuit 660 includes delay elements (not shown) for delaying the switching signals by a predetermined dead time. Preferably, the delay is applied to the rising (transition from low to high) edges of the MUXA and MUXB signals. This dead time delay creates a time gap between the transition of the delayed first pulse signal and the transition of the second pulse signal to prevent simultaneously turning on or off the transistors in an audio sound regenerating apparatus. The dead time controlling circuit 660 outputs first and second switching signals PWMA, PWMB to the audio sound regenerating apparatus.
FIG. 4 shows a half-bridge type audio sound regenerating apparatus 680 , which includes two MOS transistors 101 , 103 connected in series, two diodes M 1 , M 2 , a band pass filter having an inductance L and a capacitor C, and a speaker 105 . One terminal of each of the diode M 1 and M 2 is connected to a source of the transistor and the other terminal of each of the diode is connected to a drain of the transistor.
The first and second switching signals PWMA, PWMB generated from the switching signal generating circuit 600 are inputted into the gates of the MOS transistors 101 , 103 , respectively, and are amplified by the MOS transistors 101 , 103 corresponding to the first and second switching signals PWMA, PWMB. Since the first and second amplified switching signals PWMA and PWMB include a sound component and a switching frequency component, a low frequency band pass filter is used to filter the switching frequency component to recover the sound signal.
FIG. 5A shows an alternate audio sound regenerating apparatus, which is a half-bridge type having two transistors 101 , 103 , two power sources ½Vdc, ½Vdc, a band pass filter having an inductance L and a capacitor C, and a speaker 105 . FIG. 5B shows another audio sound regenerating apparatus which is a full-bridge type having one power source Vdc, four transistors 101 , 103 , 301 , 303 , and a band pass filter L 1 , L 2 , C. One skilled in the art can readily appreciate that the audio sound regenerating apparatus 680 applicable to the present invention is not limited to the apparatus shown in FIGS. 4 , 5 A and 5 B, but includes any audio sound regenerating apparatus having at least two transistors with respective gates for receiving switching signals PWMA, PWMB, and a low band pass filter.
FIG. 6 is an exemplary circuit diagram of the pulse signal generating circuit 620 of FIG. 3 . This circuit receives as inputs the power-on detect signal DET 1 and signal SEL from power detect circuit 610 to generate pulse signals PUL 1 and PUL 2 . Upon transition from ‘Low’ to ‘High’ of the DET 1 signal, the half-pulse generators 622 and 623 generate initial pulses at half width (quarter cycle) to output through MUX 626 and MUX 627 the initial pulses of PUL 1 and PUL 2 with a pulse width equal to one half (½) of the pulse width of modulated audio signal APWM. Then, MUX 626 and MUX 627 are selected to pass through signals output from the 50 : 50 pulse generators 624 in response to control signals from controllers 625 , with duty cycle the same as system clock CLK and same period as pulse period signal PPS. According to an alternative embodiment, only one of the two half-pulse generators 622 and 623 is employed, depending on whether transistors 101 , 301 , 103 , 301 are NMOS or PMOS type, to generate an initial half pulse at either PUL 1 or PUL 2 .
FIG. 7 ( a ) shows waveforms of the first detecting signal DET 1 and the first and second pulse signals PUL 1 , PUL 2 in case that the MOS transistors 101 , 303 , 103 , 301 of FIGS. 1 and 3 are NMOS transistors. It can be seen that signals PUL 1 and PUL 2 are opposite in phase at all times. FIG. 7 ( b ) shows waveforms of the first and second pulse signals PUL 1 , PUL 2 applicable when the MOS transistors 101 , 303 of FIGS. 1 and 3 are PMOS transistors and the MOS transistor 103 , 301 are NMOS transistors. It can be seen that signals PUL 1 and PUL 2 are in phase at all times.
FIG. 8 shows switching waveforms at a time of power-on for the switching signal generating apparatus 600 and switching signals PWMA, PWMB. With select signal SEL initially at logic level ‘Low’, signals PUL 1 and PUL 2 are output through first select circuit 630 and second select circuit 650 as PWMA and PWMB.
Operation of the switching signal generating apparatus 600 is further described with reference to FIGS. 3 , 6 , 7 , and 8 . When power PW is supplied to the switching signal generating apparatus 600 , the power detecting circuit 610 outputs the first detecting signal DET 1 with transition from logic level ‘Low’ to logic level ‘High’ to the pulse signal generating circuit 620 . The power detecting circuit 610 also outputs signal SEL, initially having logic level ‘Low’, to the pulse signal generating circuit 620 , the first selection circuit 630 , and the second selection circuit 650 .
The pulse signal generating circuit 620 generates the first pulse signal PUL 1 and the second pulse signal PUL 2 in response to the first detecting signal DET 1 , as shown in FIGS. 7 ( a ) and 7 ( b ). The audio signal processor 640 outputs the pulse width modulated audio signal APWM.
The first selection circuit 630 outputs the first selected signal MUXA to the dead time controlling circuit 660 and the second selected signal MUXB to the dead time controlling circuit 660 in response to the ‘Low’ level of the control signal SEL.
The dead time controlling circuit 660 outputs the first and second switching signals PWMA, PWMB to the MOS transistors of the audio sound regenerating apparatus 680 ( FIGS. 4 , SA and 5 B).
It can be seen from FIGS. 7 ( a ) and 8 that a width Tonf of a first pulse 701 of the first pulse signal PUL 1 is about Ton/2, and is smaller than each width (Ton) of other pulses 702 , 703 , 704 , 705 . The first pulse 701 represents a first generated pulse of the first pulse signal PUL 1 at the pulse signal generating circuit 620 when the power PW is supplied. The pulses 703 , 705 represent second and third pulses, respectively, of the first pulse signal PUL 1 . The pulse 702 represents a first pulse of the second pulse signal PUL 2 , and the pulse 704 represents a second pulse of the second pulse signal PUL 2 . Preferably, the pulse width Tonf of the first pulse 701 of the first pulse signal PUL 1 is about one half the width of the other pulses 702 , 703 , 704 , 705 . Further, the width Tonf of the first pulse 701 of the first pulse signal PUL 1 is about a quarter (¼) cycle of the other pulses 702 , 703 , 704 . Each cycle (Tsw) of the other pulses 702 , 703 , 704 , 705 is the same as a cycle of the pulse width modulated audio signal APWM. A width of an (n)-th pulse is substantially the same as a width of an (n+1)-th pulse. The initial pulse width 701 applied to the transistor of a class-D amplifier (e.g., 101 in FIG. 4 ) acts to turn on the transistor at reduced energy upon application of power, thus the pop-noise is minimized since an excess response is minimized. Although the initial pulse width of PUL 1 or PUL 2 is reduced to one half pulse width as described, other pulse width reductions, such as one quarter to one third pulse width can also be applicable to reduce pop noise.
After a predetermined time is passed, the control signal SEL is changed from logic ‘Low’ to logic ‘High’, and the pulse signal generating circuit 620 is disabled in response to the active (logic ‘High’) control signal SEL. Then, the output of the audio signal processor 640 , the pulse width modulated audio signal APWM, is selected by the first and second selector circuits 630 and 650 to the dead time control circuit 660 . According to an embodiment of the present invention, the predetermined time is set by a manufacturer as a default value or by a user as any value. According to the embodiment as shown in FIG. 8 , the predetermined time is about 2½ cycles.
The dead time control circuit 660 outputs the first and second switching signals PWMA, PWMB to the MOS transistors of the class-D amplifiers 408 (FIGS. 4 and 5 ). According to an embodiment of the present invention, the predetermined dead time (DT) is a time for protecting simultaneously turning-on or off of the MOS transistors 101 , 103 , 301 , 303 . The dead time control circuit 660 makes smaller the width of at least one the first and second switching signals PWMA, PWMB by the predetermined dead time (DT), thus preventing simultaneously turning-on or off the MOS transistors 101 , 103 , 301 , 303 . The dead time controlling circuit 660 includes delay elements for implementing the delay (dead time) to make smaller one or both switching signals PWMA and PWMB shorter in pulse width at logic ‘High’. According to one embodiment, the delay is applied to the rising edges of both switching signals PWMA and PWMB.
Referring again to FIG. 8 , the switching signal generating apparatus 600 outputs the first and second switching signals PWMA, PWMB during the predetermined period “Tp” (or “Starting Mode”). During the “Tp” period, the first and second switching signals PWMA, PWMB are substantially the same as the first and second pulse signals PUL 1 , PUL 2 . After “Tp” period, the switching signal generating apparatus 600 outputs the first and second switching signals PWMA, PWMB during a “Ta” period (or “Sound PWM Mode”). During the “Ta” period, the first and second switching signals PWMA, PWMB are substantially the same as the pulse width modulated audio signal APWM. According to an embodiment of the present invention, the pulse widths 702 , 704 of the second switching signal PWMB are smaller than the signal PWMA, preferably at an amount of 2*DT, as compared to switching signal PWMA, pulses 703 and 705 .
Protective measures applicable to power-off from the amplifier is described with reference to FIG. 9 , which shows switching waveforms at a time of power-off for the switching signal generating apparatus 600 .
According to a preferred embodiment of the invention, the audio signal processor 640 estimates on-periods Ton 1 , Ton 2 of signal APWM and outputs an estimated value PPS to the power detecting circuit 610 . Preferably, the pulse period or duration of each cycle of the first and second switching signals PWMA, PWMB are substantially constant, and the on-periods Ton 1 , Ton 2 are variable according to an audio signal AUDIO. The cycle duration is preferably estimated by using a counter (not shown). This counter value can be stored in a buffer unit (not shown) and the buffer is updated with the estimated value PPS every cycle. The estimated value PPS is used for controlling a pulse width 903 to reduce pop-noise when the supplied power PW is turning off, that is, the power PW transitions from level ‘High’ to level ‘Low’.
During power-off, the power detecting circuit 610 , the pulse signal generating circuit 620 , and the audio signal processor 640 can be disabled. The power detecting circuit 610 detects the power-off and outputs a second detecting signal DET 2 to the audio signal processor 640 . The audio signal processor 640 stops the operation of pulse width modulation in response to the second detecting signal DET 2 . According to an embodiment of the present invention, the second detecting signal DET 2 is changed to a logic ‘Low’ (or inactivated) at a reduced pulse width, preferably at half period of the on-period Ton 2 or at quarter-cycle. Thus, the width of a pulse 903 is smaller than the width Ton 2 of the pulse 902 , pulse 903 , being the last pulse before the power is off. Preferably, the width of the pulse 903 is substantially a half-width of the pulse 902 or a quarter of a period of a normal cycle of the first or second switching signal PWMA or PWMB. The reduced pulse width is a function of the counter value stored in the buffer. For example, an one third pulse width in pulse 903 is obtained by transitioning DET 2 from ‘High’ to ‘Low’ at one third the time value stored in the buffer.
FIG. 10 is a block diagram of a switching signal generating apparatus 1000 according to another embodiment of the present invention. The switching signal generating apparatus 1000 controls an on-period of first and second switching signals PWMA, PWMB in response to a mute signal/MUTE.
Referring to FIG. 10 , the switching signal generating apparatus 1000 includes a power detecting circuit 610 , a pulse signal generating circuit 620 , a first selection circuit 630 , a audio signal processor 641 , a second selection circuit 650 , a dead time controlling circuit 660 , and a logic gate 1010 .
The power detecting circuit 610 detects a supplied power PW and generates a pre-control signal PSEL. The pre-control signal PSEL is input to one of two inputs of logic gate 1010 . The output of the logic gate 1010 is control signal SEL, which functions similarly as the SEL signal in FIG. 3 to select between PUL 1 and PUL 2 or APWM to output from selectors 630 and 650 , respectively.
The audio signal processor 641 outputs a mute control signal CMUTE to the logic gate 1010 in response to mute signal/MUTE. The audio signal processor 641 controls the time when CMUTE is active or inactive. The operations and functions of the audio signal processor 641 of the present embodiment are substantially the same as the audio signal processor 640 in FIG. 3 , with the exception of the ability to disable the control signal (SEL) by the audio signal processor 641 via the CMUTE signal. According to the present embodiment, the logic gate 1010 is preferably an AND gate or an equivalent gate of the AND gate. The logic gate 1010 receives the mute control signal CMUTE and the pre-control signal PSEL, and generates a control signal SEL.
FIG. 11 shows switching waveforms at mute-on and mute-off for the switching signal generating apparatus 1000 in FIG. 10 . Referring to FIGS. 10 and 11 , when the switching signal generating apparatus 1000 is operated as a “sound pulse width modulating (PWM) mode”, the PSEL signal is at logic ‘High’ and mute signal/MUTE is inactive at logic ‘High’ (or “mute-off mode”). During the mute-off mode, the switching signal generating apparatus 1000 outputs first and second switching signals PWMA, PWMB substantially the same as pulse width modulated audio signal APWM outputted from the audio signal processor 641 .
When the mute signal/MUTE is transited to a logic ‘Low’ (or “mute-on mode”), the audio signal processor 641 in turn outputs a mute control signal CMUTE to the logic gate 1010 . When the mute control signal CMUTE is transited to a logic ‘Low’, the control signal SEL is transited to a logic ‘Low’. During a sound PWM mode, the pre-control signal is at a ‘High’ level, the control signal SEL is transited to the same logic level as the logic level of the mute control signal CMUTE. As in the embodiment described above for power turn-off with reference to FIG. 9 , the audio signal processor 641 estimates the pulse width of an “on-period” (Ton 1 ). The audio signal processor 641 can further generate the mute control signal CMUTE to control the “on-period” of the last pulse 1103 at a reduced pulse width prior to the mute controller.
The first selection circuit 630 and the second selection circuit 650 are switched in response to the control signal SEL. Preferably, the first selection circuit 630 and the second selection circuit 650 are switched when the pulse width Ton 1 f (or on-period) of the pulse 1103 is less than the pulse width Ton 1 (or on-period) of the pulse 1101 , preferably, Ton 1 f is one half of Ton 1 . The audio signal processor 641 outputs the pulse width modulated audio signal APWM. Thus, pop-noise generated the class-D amplifier is reduced in response to the pulse 1103 .
Further, when the mute-on mode is transited to the mute-off mode, the mute signal/MUTE is transited to a logic ‘High’. The audio signal processor 641 outputs the mute control signal CMUTE to the AND gate 1010 for transiting the control signal to a logic ‘High’ in response to the mute signal/MUTE. The audio signal processor 641 can thus generate the mute control signal CMUTE to control “on-period” of pulse 1105 .
The AND gate 1010 outputs the control signal SEL having a logic ‘High’ in response to the mute control signal CMUTE having a logic ‘High’ and the pre-control signal PSEL having a logic ‘High’.
The first selection circuit 630 and the second selection circuit 650 are switched in response to the control signal SEL having a logic ‘High’. The first selection circuit 630 and the second selection circuit 650 is switched when pulse width Ton 3 f (or on-period) of the pulse 1105 is less than the pulse width Ton 3 (or on-period) of the pulse 1107 . According to a preferred embodiment of the present invention, the on-period of the pulse 1105 is about a half of the on-period of the pulse 1107 . Thus, any pop-noise that may be generated by the pulse 1105 would be less as compared to pop-noise that may be generated by the pulse 1107 .
FIG. 12 is a graph showing a response of speaker voltage in an audio sound regenerating apparatus according to an embodiment of the present invention. Voltage Vc 1 in FIG. 12 is smaller than voltage Vc 1 in FIG. 2 and the overshoot response is considerably reduced compared to the conventional overshoot response in FIG. 2 . Therefore, pop-noise for the sound signal generating apparatus (class-D amplifier) is reduced by using the switching signal generating apparatus 600 or 1000 .
FIG. 13 is a flowchart showing a method of generating a switching signal according to an embodiment of the present invention. Referring to FIGS. 3 , 10 , and 13 , first, power is on (Step 1400 ). The power detecting circuit 610 detects whether the power is on (Step 1401 ). When the power is on, the power detecting circuit 610 outputs a first detecting signal DET 1 (Step 1403 ). The pulse signal generating circuit 620 generates pulse signals PUL 1 , PUL 2 (Step 1405 ). An initial first pulse 701 has a half width as compared to pulses 702 , 703 , 704 .
The control signal SEL generated from the power detecting circuit 610 transits from a logic ‘Low’ to a logic ‘High’ after passing a predetermined period. The predetermined period is a period for stabilizing the pulse width modulated audio signal APWM generated from the audio signal processor 640 or 641 . Regular pulse signals PUL 1 and PUL 2 are output after the initial reduced width signals (Step 1407 ).
Upon stabilization of the pulse width modulated audio signal APWM, the first selection circuit 630 and the second selection circuit 650 are selected to output PWM signals in sound PWM mode in response to the control signal SEL at logic ‘High’ (Step 1409 ).
When power PW is disconnected or being burned-off, the power detecting circuit 610 detects power-off and outputs the second detecting signal DET 2 to the audio signal processor 640 (Step 1410 ). As shown in FIG. 9 , the second detecting signal DET 2 transits to inactive level when the last pulse width 903 is about half width of the pulse width 902 . Then, the sound PWM mode is stopped when power is completely off (Step 1411 ).
The audio signal processor 640 detects a state of the mute signal/MUTE and determines whether the mute signal/MUTE is in a state of mute-on. If the mute signal/MUTE is not in a state of mute-on, the switching signal generating apparatus 1000 performs a sound PWM mode. While the switching signal generating apparatus 1000 is in a state of mute-on, the audio signal processor 641 outputs a mute controlling signal CMUTE to the AND gate 1010 . The first selection circuit 630 and the second selection circuit 650 are switched in response to the control signal SEL.
Although the present invention has been described herein with reference to the accompanying drawings, it is to be understood that the present invention is not limited to those precise embodiments, and various other changes and modifications may be affected therein by one skilled in the art without departing from the scope and spirit of the invention. All such changes and modifications are intended to be included within the scope of the invention as defined by the appended claims.
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A circuit for handling pulse width modulation (PWM) first signal and PWM second signal for outputting to an amplifier, the PWM first signal having one of a same phase and an opposite phase relationship with the PWM second signal, the circuit comprising a power detector for detecting power turn on to the amplifier and outputting a power on signal and detecting a power turn off to the amplifier and outputting a power off signal; a pulse generator having: a duty cycle generator for generating a first pulse signal corresponding to the PWM first signal and a second pulse signal corresponding to the PWM second signal, and a reduced-width generator for generating at least one of a reduced-width first pulse and a reduced-width second pulse; a controller for selecting one of the reduced-width first pulse and the reduced-width second pulse for outputting to the amplifier upon receipt of the power on signal and for selecting the first pulse signal and the second pulse signal for outputting to the amplifier thereafter; and a counter for counting the duration of the pulse width of the PWM first signal, the counter being activated upon detection of the power off signal and a select circuit for outputting an off select signal upon reaching a predetermined reduced-width time count to cause an output of one of a reduced-width PWM first signal and a reduced-width PWM second signal.
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CROSS-REFERENCE TO A RELATED APPLICATION
This application claims the benefit of the filing date of Japanese Patent Application No. 2004-217240 filed on Jul. 26, 2004, which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a component and material traceability control apparatus, control method, control program, and control program memory medium for controlling manufacturing lot identification information of a component and material constituting a product.
2. Description of the Related Art
When there is a defect in a produced and sold product, an enterprise that has manufactured or sold the product receives not a little damage on a management thereof. Therefore, an enterprise of a manufacturing industry performs quality control in all processes from a product design to a manufacturing till a packaging. However, even how the quality control is reinforced, a possibility of an inferior quality product flowing into a market cannot be completely made zero. If the possibility of the inferior quality product flowing into the market is not completely zero, it becomes a big problem how to swiftly inquire into a cause thereof and how to recover the inferior quality product from the market without cost.
Generally, when an inferior quality problem occurs in a product, a measure of a product recovery and change is taken for a product already delivered to a market; and a measure such as a delivery stop, manufacturing stop, and the like is taken for a product before a delivery. In addition, with respect to a product made as an inferior quality product, a manufacturing date of the product, an apparatus used in a manufacturing thereof, an origin of a component and material constituting the product, and the like are traced back, and thereby a cause of the inferior quality is inferred or specified. And when the cause of the inferior quality is specified, a treatment for removing the cause is performed. In addition, when there is a defect in some of a component of a product, upon recovering the component based on a manufacturing number and manufacturing lot number thereof for the product having flowed into the market, some defective component is changed. In addition, at a manufacturing job site the manufacturing is reopened, upon changing the component used.
Thus in order to inquire into a cause of the inferior quality and to recover an inferior quality product from a market, the manufacturing number or the manufacturing lot number plays an important role.
In this connection, many industrial products are manufactured by working or assembling many components and materials (hereinafter referred to as “component/material (part)”). And in many cases the “component/material” is manufactured in other enterprises and is purchased. Accordingly, in the inferior quality of a product there are something originated in a design or a manufacturing process and something brought from outside as the inferior quality of a purchase “component/material.” Therefore, when intending to swiftly inquire into the cause and to recover the product at low cost, it is necessary to control each manufacturing number and each manufacturing lot number of the “component/material” used for each product manufactured.
Conventionally, it is already known a system of controlling each manufacturing number and manufacturing lot number of the “component/material” used for each product. For example, at paragraphs 0006 to 0026 and FIGS. 1 to 3 of Japanese Patent Laid-Open Publication No. 2004-134509 (hereinafter referred to as patent document 1), at a portion where a conventional technology is described is shown an example of a traceability system for controlling the manufacturing lot number of the “component/material” used for an electronic circuit board with respect to the board manufactured. And as a technology of the patent document 1, instead of controlling the manufacturing lot number, is shown an example of the traceability system, where a manufactured electronic circuit board is designed to control a process by its passing time and to simultaneously control the manufacturing lot number of the “component/material” in each process.
In addition, at paraphrases 0006 to 0026 and FIGS. 1 to 7 of Japanese Patent Laid-Open Publication Hei. 9-252195 (hereinafter referred to as patent document 2) is shown, in an apparatus for mounting the “component/material” on an electronic circuit board, a control system of a resupply “component/material” where a history of an identification number of the “component/material” actually mounted is designed to be kept in order to enable a trace of the “component/material” mounted, when there occurs a trouble in the electronic circuit board manufactured, and to prevent an erroneous mount.
In the patent documents 1 and 2 one manufacturing number or manufacturing lot number is made to correspond to each “component/material” used in a product. Thus the “component/material” can be accurately made to correspond to the manufacturing number or manufacturing lot number. However, if attempting to accurately make the “component/material” correspond to the manufacturing number or manufacturing lot number, a manufacturing apparatus and control procedure for make the correspondence become complicated. As a result, the manufacturing cost and control cost of the product result in becoming large.
For example, with respect to a pass capacitor and the like used in an electronic circuit board, because the “component/material” itself is small, there is no space for affixing a barcode and the like for indicating a manufacturing lot number thereof. If so, the control of the manufacturing lot number can be performed in nothing but a level of a storage case for packaging the “component/material.” In that case “component/material” with a plurality of manufacturing lot numbers cannot be put in one storage case. Or, even if the “component/material” with the plurality of the manufacturing lot numbers can be put in one storage case, it results in standing extra control cost for such as being stored in specific order and making a table of the manufacturing lot numbers matching storage positions.
Consequently, for example, there is some idea of not controlling a manufacturing lot number for “component/material” such as a pass capacitor similar to “a screw and a nail.” However, in that case, when there occurs an inferior quality problem in the “component/material” not controlled, a clue for inquiring into a cause thereof is lost. In addition, for example, even when the manufacturing lot number and the like of the “component/material” with the inferior quality become clear, product recovery cost results in becoming larger because the manufacturing number of the product using the “component/material” of the inferior quality cannot be narrowed down.
Thus considering the problems of conventional technologies, it is strongly requested a traceability control apparatus, control method, control program, and control program memory medium that simplify the manufacturing lot number control of the “component/material” constituting a product, and thereby that can reduce control cost thereof.
SUMMARY OF THE INVENTION
In order to solve the above problems, a “component/material (part)” traceability control apparatus of the present invention is an apparatus for controlling manufacturing lot identification information of “component/material,” which constitutes a product, in the product manufactured according to a process where a manufacturing apparatus comprising not less than one “component/material” reserve unit takes out a needed amount out of the “component/material” reserved in the “component/material” reserve unit and thereby manufactures the product; wherein the “component/material” traceability control apparatus is designed to be a configuration of comprising at least a processing unit, a memory unit used as a working area by the processing unit, a manufacturing performance information memory unit, a “component/material” supply performance information memory unit, and a manufacturing lot trace information memory unit. And with respect to the product manufactured by the manufacturing apparatus, information of manufacturing start time and end time by the manufacturing apparatus is made to correspond to manufacturing apparatus identification information of the manufacturing apparatus and manufactured article (assemble module) identification information of the product manufactured, and thus is memorized in the manufacturing performance information memory unit; and in addition, “component/material” supply start time and stop time when a supply of predetermined “component/material” is started and stopped in a “component/material” reserve unit of the manufacturing apparatus are made to correspond to the manufacturing lot identification information of the “component/material,” the manufacturing apparatus identification information of the manufacturing apparatus, the “component/material” reserve unit identification information of the “component/material” reserve unit, and a name of the “component/material” supplied and thus are memorized in the “component/material” supply performance information memory unit. And a product manufactured by the manufacturing apparatus is designed so that not less than one piece of manufacturing lot identification information of “component/material” usable in the product is extracted, and not less than the one piece of manufacturing lot identification information extracted is made to correspond to the manufactured article identification information and the name of the “component/material” and is memorized in the manufacturing lot trace information memory unit, based on the information of the manufacturing start time and end time of a product memorized in the manufacturing performance information memory unit and the information of the “component/material” supply start time and stop time memorized in the “component/material” supply performance information memory unit.
Thus the “component/material” traceability control apparatus of the present invention obtains the information of a basis of manufacturing lot trace information, matching timings of major events in any of a manufacturing apparatus and a manufacturing process, that is, a manufacturing start and end of a product, and “component/material” supply start and stop of “component/material” in a “component/material” reserve unit. And at that time the control apparatus does not make manufacturing lot identification information correspond to each “component/material.” As a result, although a plurality of manufacturing lot identification information are made to correspond to one “component/material” in some case, the cost of the manufacturing apparatus and the control cost for obtaining traceability control information can be reduced.
In addition, when in the present invention, in a “component/material” reserve unit of a manufacturing apparatus, the manufacturing lot trace information memory unit makes “component/material” supply start time of a supply of a predetermined “component/material” being started and “component/material” supply stop time of the supply being stopped correspond to the manufacturing lot identification information of the “component/material,” the manufacturing apparatus identification information of the manufacturing apparatus, the “component/material” reserve unit identification information of the “component/material” reserve unit, and the name of the “component/material” supplied and thus memorizes the start time and stop time in the “component/material” supply performance information memory unit, the manufacturing lot identification information is designed to be not less than one piece of manufacturing lot identification information.
In other words, a plurality of manufacturing lot identification information is designed to be able to correspond to one “component/material” supplied to a “component/material” reserve unit. Therefore, it becomes enabled to mix “component/material” with a plurality of manufacturing lot numbers into a package case and a storage case. Or it also becomes enabled to mix a “component/material” with a plurality of manufacturing lot numbers in a “component/material” reserve unit of a manufacturing apparatus. Therefore, the control of the manufacturing lot identification information of the “component/material” is simplified and the cost of the manufacturing apparatus is reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a drawing exemplifying a manufacturing model of an electronic circuit board using a manufacturing apparatus where the present invention is applied.
FIG. 2 is a drawing showing a configuration example of a “component/material (part)” traceability control apparatus in an embodiment of the present invention.
FIG. 3 is a drawing exemplifying a time chart of a manufacturing procedure of a manufactured article (assembled module) and that of a “component/material” supply procedure to a “component/material” reserve unit by a manufacturing apparatus in an embodiment of the present invention.
FIG. 4 is a drawing showing a configuration example of records memorized in a manufacturing performance information memory unit in an embodiment of the present invention.
FIG. 5 is a drawing showing a configuration example of records memorized in a “component/material” supply performance information memory unit in an embodiment of the present invention.
FIG. 6 is a drawing showing a configuration example of records memorized in a manufacturing lot trace information memory unit in an embodiment of the present invention.
FIG. 7 is a drawing showing a configuration example of records memorized in a manufactured article configuration information memory unit in an embodiment of the present invention.
FIG. 8 is an example of a flowchart showing a procedure for obtaining traceability information of “component/material” memorized in a manufacturing lot trace information memory unit in an embodiment of the present invention.
FIG. 9 is a drawing showing a configuration example of records memorized in a purchase lot trace information memory unit in a variation example of an embodiment of the present invention.
FIG. 10 is a drawing exemplifying a time chart of a manufacturing procedure of an electronic circuit board when the present invention is applied to a flow soldering process.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Here will be described embodiments of the present invention in detail, referring to drawings as needed.
FIG. 1 is a drawing exemplifying a manufacturing model of an electronic circuit board using a manufacturing apparatus where the present invention is applied. In FIG. 1 a manufacturing apparatus 1 is an electronic circuit board manufacturing apparatus and comprises a working unit 11 and a plurality of “component/material (part)” reserve units 12 ; and in addition, a manufacturing control personal computer 2 is connected to the manufacturing apparatus 1 .
The manufacturing apparatus 1 of this case is an apparatus for mounting an electronic circuit component on a before-working electronic circuit board 4 where a through hole is already formed and which is print-wired, for performing soldering by a reflow solder and a flow solder, and for manufacturing a working-completion electronic circuit board 5 . Although in FIG. 1 the working unit 11 is shown only one, it actually comprises a plurality of working units consisting of a chip mounting apparatus, a soldering tool, and the like. Here to make a description easily understandable, the working unit 11 is assumed to comprise one chip mounting apparatus.
The “component/material” reserve unit 12 is a container for temporary keeping an electronic circuit component mounted on the before-working electronic circuit board 4 . As electronic circuit components, there are LSI (Large Scale Integrated Circuits), IC (Integrated Circuits), diodes, resistances, capacitors, and the like. These electronic circuit components are usually delivered from an electronic component manufacturer in a form contained in a carrier tape and a feeder cart (called a magazine in some case). Therefore, many actual “component/material” reserve units 12 are designed so that these carrier tape and feeder cart can be directly set. Accordingly, manufacturing lot numbers of electronic circuit components are usually added to the carrier tape and the feeder cart, and in the embodiment it is assumed that a barcode of a manufacturing lot number is added to a “component/material” containing case such as the carrier tape and the feeder cart. Here, the barcode may also be a two-dimensional one.
The chip mounting apparatus of the working unit 11 takes out electronic circuit components one by one contained in the “component/material” reserve unit 12 and mounts them on predetermined positions of the before-working electronic circuit board 4 . Meanwhile, there are also a plurality of types in the chip mounting apparatus, and when manufacturing a usual electronic circuit board, two kinds of chip mounting apparatuses are used in many cases. Here, even when chip mounting apparatuses used are plural, this is regarded as one chip mounting apparatus, totally including this.
In FIG. 1 the manufacturing control personal computer 2 is connected to the working unit 11 and each of the “component/material” reserve units 12 through lines not shown and monitors each operation situation thereof. In addition, the personal computer 2 comprises barcode readers 3 and, through them, reads a barcode of a manufactured article (assemble module) identification number printed on the before-working electronic circuit board 4 and the working-completion electronic circuit board 5 . In addition, through the barcode readers 3 , the personal computer 2 reads a barcode of a manufacturing lot identification number added to a carrier tape and a feeder cart set at the “component/material” reserve unit 12 .
Meanwhile, here instead of the barcode readers 3 , a monitor camera and a character recognition apparatus may be used. In this case a manufactured article identification number and the like according to a character may be printed on an electronic circuit board and the like instead of a barcode. In addition, an IC tag reader may be used instead of the barcode readers 3 . In this case an IC tag is assumed to be affixed to a containing case of an electronic circuit board and an electronic circuit component.
FIG. 2 is a drawing showing a configuration example of a “component/material” traceability control apparatus in the embodiment. In FIG. 2 a “component/material” traceability control apparatus 7 is a computer comprising a processing unit 71 , a memory unit 72 , an input/output interface unit 73 , a liquid crystal display unit 74 , a keyboard 75 , a manufacturing performance information memory unit 76 , a “component/material” supply performance information memory unit 77 , a manufacturing lot trace information memory unit 78 , a purchase lot trace information memory unit 79 , and a manufactured article configuration information memory unit 80 .
Here, the memory unit 72 comprises a semiconductor memory and a magnetic hard disk device, and a program and operating system for realizing a function of the “component/material” traceability control apparatus 7 are stored therein. And the memory unit 72 is also used as a working area when the processing unit 71 runs the program.
Here, the input/output interface unit 73 comprises interfaces for connecting outside peripherals such as an interface with the liquid crystal display unit 74 and the keyboard 75 and an interface with a network 8 . In addition, the liquid crystal display unit 74 and the keyboard 75 are used for a user's inputting information in the “component/material” traceability control apparatus 7 and consulting information. Here, instead of the liquid crystal display unit 74 , another display unit such as a CRT (Cathode Ray Tube) and the like may be used.
The performance information memory unit 76 , “component/material” supply performance information memory unit 77 , manufacturing lot trace information memory unit 78 , purchase lot trace information memory unit 79 , and manufactured article configuration information memory unit 80 are configured on a large capacity memory device such as a magnetic hard disk device and memorize information for realizing the function of the “component/material” traceability control apparatus 7 . With respect to a content of information which each of the memory units 76 to 80 memorizes, it will be separately described in detail, using drawings.
In FIG. 2 the “component/material” traceability control apparatus 7 is connected to the network 8 such as a LAN (Local Area Network) through the input/output interface unit 73 , and further connected to the manufacturing control personal computer 2 of the manufacturing apparatus 1 through the network 8 . Although in FIG. 2 only one personal computer 2 is depicted, a configuration of a plurality of manufacturing control personal computers 2 being connected is also available. In addition, the manufacturing control personal computers 2 may control manufacturing information of a plurality of manufacturing apparatuses 1 .
FIG. 3 is a drawing exemplifying a time chart of a manufacturing procedure of a manufactured article and that of a “component/material” supply procedure to a “component/material” reserve unit by a manufacturing apparatus in the embodiment. Here will be described the manufacturing procedure in the electronic circuit board manufacturing apparatus shown in FIG. 1 , using FIG. 3 .
In FIG. 3 a time chart at an utmost stage is the chart showing a manufacturing procedure of an electronic circuit board with a manufactured article name PB00A. In accordance with the time chart, a manufacturing of an electronic circuit board with a manufactured article identification number A0001 is finished at eight fifty five in the working unit 11 of the manufacturing apparatus 1 and is removed from the working unit 11 . Next, another electronic circuit board with a manufactured article identification number A0002 is set in the working unit 11 , and a manufacturing thereof is started at nine o'clock. And the manufacturing of the electronic circuit board with the manufactured article identification number A0002 is finished at nine fifty five and is removed from the working unit 11 . Next, still another electronic circuit board with a manufactured article identification number A0003 is set in the working unit 11 , and a manufacturing thereof is started at ten o'clock.
A manufactured article identification number (for example, A0001) is printed with a barcode at a predetermined position of a surface of the before-working electronic circuit board 4 . Consequently, when the before-working electronic circuit board 4 is set in the working unit 11 , the manufacturing control personal computer 2 reads the barcode through one of the barcode readers 3 and memorizes time then as manufacturing start time. In addition, when the manufacturing of the electronic circuit board is finished and the working-completion electronic circuit board 5 thereof is removed from the working unit 11 , the manufacturing control personal computer 2 again reads the barcode through the barcode reader 3 and memorizes time then as manufacturing end time.
In FIG. 3 time charts below a third stage are the charts showing a procedure for supplying “component/material” with respective “component/material” names IC001, DI003, and CA789 to the “component/material” reserve units 12 with respective identification numbers 123A, 123B, and 123C.
In accordance with FIG. 3 , in the “component/material” reserve unit 12 with the identification number 123A is at first reserved “component/material” (for example, an IC chip) with the “component/material” name IC001 and a manufacturing lot identification number LOT012A1 in a state of being contained in any of a carrier tape and a feeder cart; and the “component/material” is completely used at nine thirty, and a supply thereof is stopped from the “component/material” reserve unit 12 . And “component/material” with the “component/material” name IC001 and a manufacturing lot identification number LOT012A2 is newly set in the “component/material” reserve unit 12 with the identification number 123A in a state of being contained in any of a carrier tape and a feeder cart; and a supply thereof is started at nine forty.
Similarly, in the “component/material” reserve unit 12 with the identification number 123B is at first reserved “component/material” (for example, a diode chip) with the “component/material” name DI003 and a manufacturing lot identification number LOT123B1, and a supply thereof is stopped at eight fifty five. And “component/material” with the “component/material” name DT003 and the manufacturing lot identification number LOT123B1 or LOT123B2 is set at the “component/material” reserve unit 12 with the identification number 123B in a state of being contained in any of a carrier tape and a feeder cart, a supply thereof is started at nine o'clock, and the supply is stopped at ten fifteen. Furthermore similarly, the supply of “component/material” with the “component/material” name DI003 and a manufacturing lot identification number LOT123B3 is started at ten twenty.
In addition, in the “component/material” reserve unit 12 with the identification number 123C is started and stopped the supply of “component/material” (for example, a capacitor) with the “component/material” name CA789 according to the similar procedure. However, the example of this time chart is different from other ones in a point that time from the supply stop to supply start of the “component/material” is zero.
In the embodiment a manufacturing lot identification number of relevant “component/material” is added to any of a carrier tape and feeder cart of a “component/material” containing case with a barcode. Consequently, when the “component/material” containing case is set in the “component/material” reserve unit 12 , the manufacturing control personal computer 2 reads the barcode added to the “component/material” containing case through the barcode reader 3 and memorizes time then as “component/material” supply start time. In addition, if the manufacturing control personal computer 2 detects that the “component/material” in the “component/material” reserve unit 12 runs short, it memorizes time then as “component/material” supply stop time and request for an operator or an automatic loader not shown to remove an empty “component/material” containing case and to set a new one.
In addition, FIG. 3 shows that “component/material” with different manufacturing lot identification numbers (LOT123B1 and LOT123B2) is mixed in the “component/material” reserve unit 12 with the identification number 123B from nine o'clock to ten fifteen.
In such the case the manufacturing control personal computer 2 of the present invention does not discriminate the “component/material” with the manufacturing lot identification number LOT123B1 from one with the manufacturing lot identification number LOT123B2 that are mixed in the “component/material” reserve unit 12 . Because this makes the configuration of the manufacturing apparatus 1 simpler, the cost of the manufacturing apparatus 1 results in being lower. Here, because if it is designed that a manufacturing lot identification number can be discriminated, various burdens and restrictions are added to a supply mechanism and supply procedure of “component/material” in the “component/material” reserve unit 12 , an apparatus configuration thereof becomes complicated, and apparatus cost thereof becomes larger.
Consequently, in such the case the embodiment makes a plurality of manufacturing lot identification numbers correspond to one “component/material.” In other words, the manufacturing control personal computer 2 assumes that a manufacturing lot identification number of the “component/material” with the “component/material” name DI003 used in an electronic circuit board with the manufactured article identification number A0002 is any of LOT123B1 and LOT123B2, and the personal computer 2 memorizes both manufacturing lot identification numbers.
Thus there occurs a situation that “component/material” with different manufacturing lot identification numbers is mixed in one “component/material” reserve unit 12 in following cases:
a case that “component/material” with a plurality of manufacturing lot identification numbers is mixed and contained in a carrier tape, a feeder cart, and another “component/material” containing case;” a case of not a configuration that a plurality of carrier tapes and feeder carts can be set in the “component/material” reserve unit 12 and that the working unit 11 can discriminate the carrier tapes and feeder carts, even if “component/material” with a same manufacturing lot identification number is contained in the carrier tapes and the feeder carts; and a case of replenishing another “component/material” with a different manufacturing lot identification number notwithstanding “component/material” remaining in the “component/material” reserve unit 12 .
Meanwhile, the case (3) is such a case that “component/material” is replenished at a manufacturing start timing in the working unit 11 , and such the case may be thought to actually often happen.
Furthermore, on the way of the working unit 11 manufacturing the electronic circuit board with the manufactured article identification number A0002, in the “component/material” reserve unit 12 with the identification number 123A, the manufacturing lot identification number of the “component/material” with the “component/material” name IC001 is changed from LOT012A1 to LOT012A 2. In such the case there is a possibility that not only the “component/material” with the manufacturing lot identification number LOT012A1 but also the “component/material” with the manufacturing lot identification number LOT012A2 are used in the electronic circuit board with the manufactured article identification number A0002. In such the case the embodiment does not discriminate the manufacturing lot identification numbers of the “component/material,” and the manufacturing control personal computer 2 memorizes both of two manufacturing lot identification numbers LOT012A1 and LOT012A 2 as the manufacturing lot identification number of the “component/material” with the “component/material” name IC001 used in the electronic circuit board with the manufactured article identification number A0002.
Thus as described in FIG. 3 , when a manufactured article manufactured by the manufacturing apparatus 1 is put in and taken out from the working unit 11 , the manufacturing control personal computer 2 reads a manufactured article identification number added to the manufactured article and memorizes the manufacturing lot identification number read, together with time then (manufacturing start time and end time). In addition, when “component/material” is supplied to the “component/material” reserve unit 12 , and it becomes empty or it becomes necessary to replenish new “component/material,” the manufacturing control personal computer 2 reads a manufacturing lot identification number of “component/material” added to any of the “component/material” and a containing case thereof and memorizes the manufacturing lot identification number read, together with time then (“component/material” supply start time and stop time).
Furthermore, the manufacturing control personal computer 2 sends information, where the manufacturing apparatus identification number of the manufacturing apparatus 1 and a manufactured article name manufactured are added to a manufactured article identification number memorized, manufacturing start time, and manufacturing end time that are memorized, to the “component/material” traceability control apparatus 7 through the network 8 . In addition, similarly, the manufacturing control personal computer 2 sends information, where the manufacturing apparatus identification number of the manufacturing apparatus 1 , the “component/material” reserve unit identification number of the “component/material” reserve unit 12 , and the “component/material” name are added to the “component/material” manufacturing lot identification number, “component/material” supply start time, and “component/material” supply stop time that are memorized, to the “component/material” traceability control apparatus 7 through the network 8 .
FIG. 4 is a drawing showing a configuration example of records memorized in the manufacturing performance information memory unit 76 in the embodiment. Here, a record means a plurality of information collected up to one set as interrelated information, and when memorized in a memory device such a magnetic hard disk, it is handled as one set of information to be memorized. In addition, one record is constituted of a plurality of fields, and in one field is usually memorized one piece of information.
In FIG. 4 a record of the manufacturing performance information memory unit 76 is constituted of fields comprising a manufacturing apparatus identification number 761, a manufactured article name 762, a manufactured article identification number 763, a manufacturing start time 764, and a manufacturing end time 765, respectively.
The “component/material” traceability control apparatus 7 receives the information of a manufactured article identification number, manufacturing start time, manufacturing end time, manufacturing apparatus identification number, and manufactured article name relating to a product manufactured by the manufacturing apparatus 1 out of information sent from the manufacturing control personal computer 2 and memorizes the information as one record in the manufacturing performance information memory unit 76 . In other words, in the field of the manufacturing apparatus identification number 761 is memorized the manufacturing apparatus identification number of the manufacturing apparatus 1 , in the field of the manufactured article name 762 is memorized the name of the manufactured article manufactured by the manufacturing apparatus 1 , and in the field of the manufactured article identification number 763 is memorized the manufactured article identification number of the manufactured article manufactured by the manufacturing apparatus 1 . In addition, in the fields of the manufacturing start time 764 and the manufacturing end time 765 are respectively memorized the manufacturing start time and manufacturing end time of the manufactured article with a manufactured article identification number specified by the field of the manufactured article identification number 763.
For example, a second record of manufacturing information of FIG. 4 indicates that a manufacturing of an electronic circuit board with the manufactured article name PB00A and the manufactured article identification number A0002 is started at nine o'clock on the tenth of June, 2004 and finished at nine fifty five on the same day by the manufacturing apparatus 1 with a manufacturing apparatus identification number M0123.
FIG. 5 is a drawing showing a configuration example of records memorized in the “component/material” supply performance information memory unit 77 in the embodiment. In FIG. 5 a record of the “component/material” supply performance information memory unit 77 is constituted of fields comprising a manufacturing apparatus identification number 771, a “component/material” reserve unit identification number 772, a “component/material” name 773, a manufacturing lot identification number 774, a “component/material” supply start time 775, and a “component/material” supply stop time 776, respectively.
The “component/material” traceability control apparatus 7 receives the information of a manufacturing lot identification number, “component/material” supply start time, “component/material” supply stop time, manufacturing apparatus identification number, “component/material” reserve unit identification number, and “component/material” name relating to “component/material” supplied to the “component/material” reserve unit 12 out of information sent from the manufacturing control personal computer 2 and memorizes the information as one record in the “component/material” supply performance information memory unit 77 . In other words, in the field of the manufacturing apparatus identification number 771 is memorized the manufacturing apparatus identification number of the manufacturing apparatus 1 , in the field of the “component/material” reserve unit identification number 772 is memorized the identification number of the “component/material” reserve unit 12 where the “component/material” is supplied, and in the field of the “component/material” name 773 is memorized the name of the “component/material.” In addition, in the field of the manufacturing lot identification number 774 is memorized the manufacturing lot identification number of the “component/material” actually supplied to the “component/material” reserve unit 12 , and in the fields of the “component/material” supply start time 775 and the “component/material” supply stop time 776 are respectively memorized time, when any of the “component/material” and a containing case thereof is set, and time, when the “component/material” runs short or the containing case is removed.
For example, a second record of the “component/material” supply performance information of FIG. 5 indicates that “component/material” with the “component/material” name IC001 and the manufacturing lot identification number LOT012A2 is started to be supplied at nine forty on the tenth of June, 2004 and stopped to be supplied at eleven twenty on the same day in the “component/material” reserve unit 12 of the manufacturing apparatus 1 with the “component/material” reserve unit identification number 123A and the manufacturing apparatus identification number M0123, respectively. In addition, forth and fifth records of the “component/material” supply performance information of FIG. 5 indicate that “component/material” with the same “component/material” name (DI003) and two different manufacturing lot identification numbers (LOT123B1 and LOT123B2) is supplied at the same time zone (from nine o'clock till ten fifteen on the tenth of June, 2004).
Thus if the “component/material” traceability control apparatus 7 memorizes information sent from the manufacturing control personal computer 2 in the manufacturing performance information memory unit 76 and the “component/material” supply performance information memory unit 77 , it obtains manufacturing lot trace information, based on the information memorized, and memorizes a result thereof in the manufacturing lot trace information memory unit 78 .
FIG. 6 is a drawing showing a configuration example of records memorized in the manufacturing lot trace information memory unit 78 in the embodiment; FIG. 7 is a drawing showing a configuration example of records memorized in a manufactured article configuration information memory unit 80 in the embodiment; and FIG. 8 is an example of a flowchart showing a procedure for obtaining traceability information of a “component/material” memorized in the manufacturing lot trace information memory unit 78 in the embodiment.
In FIG. 6 a record of the manufacturing lot trace information memory unit 78 is constituted of fields comprising a manufactured article name 781, a manufactured article identification number 782, a “component/material” name 783, and a manufacturing lot identification number 784. And the record means, for example, that in a case of a fourth record “a manufacturing lot identification number of “component/material” with the name IC001 constituting a manufactured article (electronic circuit board) with the manufactured article name PB00A and the manufactured article identification number A0002 is any of LOT012A and LOT012A2.” Accordingly, if there is the information of the manufacturing lot trace information memory unit 78 , manufacturing lot identification information of “component/material” used in a manufactured article can immediately be known according to a manufactured article identification number thereof; on the contrary, a manufactured article name and manufactured article identification number where the “component/material” is used can be known according to a “component/material” name and a manufacturing lot identification number thereof. In other words, the information of the manufacturing lot trace information memory unit 78 can be said to be traceability information of “component/material” constituting a manufactured article.
Meanwhile, in the field of the manufacturing lot identification number 784, a memorable area of a plurality of manufacturing lot identification numbers is assumed to be ensured, and the plurality of manufacturing lot identification numbers are memorized as needed. That in the field of the manufacturing lot identification number 784 a plurality of manufacturing lot identification numbers is memorized means that in some case a resolution of the traceability information is lowered. However, when constituting a product with specifically using small “component/material” such as “a screw and a nail,” an effect of reducing cost for obtaining the traceability information is larger.
In FIG. 7 the manufactured article configuration information memory unit 80 is constituted of fields comprising a manufactured article name 801 and a “component/material” name 802, respectively. Manufactured article configuration information memorized in the manufactured article configuration information memory unit 80 is a so called component table and a list of “component/material” constituting a manufactured article specified by a manufactured article name. Although the component table is often expressed in a hierarchical structure description, the manufactured article configuration information is here assumed to be a flat (one hierarchical) structure. Meanwhile, because information of the component table memorized in the manufactured article configuration information memory unit 80 is made in designing, it is here assumed to simplify a description that the information made is used as it is (in some case the hierarchical structure is converted to the flat structure).
Next, according to the flowchart of FIG. 8 , information to be memorized in the manufactured article trace information memory unit 78 of FIG. 6 is obtained, based on information memorized in the manufactured article configuration information memory unit 80 of FIG. 7 , the manufacturing performance information memory unit 76 of FIG. 4 , and the “component/material” supply performance information memory unit 77 of FIG. 5 . Meanwhile, a procedure shown therein is a run procedure of a computer program, and usually such the program is stored in the memory unit 72 (see FIG. 2 ), and the processing unit 71 reads the program from the memory unit 72 as needed and runs it. In addition, the program is memorized in a computable-readable memory medium such as a CD-ROM (Compact Disk Read Only Memory) and is read as needed into the memory unit 72 through a CD-ROM drive dive and the like not shown in FIG. 2 .
In FIG. 8 , firstly receive an input of a manufactured article name, and make the manufactured article name # a (step S 11 ). Meanwhile, an operator may perform the input through the key board 75 or another program may input the data #a as a parameter. And refer to the manufactured article configuration information memory unit 80 , and extract a “component/material” name #b configuring a manufactured article with the manufactured article name #a (step S 12 ). Here, as the “component/material” name #b, a plurality of “component/material” names are extracted. Next, refer to the manufacturing performance information memory unit 76 , and extract records with the manufactured article name # a, and sort them according to an order of manufactured article identification numbers (step S 13 ).
Next, out of the records extracted and sorted in the step S 13 , pick up one of the manufactured article identification numbers, make it #c, and pick up a manufacturing apparatus identification number, manufacturing start time, and manufacturing end time that are made to correspond to the #c by a record comprising it, and make them #d, #e, and #f, respectively (step S 14 ). Next, pick up one piece of “component/material” with the “component/material” name #b, and make it #g (step S 15 ).
Refer to the “component/material” supply performance information memory unit 77 , and extract a record with the manufacturing apparatus identification number #d and the “component/material” name #g, and make it a record #h (step S 16 ). Here, as the record #h are usually extracted a plurality of records. Consequently, out of the records #h extracted in the step S 16 , pick up a record where time from supply start time to supply stop time of the “component/material” overlaps time from manufacturing start time to manufacturing end time specified by the #e and the #f, and make it a record #i (step S 17 ). Here, as the record #i are extracted a plurality of records in some case. Next, pick up a manufacturing lot identification number for the record #i, make it #j, and memorize the #a, #c, #g, and #j in the manufacturing lot trace information memory unit 78 (step S 18 ). Meanwhile, although when the record #i is plural records, the #j also becomes plural, in this case the manufacturing lot trace information memory unit 78 memorizes a plurality of the #i for the #a, #c, and #g.
Next, determine whether or not the “component/material” names extracted as the “component/material” names #b in the step S 12 is all picked up and made the #g in the step S 15 (step S 19 ). In a determination thereof, if all the “component/material” names are not picked up and not made the #g (No in the step S 19 ), return to the step S 15 , and again run the procedure from the step S 15 . On the other hand, in a determination of the step S 19 , if all the “component/material” names are picked up and made the #g (Yes in the step S 19 ), determine whether or not all the manufactured article identification numbers are picked up out of the records extracted and sorted in the step S 13 and are made the #c (step S 20 ). And in a determination thereof, if there is still a manufactured article identification number not made the #c (No in the step S 20 ), return to the step S 14 , and again run the procedure from the step S 14 . On the other hand, if in a determination of the step S 20 all the manufactured article identification numbers are picked up and made the #c (Yes in the step S 20 ), end the procedure.
Thus the manufactured article trace information for the manufactured article name #a firstly specified results in being made in the manufactured article trace information memory unit 78 . Similarly, if specifying another name as a manufactured article name, the manufactured article trace information can be made for manufactured articles with another name. And according to information memorized in the manufactured article trace information memory unit 78 , a manufacturing lot identification number of “component/material” used can be controlled for each product manufactured.
VARIATION EXAMPLE OF EMBODIMENT
In the embodiment thus described is not used the purchase lot trace information memory unit 79 (see FIG. 2 ). The purchase lot trace information memory unit 79 is used in a variation example of an embodiment described below.
FIG. 9 is a drawing showing a configuration example of records memorized in the purchase lot trace information memory unit 79 in a variation example of the embodiment. In FIG. 9 a record of the purchase lot trace information memory unit 79 is constituted of fields comprising a purchase lot identification number 791, a “component/material” name 792, and a manufacturing lot identification number 793, respectively. Here, a purchase lot means a set of “component/material” in a purchase unit purchased from a “component/material” manufacturer. Accordingly, there are many cases that any of an order form number and a purchase form number is used as a purchase lot identification number.
The purchase lot identification number and the manufacturing lot identification number do not always correspond to each other. Consequently, in the purchase lot trace information memory unit 79 the purchase lot identification number is made to correspond to the manufacturing lot identification number. For example, in a second record of FIG. 9 a purchase lot identification number PO1002 of “component/material” with the “component/material” IC001 corresponds to the manufacturing lot identification number LOT012A2. Meanwhile, here is assumed that like a fourth record of FIG. 9 , a plurality of manufacturing lot identification numbers can also be made to correspond to one purchase lot identification number. This signifies that “component/material” with a plurality of manufacturing lot identification numbers may be mixed in “component/material” of one purchase lot.
When generally purchasing “component/material,” a barcode of a manufacturing lot identification number and the like are not always added to any of a package and containing case of the “component/material.” To the package and containing case of the “component/material” is added any barcode of an order form number and purchase form number instead of a manufacturing lot identification number, and the manufacturing lot identification number is provided as additional data of the form. In such the case the purchase lot trace information memory unit 79 is made in advance, based on the additional data of the form. If so, a purchase lot identification number can be used instead of a manufacturing lot identification number in the embodiment described in FIGS. 1 to 8 . If so, although information obtained as traceability information of “component/material” constituting a manufactured article is the purchase lot identification number, the number can easily be converted to the manufacturing lot identification number by using the purchase lot trace information memory unit 79 .
[Application to a Case of Indefinite Shape “Component/Material”]
The “component/material” traceability control apparatus 7 in the embodiments thus described is also applicable to a case of indefinite “component/material” such as a solder. In a flow soldering process a reverse side of an electronic circuit board where components are mounted is immersed in a molten solder bath, and thereby soldering of a through hole and the like is performed. In this case the working unit 11 is the molten solder bath, and in addition, the bath doubles as the “component/material” reserve unit 12 . In the molten solder bath, as new “component/material” is thrown in a solder bar every time when an amount of a molten solder decreases by a predetermined amount, in order to keep the amount of the molten solder approximately constant.
FIG. 10 is a drawing exemplifying a time chart of a manufacturing procedure of an electronic circuit board when the present invention is applied to a flow soldering process. In FIG. 10 a time chart of an upper stage is the chart showing a manufacturing of an electronic circuit board with the manufactured article name PB00A same as in the case of FIG. 3 , that is, a time chart by which flow soldering is performed. For example, the flow soldering of an electronic circuit board with the manufactured article identification number A0002 is started at nine o'clock and finished at nine fifty five (actually it does not take time this much).
On the other hand, as shown in a time chart of a lower stage, in the “component/material” reserve unit 12 , that is, a molten solder bath with an identification number 456A, a solder bar with a manufacturing lot identification number LOTHA02 becomes thrown in after nine o'clock, instead of a solder bar with a manufacturing lot identification number LOTHA01 being thrown in till then. In such the case a condition of a solder with the manufacturing lot identification number LOTHA01 and one with the manufacturing lot identification number LOTHA02 being mixed results in continuing some time after nine o'clock in the molten solder bath. In other words, the electronic circuit board with the manufactured article identification number A0002 results in containing as “component/material” thereof the solder bar with the manufacturing lot identification number LOTHA01 and one with the manufacturing lot identification number LOTHA02.
In the present invention, because a plurality of manufacturing lot identification numbers are made to correspond to each product manufactured, it is enabled to easily apply the embodiments described in FIGS. 1 to 8 to such the case described above. However, in order to apply the procedure shown in FIG. 8 as it is for obtaining the traceability information shown in FIG. 8 , it is necessary for the “component/material” traceability control apparatus 7 not to memorize time as it is, which the manufacturing control personal computer 2 sends as “component/material” supply stop time in the “component/material” reserve unit 12 , but to memorize time, where time when a mixture of “component/material” with different manufacturing lot identification numbers continues is added to the time sent by the computer 2 , as information to be memorized in the field of the “component/material” supply stop time 776 of the “component/material” supply performance information memory unit 77 .
In the case of FIG. 10 , the “component/material” traceability control apparatus 7 memorizes in the field of the “component/material” supply stop time 776 of the “component/material” supply performance information memory unit 77 that if the condition of the solder with the manufacturing lot identification number LOTHA01 and one with the manufacturing lot identification number LOTHA02 being mixed is eliminated, for example, at nine fifty five, the supply stop time of the solder bar with the manufacturing lot identification number LOTHA01 is not at nine o'clock but nine fifty. Meanwhile, not limited to a solder within a molten solder bath, it is difficult in many cases to specify time when a mixture of “component/material” with different manufacturing lot identification numbers is actually eliminated. Consequently, in such the cases the time of the mixture elimination of the “component/material” is substituted by an expectation value obtained in advance through a numerical calculation, a simulation, and the like.
Thus also in the case of the indefinite shape “component/material,” according to the procedure shown in FIG. 8 , the information of the manufacturing lot trace information memory unit 78 , that is, the traceability information of relevant “component/material” can be made for each product. Meanwhile, this embodiment can also be applied to control of the traceability information of a material not remaining as “component/material” of a product, for example, cleaning liquid used in a manufacturing process.
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The present invention is related to a component and material traceability control apparatus for controlling manufacturing lot identification information of any of a component and material constituting a product manufactured according to a process where a manufacturing apparatus with not less than one component and material reserve unit picks up a needed amount out of the component and material reserved in the component and material reserve unit and manufactures the product, and the component and material traceability control apparatus is equipped with at least a processing unit, a memory unit used as a work area by the processing unit, a manufacturing performance information memory unit, a component and material supply performance information memory unit, and a manufacturing lot trace information memory unit.
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BACKGROUND
[0001] 1. Field of the Invention
[0002] The systems and methods disclosed herein relate generally to preserving battery charge and particularly to deferring power consumption of an electronic device to a later time by post-processing sensor data.
[0003] 2. Description of the Related Art
[0004] In today's fast moving technology development for the mobile sector, user experience and battery life are two of the most important metrics of an electronic device, for example a mobile phone. Some applications run on an electronic device, for example camera applications, can rapidly deplete battery charge. Depletion of the battery charge may result in failure of the electronic device, which can inconvenience the user. Actively managing the power consumption of a feature or application may add value to the system by contributing to longer battery life through smarter use of features. In addition, by customizing the response of a mobile device based on a more context-aware method or system the device can deliver a more compelling user experience.
SUMMARY
[0005] The systems, methods and devices of the disclosure each have several innovative aspects, no single one of which is solely responsible for the desirable attributes disclosed herein. Combinations of the innovations, aspects and features described herein can be incorporated in various embodiments of systems, methods, and devices, and such combinations are not limited by the examples of embodiments described herein.
[0006] Embodiments and innovations described herein relate to systems and methods that may be run in a processor for an electronic device for deferring battery consumption when the user or the device learns or knows that the battery will be depleted before the next possible charge cycle. Deferring battery consumption to a later time could be accomplished by accessing an application requiring less power consumption and/or delaying post-processing of sensor data related to that application, for example an image or video capture application or an audio application. Aspects of the disclosure also relate to the prediction of battery life of an electronic device. Prediction of battery life could include determining the time to the next expected battery charge and delaying the processing of sensor data until the electronic device is plugged in and charging or has reached a predetermined charge level. Other aspects of the disclosure relate to processes, applications, daemons, and libraries that could be modified depending on the mode of operation of the electronic device.
[0007] As discussed below, some embodiments incorporate a look-up table to control which application is launched when the user selects the application icon. A person of skill in the art will appreciate that other embodiments could be used to control which application is launched for a given battery life condition.
[0008] One innovation relates to systems and methods for reducing power consumption of an electronic device when a user, or the device, knows that the battery will be depleted before the next possible charge cycle. For example, some methods to reduce battery consumption can include determining whether a full-power or reduced-power version of an application is run and/or delaying the post-processing of sensor data to a time when conserving power is not an issue.
[0009] One aspect relates to a system for deferring power consumption of an electronic device. The system includes a memory component configured to store sensor data and a processor coupled to the memory component. The processor is configured to retrieve the sensor data from the memory component and perform processing of the sensor data in at least two operational modes including a sensor data processing normal power operation mode and a sensor data processing low power operation mode, the low power operation mode consuming less power than the normal power operation mode. The system also includes a control module stored in the memory component. The control module includes instructions configured to operate the processor to determine a low power condition that is based on at least one of a threshold battery charge level below which the electronic device will enter the low power operation mode or a threshold time after which the device will enter the low power operation mode and operate the device in the low power operation mode based on whether the low power condition occurs. Operating the device in the low power operation mode includes storing sensor data in the memory component and performing less processing of the sensor data than when the device is operated in the normal power operation mode. The system further includes an imaging device in communication with the processor and configured to generate image data, the imaging device including at least one imaging sensor. The control module is further configured to accept user preferences for a low power operation mode of the electronic device. The control module is further configured to, when in the low power operation mode, store the sensor data in the memory component for later processing. The control module is further configured to store the sensor data for delayed high quality post-processing during a later charging cycle of the electronic device. The low power operation mode may include operating a camera application for a light-field or plenoptic camera. The low power operation mode may include operating a camera application for a stereoscopic camera. The low power operation mode may include operating a heart rate monitor application. The low power operation mode may include operating an audio application. The low power operation mode may include operating a camera application for a mobile device.
[0010] In another aspect, a method for deferring power consumption of an electronic device includes the steps of storing sensor data in a memory component of the electronic device, retrieving the sensor data from the memory component and performing processing of the sensor data in at least two operational modes including a sensor data processing normal power operation mode and a sensor data processing low power operation mode, the low power operation mode consuming less power than the normal power operation, determining a low power condition that is based on at least one of a threshold battery charge level below which the electronic device will enter the low power operation mode or a threshold time after which the device will enter the low power operation mode, and operating the device in the low power operation mode based on whether the low power condition occurs. Operating the device in the low power operation mode may include storing the sensor data in the memory component and performing less processing of the sensor data than when the device is operated in the normal power operation mode. The method may further include the step of accepting user preferences for a low power operation mode of the electronic device. The method may further include the step of storing the sensor data in the memory component for later post-processing during low power operation of the electronic device. The method may further include the step of storing the sensor data in the memory component of the electronic device for delayed post-processing during a later charging cycle of the electronic device. The low power operation mode may include operating a camera application for a light-field or plenoptic camera. The low power operation mode may include operating a camera application for a stereoscopic camera. The low power operation mode may include operating a heart rate monitor application. The low power operation mode may include operating an audio application. The low power operation mode may include operating a camera application for a mobile device.
[0011] In yet another, an apparatus for deferring power consumption of an electronic device may include means for storing sensor data, means for retrieving the sensor data from the memory component and performing processing of the sensor data in at least two operational modes including a sensor data processing normal power operation mode and a sensor data processing low power operation mode, the low power operation mode consuming less power than the normal power operation, means for determining a low power condition that is based on at least one of a threshold battery charge level below which the electronic device will enter the low power operation mode or a threshold time after which the device will enter the low power operation mode, and means for operating the device in the low power operation mode based on whether the low power condition occurs.
[0012] In another aspect, a non-transitory computer-readable medium stores instructions that, when executed, cause at least one physical computer processor to perform a method of deferring power operation of an electronic device. The method may include the steps of storing sensor data in a memory component of the electronic device, retrieving the sensor data from the memory component and performing processing of the sensor data in at least two operational modes including a sensor data processing normal power operation mode and a sensor data processing low power operation mode, the low power operation mode consuming less power than the normal power operation, determining a low power condition that is based on at least one of a threshold battery charge level below which the electronic device will enter the low power operation mode or a threshold time after which the device will enter the low power operation mode, and operating the device in the low power operation mode based on whether the low power condition occurs. Operating in the low power operation mode may include storing sensor data in the memory component and performing less processing of the sensor data than when the device is operated in the normal power operation mode. The method may further include accepting user preferences for the low power operation mode of the electronic device. The method may further include storing the sensor data in the memory component for later processing. The method may further include storing the sensor data in the memory component for delayed high quality post-processing during a later charging cycle of the electronic device. The low power operation mode may include operating a camera application for a light-field or plenoptic camera. The low power operation mode may include operating a camera application for a stereoscopic camera. The low power operation mode may include operating a heart rate monitor application. The low power operation mode may include operating an audio application.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The disclosed aspects will hereinafter be described in conjunction with the appended drawings, provided to illustrate and not to limit the disclosed aspects, wherein like designations denote like elements.
[0014] FIG. 1 is a block diagram depicting a system implementing some operative elements for reducing power consumption of an electronic device.
[0015] FIG. 2 is a flow chart illustrating a process for reducing power consumption of an electronic device by post-processing sensor data.
[0016] FIG. 3 is an example of a user interface depicting partial processing and delayed processing of image data to reduce power consumption.
[0017] FIG. 4 is a flow chart illustrating a process for reducing power consumption of an electronic device by post-processing sensor data.
[0018] FIG. 5 is an example of a user interface illustrating one embodiment of a photo gallery of an electronic device implementing delayed post-processing of sensor data.
[0019] FIG. 6 is an example of an image processing pipeline that may be implemented shortened by an electronic device having a camera that can operate in a regular and low power mode.
DETAILED DESCRIPTION
[0020] Depletion of battery charge can be an issue or inconvenience for a user of an electronic device. At times, circumstances may prevent a user from timely recharging the electronic device, for example when the user is traveling or actively away from a charging station. Prolonged use of the electronic device without access to charging facilities can result in depletion of the battery before the user is able to recharge the device. The methods and systems discussed below provide solutions to reduce or defer battery consumption in light of the anticipated timing of the next possible charge cycle.
[0021] In some embodiments, a device may include a power consumption deferment process that may include a configuration stage and a running stage. In the configuration stage, the device may provide an interface that receives a user selection of which features may be limited if the battery is low on charge. Additionally, during the configuration stage, the user interface of the device may allow the device to receive a user may selection of a threshold beyond which the device enters a low power mode. During the running stage, the electronic device has been instructed (or configured) to enter a low power mode. In the low power mode, the device may be configured to limit available features and/or functionality, run alternative low power applications, adjust which libraries are accessed, modify other processing functions including background processing (for example, daemons), or adjust any other function currently running on a processor of the device. In some embodiments, a processor of the electronic device may be instructed (or configured) to delay post-processing of sensor data until a time when the battery is recharged.
[0022] It is also noted that the examples may be described as a process, which is depicted as a flowchart, a flow diagram, a finite state diagram, a structure diagram, or a block diagram. Although a flowchart may describe the operations as a sequential process, many of the operations can be performed in parallel, or concurrently, and the process can be repeated. In addition, the order of the operations may be re-arranged. A process is terminated when its operations are completed. A process may correspond to a method, a function, a procedure, a subroutine, a subprogram, etc. When a process corresponds to a software function, its termination corresponds to a return of the function to the calling function or the main function.
[0023] Embodiments may be implemented in System-on-Chip (SoC) or external hardware, software, firmware, or any combination thereof. Those of skill in the art will understand that information and signals may be represented using any of a variety of different technologies and techniques. For example, data, instructions, commands, information, signals, bits, symbols, and chips that may be referenced throughout the above description may be represented by voltages, currents, electromagnetic waves, magnetic fields or particles, optical fields or particles, or any combination thereof.
[0024] In the following description, specific details are given to provide a thorough understanding of the examples. However, it will be understood by one of ordinary skill in the art that the examples may be practiced without these specific details. For example, electrical components/devices may be shown in block diagrams in order not to obscure the examples in unnecessary detail. In other instances, such components, other structures and techniques may be shown in detail to further explain the examples.
System Overview
[0025] FIG. 1 illustrates one example of a power management system 100 configured to estimate the power consumption of an electronic device and implement power reduction strategies based on the estimated power consumption or battery level remaining. The illustrated embodiment is not meant to be limiting, but is rather illustrative of certain components in some embodiments. The power management system 100 may include a variety of other components for other functions which are not shown for clarity of the illustrated components.
[0026] The power management system 100 may include an imaging device 110 and an electronic display 130 . Certain embodiments of electronic display 130 may be any flat panel display technology, for example an LED, LCD, plasma, or projection screen. Electronic display 130 may be coupled to a processor 120 for receiving information for visual display to a user. Such information may include, but is not limited to, visual representations of files stored in a memory location, software applications installed on the processor 120 , user interfaces, and network-accessible content objects.
[0027] The imaging device 110 may include one or a combination of imaging sensors. The processor 120 of the power management system 100 can also be coupled to, and in data communication with, the imaging device 110 . The power management system 100 can also include a working memory 135 and a program memory 140 also in communication with processor 120 . The power management system 100 may be a mobile device, for example, a portable wireless device including but not limited to a tablet computer, a laptop computer, or a cellular telephone (for example a smartphone).
[0028] In some embodiments the processor 120 may be a general purpose processing unit, or in some embodiments the processor 120 may be specially designed for power management or image processing applications for a handheld electronic device. In some embodiments, processor 120 may include an image signal processor (ISP) used for digital processing of image data in digital cameras, mobile phones, or other devices having a camera. As shown, the processor 120 is connected to, and in data communication with, program memory 140 and a working memory 135 . In some embodiments, the working memory 135 may be incorporated in the processor 120 , for example, cache memory. The working memory 135 may also be a component separate from the processor 120 and coupled to the processor 120 , for example, one or more RAM or DRAM components. In other words, although FIG. 1 illustrates two memory components, including memory component 140 comprising several modules and a separate memory 135 comprising a working memory, one with skill in the art would recognize several embodiments utilizing different memory architectures. For example, a design may utilize ROM or static RAM memory for the storage of processor instructions implementing the modules contained in memory 140 . The processor instructions may then be loaded into RAM to facilitate execution by the processor. For example, working memory 135 may be a RAM memory, with instructions loaded into working memory 135 before execution by the processor 120 .
[0029] In the illustrated embodiment, the program memory 140 stores an image capture module 145 , a battery level determination module 150 , a post-processing determination module 155 , a low power application module 160 , operating system 165 , and a user interface module 170 . These modules may include instructions that configure the processor 120 to perform various image processing and device management tasks. Program memory 140 can be any suitable computer-readable storage medium, for example a non-transitory storage medium. Working memory 135 may be used by processor 120 to store a working set of processor instructions contained in the modules of memory 140 . Alternatively, working memory 135 may also be used by processor 120 to store dynamic data created during the operation of power management system 100 .
[0030] As mentioned above, the processor 120 may be configured by several modules stored in the memory 140 . In other words, the process 120 can run instructions stored in modules in the memory 140 . Image capture control module 145 may include instructions that configure the processor 120 to obtain images from the imaging device. Therefore, processor 120 , along with image capture control module 145 , imaging device 110 , and working memory 135 , represent one means for obtaining image sensor data.
[0031] Still referring to FIG. 1 , memory 140 may also contain battery level determination module 150 . The battery level determination module 150 may include instructions that configure the processor 120 to determine an amount of charge remaining in the electronic device, as will be described in further detail below. Therefore, processor 120 , along with battery level determination module 150 and working memory 135 , represent one means for estimating the amount of battery level or charge remaining on a battery of an electronic device.
[0032] Memory 140 may also contain post-processing determination module 155 . The post-processing determination module 155 may include instructions that configure the processor 120 to perform limited post-processing or delay post-processing of acquired image data based on the amount of battery charge remaining. For example, if a battery charge remaining is less than a predetermined threshold level, or a threshold that is determined during operation, (for example, a dynamically determined threshold), the processor 120 may be instructed by the post-processing determination module 155 to delay post-processing functions, for example robust demosaic filtering, motion-stabilization, skin-tone correction, etc. Therefore, processor 120 , along with battery level determination module 150 , post-processing determination module 155 , and working memory 135 represent one means for determining which post-processing functions to apply to an acquired image and when to apply such functions. In some embodiments, a dynamically determined threshold can be determined based on one or more factors, for example but not limited to, the rate of the battery depletion, how fast the battery has been depleted during previous usage, and/or what other processes are running on the electronic device or the processor. Such thresholds may be dynamically determined for limited post-processing or delay post-processing, or other processes and/or functionality described herein.
[0033] Memory 140 may also contain a low power application module 160 . The low power application module 160 illustrated in FIG. 1 may include instructions that configure the processor 120 to switch from an application that consumes a large amount of power to an application that consumes a low amount of power based on the battery charge remaining. Some embodiments incorporate information in, for example, a look-up table, a file, a database, or in another hardware or software storage component (all of such components referred to as a look-up table for ease of reference) to control which application is launched when the user selects the application icon. In other embodiments, a running process could use a system property to identify whether to operate in a low-power or regular mode. The system property could include information about the current battery level, for example. The process could include an argument that could be passed in to determine the mode of operation. In some embodiments, if a battery charge remaining is less than a predetermined threshold level, the processor 120 may be instructed by the low power application module 160 to access the information stored in the look-up table that controls whether a low power or full power application is launched when the user selects the application icon, and launch the appropriate application. Therefore, processor 120 , along with battery level determination module 150 , low power application module 160 , and working memory 135 represent one means for determining whether to launch a low power or full power application.
[0034] Memory 140 may also contain user interface module 170 . The user interface module 170 illustrated in FIG. 1 may include instructions that configure the processor 120 to provide a collection of on-display objects and soft controls that allow the user to interact with the device. An operating system module 165 may also reside in memory 140 and operate with processor 120 to manage the memory and processing resources of the system 100 . For example, operating system 165 may include device drivers to manage hardware resources for example the electronic display 130 or imaging device 110 . In some embodiments, instructions contained in the battery level determination module 150 and post-processing determination module 155 may not interact with these hardware resources directly, but instead interact through standard subroutines or APIs located in operating system 165 . Instructions within operating system 165 may then interact directly with these hardware components.
[0035] Processor 120 may write data to storage module 125 . While storage module 125 is represented graphically as a traditional disk drive, those with skill in the art would understand multiple embodiments could include either a disk-based storage device or one of several other types of storage mediums, including a memory disk, USB drive, flash drive, remotely connected storage medium, virtual disk driver, or the like.
[0036] Although FIG. 1 depicts a device comprising separate components to include a processor, imaging device, electronic display, and memory, one skilled in the art would recognize that these separate components may be combined in a variety of ways to achieve particular design objectives. For example, in an alternative embodiment, the memory components may be combined with processor components to save cost and improve performance.
[0037] Additionally, although FIG. 1 illustrates two memory components, including memory component 140 comprising several modules and a separate memory 135 comprising a working memory, one with skill in the art would recognize several embodiments utilizing different memory architectures. For example, a design may utilize ROM or static RAM memory for the storage of processor instructions implementing the modules contained in memory 140 . Alternatively, processor instructions may be read at system startup from a disk storage device that is integrated into power management system 100 or connected via an external device port. The processor instructions may then be loaded into RAM to facilitate execution by the processor. For example, working memory 135 may be a RAM memory, with instructions loaded into working memory 135 before execution by the processor 120 .
Method Overview
[0038] Certain functionality of the examples of embodiments described herein relate to predicting how long the battery charge of an electronic device will last and from that prediction, performing full or limited functions on the electronic device, for example, launching and running a low-power or full-power application or performing full or limited post-processing of sensor data for example images. The examples may be described as a process, which may be depicted as a flowchart, a flow diagram, a finite state diagram, a structure diagram, or a block diagram. Although a flowchart may describe the operations as a sequential process, many of the operations can be performed in parallel, or concurrently, and the process can be repeated. In addition, the order of the operations may be re-arranged. A process is terminated when its operations are completed. A process may correspond to a method, a function, a procedure, a subroutine, a subprogram, etc. When a process corresponds to a software function, its termination corresponds to a return of the function to the calling function or the main function.
[0039] FIG. 2 illustrates one embodiment of a process 200 to configure an electronic device into a low power or a full or normal power operation mode that may be implemented in one or more of the modules depicted in FIG. 1 . The low power operating mode desirably consumes less power than the normal power operation mode. The electronic device may be a handheld communication device, e.g., a cellular phone or “smartphone,” or a mobile personal data assistant (PDA) including a tablet computer. In some examples, the process 200 may be run on a processor, for example, processor 120 ( FIG. 1 ), and on other components illustrated in FIG. 1 that are stored in memory 140 or that are incorporated in other hardware or software. The configuration process 200 begins at start block 202 and transitions to block 204 wherein the user first indicates one or more low power operation preferences. In some embodiments, the user may select which feature(s) of the electronic device may be limited during a low power operation. For example, the user may indicate that post-processing of sensor data, for example camera data acquired by an imaging device, for example imaging device 110 ( FIG. 1 ) of the electronic device, may be delayed if the device is in a low power mode of operation. In another example, the user may indicate that a low power application, for example a less graphics-intensive game, may be launched during a low power mode of operation instead of the full game or more graphics-intensive version. In other embodiments, the electronic device may, by default, run low power applications and processes. In this implementation, the user may select which applications, features, or processes to be run in a regular or high power mode. For example, the user may indicate that full post-processing of an image is desired by selecting an image icon or text displayed in a photo gallery (as illustrated in FIG. 5 and discussed in greater detail below). The process 200 then transitions to block 206 , wherein the user indicates a threshold beyond which the device has entered a “usable despite low power” mode. In some embodiments, the threshold could be a battery level threshold. The user may indicate, via a selection, a battery level threshold below which the device would enter a low power mode of operation. In some embodiments, the battery level threshold could be 30% battery charge, 25% battery charge, 20% battery charge, or any other user-defined threshold battery charge percentage. In other embodiments, the user may indicate a time threshold. A time threshold may represent the minimum amount of time the device must continue to function at the current power usage. For example, the user may indicate that the device needs to operate at the current power usage for a specified time to accommodate the user's travel plans, for example air travel. In another example, the user may indicate that the device needs to operate at the current power usage for a specified time to accommodate usage of the device while the user is at a business meeting. In another example, the user could indicate a time threshold when the user is at a theme park and will want to have use of the device to take photos or video for a specified length of time. Once the user has indicated a threshold, either battery-level or time or both, the process 200 transitions to block 208 and ends.
[0040] After the configuration stage is complete, for example when process 200 is complete, in some embodiments the device may run a battery level determination process, for example process 300 shown in FIG. 3 . Process 300 may be used in some embodiments to estimate the amount of battery life remaining in an electronic device or predict how long the battery charge of an electronic device will last. This prediction may be based on data representing historical usage and charging patterns of the electronic device or from location indications or other factors. In some examples, the process 300 may be run on a processor, for example, processor 120 ( FIG. 1 ), and on other components illustrated in FIG. 1 that are stored in memory 140 or that are incorporated in other hardware or software. The battery-level determination process 300 begins at start block 302 and transitions to block 304 wherein a decision is made as to the level of battery charge of the electronic device. If the battery level is low, as defined by a user-defined threshold established during the configuration process 200 , process 300 transitions to block 310 , wherein the device enters a “usable despite low power” mode. In this mode, features or applications may be limited or disabled, as identified by the user in the configuration process 200 , described above. Additional details of operation of the device during a low-power mode will be discussed below. The process 300 then transitions to block 314 and ends.
[0041] If the battery level is not low, as defined by a user-defined threshold, or a dynamically determined threshold, the process 300 transitions to block 306 , wherein the device predicts whether it will deplete the battery prior to the next charge. For example, if the user normally charges the device at 7 pm and the current time is 1 pm with 30% of battery charge left, the device may determine, based on historical usage records of the device, that the device will deplete the battery prior to the next charge cycle when operating at the current, full power usage mode. If this is true, the process 300 transitions to block 310 , where, as discussed above, the device enters a “usable despite low power” mode and disables certain features or processes based on user preferences or device settings, as will be discussed below. The process 300 then transitions to block 314 and may end.
[0042] If the device predicts that it will not deplete the battery prior to the next anticipated charge cycle, the process 300 transitions to block 308 , wherein a determination is made as to whether the user has specified that it will be longer than normal until the next charging cycle. For example, if the user is traveling and selects a longer time threshold in the configuration stage outlined in process 200 and/or a GPS reading from the electronic device indicates that the electronic device is away from the home area, the device may deplete the battery prior to the next charging cycle. In some embodiments, determining a battery level and power usage may include determining historical power usage or current power usage (for example, if the user is taking a large number of pictures in a short time frame). If this is true, the process 300 transitions to block 310 , where, as discussed above, the device enters a “usable despite low power” mode and disables certain features or processes based on user preferences or device settings, as will be discussed below. The process 300 then transitions to block 314 and may end.
[0043] If the user has not specified that it will be longer than normal until the next charge cycle and the device has not determined that it will be longer than normal until the next charge cycle, the process 300 transitions to block 312 , wherein the device enters or remains in a full power mode. In the full power mode, no limitation of features or delayed post-processing is instructed. The process 300 then transitions to block 314 and may end.
[0044] In some embodiments, prediction of time to the next charging cycle and determination of whether the device will deplete the battery prior to the next charge could be based on location information. For example, the user may be at home as determined by GPS coordinates and therefore is likely to recharge the device soon. In other embodiments, prediction of time to the next charging cycle could also be based on time and date information. For example, the user may typically charge the device at 7pm each evening. In other embodiment, prediction of time to the next charging cycle could be based on other historical device usage information.
Operation in Low-Power Mode
[0045] When the device has been alerted that power should be conserved, based on one of the battery-level determination steps of process 300 , discussed above, the device may run a low-power operation process 400 , one example of which is shown in FIG. 4 . Operation in a low power operation mode desirably consumes less power than operation in a normal power operation mode. Process 400 may be used in some embodiments to delay post-processing of sensor data to a time when the device is plugged in or is fully charged. For example, if the user is at a theme park and taking multiple photos and videos without an opportunity to recharge the electronic device, the device may determine, using the battery-level determination process 300 described above, that the device may not have sufficient battery charge to continue to operate in a full power mode until the user can recharge the device. In this situation, the device may switch from a full-power mode, in which sensor data is post-processed shortly after acquisition, to a low-power mode, in which minimal post-processing is performed on the sensor data to conserve battery power such that the device can continue to operate until the user can recharge the device. In some embodiments, the device may run a low-power camera operation according to the steps outlined in the process 400 . In some examples, the process 400 may be run on a processor, for example, processor 120 ( FIG. 1 ), and on other components illustrated in FIG. 1 that are stored in memory 140 or that are incorporated in other hardware or software.
[0046] The low-power operation process 400 begins at start block 402 and transitions to block 404 , wherein the device is operated in a low-power mode. For example, in some embodiments, an imaging device 110 and camera application may be operated in a low-power mode. In a low power operation mode, processes that utilize a large amount of power, for example image processing functions including auto white balance, CFA demosaicing, and storing the processed image as a JPEG, may be delayed until the battery of the device is fully charged or the device is plugged in. In some embodiments, operation in low power operation mode shuts down or bypasses high power consumption processes of the image signal processor of processor 120 that may be run during a normal power operation mode.
[0047] The process 400 then transitions to block 406 , wherein sensor data is obtained. The sensor data may include, for example, still image data or video image data acquired by an imaging device 110 , audio data acquired by a microphone 115 , or any other additional sensor data for example temperature or pressure. In other embodiments, other sensor data may also be obtained. The process 400 then transitions to block 408 , wherein the sensor data is stored in a memory for later processing. Using a camera application as an example, in some embodiments, the low-power application system may configure the imaging device 110 through the API to capture the raw image data and store the data in memory, for example memory 125 for processing at a later time. For example, the low-power camera application may not utilize a view-finder, run auto white balance, run auto focus, or process the raw BGGR Bayer data immediately. Unlike a full-power camera application that may process the raw BGGR data using the camera's image processing pipeline and store the image data as a JPEG file in memory, the raw BGGR data acquired by the imaging device 110 may be stored in memory and processed at a later time. One example of a generic image data processing pipeline 600 that may be bypassed when the device is in a low power operation mode is shown in FIG. 6 . Typically, during a normal power operation mode of an imaging system, significant preprocessing and post-processing is performed on the sensor data acquired by the image sensor. This typical processing operation is illustrated in FIG. 6 .
[0048] In a full or normal power operation mode, the pipeline 600 receives raw image data 602 from the camera sensor and preferably performs full post-processing of the image data. This post-processing may include white balancing the image data 606 , CFA demosaicing 608 , color conversion 610 , and color correction of the image data 612 before storing the image data to memory 616 . This typical process is indicated by the white arrows in FIG. 6 . As discussed above, these processing steps consume battery power and may be bypassed as discussed with respect to process 400 to conserve battery power. For example, during a low power operation mode, the device may bypass one or more steps of the full image processing pipeline shown in FIG. 6 . In one embodiment, in one embodiment of a low power operation mode, the processor may be instructed to perform limited preprocessing 604 of the raw image data 602 and then save the image data to memory 616 , as indicated by the solid black lines 620 in FIG. 6 . In another embodiment, when a device is operating in another embodiment of a low power operation mode, the processor may be instructed to immediately store the raw image data without performing any processing of the raw image data, as indicated by the dashed line 622 in FIG. 6 . A command to post-process the image data, for example a direct command from the user or an instruction received by the processor 120 to enter a high or normal power operation due to the device reaching or exceeding a battery level threshold, may trigger instructions to the processor 120 to inject the sensor data back into the image signal processor (ISP) for post-processing. Once injected back into the ISP for post-processing, the sensor data may be fully processed as indicated in FIG. 6 by the white arrows.
[0049] In some embodiments, a thumbnail photo could be processed and displayed in the photo gallery of an electronic device while higher-quality processing using a more robust demosaic filter, a motion-stabilization filter, skin-tone correction filter, etc. is performed when the device is charging or when the user manually selects a picture for sharing. In one example, a photo gallery of an electronic device, for example a mobile phone, may display text to the user indicating delayed post-processing of image data based on battery charge level, as shown in FIG. 5 . For example, to produce a camera preview picture, the image data may be processed in a reduced quality at the time the photo is taken to produce a temporary image. The temporary image may be formed by reducing the resolution of the displayed images using, for example, a nearest-neighbor Bayer-pattern demosaic filter, or another image resolution process. This temporary image may be displayed in a user's photo gallery as shown in FIG. 5 . The photo gallery may display instructional text to the user indicating that the image will be displayed when the device is plugged in or fully charged. However, in other embodiments, the user may select the text or icon indicating that the image data has not been post-processed to demand full post-processing of the image so that the image can be emailed, uploaded to a website, etc. This will direct the system to post-process the image and display a thumbnail image in the photo gallery in place of an icon or text indicating that the image data has not been fully post-processed.
[0050] In another example, a microphone, for example microphone 115 , may be used to capture raw audio data. If the device is in a low power mode, the system can store the raw audio data in a memory storage, for example memory 125 , for later post-processing at a time when battery charge is full, the device is plugged in and charging, or upon user demand.
[0051] In yet another example, an imaging sensor, for example imaging sensor 110 , may record raw video data. If the device is in a low-power mode, the system can store the raw video data in a memory storage, for example memory 125 , for processing at a time when the battery charge of the device is full, the device is plugged in and charging, or upon user demand.
[0052] The process 400 then transitions to block 412 , wherein a decision is made as to whether the battery level of the electronic device is low. If the battery level is low, the process 400 transitions to block 404 and the process repeats as discussed above. However, if the device is charged or is plugged in and being charged, the process 400 transitions to block 414 , wherein the device can then perform post-processing of raw image data. Post-processing could include applying a more robust demosaic filter, applying a motion-stabilization filter, applying a skin-tone correction filter, along with other post-processing filters and functions. Post-processing could include loading image data from memory and providing image data to the image signal processor (ISP). In one embodiment, the processor may be instructed to load the raw image data 630 and insert the raw image data 630 into the pipeline 600 , as indicated by the line 631 in FIG. 6 . The process 400 then transitions to block 416 and ends.
[0053] In some embodiments, post-processing of the sensor data may also be initialized if the user manually initiates an action that requires the full quality version of the data even when the battery level is low. For example, the device may perform higher-quality post-processing of the image data if the user attempts to email the image.
[0054] In some embodiments, if the battery level is below a user-defined threshold or the device predicts it is not going to have enough charge to last until the next charging cycle, the system can change the look-up table (LUT) that defines which application is launched when the user clicks the application icon. In other embodiments, a running process could use a system property to identify whether to operate in a low-power or regular mode. In some embodiments, the system property could include a battery level indication. The process could include an argument that could be passed in to determine the mode of operation. For example, when the system is in a low power situation, a low-power version of an application for example a camera could be launched. In other embodiments, a low-power version of a gaming application could also be launched when the device is in a low-power mode. The low-power version of these applications could include a shorter game and/or less complex graphics. When the battery level is above a defined threshold or the device is charged, the LUT could be changed so that the application that is launched when the user selects the application icon is the full-power operation application.
[0055] In another example, the processor of an electronic device (for example processor 120 ) could receive instructions to operate a display of an electronic device (for example electronic display 130 ) in a low-power mode. In some embodiments, during a low-power mode of operation, a color format could be changed or the frames per second (fps) could be reduced to conserve battery power. For example, changing from a color format of RGBX8888 at 60 fps to a color format of RGB565 at 30 fps could reduce the amount of bandwidth consumed by a display processing pipeline. Additionally, this color format change and fps reduction could reduce the clock rate at which the hardware operates. In some embodiments incorporating AMOLED displays, the pixels of the electronic display could be dimmed to conserve battery power. In other embodiments, a screen resolution of the electronic display could be adjusted. For example, a 720p screen could display at a lower resolution such that part of the viewing surface of the electronic display is black.
[0056] Embodiments of this predictive battery life and delayed post-processing approach could be implemented on mobile devices for example phones, cameras (including plenoptic or light-field cameras and stereo cameras), tablets, computers, heart rate monitors, etc. These examples are meant to be illustrative and are not limiting.
Clarifications Regarding Terminology
[0057] Unless indicated otherwise, any disclosure of an operation of an apparatus having a particular feature is also expressly intended to disclose a method having an analogous feature (and vice versa), and any disclosure of an operation of an apparatus according to a particular configuration is also expressly intended to disclose a method according to an analogous configuration (and vice versa). The term “configuration” may be used in reference to a method, apparatus, and/or system as indicated by its particular context. The terms “method,” “process,” “procedure,” and “technique” are used generically and interchangeably unless otherwise indicated by the particular context. The terms “apparatus” and “device” are also used generically and interchangeably unless otherwise indicated by the particular context. The terms “element” and “module” are typically used to indicate a portion of a greater configuration. Unless expressly limited by its context, the term “system” is used herein to indicate any of its ordinary meanings, including “a group of elements that interact to serve a common purpose.” Any incorporation by reference of a portion of a document shall also be understood to incorporate definitions of terms or variables that are referenced within the portion, where such definitions appear elsewhere in the document, as well as any figures referenced in the incorporated portion.
[0058] Those having skill in the art will further appreciate that the various illustrative logical blocks, modules, circuits, and process steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both. To clearly illustrate this interchangeability of hardware and software, various illustrative components, blocks, modules, circuits, and steps have been described above generally in terms of their functionality. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the overall system. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention. One skilled in the art will recognize that a portion, or a part, may comprise something less than, or equal to, a whole. For example, a portion of a collection of pixels may refer to a sub-collection of those pixels.
[0059] The various illustrative logical blocks, modules, and circuits described in connection with the embodiments disclosed herein may be implemented or performed with a general purpose processor, a digital signal processor (DSP), an application specific integrated circuit (ASIC), a field programmable gate array (FPGA) or other programmable logic device, discrete gate or transistor logic, discrete hardware components, or any combination thereof designed to perform the functions described herein. A general purpose processor may be a microprocessor, but in the alternative, the processor may be any conventional processor, controller, microcontroller, or state machine. A processor may also be implemented as a combination of computing devices, e.g., a combination of a DSP and a microprocessor, a plurality of microprocessors, one or more microprocessors in conjunction with a DSP core, or any other such configuration.
[0060] The steps of a method or process described in connection with the embodiments disclosed herein may be embodied directly in hardware, in a software module executed by a processor, or in a combination of the two. A software module may reside in RAM memory, flash memory, ROM memory, EPROM memory, EEPROM memory, registers, hard disk, a removable disk, a CD-ROM, or any other form of non-transitory storage medium known in the art. An exemplary computer-readable storage medium is coupled to the processor such the processor can read information from, and write information to, the computer-readable storage medium. In the alternative, the storage medium may be integral to the processor. The processor and the storage medium may reside in an ASIC. The ASIC may reside in a user terminal, camera, or other device. In the alternative, the processor and the storage medium may reside as discrete components in a user terminal, camera, or other device.
[0061] Headings are included herein for reference and to aid in locating various sections. These headings are not intended to limit the scope of the concepts described with respect thereto. Such concepts may have applicability throughout the entire specification.
[0062] The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
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Systems and methods for determining a battery-level of an electronic device and conserving the battery charge of the electronic device are disclosed. The battery consumption of an electronic device may be reduced when the user or the device learns via user input or determines via prediction that the battery will be depleted before the next possible charge cycle. Reducing battery consumption could be accomplished by accessing an application requiring less power consumption and/or delaying post-processing of sensor data related to that application, for example a camera application. Prediction of battery life could include determining the time to the next expected battery charge and delaying the processing of sensor data until the electronic device is plugged in and charging or has reached a predetermined charge level.
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[0001] This application claims the benefit of U.S. Provisional Application No. 60/509,202,filed Oct. 7, 2003.
TECHNICAL FIELD
[0002] The invention generally relates to optical detectors and methods of fabricating such detectors.
BACKGROUND OF THE INVENTION
[0003] To build an optical signal distribution network within a semiconductor substrate, one needs to be able to make good optical waveguides to distribute the optical signals and one needs to be able to fabricate elements that get the optical signals into and out of the waveguides to interface with other circuitry. Extracting the optical signals can be accomplished in at least two ways. Either the optical signal itself is extracted out of the waveguide and delivered to other circuitry that can convert it to the required form. Or the optical can be converted into electrical form in the waveguide and the electrical signal delivered to other the circuitry. Extracting the optical signal as an optical signal involves the use of mirrors within the waveguides or elements that function like mirrors. The scientific literature has an increasing number of examples of technologies that can be used to construct such mirrors. Extracting the optical signal as an electrical signal involves the use of detector within the waveguide, i.e., circuit elements that convert the optical signal to an electrical form. The scientific literature also has an increasing number of examples of detector designs that can be used to accomplish this.
[0004] The challenge in finding the combination of elements that produces an acceptable optical distribution network becomes greater, however, when one limits the frame of reference to particular optical signal distribution network designs and to the financial reality that any such designs should be easy to fabricate and financially economical.
[0005] The combination of silicon and SiGe has attracted attention as useful combination of materials from which one might be able to easily and economically fabricate optical signal distribution networks. With SiGe it is possible to fabricate waveguides in the silicon substrates. The index of refraction of SiGe is slightly higher than that of silicon. For example, SiGe with 5% Ge has a index of refraction of about 3.52 at an optical wavelength of about 1300 nm while crystalline silicon has an index of refraction that is less than that, e.g. about 3.50. So, if a SiGe core is formed in a silicon substrate, the difference in the indices of refraction is sufficient to enable the SiGe core to contain an optical signal through internal reflections. Moreover, this particular combination of materials lends itself to the use of conventional semiconductor fabrication technologies to fabricate the optical circuitry.
[0006] Of course, for such a system to work as an optical signal distribution network, the optical signal must be at a wavelength at which the Si and SiGe are transparent. Since the bandgap of these materials is about 1.12 eV, they appear transparent to the commonly used optical wavelengths of greater than about 1100 nm. But, the transparency of these materials to optical signals having those wavelengths brings with it another problem. These materials are generally not suitable for building detectors that can convert the optical signals to electrical form. To be a good detector, the materials must be able to absorb the light. That is, the optical signal must be capable of generating electron transitions from the valence band to the conduction band within the detector to produce an electrical output signal. But the wavelengths of greater than about 1100 nm are too long to produce electron transitions in silicon. For example, at a wavelength of 1300 nm, the corresponding photon energy is about 0.95 eV, which is well below the bandgap of silicon or SiGe and consequently well below the amount necessary to cause transitions from the valence band into the conductor band.
[0007] One class of detectors that has attracted some interest is the class of SiGe super lattice detectors. These detectors are made up of alternating thin layers of Si and SiGe. Because the lattice constant of these materials is not the same, when the two layers are grown on top of each other the lattice mismatch causes a strain in the SiGe layer. If the Si and SiGe layers are sufficiently thin (e.g. on the order of about 6 nm), and if the process temperatures to which the structure is exposed are sufficiently low (e.g. below about 800° C.), then the induced strain will be permanent. The induced strain reduces the bandgap of the SiGe material. As the percentage of Ge in the SiGe increases, the mismatch becomes greater, the induced strain increases and the bandgap decreases further.
[0008] FIG. 1 illustrates how the percentage of Ge impacts the bandgap in the super lattice structures. If the induced strain is maintained in the SiGe, as the percentage of Ge increases, the bandgap decreases along the lower curve. At some point the percentage of Ge will be enough to reduce the bandgap sufficiently so that it can serve as a detector for light having wavelengths of about 1200 nm (about 0.9 eV). However, if the lattice is allowed to relax thereby relieving the strain, the affect of increasing amounts of Ge on the bandgap will be less dramatic as indicated by the upper curve and it will not be possible fabricate an effective detector for that wavelength.
SUMMARY OF THE INVENTION
[0009] In general, in one aspect, the invention features a method of fabricating a detector. The method involves forming an island of detector core material on a substrate, the island having a horizontally oriented top end, a vertically oriented first sidewall, and a vertically oriented second sidewall that is opposite said first sidewall; implanting a first dopant into the first sidewall to form a first conductive region that has a top end that is part of the top end of the island; implanting a second dopant into the second sidewall to form a second conductive region that has a top end that is part of the top end of the island; fabricating a first electrical connection to the top end of the first conductive region; and fabricating a second electrical connection to the top end of the second conductive region.
[0010] Embodiments have one or more of the following additional features. The process of forming of the island involves forming a layer of the detector core material on the substrate; and etching away selective portions of the detector core material layer to form the island of detector core material. The process of forming of the island also involves, after forming the layer of the detector core material on the substrate, forming a hard mask layer over the top end of the detector core material layer, and the etching away involves etching away selective portions of the hard mask layer and the detector core material layer to form the island of detector core material. The method further involves, after implanting the first and second dopants, removing the hard mask layer from the top end of the island; depositing an isolation material onto the substrate and covering the island; and planarizing the deposited isolation material so that the top ends of the first and second conductive regions are exposed. The method also involves depositing an insulator onto the planarized material; forming a first opening in the insulator above and extending down to the first conductive regions and a second opening in the insulator above and extending down to the second conductive regions; and depositing a metal in the first and second openings to make electrical contact to the first conductive regions. The process of implanting the first dopant involves implanting a p-type dopant and the process of implanting the second dopant involves implanting an n-type dopant. Alternatively, the first and second dopants are the same materials.
[0011] In general, in another aspect, the invention features an optical detector including a substrate; and an island of detector material formed on the substrate, wherein the island has (1) a horizontally oriented top end, a vertically oriented first sidewall, and vertically oriented second sidewall that is opposite said first sidewall, (2) a first doped region extending into the island through first sidewall and forming a first conductive region that extends down into the island of detector material, and (3) a second doped region extending into the island through the second sidewall and forming a second conductive region that extends down into island of the detector material, the first and second conductive regions each having a top end that is part of the top end of the island. The optical detector also includes a first electrical connection to the top end of the first conductive region; and a second electrical connection to the top end of the second conductive region.
[0012] Embodiments include one or more of the following additional features. The optical detector also includes an isolation material covering the first sidewall and the second sidewall of the island and forming a upper surface that is level with the top end of the island; an insulating layer over the isolation material and the island, the insulating layer including a first hole down to the first conductive region and a second hole down to the second conductive region; a first conductor filing the first hole and electrically connecting to the first conductive region; and a second conductor filing the second hole and electrically connecting to the second conductive region. The first conductive region is doped with a p-type dopant and the second conductive region is doped with an n-type dopant. Alternatively, the first and second conductive regions are doped with the same dopant.
[0013] One advantage of some embodiments of the invention is that one can avoid having to use separate masks for the N + and P + implants in the N + —I—N 30 and P + —I—N + structures.
[0014] Another advantage is that it provides a way of fabricating horizontally oriented detectors on a semiconductor substrate.
[0015] Other features and advantages of the invention will be apparent from the following detailed and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 shows the affect on bandgap of the percentage of Ge in a SiGe super lattice structure.
[0017] FIGS. 2 A-G illustrate the process for fabricating a SiGe super lattice detector.
[0018] FIG. 3 illustrates use of a narrower hard mask so as to allow implantation of electrode dopants over more of the top of the structure.
DETAILED DESCRIPTION
[0019] Referring to FIG. 2A , starting with a substrate 100 , e.g. a silicon substrate, a SiGe super lattice structure 102 is deposited onto the upper surface of substrate 100 . Procedures for fabricating such a structure are generally known in the art and thus will not be described in detail here. In the described embodiment, the basic building block of the super lattice is a SiGe layer grown on top of a Si layer. The SiGe layer is thin enough to sustain the induced strain without relaxing (e.g. about 6 nm) with the percentage of Ge being about 60%. The Si layer is about 29 nm think. This basic two-layer building block is repeated about 29 times to fabricate a stack that is about 1 micron high. In the described embodiment, an epitaxial process is used to grow these layers with the composition of the feed gas varied throughout the process to deposit the individual layers.
[0020] After the super lattice is deposited, a hard mask protective layer 104 is formed over the entire surface of the super lattice structure. The purpose of hard mask is to protect the upper surface of the Si/SiGe super lattice structure from being doped during subsequent implantations that are use to form vertically oriented electrodes on either side of the structure. The hard mask can be, for example, SiO 2 which can be formed in one of a number of different ways including oxidizing the surface or epitaxially growing an oxide layer on the surface. Using standard photolithographic techniques, hard mask layer 104 is patterned to define islands 108 of material that are located where the detectors are required. Material outside of the islands defined by the patterned hard mask layer is removed by etching it away (see FIG. 2B ).
[0021] Each island 108 defines the core 103 of the to-be-formed detector, which in this embodiment is a Si/SiGe super lattice detector.
[0022] With the islands now formed at appropriate predefined locations on the surface of the substrate, the substrate is exposed to two separate ion implantation processes. In the first ion implantation process, the substrate is oriented within the ion implantation chamber so one side of the island is exposed to the beam and oriented about at about 45° relative to the ion beam while the other side of the island is protected from the ion beam by being within the shadow of the island, as illustrated in FIG. 2C . In this orientation, a p-type dopant (e.g. boron) 110 is implanted into one side of the island to form a vertically oriented p-type electrode 111 . In the described embodiment, the ion beam energy is about 100-200 kV and the dopant (e.g. boron or phosphorous) is implanted to a depth of about 200 nm. and with a sufficient dose so the resulting doping levels will be above about 10 18 cm −3 .
[0023] After the P + side is implanted, the same procedure is used to implant an n-type dopant (e.g. phosphorus) on the other side of island 108 (see FIG. 2D ) to form a vertically oriented n-type electrode 113 . This time the substrate is oriented within the corresponding ion implantation chamber so the other non-implanted side of the island is exposed to the beam and oriented about at about 45° relative to the ion beam while the previously implanted side is protected from the ion beam by being within the shadow of the island, as illustrated in FIG. 2D .
[0024] During these two implantation processes, the portion of hard mask layer 104 that remains on top of island 108 protects the top of island 108 from being implanted with dopants.
[0025] After the implantation of the dopants for the electrodes, an optional low temperature anneal can be used to diffuse the dopants into the structure to a deeper level, e.g. 300 nm. Of course, the temperature used for the anneal must be low enough so that the induced strain in the Si/SiGe super lattice structure does not relax during the anneal process.
[0026] After both sides of the island are implanted, hard mask 104 is stripped off (see FIG. 2E ) exposing the top portions of the two implanted regions. Then, an isolation material 112 (e.g. epitaxial silicon or SiO 2 ) is formed over the surface of the substrate and having a thickness that is at least as great as the height of the islands. One purpose of this material is to fill in the regions between the regions between the detector structures and other devices.
[0027] After the isolation material has been formed over the substrate, the substrate is then planarized using, for example, chemical mechanical polishing (CMP) to remove isolating material 112 down to the top surface of the island, exposing the top portions to the two vertically oriented electrodes 111 and 113 .
[0028] At some point during subsequent fabrication, electrical connection will be made to the top portions of the two vertically oriented electrodes 111 and 113 . When this happens depends on what other circuitry is to be fabricated on the substrate. In essence, the subsequent steps will involve (referring to FIG. 2G ) forming an insulating layer 120 (e.g. SiO 2 ) over the detector, patterning openings 122 through that insulating layer and extending down to the electrodes, and then depositing a metal 124 within the openings to make electrical contact to the two electrodes. Using a silicide process to improve the ohmic character of the electrical contacts at the top of the electrodes is also an option.
[0029] For an optical mode to sit comfortably within the detector region, that region needs to be tall (M) and narrow (L). Also, the width L of the detector region impacts the speed of the device. That is, a narrower detector region yields a quicker transit time for the electrons. So to produce faster detectors L must be kept sufficiently small. In the described embodiment, L≈0.5μ and M≈1-2μ.
[0030] In the embodiments shown in FIGS. 2 A-G, hard mask 104 shadows the upper portions of islands 108 just under mask 104 . To increase the coverage of the implanted dopants at the top of the electrodes, one can etch back the hard mask as shown in FIG. 3 . This would allow the side implants to more effectively reach the topmost portions of the electrodes.
[0031] The detectors described above are considered to particularly useful in fabrication of the optical ready substrates such as are described in detail in U.S. patent application Ser. No. 10/280,505, filed Oct. 25, 2002, entitled “Optical Ready Substrates,” and U.S. patent application Ser. No. 10/280,492, filed Oct. 25, 2002, entitled “Optical Ready Wafers,” both of which are incorporated herein by reference. Some of the waveguides that are mentioned in connection with the optical ready substrates are SiGe waveguides. Methods of making such waveguides are described in publicly available scientific literature including, for example, U.S. patent application Ser. No. 09/866,172, filed May 24, 2001, entitled “Method for Fabricating Waveguides,” and to U.S. patent application Ser. No. 10/014,466, filed Dec. 11, 2001, entitled “Waveguides Such As SiGeC Waveguides and Method of Fabricating Same,” both of which are incorporated herein by reference.
[0032] If used in connection with waveguides such as are described above, one option is to first fabricate the detectors on the substrate and then fabricate the waveguides to which the detectors are coupled. The detector is aligned with the waveguide so that an electrode is positioned on either side of the waveguide. In FIG. 2G that would mean that the axis of the waveguide is normal to the plane of the figure and aligned with the detector core (i.e., SiGe super lattice 102 ). The detector is made sufficiently long along the axis of the waveguide to yield the desired absorption/sensitivity.
[0033] The specifics of the implantation process described above are meant to merely be illustrative. As is known to persons skilled in the art, a wide range of alternative process conditions can be used to accomplish the implantation of the dopants in the vertical regions that will constitute the electrodes. In general during the implantation phase of the fabrication process, the goal is to choose the ion implanting energies, the doses, the times and the temperatures so as to produce heavily doped, low resistivity regions which will function as electrodes. A typical energy for implanting the dopants is between 100 kV and 200 kV, which is the range of energies in which of many commercially available implantation systems operate. In general, the ion energy needs to be sufficient to get adequate projected range into the host SiGe (e.g. at least about 0.1μ) so the dopant remains in the host material during subsequent processing.
[0034] In reality, the implant energies can be as low as a few hundred eV or as high as a few MeV. If low implant energies are used, then other known techniques will likely have to be employed to prevent that shallow implanted material from evaporating during subsequent processing before it is able to diffuse into the host material. A commonly used well-known technique to address this problem is to use a capping layer (e.g. SiO 2 or Si 3 N 4 ) to hold the implant in place until the diffusion into the host material has taken place.
[0035] The hard mask is used to protect against forming an electrical short across the top of the island between the two conductive regions on opposite sides of the island. In the case of a P + —I—N + structure, however, the hard mask may be omitted since there would be less risk of producing an electrical short between the two conductive regions of opposite conductivity types.
[0036] The structure described herein and the method of fabricating it can be used for a wide variety of optical detectors other than optical detectors that employ Si/SiGe super lattice cores 103 . For example, it can also be used for N + —I—N + and P + —I—N + structures, where the I-region is made of any suitable material that is appropriate for performing the optical detection function of the device.
[0037] Other embodiments are within the following claims.
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A method of fabricating a detector, the method including forming an island of detector core material on a substrate, the island having a horizontally oriented top end, a vertically oriented first sidewall, and a vertically oriented second sidewall that is opposite said first sidewall; implanting a first dopant into the first sidewall to form a first conductive region that has a top end that is part of the top end of the island; implanting a second dopant into the second sidewall to form a second conductive region that has a top end that is part of the top end of the island; fabricating a first electrical connection to the top end of the first conductive region; and fabricating a second electrical connection to the top end of the second conductive region.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an air volume control module for controlling the rotational speed of the blower of a vehicular air conditioning apparatus.
2. Description of the Related Art
Vehicular aid-conditioning systems include a blower unit and a cooling/heating unit. Air delivered from the blower of the blower unit is adjusted in temperature by the evaporator and heater of the cooling/heating unit and introduced as conditioned air from air outlets into the passenger compartment of the vehicle.
The blower is rotated by a motor whose rotational speed is controlled by an air volume control module for use with the vehicular air conditioning apparatus, as disclosed in Japanese Laid-Open Patent Publication No. 2005-289243.
One known air volume control module of the type described above is shown in FIGS. 7 and 8 of the accompanying drawings. As shown in FIGS. 7 and 8 , the air volume control module, generally denoted by 1 , comprises a circuit board 2 including a control circuit, a heat sink 3 on which the circuit board 2 is mounted, and a base housing 5 surrounding a portion 4 of the heat sink 3 on which the circuit board 2 is mounted. The portion 4 will hereinafter be referred to as “board mount 4 ”.
The base housing 5 is generally made of a resin material and has an insertion opening 6 defined in one end thereof for the insertion therein of the heat sink 3 . The heat sink 3 has a support base 7 disposed on the board mount 4 and a plurality of fins 8 mounted on the support base 7 . The support base 7 is wider than the insertion opening 6 . When the support base 7 is secured to the base housing 5 with the board mount 4 inserted in the insertion opening 6 , the heat sink 3 is supported on the base housing 5 with the fins 8 projecting therefrom (see FIG. 8 ).
The board mount 4 includes a pair of parallel support plates 9 , 10 (see FIG. 7 ) extending parallel to each other away from the support base 7 . The circuit board 2 is firmly mounted on the parallel support plates 9 , 10 . Four terminals 11 through 14 are joined to the circuit board 2 and extend away from the board mount 4 . When the board mount 4 is housed in the base housing 5 , the terminals 11 through 14 project into a terminal protector 36 of the base housing 5 . In FIG. 7 , the terminals 12 , 14 are positioned behind the respective terminals 11 , 13 and hence concealed from view.
A power transistor, not shown, is mounted on the circuit board 2 . The terminals 11 , 12 , the terminal 13 , and the terminal 14 are electrically connected respectively to the drain, gate, and source electrodes of the power transistor. A capacitor 15 is also mounted on the circuit board 2 .
A plurality of resistors, not shown, are also mounted on the circuit board 2 . The power transistor, the capacitor 15 , and the resistors are electrically connected, making up a control circuit for controlling the rotational speed of the motor.
The base housing 5 has a pair of through screw holes 16 , 17 defined therein. The heat sink 3 includes a pair of internally threaded legs 18 , 19 disposed adjacent to the respective parallel support plates 9 , 10 and positioned diagonally opposite to each other across the heat sink 3 . Screws 20 , 21 are inserted respectively through the through screw holes 16 , 17 and threaded respectively into the internally threaded legs 18 , 19 , thereby fastening the base housing 5 to the heat sink 3 .
The air volume control module 1 thus constructed is installed at a given position in the vehicular air conditioning apparatus, and an electric power source is electrically connected to the terminals 11 through 14 .
The base housing 5 has an end flange having a triangular end and a trapezoidal end which are opposite to each other. When an attempt is made to install the base housing 5 in a wrong orientation in the vehicular air conditioning apparatus, the triangular end of the end flange of the base housing 5 physically interferes with a certain surface of the vehicular air conditioning apparatus, preventing the base housing 5 from being installed in the vehicular air conditioning apparatus. Consequently, the base housing 5 can be installed in the vehicular air conditioning apparatus only when the base housing 5 is properly oriented with respect to the vehicular air conditioning apparatus.
The base housing 5 is fastened to the heat sink 3 by the screws 20 , 21 . However, the fastening process is tedious and time-consuming to perform because it is necessary to position the screws 20 , 21 with respect to the through screw holes 16 , 17 and turn the positioned screws 20 , 21 to tighten them in the internally threaded legs 18 , 19 .
SUMMARY OF THE INVENTION
It is a general object of the present invention to provide an air volume control module for use with a vehicular air conditioning apparatus, which includes a base housing that can easily be installed on a heat sink.
A major object of the present invention is to provide an air volume control module for use with a vehicular air conditioning apparatus, which can be assembled according to a highly simple assembling process.
According to the present invention, there is provided an air volume control module for controlling the rotational speed of a blower of a vehicular air conditioning apparatus, comprising a circuit board including a control circuit for controlling the rotational speed of the blower, a heat sink connected to the circuit board and including a fin for radiating heat generated by the circuit board, and a base housing surrounding the circuit board, the heat sink being inserted in the base housing with the fin projecting from the base housing, wherein the base housing has an insertion opening for inserting the heat sink therethrough into the base housing, and includes a locking finger disposed adjacent to the insertion opening for locking the heat sink in the base housing, the base housing is mounted on the heat sink only by the locking finger, and either one of the base housing and the fin of the heat sink has a protective projection having a heightwise dimension greater than that of the locking finger.
In the present invention, the heat sink is mounted on the base housing by the locking finger. Thus, the heat sink and the base housing do not need to be fastened to each other by screws. In other words, it is not necessary to position screws and turn the positioned screws in securing the heat sink to the base housing. The heat sink may be installed on the base housing simply by inserting a board mount of the heat sink into the base housing.
Since no process is required to position screws and no process is required to turn the positioned screws, the air volume control module can be assembled highly efficiently according to a highly simple assembling process.
The air volume control module includes the protective projection which has a heightwise dimension greater than that of the locking finger. When the air volume control module is installed on a predetermined position of a structural member of the vehicular air conditioning apparatus, only the protective projection hits the structural member, but the locking finger does not hit the structural member. The locking finger is thus prevented from being broken by the structural member, preventing the heat sink from being dislodged from the base housing.
According to the related art, the air volume control module is prevented from being assembled in error in the vehicular air conditioning apparatus because the end surface (flange) of the base housing physically interferes with a certain portion of the vehicular air conditioning apparatus if the air volume control module is wrongly oriented. Therefore, the end flange of the base housing needs to be of a dimension which can physically interfere with the certain portion of the vehicular air conditioning apparatus. According to the present invention, the protective projection should be disposed in a position which physically interferes with the vehicular air conditioning apparatus when an attempt is made to install the air volume control module in a wrong orientation in the vehicular air conditioning apparatus.
Because of the protective projection thus positioned, an end flange of the base housing is not required to be of an excessive dimension for physical interference with a certain region of the vehicular air conditioning apparatus. As a result, the amount of a material which the base housing is made of may be reduced. The air volume control module according to the present invention is, therefore, a resource saver and a cost saver.
The above and other objects, features, and advantages of the present invention will become more apparent from the following description when taken in conjunction with the accompanying drawings in which preferred embodiments of the present invention are shown by way of illustrative example.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an air volume control module according to a first embodiment of the present invention;
FIG. 2 is an enlarged fragmentary cross-sectional view of the air volume control module shown in FIG. 1 ;
FIG. 3 is a plan view, partly in cross section, showing the manner in which the air volume control module shown in FIG. 1 is installed, with a base housing being directed in a normal orientation, on a structural member of a vehicular air conditioning apparatus;
FIG. 4 is a plan view, partly in cross section, showing the manner in which an attempt is made to install the air volume control module shown in FIG. 1 , with the base housing being directed in a wrong orientation, on the structural member of the vehicular air conditioning apparatus;
FIG. 5 is a perspective view of an air volume control module according to a second embodiment of the present invention;
FIG. 6 is an enlarged fragmentary cross-sectional view of the air volume control module shown in FIG. 5 ;
FIG. 7 is an exploded plan view of an air volume control module according to the related art; and
FIG. 8 is a perspective view of the air volume control module shown in FIG. 7 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Air volume control modules according to preferred embodiments of the present invention will be described in detail below with reference to FIGS. 1 through 6 . Those parts shown in FIGS. 1 through 6 which are identical to those shown in FIGS. 7 and 8 are denoted by identical reference characters, and will not be described in detail below. Furthermore, like or corresponding parts are denoted by like or corresponding reference characters throughout views.
FIG. 1 shows in perspective an air volume control module 30 according to a first embodiment of the present invention. As shown in FIG. 1 , the air volume control module 30 generally comprises a heat sink 32 of metal and a base housing 34 connected to the heat sink 32 .
The heat sink 32 is structurally similar to the heat sink 3 shown in FIGS. 7 and 8 except that the heat sink 32 is free of the internally threaded legs 18 , 19 . Specifically, the heat sink 32 has a wide support base 7 , a board mount 4 disposed beneath the support base 7 , and a plurality of fins 8 mounted on the support base 7 . The board mount 4 is inserted through an insertion opening 6 defined in an end flange of the base housing 34 and finally placed in the base housing 34 .
The board mount 4 includes a pair of parallel support plates 9 , 10 (see FIG. 7 ) extending parallel to each other away from the support base 7 as with the heat sink 3 . The circuit board 2 is firmly mounted on the parallel support plates 9 , 10 . When the board mount 4 is placed in the base housing 34 , terminals that are electrically connected to the drain, gate, and source electrodes of the power transistor mounted on the circuit board 2 project into a terminal protector 36 of the base housing 34 .
The fins 8 of the heat sink 32 project from the base housing 34 (see FIG. 1 ). The fins 8 , which are arranged parallel to each other at spaced intervals in an array, include second fins 8 a , 8 b and third fins 8 c , 8 d from respective opposite ends of the array. As shown in FIGS. 1 and 2 , an engaging tooth 38 is mounted on and extends between side edges of the second and third fins 8 a , 8 c at their lower ends, and an engaging tooth 40 is also mounted on and extends between side edges of the second and third fins 8 b , 8 d at their lower ends. Similarly, an engaging tooth 42 is mounted on and extends between opposite side edges of the second and third fins 8 a , 8 c at their lower ends, and an engaging tooth 44 is also mounted on and extends between opposite side edges of the second and third fins 8 b , 8 d at their lower ends. The engaging teeth 42 , 44 are positioned in line-symmetric relationship to the engaging teeth 38 , 40 with respect to the axis of the array of fins 8 .
The base housing 34 , which is made of a resin material, has four locking fingers 46 , 48 , 50 , 52 integrally formed therewith which project from a surface of the base housing 34 that faces away from the board mount 4 . The locking fingers 46 , 48 , 50 , 52 , which are shaped identically to each other, are positioned closely to the insertion opening 6 and held in alignment with the engaging teeth 38 , 40 , 42 , 44 . The locking fingers 50 , 52 are positioned in line-symmetric relationship to the locking fingers 46 , 48 with respect to the axis of the array of fins 8 .
As shown in FIG. 2 , the locking fingers 46 , 48 , 50 , 52 have respective hooks 54 projecting toward the fins 8 and engaging the upper end surfaces of the respective engaging teeth 38 , 40 , 42 , 44 . Since the engaging teeth 38 , 40 , 42 , 44 of the heat sink 32 are locked by the respectively hooks 54 of the locking fingers 46 , 48 , 50 , 52 , the heat sink 32 is securely mounted on the base housing 34 .
The second fin 8 a includes a pair of protective projections 56 , 60 on the respective longitudinal side edges thereof. The protective projections 56 , 60 have a heightwise dimension greater than the locking fingers 46 , 50 . Similarly, the second fin 8 b includes a pair of protective projections 58 , 62 on the respective longitudinal side edges thereof. The protective projections 58 , 62 have a heightwise dimension greater than the locking fingers 48 , 52 . The protective projections 56 , 58 , 60 , 62 are positioned adjacent to the locking fingers 46 , 48 , 50 , 52 , respectively, with small clearances therebetween.
The air volume control module 30 according to the first embodiment is basically constructed as described above. A process of assembling the air volume control module 30 and advantages of the air volume control module 30 will be described below.
For assembling the air volume control module 30 , the board mount 4 of the heat sink 32 is inserted into the insertion opening 6 of the base housing 34 . At this time, the locking fingers 46 , 48 , 50 , 52 , which are integrally formed with the base housing 34 of resin material, are resiliently flexed away from the insertion opening 6 because the hooks 54 are pressed and laterally displaced by the respective engaging teeth 38 , 40 , 42 , 44 .
When the engaging teeth 38 , 40 , 42 , 44 move past the respective hooks 54 , the locking fingers 46 , 48 , 50 , 52 resiliently snap back, bringing the hooks 54 into engagement with the upper end surfaces of the respective engaging teeth 38 , 40 , 42 , 44 . As a result, the engaging teeth 38 , 40 , 42 , 44 are locked by the respective locking fingers 46 , 48 , 50 , 52 , so that the heat sink 32 is securely mounted on the base housing 34 . Therefore, the heat sink 32 does not need to be fastened to the base housing 34 by screws.
According to the first embodiment, as described above, the heat sink 32 can easily be installed on the base housing 34 simply by inserting the board mount 4 of the heat sink 32 into the insertion opening 6 of the base housing 34 . It is not necessary to perform a tedious and time-consuming process of positioning and tightening screws in assembling the air volume control module 30 .
As shown in FIG. 3 , the assembled air volume control module 30 is then installed at a given position on a structural member 70 of a vehicular air conditioning apparatus, with the heat sink 32 being placed in a predetermined position in the structural member 70 .
If it were not for the protective projections 56 , 58 , 60 , 62 , then the locking fingers 46 , 48 , 50 , 52 would be fully exposed and might possibly be broken when the locking fingers 46 , 48 , 50 , 52 hit the structural member 70 of the vehicular air conditioning apparatus.
According to the first embodiment, however, the protective projections 56 , 58 , 60 , 62 which have a heightwise dimension greater than the locking fingers 46 , 48 , 50 , 52 are positioned adjacent to the locking fingers 46 , 48 , 50 , 52 , respectively, as described above. Therefore, only the protective projections 56 , 58 , 60 , 62 , but not the locking fingers 46 , 48 , 50 , 52 , will hit the structural member 70 of the vehicular air conditioning apparatus. Consequently, the locking fingers 46 , 48 , 50 , 52 are protected against being broken, preventing the heat sink 32 from being dislodged from the base housing 34 .
In FIG. 3 , the air volume control module 30 is shown as being installed, with the base housing 34 being directed in a normal orientation, on the structural member 70 of the vehicular air conditioning apparatus. When an attempt is made to install the air volume control module 30 , with the base housing 34 being directed in an opposite orientation, i.e., a wrong orientation, on the structural member 70 of the vehicular air conditioning apparatus, as shown in FIG. 4 , some of the protective projections 56 , 58 , 60 , 62 physically interfere with the structural member 70 . Accordingly, the air volume control module 30 cannot properly be installed on the structural member 70 of the vehicular air conditioning apparatus, or stated otherwise is prevented from being assembled in error on the vehicular air conditioning apparatus.
When an attempt is made to install the air volume control module 30 which is free of the protective projections 56 , 58 , 60 , 62 , with the base housing 34 being directed in the wrong orientation, on the structural member 70 of the vehicular air conditioning apparatus, as shown in FIG. 4 , some of the locking fingers 46 , 48 , 50 , 52 would possibly hit the structural member 70 and be broken thereby. According to the first embodiment, however, since some of the protective projections 56 , 58 , 60 , 62 physically interfere with the structural member 70 , the heat sink 32 will not be further inserted into the hole in the structural member 70 . The locking fingers 46 , 48 , 50 , 52 will not be brought into hitting engagement with the structural member 70 and hence will not be broken thereby.
In addition, the end flange of the base housing 34 is not required to be of such a dimension as to extend to and interfere with a certain region of the structural member 70 , e.g., a rib 72 (see FIGS. 3 and 4 ), when an attempt is made to install the air volume control module 30 in a wrong orientation on the structural member 70 . As a result, in forming the base housing 34 , the amount of the resin material which the base housing 34 is made of may be reduced. The air volume control module 30 according to the first embodiment is, therefore, a resource saver and a cost saver.
The protective projections may be integrally formed with the base housing 34 . Such a modification will be described below.
FIG. 5 shows in perspective an air volume control module 80 according to a second embodiment of the present invention. The air volume control module 80 is similar to the air volume control module 30 according to the first embodiment except that the fins 8 a , 8 b are free of the protective projections 56 , 58 , 60 , 62 and the base housing 34 has protective projections 82 , 84 , 86 , 88 integrally formed therewith and disposed adjacent to the locking fingers 46 , 48 , 50 , 52 , respectively. Those parts of the air volume control module 80 which are identical to those of the air volume control module 30 according to the first embodiment are denoted by identical reference characters and will not be described in detail below.
As shown in FIGS. 5 and 6 , the protective projections 82 , 84 , 86 , 88 are positioned adjacent to the opposite longitudinal ends of the second fins 8 a , 8 b from respective opposite ends of the array of the fins 8 . The protective projections 82 , 84 , 86 , 88 are spaced from the locking fingers 46 , 48 , 50 , 52 with small clearances therebetween to allow the locking fingers 46 , 48 , 50 , 52 to remain resiliently flexible.
The protective projections 82 , 84 , 86 , 88 have a heightwise dimension greater than that of the locking fingers 46 , 48 , 50 , 52 . Therefore, when the air volume control module 80 is to be installed on the structural member 70 of the vehicular air conditioning apparatus, only the protective projections 82 , 84 , 86 , 88 , but not the locking fingers 46 , 48 , 50 , 52 , will hit the structural member 70 of the vehicular air conditioning apparatus. Consequently, the locking fingers 46 , 48 , 50 , 52 are protected against being broken, preventing the heat sink 32 from being dislodged from the base housing 34 .
When an attempt is made to install the air volume control module 80 , with the base housing 34 being directed in a wrong orientation, on the structural member 70 of the vehicular air conditioning apparatus, some of the protective projections 82 , 84 , 86 , 88 physically interfere with the structural member 70 , as shown in FIG. 4 . Accordingly, the air volume control module 80 is prevented by the protective projections 82 , 84 , 86 , 88 from being assembled in error on the vehicular air conditioning apparatus.
Stated otherwise, if it were not for the protective projections 82 , 84 , 86 , 88 , then when an attempt is made to install the air volume control module 80 , with the base housing 34 being directed in the normal orientation but displaced from a predetermined position or with the base housing 34 being directed in a wrong orientation, on the structural member 70 , some of the locking fingers 46 , 48 , 50 , 52 would possibly hit the structural member 70 and be broken thereby. According to the second embodiment, however, since some of the protective projections 82 , 84 , 86 , 88 physically interfere with the structural member 70 , the heat sink 32 will not be further inserted into the hole in the structural member 70 . The locking fingers 46 , 48 , 50 , 52 will not be brought into hitting engagement with the structural member 70 and hence will not be broken thereby.
In the first and second embodiments, as described above, when an attempt is made to install the air volume control module 30 or the air volume control module 80 in a wrong orientation on the structural member 70 , some of the protective projections 56 , 58 , 60 , 62 or the protective projections 82 , 84 , 86 , 88 physically interfere with the structural member 70 , preventing the air volume control module 30 or the air volume control module 80 from being assembled in error on the vehicular air conditioning apparatus. However, the end flange of the base housing 34 may be of such a dimension as to extend to and interfere with a certain region of the structural member 70 , e.g., the rib 72 (see FIGS. 3 and 4 ), when an attempt is made to install the air volume control module 30 or the air volume control module 80 in a wrong orientation on the structural member 70 .
Although certain preferred embodiments of the present invention have been shown and described in detail, it should be understood that various changes and modifications may be made therein without departing from the scope of the appended claims.
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An air volume control module for use with a vehicular air conditioning apparatus includes a circuit board including a control circuit for controlling the rotational speed of the blower of the vehicular air conditioning apparatus, a heat sink connected to the circuit board and including a fin for radiating heat generated by the circuit board, and a base housing surrounding the circuit board, the heat sink being inserted in the base housing with the fin projecting from the base housing. The base housing is mounted on the heat sink only by a locking finger. Either one of the base housing and the fin of the heat sink has a protective projection having a heightwise dimension greater than that of the locking finger.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the priority benefit of U.S. Provisional Patent Application 61/424,464 filed 17 Dec. 2010 entitled SYSTEMS AND METHODS FOR INJECTING A PARTICULATE MIXTURE, the entirety of which is incorporated by reference herein.
FIELD
[0002] The present techniques relate to permeability control of a solid-liquid slurry. More specifically, the techniques relate to methods and systems of permeability control of a slurry stream formed by mixing two or more different solid-fluid mixture streams.
BACKGROUND
[0003] This section is intended to introduce various aspects of the art, which may be associated with exemplary embodiments of the present techniques. This discussion is believed to assist in providing a framework to facilitate a better understanding of particular aspects of the present techniques. Accordingly, it should be understood that this section should be read in this light, and not necessarily as admissions of prior art.
[0004] Modern society is greatly dependant on the use of hydrocarbons for fuels and chemical feedstocks. Hydrocarbons are generally found in subsurface rock formations that can be termed “reservoirs.” Removing hydrocarbons from the reservoirs depends on numerous physical properties of the rock formations, such as the permeability of the rock containing the hydrocarbons, the ability of the hydrocarbons to flow through the rock formations, and the proportion of hydrocarbons present, among others.
[0005] Easily harvested sources of hydrocarbon are dwindling, leaving less accessible sources to satisfy future energy needs. However, as the costs of hydrocarbons increase, these sources become attractive. Recently, the harvesting of oil sands to remove bitumen has become economical. Hydrocarbon removal from the oil sands may be performed by several techniques. For example, a well can be drilled to an oil sand reservoir and steam, hot air, solvents, or a combination thereof, can be injected to release the hydrocarbons. The released hydrocarbons may then be collected and brought to the surface. In another technique, strip or surface mining may be performed to access the oil sands, which can then be treated with hot water or steam to extract the oil. However, this technique produces a substantial amount of waste or tailings that must be disposed. Traditionally in the oil sand industry, tailings are disposed of in tailings ponds.
[0006] One process for harvesting oil sands that generates less waste is the slurrified heavy oil reservoir extraction process. In the slurrified heavy oil reservoir extraction process, the entire contents of a reservoir, including sand and hydrocarbon, can be extracted from the subsurface via wellbores for processing at the surface to remove the hydrocarbons. The tailings are then reinjected via wellbores back into the subsurface to prevent subsidence of the reservoir and allow the process to sweep the hydrocarbon bearing sands from the reservoir to the wellbores producing the slurry.
[0007] U.S. Pat. No. 5,832,631 to Herbolzheimer et al. discloses one such slurrified hydrocarbon recovery process that uses a slurry that is injected into a reservoir. In this process, hydrocarbons that are trapped in a solid media, such as bitumen in tar sands, can be recovered from deep formations. The process is performed by relieving the stress of the overburden and causing the formation to flow from an injection well to a production well, for example, by fluid injection. A tar sand/water mixture is recovered from the production well. The bitumen is separated from the sand and the remaining sand is reinjected in a water slurry.
[0008] International Patent Application No. WO/2007/050180, by Yale and Herbolzheimer, discloses an improved slurrified heavy oil recovery process. The application discloses a method for recovering heavy oil that includes accessing a subsurface formation, from two or more locations. The formation may include heavy oil and one or more solids. The formation is pressurized to a pressure sufficient to relieve the overburden stress. A differential pressure is created between the two or more locations to provide one or more high pressure locations and one or more low pressure locations. The differential pressure is varied within the formation between the one or more high pressure locations and the one or more low pressure locations to mobilize at least a portion of the solids and a portion of the heavy oil in the formation. The mobilized solids and heavy oil then flow toward the one or more low pressure locations to provide a slurry comprising heavy oil, water and one or more solids. The slurry comprising the heavy oil and solids is flowed to the surface where the heavy oil is recovered from the one or more solids. The one or more solids are recycled to the formation, for example, as backfill.
[0009] Backfill systems for reinjection of tailings in mining operations fall into two major flow categories. See Cooke, “Design procedure for hydraulic backfill distribution systems,” The Journal of The South African Institute of Mining and Metallurgy, March/April 2001, pp. 97-102 (hereinafter “Cooke 2001”). The first category is a free fall flow and the second category is a full flow or continuous flow.
[0010] The free fall systems are categorized by low flow rates such that gravity force is larger than friction force on a slurry, so that the slurry falls freely in the pipe until it reaches the free surface. The advantage of such a system is its tolerance to variations in tailings stream properties, such as solids volume concentration and flow rate. However, the backfilling pipes may often have a short life span. The reasons behind the short pipe life span include the impact damage of slurry freely falling with speeds of up to 45 m/s, high impact pressure when slurry hits the free surface, high erosion rates when slight deviations from vertical occur in free fall region, and excessive pressure in the event of pipeline blockage.
[0011] The continuous systems are categorized by slurry occupying the full length of the reinjection well and the pipelines without any area of free fall. The advantage of this method is a much longer pipe life span as the free fall associated modes of pipe wear may be decreased. However, a fairly high backfill flow rate must be maintained so that friction loss is equal or greater than the backfill weight. Such systems may be sensitive to changes in flow rate and slurry rheology. Therefore, friction regulating/augmenting devices such as liners, valves, breaks or, more often, through solids volume concentration regulation are common However, if the formation in the immediate vicinity of the injection represents a significant resistance to the backfill flow, then a large backpressure will develop which will support the weight of the backfill.
[0012] Most modern backfilling systems in mining operations are of the continuous type. Generally, hydraulic backfills are classified as slurries and pastes (See Cooke 2001). Slurries are characterized by a low fraction of small particles or fines, for example, less than about 75 μm, and volume concentrations equal to or less than particle constant contact solid concentration, i.e., the volume concentration at or above which particles start developing permanent contacts with each other. Pastes, on the other hand, have large fines content and volume concentrations exceeding constant contact solid concentration, for example, about 45-50%. Previous art in this area is strongly related to particle size control and slurry distribution systems.
[0013] As suggested above, many efforts have been made previously in this area. Among the prior U.S. patents related to the technology disclosed herein, the following non-exclusive list is representative of those efforts: U.S. Pat. Nos. 3,508,407; 4,968,187; 3,340,693; 6,168,352; 3,786,639; 3,440,824; 5,141,365 4,101,333; 3,608,317; 5,340,235; 6,297,295; 6,431,796; 6,554,368; 6,640,912; 6,910,411; 7,069,990; and 7,571,080. Additionally, published U.S. Patent Application Publication Nos. 2007/0197851 and 2008/0179092 are representative of more recent efforts in this area.
SUMMARY
[0014] A method of injecting a particulate mixture. The method includes forming a mixture comprising coarse particles and fine particles, wherein the mixture has a permeability in a predefined range. A fluid content of the mixture is controlled to control a rheological property of the mixture. The mixture is injected through a pipe into a target location.
[0015] The target location may be a subsurface formation comprising bitumen and may be located at a depth of least about 50 meters. At least one solids stream comprises residual hydrocarbons. A mass-averaged median diameter of the coarse particles may be larger than a mass-averaged median diameter of the fine particles.
[0016] In some embodiments, fluid may be added to various components to control various properties. For example, a fluid stream may be added to the mixture to adjust a rheological property of the mixture, a density of the mixture, or both. A fluid stream may be added to a stream comprising the coarse particles to adjust a rheological property of the mixture, the density of the mixture, or both. A fluid stream may be added to a stream comprising the fine particles to adjust a rheological property of the mixture, the density of the mixture, or both.
[0017] In some embodiments, fluid may be removed from various components to control various properties. A fluid may be removed from the mixture to adjust a rheological property of the mixture, the density of the mixture, or both. A fluid may be removed from a stream comprising the coarse particles to adjust a rheological property of the mixture, the density of the mixture, or both. The fluid can be removed from the stream comprising the coarse particles by a centrifuge, a vacuum belt, a vibrating screen filter, or any combinations thereof. A fluid can be removed from a stream comprising the fine particles to adjust a rheological property of the mixture, the density of the mixture, or both. The fluid can be removed in a thickener. The fluid can be removed with an addition of coagulation agents. The rheological property of the mixture, a density of the mixture, or both, can be controlled to adjust a frictional pressure loss of the mixture during a flow through a pipe or a wellbore.
[0018] The ratio of mixing of particle sources may be controlled in embodiments to adjust a number of responses. For example, a ratio of mixing between particle sources can be controlled based, at least in part, on a real-time estimate of averaged particle sizes, particle size distributions, permeability, rheology, or density for at least one of the plurality of particle sources. A ratio of mixing between particle sources can be controlled to control, at least in part, an injection rate of the mixture. A ratio of mixing between particle sources can be controlled to control, at least in part, an erosion rate of the pipe due to the mixture flow. A ratio of mixing between particle sources can be controlled based, at least in part, on a real-time measurement of averaged particle sizes, particle size distributions, or rheology of one or more particle sources or the resulting mixture.
[0019] The permeability of the mixture may be between about 0.01 and about 10 times an initial permeability of a material in a subsurface formation. The rheological property of the mixture can be controlled so that the mixture does not free fall in the pipe during injection. The rheological property can be controlled, at least in part, by addition of a chemical additive. The chemical additive includes a polymer, a gelling agent, a flocculent, a pH modifier, or any combinations thereof. An injection pipe used to inject the mixture can include an inner pipe to reduce a cross-sectional flow space. The mixing may be performed at the surface in a blending apparatus or in a subsurface region by commingling of the outlets of two or more pipes.
[0020] Another embodiment provides a system for injecting a particulate mixture. The system includes a source of coarse particles, a source of fine particles, and a mixing subsystem which mixes coarse particles with fine particles to form a particulate mixture. The system includes an apparatus that can be used to alter a water content of a particulate flow; and a measurement system measuring a property of a particulate flow. A control system can adjust the mixing subsystem and/or a water content of at least one particular flow based, at least in part, on the measured property. An injection pipe injects the particulate mixture into a target location. The particulate flow can include the coarse particles, the fine particles, the particulate mixture, or any combinations thereof.
[0021] The measured property can include particle sizes, permeability, rheology, or flow rate of a particulate flow, or any combinations thereof. The apparatus to alter a fluid content can include a water source. The apparatus to alter a fluid content can include a water removal system. The measured property can include a ratio of mixing between a plurality of particle sources.
[0022] The control system can adjust the rheology of a particulate flow through addition of chemical additives.
[0023] Another embodiment provides a method for harvesting hydrocarbons from a reservoir. The method comprises drilling at least one injection well to a reservoir, drilling at least one production well to the reservoir, and producing a material from the production well, wherein the material comprises a mixture of particulate solids and hydrocarbons. At least a portion of the hydrocarbons may be removed from the material, and particulate streams are formed from the material. A mixture comprising at least two of the plurality of particulate streams is formed, wherein the ratio between each of the plurality of particulate streams is controlled to control a permeability of the mixture. A water content of the mixture is controlled to adjust a rheological property of the mixture. The mixture is injected through the injection well into the reservoir at substantially the same rate as production of the material from the reservoir.
[0024] A hydrocarbon removed from the material may be processed. The reservoir may include a hydrocarbon and a sand. For example, the reservoir may include bitumen. The re-injected mixture may include residual hydrocarbons.
DESCRIPTION OF THE DRAWINGS
[0025] The advantages of the present techniques are better understood by referring to the following detailed description and the attached drawings, in which:
[0026] FIG. 1 is a diagram showing a slurrified backfilling process, illustrating three distinct streams that can be used;
[0027] FIG. 2 is a diagram showing the use of a slurrified heavy oil reservoir extraction process to harvest hydrocarbons from a reservoir, such as an oil-sands deposit;
[0028] FIG. 3 is a diagram showing a pattern of injection wells and production wells over a hydrocarbon field;
[0029] FIG. 4 is a graph of different rheological behaviors for various materials;
[0030] FIG. 5 is a graph comparing different particle size distributions, including total tailings, classified tailings resulting from hydrocyclone fines separation from total tailings, and sieved, i.e., nearly monosized Sand 2 ;
[0031] FIG. 6 is a graph that displays the rheological behavior of slurries that may be formed from the solid distributions shown in FIG. 5 ;
[0032] FIG. 7 is a graph comparing the calculated friction loss for a number of systems versus a measured friction loss;
[0033] FIG. 8 is a graph comparing measured pressure gradients to predicted pressure gradients over a range of slurry velocities for two mixtures of tailings;
[0034] FIG. 9 is a set of two graphs that depict a range of equilibrium flow rates and slurry velocities that can be achieved if Sand 2 were injected through pipes of various diameters;
[0035] FIG. 10 is a set of two graphs that depict a range of friction/static ratios and slurry velocities that can be achieved if total paste tailings are injected at various volume concentrations in the range 47-48%;
[0036] FIG. 11 is a series of graphs displaying the contribution of the coarse stream ({dot over (Q)} 1 ), fines stream ({dot over (Q)} 2 ), and the water stream ({dot over (Q)} f3 ) to a total flow rate ({dot over (Q)} 4 ) at a fixed fines volume concentration, c 2 , of about 14%, for a number of backfill concentrations;
[0037] FIG. 12 is a block diagram of a slurrified backfill process;
[0038] FIG. 13 is a block diagram of a method for controlling a backfill injection process, as described herein; and
[0039] FIG. 14 is a block diagram of a control system that may be used to control a backfill process.
DETAILED DESCRIPTION
[0040] In the following detailed description section, specific embodiments of the present techniques are described. However, to the extent that the following description is specific to a particular embodiment or a particular use of the present techniques, this is intended to be for exemplary purposes only and simply provides a description of the exemplary embodiments. Accordingly, the techniques are not limited to the specific embodiments described below, but rather, include all alternatives, modifications, and equivalents falling within the true spirit and scope of the appended claims.
[0041] At the outset, for ease of reference, certain terms used in this application and their meanings as used in this context are set forth. To the extent a term used herein is not defined below, it should be given the broadest definition persons in the pertinent art have given that term as reflected in at least one printed publication or issued patent. Further, the present techniques are not limited by the usage of the terms shown below, as all equivalents, synonyms, new developments, and terms or techniques that serve the same or a similar purpose are considered to be within the scope of the present claims.
[0042] “Bitumen” is a naturally occurring heavy oil material. Generally, it is the hydrocarbon component found in oil sands. Bitumen can vary in composition depending upon the degree of loss of more volatile components. It can vary from a very viscous, tar-like, semi-solid material to solid forms. The hydrocarbon types found in bitumen can include aliphatics, aromatics, resins, and asphaltenes. A typical bitumen might be composed of:
[0043] 19 wt. % aliphatics (which can range from 5 wt. %-30 wt. %, or higher);
[0044] 19 wt. % asphaltenes (which can range from 5 wt. %-30 wt. %, or higher);
[0045] 30 wt. % aromatics (which can range from 15 wt. %-50 wt. %, or higher);
[0046] 32 wt. % resins (which can range from 15 wt. %-50 wt. %, or higher); and
[0047] some amount of sulfur (which can range in excess of 7 wt. %).
[0000] In addition, bitumen can contain some water and nitrogen compounds ranging from less than 0.4 wt. % to in excess of 0.7 wt. %. The metals content, while small, must be removed to avoid contamination of the product synthetic crude oil (SCO). Nickel can vary from less than 75 ppm (part per million) to more than 200 ppm. Vanadium can range from less than 200 ppm to more than 500 ppm. The percentage of the hydrocarbon types found in bitumen can vary.
[0048] “Clark hot water extraction process” (“CHWE”) was originally developed for releasing bitumen from oil sands, based on the work of Dr. K. A. Clark, and discussed in a paper by Corti et al., “Athabasca Mineable Oil Sands: The RTR/Gulf Extraction Process Theoretical Model of Bitumen Detachment,” The 4th UNITAR/UNDP International Conference on Heavy Crude and Tar Sands Proceedings, vol. 5, Edmonton, AB, Aug. 7-12, 1988, pp. 41-44, 71. The process, which is also described in U.S. Pat. No. 4,946,597, uses vigorous mechanical agitation of the oil sands with water and caustic alkali to disrupt the granules and form a slurry, after which the slurry is passed to a separation tank for the flotation of the bitumen, or other hydrocarbons, from which the bitumen is skimmed. The process may be operated at ambient temperatures, with a conditioning agent being added to the slurry. Earlier methods used temperatures of 85° C., and above, together with vigorous mechanical agitation and are highly energy inefficient. Chemical adjuvants, particularly alkalis, have to be utilized to assist these processes.
[0049] The “front end” of the CHWE, leading up to the production of cleaned, solvent-diluted bitumen froth, will now be generally described. The as-mined oil sand is firstly mixed with hot water and caustic in a rotating tumbler to produce a slurry. The slurry is screened, to remove oversize rocks and the like. The screened slurry is diluted with additional hot water and the product is then temporarily retained in a thickener vessel, referred to as a primary separation vessel (“PSV”). In the PSV, bitumen globules contact and coat air bubbles which have been entrained in the slurry in the tumbler. The buoyant bitumen-coated bubbles rise through the slurry and form a bitumen froth. The sand in the slurry settles and is discharged from the base of the PSV, together with some water and a small amount of bitumen. This stream is referred to as “PSV underflow.” “Middlings,” including water containing non-buoyant bitumen and fines, collect in the mid-section of the PSV.
[0050] The froth overflows the lip of the vessel and is recovered in a launder. This froth stream is referred to as “primary” froth. It typically comprises 65 wt. % bitumen, 28 wt. % water, and 7 wt. % particulate solids.
[0051] The PSV underflow is introduced into a deep cone vessel, referred to as the tailings oil recovery vessel (“TORV”). Here the PSV underflow is contacted and mixed with a stream of aerated middlings from the PSV. Again, bitumen and air bubbles contact and unite to form buoyant globules that rise and form a froth. This “secondary” froth overflows the lip of the TORV and is recovered. The secondary froth typically comprises 45 wt. % bitumen, 45 wt. % water, and 10 wt. % solids. The underflows from the TORV, the flotation cells and the dilution centrifuging circuit are typically discharged as tailings into a pond system. In embodiments of the present techniques, the tailings are reinjected back into the formation as backfill. The reinjection both prevents subsidence as material is removed from the reservoir and also lowers environmental issues from the waste tailings. Water removed from the tailings during the reinjection process may be recycled for use as plant process water.
[0052] As used herein, a “compressor” includes any type of equipment designed to increase the pressure of a material, and includes any one type or combination of similar or different types of compression equipment. A compressor may also include auxiliary equipment associated with the compressor, such as motors, and drive systems, among others. The compressor may utilize one or more compression stages, for example, in series. Illustrative compressors may include, but are not limited to, positive displacement types, such as reciprocating and rotary compressors for example, and dynamic types, such as centrifugal and axial flow compressors, for example.
[0053] “Facility” as used in this description is a tangible piece of physical equipment through which hydrocarbon fluids are either produced from a reservoir or injected into a reservoir, or equipment which can be used to control production or completion operations. In its broadest sense, the term facility is applied to any equipment that may be present along the flow path between a reservoir and its delivery outlets. Facilities may comprise production wells, injection wells, well tubulars, wellhead equipment, gathering lines, manifolds, pumps, compressors, separators, surface flow lines, sand processing plants, and delivery outlets. In some instances, the term “surface facility” is used to distinguish those facilities other than wells. A “facility network” is the complete collection of facilities that are present in the model, which would include all wells and the surface facilities between the wellheads and the delivery outlets.
[0054] A “hydrocarbon” is an organic compound that primarily includes the elements hydrogen and carbon, although nitrogen, sulfur, oxygen, metals, or any number of other elements may be present in small amounts. As used herein, hydrocarbons generally refer to components found in bitumen, or other oil sands.
[0055] “Permeability” is the capacity of a rock or other material to transmit fluids through the interconnected pore spaces of the rock or material; the customary unit of measurement is the millidarcy. The term “relatively permeable” is defined, with respect to formations or portions thereof, as an average permeability of 10 millidarcy or more (for example, 10 or 100 millidarcy). The term “relatively low permeability” is defined, with respect to formations or portions thereof, as an average permeability of less than about 10 millidarcy. While permeability is typically considered in the context of a solid object, such as rock, it may also be relevant in the context of non-solid materials. For example, in the context of the present technology, the slurries injected into the formation are adapted to have selected permeabilities relative to the formation fluids. In some implementations, the slurries may be adapted to have low permeabilities relative to the formation fluids to push the formation fluids in front of the injected slurries rather than allowing the formation fluids to pass into or through the injected slurries.
[0056] “Pressure” is the force exerted per unit area by the gas on the walls of the volume. Pressure can be shown as pounds per square inch (psi). “Atmospheric pressure” refers to the local pressure of the air. “Absolute pressure” (psia) refers to the sum of the atmospheric pressure (14.7 psia at standard conditions) plus the gage pressure (psig). “Gauge pressure” (psig) refers to the pressure measured by a gauge, which indicates only the pressure exceeding the local atmospheric pressure (i.e., a gauge pressure of 0 psig corresponds to an absolute pressure of 14.7 psia). The term “vapor pressure” has the usual thermodynamic meaning. For a pure component in an enclosed system at a given pressure, the component vapor pressure is essentially equal to the total pressure in the system.
[0057] As used herein, “pressure gradient” represents the increase in back pressure seen when a flow rate of a fluid or slurry is increased. FIGS. 7 and 8 illustrate the application of pressure gradient versus superficial velocity for slurries. Pressure gradient may be measured by the methods described by Chilton, R. A. and Stainsby, R. “Pressure loss equations for laminar and turbulent non-Newtonian pipe flow,” Journal of Hydraulic Engineering, 124 (5), 522-529 (1998).
[0058] As used herein, a “reservoir” is a subsurface rock formation from which a production fluid can be harvested. The rock formation may include granite, silica, carbonates, clays, and organic matter, such as oil, gas, or coal, among others. Reservoirs can vary in thickness from less than one foot (0.3048 m) to hundreds of feet (hundreds of m). The permeability of the reservoir provides the potential for production. As used herein a reservoir may also include a hot dry rock layer used for geothermal energy production. A reservoir may often be located at a depth of 50 meters or more below the surface of the earth or the seafloor.
[0059] A “rheological property” can include numerous stress-strain relationships, such as viscosity, deformation rates, flow rates, creep rates, elasticity, plasticity, and any other properties of a material under an applied strain. Such properties are discussed, for example, with respect to FIG. 4 , below.
[0060] “Substantial” when used in reference to a quantity or amount of a material, or a specific characteristic thereof, refers to an amount that is sufficient to provide an effect that the material or characteristic was intended to provide. The exact degree of deviation allowable may in some cases depend on the specific context.
[0061] A “wellbore” is a hole in the subsurface made by drilling or inserting a conduit into the subsurface. A wellbore may have a substantially circular cross section or any other cross-sectional shape, such as an oval, a square, a rectangle, a triangle, or other regular or irregular shapes. As used herein, the term “well”, when referring to an opening in the formation, may be used interchangeably with the term “wellbore.” Further, multiple pipes may be inserted into a single wellbore, for example, to limit frictional forces in any one pipe.
Overview
[0062] Embodiments of the present invention provide a method and a system for continuous backfilling of tailings, such as sand after oil has been removed, into a subterranean reservoir with control of the solid size distribution. For effective injection of tailings, two conditions can be met. First, the permeability of the backfill solids can be controlled within a predetermined range of about 0.01 to about 10 times of the initial permeability of the injected fluid through the porous material of the subsurface formation into which the mixture is injected. Second, the slurry rheology can be controlled to manage pipe pressure losses. Control of the tailings within these ranges is discussed in greater detail, below. When both criteria are met, the backfill may be placed correctly, water consumption can be optimal, and subsidence may be prevented. As tailing streams in real injection processes may vary over time, in embodiments a model can be used to predict the backfill operation in accord with the conditions above. Embodiments also include a control system running a mathematical algorithm and associated sensor, pipe, and pump systems, which may be used as inputs and outputs for the algorithm.
[0063] The control of the permeability of the backfill slurry is determined by the number of particles within certain size range per unit of slurry volume. Slurry rheology is affected by the particle size distribution of the slurry as well as by total solids concentration. Examples of permeability and rheology control are discussed in greater detail below.
[0064] FIG. 1 is a diagram showing an embodiment of a slurry stream mixing process 100 in accordance with embodiments. A coarse particle stream 102 can be characterized by total (fluid and solid) volume flow rate, {dot over (Q)} 1 , the solids volume concentration, c 1 , solids permeability, k 1 , and characteristic solids diameter in meters, d 1 . The characteristic solids diameter can be related to a measured permeability to water, k 1 , and volume concentration, c 1 , by the Blake-Kozeny equation, shown as Eqn. 1.
[0000]
d
1
=
[
k
1
150
c
1
2
(
1
-
c
1
)
3
]
1
/
2
Eqn
.
1
[0000] In such content, the diameter d 1 can be called a permeability diameter. As an example, the known permeability and concentration of clean Athabasca sand provides a value for d 1 in the range of about 70 μm to about 80 μm. A fines particle stream 104 can be characterized by a corresponding set of variables, {dot over (Q)} 2 , c 2 , k 2 , and d 2 . The typical permeability diameter of fines, d 2 , is about 10 μm.
[0065] The resulting or mixed particulate slurry 106 can be formed by combining the coarse particle stream 102 , the fines particle stream 104 , and a fluid only stream 108 , which can be characterized by a fluid flow rate {dot over (Q)} f3 . The fluid flow rate {dot over (Q)} f3 can be positive when a fluid, such as water, is added to tailing streams, termed, “watering.” It may also be negative when a fluid, such as water, is removed from the tailings streams, termed “dewatering.” Either addition or removal of fluid ({dot over (Q)} f3 ) to either or both tailing streams may be performed before they are mixed together or after they are mixed together.
[0066] Various embodiments described herein use the fundamental fluid and solids mass conservation laws of the steady state flow. The mass conservation laws for the solid and fluid phases, respectively, are shown in Eqn. 2.
[0000]
{dot over (Q)}
1
c
1
+{dot over (Q)}
2
c
2
={dot over (Q)}
4
c
4
[0000] {dot over (Q)} 1 (1 −c 1 )+ {dot over (Q)} (1 −c 2 )= {dot over (Q)} 4 (1 −c 4 )− {dot over (Q)} f3 Eqn. 2
[0000] The conservation laws shown in Eqn. 2 can be extended to a general case of N tail streams mixing together. In the general case, the solid and fluid mass conservation equations from Eqn. 2 are as shown in Eqn. 2A.
[0000]
∑
i
=
1
N
Q
.
i
c
i
=
Q
.
c
∑
i
=
1
N
Q
.
i
(
1
-
c
i
)
=
Q
.
(
1
-
c
)
-
Q
.
f
Eqn
.
2
A
[0000] In Eqn. 2A, {dot over (Q)} represents a mixed slurry stream flow rate, corresponding to the stream {dot over (Q)} 4 in Eqn. 2 and displayed in FIG. 1 as the mixed particulate slurry 106 . The volume concentration of the solids in Eqn. 2A is represented by c, which corresponds to c 4 in Eqn. 2. The watering/dewatering rate in Eqn. 2A is represented by {dot over (Q)} f , which corresponds to {dot over (Q)} f3 in Eqn. 2.
[0067] In general, the system in Eqn. 2A can be considered as incomplete as only two independent equations for N+1 unknown flow rates ({dot over (Q)} l=1,N , {dot over (Q)} f ) are present. Therefore, the two equations in Eqn. 2A can be complemented by information about the desired solid size composition of the mixed slurry, which is characterized by N−1 known solid volume fractions
[0000]
{
f
i
,
i
=
1
,
N
-
1
_
,
f
N
≡
1
-
∑
i
=
1
N
-
1
f
i
}
[0000] of the i-th tail stream in the mixed stream, as shown in Eqn. 3.
[0000]
f
i
=
Q
.
i
c
i
∑
i
=
1
N
Q
.
i
c
i
,
i
=
1
,
N
-
1
_
Eqn
.
3
[0068] The solution of the linear system represented by Eqns. 2A and 3 is shown in Eqn. 4.
[0000]
Q
.
i
=
Q
.
cf
i
c
i
Q
.
f
=
Q
.
[
1
-
c
∑
i
=
1
N
f
i
c
i
]
Eqn
.
4
[0000] The formulas shown in Eqn. 4 provide flow rates for tailings streams plus fluid flow rate. These stream rates are computed given the volume concentrations of the streams and desired mixed slurry rate {dot over (Q)} and its volume concentration, c.
[0069] Simplifying the general solution shown in Eqn. 4 to the case of coarse and fines tail streams leads to the formulas shown in Eqn. 4A.
[0000]
Q
.
1
=
Q
.
4
c
4
(
1
-
f
4
)
c
1
Q
.
2
=
Q
4
c
4
f
4
c
2
Q
.
f
3
=
Q
.
4
[
1
-
c
4
(
(
1
-
f
4
)
c
1
+
f
4
c
2
)
]
Eqn
.
4
A
[0070] In Eqn. 4A,
[0000]
f
4
=
Q
.
2
c
2
Q
.
1
c
1
+
Q
.
2
c
2
,
[0000] which is the known fines content related to the mixed stream permeability. In an embodiment, Eqns. 4 and 4A may be used to provide a basis of the solid size distribution control dictated by the known solid volume fraction from each slurry stream. Solid size distribution of the mixed particulate slurry 106 affects the permeability of the mixed particulate slurry 106 and its rheology. Thus, permeability of the mixed particulate slurry 106 can be controlled by mixing of slurries containing two or more differently sized solid particle distributions, such as the coarse particle stream 102 and the fines particle stream 104 . In contrast, in past studies, permeability has generally been controlled by modifying size distribution of a solid-liquid stream containing a single particle size distribution, for example, by the addition of bonding agents, polymers, and the like. Control of the slurry rheology is accomplished subsequent to the control of the permeability by controlling the solids concentration through adding or removing water.
Slurrified Reinjection of Tailings
[0071] Some embodiments of current invention include various mining or civil engineering operations which rely on backfilling (or reinjection or replacement) of part or the whole of material produced from the subsurface formation. In particular, in situ heavy oil mining operations, such as a slurrified heavy oil reservoir extraction method shown in FIG. 2 , may benefit from the current invention.
[0072] FIG. 2 is a diagram 200 showing the use of a slurrified heavy oil reservoir extraction process to harvest hydrocarbons from a reservoir, such as an oil sands deposit. The techniques described herein are not limited to the slurrified reservoir process but may be used with any number of other processes. For example, techniques described herein may be used to fill a separation column, fill in a subsurface cavity, or perform any number of other filling operations. In the diagram 200 , a reservoir 202 is accessed by an injection well 204 and a production well 206 . The reservoir is a subsurface formation that may be at a depth greater than about 50 meters. Water and tailings are injected through the injection well 204 , for example, from a pumping station 208 at the surface 210 . At the same time, hydrocarbon containing materials 212 , such as oil sands, are harvested from the reservoir 202 , for example, through another pumping station 214 . The hydrocarbon containing materials 212 may be processed in a facility 216 to remove at least a portion of the hydrocarbons 218 . The hydrocarbons 218 can be sent to other facilities for refining or further processing. The cleaned tailings 220 , such as sand, or other particulates, may then be backfilled, i.e., reinjected into the reservoir 202 , for example, to prevent subsidence of the surface 210 . The injection and production wells are illustrated as single lines to the reservoir 202 , but may include multiple wells.
[0073] FIG. 3 is a diagram showing a pattern 300 of injection wells 302 and production wells 304 over a hydrocarbon field 306 . Generally, the number of injections wells 302 and production wells 304 may be matched to assist with maintaining a mass balance of material entering and exiting the reservoir. As shown in FIG. 3 , the pattern may be regularly spaced across a field. In other embodiments, the wells 302 and 304 may be irregularly spaced, for example, placed to improve interaction with the reservoir geometry. Any number of other patterns may be used in embodiments.
[0074] Particle size distribution of the backfill solids (tailings) is a useful parameter as it determines a fluid-solid interaction. Therefore, control of the size distribution of the backfill solids is a desired capability. Solids concentration and size distribution are also parameters that influence frictional pressure loss. Therefore, continuous backfill considered along with pipe erosion influences the choice of the backfill piping size and design. Embodiments of the present techniques provide a methodology for backfill design that accounts for all three considerations, i.e., particulate size control, frictional pressure loss, and pipe erosion. Further, the rheology, or flow properties, of the tailings are affected by the particle size distribution and controlled by regulation of the water content.
[0075] FIG. 4 is a graph 400 of different rheological behaviors for various solid-fluid mixtures. In the graph 400 , the x-axis 402 represents an applied shear rate, while the y-axis 404 represents the shear stress resulting from the applied shear rate. In general, the rheology of tailings is frequently described by the Herschel-Bulkley model, known to those of skill in the art, which follows the formula shown in Eqn. 5.
[0000] τ=τ Y +K{dot over (y)} n Eqn 5.
[0000] In Eqn. 5, τ represents the measured shear stress, τ Y represents the yield stress, K represents a consistency factor, and n represents a power law exponent. The yield stress τ Y may be a function of various binders added to tailings for better strength. The yield stress may also be affected by tailings concentration. The consistency factor, K, and the power, n, are each a function of solids concentration and size distribution. For highly concentrated slurries and pastes, for example, with a solids concentration above the constant-contact solid concentration of about 45%, backfill behaves like a Bingham fluid 406 , as understood by one of skill in the art, i.e., n=1 and τ Y >0. For lower solid concentrations dilatant flow 408 is often observed, in which n>1. In some cases, a slurry may function as a pseudoplastic fluid 410 , in which n<1, as discussed further with respect to FIG. 7 , below. Control of the rheological properties of the backfill may be achieved by controlling the content of particles of different sizes in the paste or slurry. The control may be assisted by the addition of chemical additives that change the rheology of the mixture, including materials such as polymers, gelling agents, coagulation agents (flocculants), or pH modifiers.
[0076] The slurrified reservoir process produces at least two streams of tailings or particles, at least one coarse tailings stream and at least one fines tailing stream, as discussed with respect to FIG. 12 . Generally, the mass-averaged median diameter of the coarse particles in the coarse tailings stream is larger than the mass-averaged median diameter of the particles in the fines tailing stream. The tailings can be watered, in which the solids concentration is reduced, or dewatered, in which the solids concentration is increased. This process is used herein as an example of a system that may be controlled by the current techniques. It will be apparent that the processes described herein are not limited to the slurrified reservoir process, but may be used with any tailings backfill process in which backfill permeability control would be useful.
[0077] Referring also to FIG. 1 , if a Clark Hot Water separation process is used to extract bitumen froth from the oil sand produced by the slurrified reservoir process, a caustic soda may be added to aid bitumen liberation and flotation. As a result, solids in the fines particle stream 104 may have a double electrical layer on their surface that can prevent them from coming in direct contact with each other resulting in dispersed fines. Thus, the fines concentration in the fines particle stream 104 or the mixed particulate slurry 106 may not exceed a certain value below the direct particle contact limit. As a result, the dewatering or mixing of dispersed fines with coarse tailings is difficult to achieve. Addition of polymers or gypsum may be used to circumvent this charge effect.
[0078] Dewatering of the coarse particle stream 102 can be implemented in standard coarse solids dewatering apparatuses such as vacuum conveyors or centrifuges. These apparatuses typically operate close to the packing limit, i.e., the maximum achievable sand concentration, which, for a monodisperse grain size, may be in a range of about 0.57 to about 0.63. Some dewatering of the fines particle stream 104 can be done in a standard fines dewatering apparatuses such as a thickener vessel.
[0079] The permeability of a mixture of coarse particles and fine particles is mainly controlled by the quantity of smaller size solids, i.e., the fines. Known permeabilities of coarse and fines solids may be connected to their characteristic diameters by the formula shown in Eqn. 1. The average backfill permeability is assumed to be a result of the uniform mixture of coarse and fines particle streams. Based on this assumption, one exemplary model for backfill permeability may be approximated based on a volume weighted mixing rule as shown in Eqn. 6.
[0000]
k
4
=
(
1
-
c
4
)
3
150
c
4
2
(
(
1
-
f
4
)
d
1
2
+
f
4
d
2
2
)
-
1
Eqn
.
6
[0000] As a condition on Eqn. 6, the fines content may be restricted so that the ratio of in-situ permeability k 5 to backfill permeability would not exceed a predetermined limit, as shown in Eqn. 7.
[0000] k 5 ε≦k 4 Eqn. 7
[0000] Therefore, to satisfy the permeability restriction given in Eqn. 7, the fines fraction satisfies the restriction shown in Eqn. 8.
[0000]
f
4
≤
f
ma
x
,
f
ma
x
=
[
(
1
-
c
4
)
3
ɛ
k
5
c
4
2
150
-
1
d
1
2
]
(
1
d
2
2
-
1
d
1
2
)
-
1
Eqn
.
8
[0000] Practically, as one of the backfill objectives is the reinjection of a maximum amount of fines, an equality can be used in Eqn. 8. Generally, the preferred range of permeability (under the conditions in the subsurface formation) of the backfill material may be about 0.01 to about 10 times of the initial permeability of the injected fluid through the porous material of the subsurface formation into which the mixture is injected.
Application to a Design of a Slurrified Reservoir Backfill Process
[0080] The algorithm described above was used for the design of a continuous flow backfill system for the slurrified reservoir process. To ensure continuous backfill flow, a force equilibrium must be established in backfill well. In particular, the weight of the backfill in the well must be balanced by the friction of the backfill slurry against the wall and by the downhole pressure, e.g., the back pressure on the slurry.
[0081] Depending on a particular production scenario a void may develop at the backfill well downhole. In such cases, continuous flow requires the backfill flow rate to be high enough to equalize gravity force with wall friction. Friction is a strong function of solids concentration so the required backfill flow rate {dot over (Q)} 4 is connected to solid concentration, c 4 . With the rheology of the dense slurries specified using the Herschel-Bulkley model, as shown in Eqn. 5, above, a pressure gradient, ∇p, which is caused by the friction of a fully developed slurry flow with a superficial velocity, U, moving downwards in a pipe of diameter, D, may be calculated by well know methods.
[0082] FIG. 5 is a graph 500 comparing different particle size distributions, including total tailings 502 , classified tailings 504 resulting from hydrocyclone fines separation from total tailings, and nearly monosized Sand 2 506 . As used herein, tailings are a particular type of particles, generally obtained from a mining or other subsurface process. Any discussion of properties or mixtures of particles applies to tailings and vice-versa. In the graph 500 , the x-axis 508 is a logarithmic scale of particle sizes in μm and the y-axis 510 is the percentage of the material passing through a screen at the particle size shown on the x-axis 508 . As discussed below, the rheological properties of slurries made from these materials may be used to model backfill properties, such as the slurrified backfilling process described herein.
[0083] FIG. 6 is a graph 600 that displays the rheological behavior of slurries that may be formed from the solid distributions shown in FIG. 5 . In the graph 600 , the x-axis 602 represents the strain rate in 1/s and the y-axis 604 represents the measured stress in Pascals. As shown in the graph 600 , both size distribution and concentration have a significant effect on rheological behavior. In particular, slurries 606 and 608 , which each have particle concentrations at or above the constant particle contact level (˜47%), act as Bingham fluids 306 ( FIG. 3 ), e.g., having much higher friction. Less concentrated slurries 610 show shear thickening behavior, acting as dilatant fluids 308 . The slurries 606 and 608 can be compared to a plot of monosized sand 612 having a concentration of 30-43% and an average size of 200 nm. Further, slurries with larger fines content show more resistance at higher strain rates.
[0084] FIGS. 7 and 8 illustrate the application of pressure gradient versus superficial velocity for slurries. FIG. 7 is a graph 700 comparing the calculated friction loss for a number of systems versus a measured friction loss. In the graph 700 , the x-axis 702 represents a logarithmic scale of a mixture velocity in meters per second and the y-axis 704 represents a logarithmic scale of a head loss in %. The friction head loss is a measure of how much pumping power is lost overcoming friction to move a slurry. In a first experiment, a predicted head loss 706 for a sewage sludge having n=0.613, and pipe diameter D=0.157 m was compared to experimental measurements 708 for the same system. Similarly, in a second experiment, a predicted head loss 710 for a kaolin slurry having n=0.843, and pipe diameter D=0.14 m was compared to experimental data 712 for the same system. Finally, a predicted head loss 714 for a kaolin slurry having n=0.613, and pipe diameter D=0.079 m was compared to experimental data 716 for the same system. All three experiments were pseudoplastic fluids 310 ( FIG. 3 ), i.e., n<1. In all three cases the agreement between the predicted head loss 706 , 710 , and 714 and the experimentally measured head loss 708 , 712 , and 716 was reasonable.
[0085] FIG. 8 is a graph 800 comparing measured pressure gradients to predicted pressure gradients over a range of slurry velocities for two mixtures of tailings. In the graph 800 , the x-axis 802 represents the slurry velocity in meters per second, while the y-axis 804 represents the pressure gradient, i.e., the back pressure caused by trying to pump a slurry at the rate shown on the x-axis 802 , in kPa/m. As shown in the graph 800 , a first experiment 806 was performed on a mixture of classified, or size sorted, tailings, resulting in a predicted curve 808 that can be compared to experimental data 810 . Further, a second experiment 812 was performed on a paste of total tailings, resulting in a predicted curve 814 that can be compared to experimental data 816 . As for the experiments discussed with respect to FIG. 7 , reasonable agreement, e.g., within about 20%, was seen between experiment and predicted values.
Exemplary Tailings Reinjection System
[0086] Two backfill materials were chosen to test a design of a continuous flow reinjection system for a slurrified reservoir process. The first test material chosen was Sand 2 , having a very narrow particle size distribution, d 50 %˜200 μm and no fines. The second test material chosen for the design test was a dense tailings mixture. The tailings were “classified” (i.e., a combination of coarse and fine tails) and the total tailings were at a concentration of c=47%.
[0087] Force equilibrium ensuring continuous backfill in the absence of the back pressure uses a slurry flow rate that matches a friction pressure gradient to a slurry static head, consistent with the formula in Eqn. 9.
[0000]
∇
p
=
2
ξ
ρ
U
2
D
=
2
ξ
ρ
D
(
Q
.
4
0.25
π
D
2
)
2
=
g
(
c
ρ
s
+
(
1
-
c
)
ρ
f
)
Eqn
.
9
[0000] It will be recognized that the friction coefficient ξ is a function of slurry concentration. Thus, the total backfill flow rate {dot over (Q)} 4 is related to the minimum backfill concentration c 4 through Eqn. 9. The backfill is achieved by a solids flow rate {dot over (Q)} 4 c 4 . The process is not limited to any single rate, as an infinite number of combinations of backfill flow rates and concentrations may be selected.
[0088] FIG. 9 is a set of two graphs that depict a range of equilibrium flow rates and slurry velocities that can be achieved if Sand 2 were injected through pipes of various diameters. In each of the graphs, the x-axis 902 represents the sand concentration, c 4 . In FIG. 9(A) , the y-axis 904 represents equilibrium slurry flow rate {dot over (Q)} 4 when there is no significant backpressure. FIG. 9(B) is based on the same basic systems shown in 9(A), except that y-axis 906 is replaced by slurry velocity. As shown in FIG. 9(A) , only a pipe of 5 cm in inner diameter (ID) allows a flow rate 908 of slurry within a nominal value for a slurrified backfilling process of 250 m 3 /day to 1100 m 3 /day. The flow range is determined by the flow rate that maintains sufficient material flow from an oil sands deposit for economical production of hydrocarbon. However, slurry velocity 910 in a 5 cm pipe will be in range 6 m/s to 8 m/s, as shown in FIG. 9(B) , which is above the recommended velocity range due to excessive pipe wear. In contrast, an ID 2.5 cm pipe ensures more or less acceptable slurry velocity 912 but with an equilibrium slurry flow rate 914 that is too low. In an embodiment, several ID 2.5 cm pipes may be used, although this may lead to unnecessary complications in design and maintenance. In other words, the rheology of Sand 2 does not allow enough friction to have an acceptable slurry flow rate at equilibrium without excessive erosion in a single pipe given no backpressure. To overcome these limitations, a mixture of particle sizes, such as in a tailings paste, may be used, as discussed with respect to FIG. 10 . In embodiments, an inner pipe string may be used to reduce the cross-sectional flow space through which the mixture flows and, thus, increase flow velocity and friction.
[0089] FIG. 10 is a set of two graphs that depict a range of friction/static ratios and slurry velocities that can be achieved if total tailings are injected at various concentrations in a concentration range 47-48%. For both graphs, the x-axis 1002 represents the pipe diameter in meters. The y-axis 1004 in FIG. 10(A) represents a logarithmic scale of a friction to gravity ratio. The y-axis 1006 in FIG. 10(B) represents a logarithmic scale of a slurry velocity. As shown, an ID 4.5 cm pipe 1008 provides a continuous flow regime without erosion for a 500 m 3 /day backfill flow rate while a pipe 1010 with an ID range of 5.5 cm to 6.5 cm is acceptable for the backfill flow rate range 1000 m 3 /day to 1500 m 3 /day.
[0090] The backfill water permeability for the slurrified backfilling process should be related to effective cold water permeability k 5 of an in-situ oil sand that is in the range of about 0.001 darcy to about 0.5 darcy. As an example, assume a coarse tailings stream has a permeability of cleaned Athabasca sand k 1 in the range of about 5 darcy to adopt 20 darcy and a related Blake-Kozeny diameter of about 80 μm, from Eqn. 2. For purposes of this example, another assumption that may be made is that the backfill permeability lies between that of the coarse stream, such as about 5 darcy, and that of in-situ oil sand, at about 0.2 darcy. This assumption stems from the consideration that, on one hand, too high backfill permeability, for example, greater than about 5 darcy, would have resulted in solids settling too quickly underground. The acceptable backfill permeability may be in the high hundreds to low thousands of millidarcies. In one embodiment k 4 may be about 1 darcy. Assuming a tailings Blake-Kozeny diameter of about 10 μm, the corresponding fines permeability would be k 2 =0.078 darcy. From Eqn. 8, a backfill permeability of this value indicates that an acceptable permeability ratio would be ε=k 4 /k 5 =1 darcy/0.2 darcy=5. Thus, the corresponding value for the fines fraction f 4 is about 0.06350.
[0091] FIG. 11 is a series of graphs displaying the contribution of the coarse particle stream ({dot over (Q)} 1 ), fines particle stream ({dot over (Q)} 2 ), and the water stream ({dot over (Q)} f3 ) to a total flow rate ({dot over (Q)} 4 ) at a fixed fines concentration, c 2 , of about 14%, for a number of backfill concentrations. In all three graphs, the x-axis 1102 represents the injector concentration of the particular stream. The y-axis 1104 for FIG. 11(A) represents the ratio of the coarse stream to the total flow. The y-axis 1106 for FIG. 11(B) represents the ratio of the fines stream to the total flow. The y-axis 1108 for FIG. 11(C) represents the ratio of the water stream to the total flow.
[0092] As an example from the graphs in FIG. 11 , if the coarse stream concentration is about 46% and the backfill concentration is about 40%, then dewatering of about 8% will be required. In this example, the coarse stream contributes about 82% of the total flow, and the fines stream contributes about 26% of the total flow, keeping the backfill permeability, k 4 , at about 1 darcy.
[0093] As a further example, if the coarse stream concentration is about 52% and the backfill concentration is about 50%, then dewatering of about 10% will be required. In this example, the coarse stream contributes 90% of the total flow, and fines stream contributes about 20% of the total flow. Such a 50% backfill concentration of paste can be continuously reinjected in a pipe having an ID of 5.5 cm at a rate of about 1000 m 3 /day with relatively moderate erosion. Therefore, assuming a backfill rate of about 1000 m 3 /day, the rate of each of the streams in this scenario are about 900 m 3 /day for the coarse stream, about 200 m 3 /day for the fines stream, and about 100 m 3 /day of a water stream obtained from dewatering the streams.
Slurrified Reservoir Backfill Process
[0094] FIG. 12 is a block diagram of a slurrified reservoir backfill process 1200 . As noted previously, the present techniques are not limited to the slurrified reservoir backfill process 1200 , but may be used with any number of filling processes in which particle slurries are injected into cavities. In the slurrified reservoir process 1200 , a mixture 1202 of oil sand and water is produced from a reservoir 1204 using an artificial lift 1206 , for example, a down well pump. Measurements of the bottom hole pressure 1208 and the sand production rate 1210 , {dot over (Q)} s , provide the information used to select a sand backfilling rate 1212 , {dot over (Q)} 4 c 4 and an allowed permeability, based on the required pore pressure to relieve the overburden. The allowed permeability determines the desired size distribution range of the backfill. Further, the allowed permeability allows choosing other parameters 1214 , such as a backfill concentration, c 4 , and flow rate {dot over (Q)} 4 , for example, based on the continuity requirement of the backfill and a given diameter 1216 for a reinjection well 1218 , as discussed with respect to FIGS. 9 and 10 . A slurrified reservoir process surface facility 1220 separates the hydrocarbon 1222 from the mixture 1202 obtained from a production well 1224 . The slurrified reservoir process surface facility 1220 produces two solids streams, a coarse tailings stream 1226 and a fines tailings stream 1228 .
[0095] The adjustment of the concentrations of the coarse tailings stream 1226 and the fine tailings stream 1228 can be accomplished by watering or dewatering in variety of ways. One scheme, shown in FIG. 12 , accomplishes dewatering using different techniques for each of the streams 1226 and 1228 . In this scheme, a standard solids separator such as a vacuum filter or centrifuge 1230 is used to remove water from the coarse stream 1226 . A settling tank 1232 is used to remove water from the fines stream 1228 . The settling tank 1232 may also serve as a storage vessel if needed. The coarse stream 1226 is fed through a coarse slurry pump 1234 which may be used to control the flow rate for mixing. Similarly, the fines stream 1228 is fed through a fines slurry pump 1236 , which controls the flow rate for mixing.
[0096] The mixing of the coarse stream 1226 and the fines stream 1228 is generally performed at the surface 1238 , for example, by commingling the streams. Static mixers may be included in the line after the streams 1226 and 1228 are commingled, to provide better mixing control. However, mixing is not limited to the surface, and in some embodiments the streams 1226 and 1228 may be reinjected independently and mixed underground. Dewatering may also be applied at the surface to the streams 1226 and 1228 separately before mixing or an already mixed stream 1240 can be dewatered above or below the surface.
[0097] The mixed stream 1240 is then injected into the reservoir 1204 through the injection well 1218 . In an embodiment, the flow rate of the mixed stream 1240 is determined from the known backfill concentration, the flow rate and concentrations of coarse and fines tailings coming from slurrified reservoir surface facilities, using the techniques described herein. The flow rates from the corresponding slurry pumps 1234 and 1236 can be used to control the mixing of the coarse stream ({dot over (Q)} 1 ) 1226 and fines stream ({dot over (Q)} 2 ) 1228 . The flow rates and the control of the pumps and filters of a watering/dewatering system ({dot over (Q)} f3 ), e.g., centrifuge 1230 or settling tank 1232 can be used to control the rheology of the mixture 1240 . The control scheme may be implemented using the method shown in FIG. 13 .
[0098] FIG. 13 is a block diagram of a method 1300 for controlling a backfill injection process, as described herein. The method 1300 begins at block 1302 with a determination of the optimum rheological behavior, for example, using the methods discussed above with respect to Eqns. 1-9. At block 1304 , the ratio of a coarse particle stream 1226 ( FIG. 12 ), a fines particle stream 1228 , and water needed to reach the rheological behavior is adjusted, for example, by changing the rates of the slurry pumps 1234 and 1236 ( FIG. 12 ) and/or by adjusting the watering/dewatering systems 1230 and 1232 . At block 1306 , the flow rate of the slurry mixture 1240 is set and/or adjusted. At block 1308 , the slurry mixture 1240 is injected into the reservoir 1204 . Process control then returns to block 1302 and repeats the method 1300 .
[0099] A continuous backfill with controlled backpressure may be designed for a slurrified reservoir process. In the slurrified reservoir process, there can be an operating range of flow rates, backfill density, and particle size distribution which allows for continuous backfill. The backfill may be performed using a single well having an inner diameter of about 4 cm to 7 cm and a velocity range of about 1 m/s to 4 m/s, which corresponds to a nominal slurrified reservoir backfill rate range of about 500-1500 m 3 /day with controllable permeability, slurry density, velocity and pressure. This analysis can be extended to higher backfill flow rates. For example, if production rate of one slurrified reservoir process producer well is 3000 m 3 /day of slurry with vol. 35% solids concentration, then, after bitumen extraction, the backfill rate of vol. 45% slurry is about 2000 m 3 /day
[0100] The backfill solids concentration can be kept high, for example, greater than 45%, to ensure high friction and still acceptable pipe erosion. Accordingly, paste backfilling with a high solids content tailings mixture, for example, >45%, provides a good option. The application of the techniques described herein to the slurrified reservoir process may use measurements obtained from online measurement of bottom hole pressure, production flow rate, and the concentrations of tailings streams coming out of surface facilities. The collected data may be combined with the calculated dependence of the backfill rheology versus the concentration and the allowable fines content, e.g., based on the permeability, to allow the present method to calculate tailings and fluid streams and give suitable commands to system pumps.
Exemplary Control System
[0101] FIG. 14 is a block diagram of a control system 1400 that may be used to control a backfill process. The control system 1400 may be a distributed control system, a direct digital control, a programmable logic controller, or any number of other types of systems. The control system 1400 will generally have a processor 1402 that is associated with a cache 1404 and a memory 1406 , such as combinations of random access memory (RAM) and read-only memory (ROM). The memory 1406 is a non-transitory, computer readable medium that may be used to hold programs associated with the techniques described herein, such as the method discussed with respect to FIG. 13 , or the techniques described with respect to Eqns. 1-14.
[0102] A bus 1408 may be used by the processor 1402 to communicate with other systems, such as a storage system 1410 . The storage system 1410 may include any combinations of hard drives, optical drives, RAM drives, holographic drives, flash drives, and the like. The storage system 1410 provides another non-transitory computer readable medium that may be used to hold code for controlling the plant and implementing the techniques described herein. For example, the storage system 1410 may hold a rheology module 1412 for calculating a predicted rheology and flow rate for a backfilling mixture, as described with respect to Eqns. 1-14. Further, the storage system 1410 may hold a mixture control module 1414 that controls slurry pumps and/or watering/dewatering systems to change the composition and rheology of the backfill, for example, based on the results from the rheology module 1412 . The storage system 1410 may also include a plant control system module 1416 that operates the specific plant equipment.
[0103] For example, the processor 1402 may access the plant control system module 1416 and use the module to communicate with a plant interface 1418 through the bus 1408 . The plant interface 1418 may include hardware, software, or both used to collect data from sensors 1420 , control pumps 1422 , open and close valves 1424 , and control motors 1426 on equipment such as mixers, conveyors, vacuum pumps, and the like.
[0104] The plant control system 1400 may have a human-machine interface 1428 that allows operators to interface to the control system. The human-machine interface 1428 may couple input and output devices, such as keyboards 1430 , displays 1432 , and pointing devices 1434 to the bus 1408 .
[0105] The plant control system 1400 may also include a network interface, such as a network interface card (NIC) 1436 to allow remote systems 1438 to communicate with the plant control system 1400 over a network 1440 . The network 1440 may be a local area network (LAN), a wide area network (WAN), the Internet, or any other appropriate network.
[0106] While the present techniques may be susceptible to various modifications and alternative forms, the exemplary embodiments discussed above have been shown only by way of example. However, it should again be understood that the techniques is not intended to be limited to the particular embodiments disclosed herein. Indeed, the present techniques include all alternatives, modifications, and equivalents falling within the true spirit and scope of the appended claims.
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An embodiment of the present techniques provides a method of injecting a particulate mixture into a target location. The method includes forming a mixture of at least two sources of particles with different size distributions wherein the mixture of solids has a permeability in a predefined range. A water content of the mixture is varied to control the rheology of the mixture. The particles are injected through one or more pipes into a target location.
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This is a continuation of application Ser. No. 08/004,699 filed on Jan. 14, 1993, abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to a tubular prosthesis and, more particularly, to a radially expandable tubular prosthesis which allows controlled expansion in a circumferential direction following implantation while limiting expansion in a longitudinal direction.
The typical prosthesis of the prior art is manufactured with a predetermined diameter, that is, prostheses are manufactured in various sizes so that the physician may choose the most appropriate-sized prosthesis to replace or repair the damaged lumen in the patient. As far as length is concerned, the physician merely cuts the chosen prosthesis to size, the prosthesis typically being oversized in the longitudinal direction.
The commonly-employed prosthesis mentioned above is suitable for use in many situations. However, several applications may demand that the prosthesis be expandable in the radial direction. For example, one such application involves intraluminal implant procedures in which the prosthesis is delivered to a damaged lumen via a catheter. The technique requires that the implant be stored within the catheter (e.g., it may be rolled or bunched) prior to insertion of the catheter into the patient. Upon advancement of the catheter to the site of the damage, the implant is expelled from the catheter, unrolled (or unfolded) and thereafter secured to the lumen. Because of the procedure, it is difficult, if not impossible, for the physician to correct any mismatch in sizing that may occur between the implant and the host lumen. For example, if the physician miscalculates the size of the lumen receiving the implant or should the lumen prove to be larger or smaller than anticipated by the physician, the physician may not be able to securely fix the implant to the host lumen.
Another application in which it would be desirable to employ an expandable prosthesis involves the area of pediatrics. A common disadvantage encountered in conventional pediatric prostheses is the inability of the device to accommodate growth changes in the surrounding tissue as the child ages. Consequently, it is often necessary to perform several surgical procedures on a child to implant ever increasingly circumferentially-larger prostheses. It has traditionally been necessary to entirely remove and replace the implanted prosthesis with a larger-sized prosthesis as the child grows. Such a series of surgeries is traumatic to the body and has a degree of risk inherently associated therewith.
Accordingly, it would be desirable to provide a tubular prosthesis which allows for circumferential expansion such that the prosthesis could be readily deployed via a catheter for intraluminal delivery and, further, such that the prosthesis could be circumferentially expanded in vivo as the child grows, thereby eliminating the need, or at least the frequency, for surgical replacement of the implant.
SUMMARY OF THE INVENTION
The present invention, which addresses the needs of the prior art, provides a radially expandable tubular prosthesis. Any type of textile pattern may be used in manufacturing the prosthesis provided its structure will allow for use of undrawn or partially drawn yarns which will provide circumferential expansion, the primary purpose being the ability to be drawn in vivo subsequent to implantation, e.g., via balloon catheter or the like. For example, woven, knitted, braided and filament wound fabrics may be used. Thus, in one embodiment, the prosthesis is made from a polymeric fabric having a sufficient portion of yarn which is capable of being drawn beyond the yield point of plastic deformation upon the application of force thereto sufficient to exceed the yield point to allow for radial expansion of the prosthesis.
The prosthesis of the present invention may be used in a wide variety of applications. For example, the prosthesis may be employed as a graft in the vascular system, as well as the esophageal, stomach and bowel areas. Alternatively, the prosthesis may be intraluminally implanted via a catheter or similar device to repair or support a weakened or damaged lumen, such as a blood vessel in the vascular system.
In one preferred embodiment, the prosthesis is made from a woven fabric having substantially drawn longitudinal yarns (warp yarns) which limit expansion or elongation of the prosthesis in the longitudinal direction, and radial yarns (fill yarns) which are at most partially drawn to allow for expansion of the prosthesis in the radial direction when the yield point of the radial yarns is exceeded.
The present invention also provides a method for intraluminally repairing a damaged lumen with an expandable prosthesis via a catheter. The method includes the step of introducing the catheter intraluminally to the damaged lumen. The method also includes the step of delivering the prosthesis intraluminally at the site of damage in the lumen. The method includes the further step of expanding the prosthesis circumferentially until its diameter substantially conforms to that of the damaged lumen.
Due to its unique features, delivery of prostheses to damaged vessels can be accomplished using less invasive methods than conventional implant surgery and with more ease and less uncertainty than conventional methods requiring coiling or folding of the device during delivery via a catheter. The prostheses of the present invention can be delivered intraluminally via a catheter without the need for conventional bunching, folding or rolling of the prosthesis for stowage in the catheter. Instead, the catheter is initially formed with a sufficiently small diameter that allows the prosthesis to be stowed on the catheter without rolling or bunching, delivered to the site of deployment, expanded to the proper size and deployed. Because the prosthesis is not rolled or bunched, the delivery process is more readily accomplished and, in addition, the prosthesis may be more easily maneuvered inside the lumen. (However, depending upon the degree of expandability, the graft may still need to be bunched or rolled, but to a lesser degree than a non-expandable graft.) Further, the prosthesis of the present invention may be implanted in a child, and, thereafter, expanded via a balloon catheter to enlarge the diameter of the implanted prosthesis to substantially conform with the enlarged diameter (due to growth) of the host lumen.
The present invention also provides a method for reducing the frequency of surgical replacement of a previously implanted prosthesis in a child. The method includes the step of implanting an expandable prosthesis in a child. The method includes the additional step of delivering internal force to the prosthesis following a period of growth in the child sufficient to expand the prosthesis in a circumferential direction until the diameter of the prosthesis substantially conforms to that of a connecting host lumen which has experienced a period of circumferential growth following a period of growth in the child. The method includes the further step of expanding the prosthesis in a circumferential direction until the diameter of the prosthesis substantially conforms to the diameter of a connecting host blood vessel which has experienced a period of circumferential growth.
It is apparent from the above discussion that the present invention overcomes important disadvantages of the prior art and satisfies a strong need in the medical industry.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a woven tubular prosthesis;
FIG. 2 is a schematic of a traditional weave pattern;
FIG. 3 is a graph illustrating the stress vs. length relationship for a typical synthetic yarn having been drawn through the yield point of plastic deformation (S o );
FIG. 4 is an illustration of an implanted tubular prosthesis;
FIG. 5 is an illustration similar to FIG. 4 following a period of growth in the host lumen;
FIG. 6 is a perspective view of a braided tubular prosthesis;
FIG. 6a is a schematic of a diamond braid;
FIG. 6b is a schematic of a regular braid;
FIG. 6c is a schematic of a hercules braid;
FIG. 7 is a perspective view of a knitted tubular prosthesis;
FIG. 7a is an enlarged detail of FIG. 7;
FIG. 8 is a perspective view of a filament wound tubular prosthesis; and
FIG. 8a is an enlarged detail of FIG. 8.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings and, in particular to FIGS. 1-2, a woven tubular prosthesis 10 is shown. The weave pattern includes warp yarns 12 running along the longitudinal length L of the woven product and fill yarns 14 running around the circumference C of the product.
As is well-known to those skilled in the art, the yarns used in a woven product are typically treated and processed prior to weaving. This treatment commonly includes the step of "drawing" the yarns, i.e., longitudinally stretching the yarns beyond their yield point until complete plastic deformation is accomplished.
Referring to FIG. 3, the force required to "draw" a yarn increases until the yield point is reached, at which point, the yarn enters a region of plastic deformation (i.e., a region in which the yarn now exhibits loss of its elasticity and ability to change appreciably in length). Once the deformation point in a yarn has been reached through stretching, the material has substantially lost its elastic memory and is more or less "fixed," neither being able to be further stretched or to return to its original length. Yarns which have experienced full deformation through the drawing process are typically used in prostheses because they are ideal for maintaining constant pressures without concern for undesirable stretching or bulging during use. Consequently, these prostheses are by necessity of fixed diameter.
As mentioned above, the present invention utilizes yarns, in the circumferential direction of the tubular prostheses, which have not been drawn or only partially drawn, allowing for future radial expansion through vivo drawing, i.e., stretching, beyond the yield point, at which time the tubular prosthesis remains fixed at the increased diameter. This type of stretching causes the yarn to undergo inelastic strain, commonly referred to as plastic deformation, whereby the polymer molecules become newly aligned. The yarn may also be stretched until a point at which the material fractures (the fracture point). The process of drawing the yarn (to a point prior to the fracture point), increases the tensile strength of the yarn and decreases the elongation to failure.
With respect to prior art prosthesis, both of these characteristics (namely, increased tensile strength and decreased elongation) are desirable in that the prior art devices are typically produced to precise diameters in order to approximately match the size of the damaged lumen being repaired. However, several situations exist in which it would be desirable to be able to implant a prosthesis of a relatively small diameter and, thereafter, expand the prosthesis while such prosthesis remains positioned in the patient's body.
As mentioned above, the first application of what may be referred to as an expandable prosthesis concerns intraluminal implantation. In this application, the present invention functions as an endoprosthetic device, i.e., it is employed to internally repair or support a weakened or damaged lumen, e.g., a blood vessel in the vascular system. More particularly, a tubular prosthesis may be implanted in the body by delivering such prosthesis to the damaged lumen via a catheter. Delivering the prosthesis in such a manner greatly reduces the invasiveness of the procedure. For example, assuming a blood vessel positioned in the thorax is damaged, the typical prior art technique would require opening of the chest and rib cage to allow access to the damaged vessel. In contrast, intraluminal implantation eliminates the need, in many situations, for the surgeon to perform highly invasive procedures on the patient. Instead of accessing the lumen at the point of damage, the physician accesses a lumen leading to the damaged site, e.g., the femoral artery in the groin region when an artery in the vascular system requires repair.
Presently, the prostheses being intraluminally implanted are substantially the same prostheses that are implanted invasively. It has been discovered however, that if a prosthesis is woven with undrawn or partially drawn radial yarns, the prosthesis will be capable of circumferential expansion following manufacture of the product. More particularly, if a balloon catheter (or similar device) is inserted into such a prosthesis and is thereafter expanded, the prosthesis will circumferentially expand a slight degree until the yield point is reached. At that point, the radial yarns, i.e., fill yarns, which were not drawn, will plasticly deform, thereby allowing substantial circumferential expansion. The fill yarns, once expanded, will retain their expanded circumferential length. In addition, as mentioned above, the expanded yarns will generally exhibit a greater tensile strength than before.
To secure the prosthesis to the host lumen, a stent may be incorporated into the prosthesis. In that way, both the prosthesis and the stent can be simultaneously and controllably expanded to the desired diameter or until the prosthesis substantially conforms to the diameter of the host lumen. Any suitable means of attaching the stent to the expandable prosthesis, such as hooks, catches, sutures or other similar means may be used. Additionally, the stent may include similar means capable of anchoring the prosthesis in place in the host lumen.
As also mentioned above, the expandable prostheses of the present invention can be used as pediatric implants. More particularly, implanting prostheses in children can prove quite challenging because as children grow, the lumens, e.g., blood vessels, in their bodies also grow (both longitudinally and circumferentially). FIG. 4 illustrates an implant 16 in a blood vessel 18 of a child. At the time of implantation, the vessel is matched to the site of the connecting host vessels. However, as the child grows, the host vessels grow circumferentially, while the implant remains the same size.
Referring to FIG. 5, this period of growth in the child results in the formation of a "bottleneck" effect in the blood vessel, In other words, the blood must pass from a vessel having a diameter D 1 , to a vessel having a reduced diameter D 2 and then to a vessel again having a diameter D 1 . This obstruction in the vessel creates a stenosis, which, in turn, reduces blood flow to distal vessels. Further, increased pressure at the junction of the host vessel and graft can be problematic, if not fatal. Insufficient blood supply distal to the stenosis can also cause fatigue and diminished activity levels.
To reduce the risks associated with this phenomenon, physicians routinely remove and replace vascular grafts that have been implanted in children. In turn, a larger-sized graft is implanted in the child, which after a period of growth, will itself have to be removed and replaced. Overall, it may be necessary to perform a large number of surgical procedures on a child requiring a vascular graft, particularly if the child is an infant (during which time rapid growth occurs). As may well be imagined, performing frequent surgical procedures on a child can severely weaken the child, both physically and psychologically.
The expandable prosthesis of the present invention therefore provides a means for reducing (or eliminating) the frequency at which surgical replacement of an implanted graft is necessary. More particularly, an expandable prosthesis is first surgically implanted in a child. After a period of growth in the child, a procedure is performed whereby internal force is delivered to the prosthesis sufficient to expand the prosthesis in a circumferential direction until the diameter of the prosthesis substantially conforms to that of a connecting host lumen which has experienced a period of circumferential growth. This procedure may be accomplished by, for example, a catheterization procedure whereby a balloon catheter is advanced to the site of the graft. The balloon catheter is thereafter inflated until the yield point of the radial fill yarns is exceeded and the graft begins to expand. The graft may then be circumferentially expanded until its diameter is made substantially equivalent to the diameter of the host vessel.
In both of the described applications, sufficient undrawn or partially drawn yarns must be present in the circumferential direction such that the yield strength would be well in excess of physiological pressure. Thus, the chosen yarn must be sufficiently strong in the radial direction of the graft in the undrawn state to resist harmful fluxuations in diameter or bulging in the unexpanded state. A minimum pressure ratio of about 10:1 yield strength to physiological pressure would suffice. For example, physiologic pressure for hypertensive patients is typically in the 2-4 psi range. This means that the hoop yield strength of the prosthesis should preferably be at least 40 psi to ensure no occurrence of premature expansion. Thus, to induce expansion of the prosthesis, a pressure of at least 40 psi would be required to be introduced. As mentioned above, while it is preferred that expansion be accomplished by balloon catheter, other means suitable to the application may be used.
Although the above discussion has been directed to weaves (i.e., woven products), the same result can be accomplished with braided prosthesis (see FIGS. 6 and 6a-6c), knitted grafts (see FIGS. 7 and 7a) and filament wound prosthesis (see FIGS. 8 and 8a). As further discussed in the following examples, each of these prostheses can be manufactured to allow circumferential expansion following implantation.
The yarns in the present invention may be selected from a wide variety of synthetic polymers. Among the useful classes of materials are polyesters, polypropylene, polyurethane, polyamide, and copolymers thereof. Those yarns which are chosen for the undrawn, expandable portion of the prosthesis must be capable of withstanding physiological pressures in the undrawn state. In essence, these yarns must in the undrawn state resist any appreciable expansion or distortion under conditions of pressure and stress encountered in the body until such time as expansion is necessary. Expansion pressures will vary depending for the most part on the physical characteristics of the chosen material, but will by necessity exceed the yield point to reach the plastic deformation state at which time the material will remain in the expanded state. As previously stated, for safety reasons, the yield point of the material should preferably exceed the inherent physiological pressures of the host lumen by a factor of at least about ten. Thus, the force required to expand the circumference of the prosthesis is sufficiently high to resist change and remain in the undrawn state until manually expanded via catheter or similar device.
In the manufacture of the prostheses of the present invention, both drawn yarns as well as undrawn or partially drawn yarns are employed. The undrawn or partially drawn yarns are incorporated into the chosen textile pattern in the direction which upon drawing will result in a larger diameter of the device. In the case of woven patterns, the undrawn materials make up the fill yarns. In the case of knitted construction, such as weft knits, or braided patterns such as two dimensional, multi-ply or three dimensional braids, the undrawn yarns may comprise part of or all of the fabric. The same applies to grafts made from filament winding construction.
As a result of drawing, the polymeric yarns become directionally aligned or oriented. Drawing is generally accomplished at elevated temperatures, although alternatively cold drawing at high speeds is possible. As the polymer cools and recrystallizes, the elongated molecular chains become arranged in a new order which gives a higher modulus and increased stiffness to the yarn. The result is a loss of elongation with a higher strength:strain ratio.
EXAMPLES
Example 1--Woven Construction
The following specifications are used to fabricate a woven prosthesis of the present invention.
Weave--1/1 Plain, Tubular
Warp Yarn--Textured 50 denier/48 filaments polyester fully oriented (drawn)
Fill Yarn--Flat 115 denier/100 filament partially oriented (partially drawn) polyester
Ends per inch--160
Picks per inch--120
Subsequent to weaving the prosthesis, the fabric is scoured in a basic solution of warm water (e.g., 120° F.) and detergent, followed by rinsing to remove the detergent. The prosthesis can then be attached to a stent fixation device and assembled into a catheter delivery system, or, alternatively surgically implanted. Thus the expandable prosthesis can then be delivered intraluminally or be implanted percutaneously.
The partially-oriented fill yarn chosen in this example has the ability to stretch about 1.7 times its original length. Thus, if the woven graft were manufactured to a diameter of 10 mm, dilation with a balloon catheter to about 17 mm can be achieved.
Example 2--Braided Construction
The following specifications are used to fabricate a braided prosthesis of the present invention:
Braid--Regular Twill Braid, Tubular
Yarn--2 ply/flat 115 denier/100 filament partially oriented (partially drawn) polyester
Carriers--96
Helix Angle--55°
Diameter--10 mm
Subsequent to braiding of the prosthesis (see FIGS. 6 and 6a-6c), the fabric is scoured in a basic solution of warm water (e.g., 120° F.) and detergent, followed by rinsing to remove the detergent. The prosthesis can then be attached to a stent fixation device and assembled into a catheter delivery system or, alternatively surgically implanted. Thus, the expandable prosthesis can then be intraluminally delivered or implanted percutaneously.
The partially-oriented fill yarn chosen in this example also has the ability to stretch about 1.7 times its original length. Thus, a braided prosthesis manufactured to a diameter of 10 mm would be capable of expanding to about 17 mm in diameter.
Example 3--Weft Knitted Construction
The following specifications are used to fabricate a knitted prosthesis of the present invention:
Knit--Tubular Jersey Weft Knit
Yarn--3 ply/flat 115 denier/100 filament partially oriented (partially drawn) polyester
Wales per inch--30
Courses per inch--40
After knitting (see FIGS. 7 and 7a), the fabric is scoured in a basic solution of warm water (e.g., 120° F.) and detergent. It would be rinsed to remove the cleaning agents. The prosthesis can then be attached to a stent fixation device and assembled into a catheter delivery system for insertion into the body or, alternatively directly implanted.
The partially-oriented fill yarn has the ability to stretch about 1.7 times its original length. The knitted fabric geometry provides an additional amount of stretch of about 50% to the overall dilation of the graft. Knitted prostheses manufactured to a diameter of about 10 mm are capable of being dilated with a balloon catheter to about 22 mm.
A warp knit construction can also be used. For example, instead of a tubular jersey weft knit construction, a tubular double tricot warp knit construction with similar stitch density can be used.
Example 4--Filament Wound Construction
A one ply/flat 115 denier/100 filament partially oriented polyester yarn is filament wound onto a mandrel of known diameter. The helix angle achieved is about 55°. The mandrel is wrapped with the yarn in both directions to provide biaxial reinforcement. To hold the yarns in place, they are passed through a solution of solvated polyurethane elastomer, such as Biomer® solution, sold by Johnson & Johnson. The solvent is removed, causing the polyurethane to dry and glue the yarns together.
After filament winding (see FIGS. 8 and 8a), the material is scoured in a basic solution of warm water (e.g., 120° F.) and detergent, followed by rinsing to remove the detergent. The prosthesis can then be attached to a stent fixation device and assembled into a catheter delivery system for delivery intraluminally or, directly implanted.
In all four examples, the prosthesis may be of a straight, bifurcated or otherwise designed configuration.
Thus, while there have been described what are presently believed to be the preferred embodiments of the invention, those skilled in the art will realize that various changes and modifications may be made to the invention without departing from the spirit of the invention, and it is intended to claim all such changes and modifications which fall within the scope of the invention.
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A radially expandable tubular prosthesis which allows for controlled expansion in a circumferential direction following implantation while limiting expansion in a longitudinal direction. The prosthesis is particularly suited to intraluminal implantation via a catheter and is also particularly suited for percutaneous implantation in children.
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FIELD OF THE INVENTION
The present invention relates to novel phosphate derivatives of 2-aryl-4-quinolones, and novel intermediates, 2-selenophene 4-quinolones and N,N-dialkylaminoalkyl derivatives of 2-phenyl-4-quinolones; and in particular to their uses in treating human cancers.
BACKGROUND OF THE INVENTION
Quinolone derivatives were initially discovered as the agents to act on bacterial DNA gyrase, and thus developed as anti-bacterial agents. Recently DNA topoisomerase II has emerged as the pharmacological target for this class of quinolone compounds. We have synthesized a series of substituted 2-phenyl-4-quinolone (A) which appeared to function as novel antimitotic agents. [Kuo, S. C., Lee, H. Z., Juang, J. P., Lin, Y. T., Wu, T. S., Chang, J. J., Lednicer, D., Paull, K. D., Lin, C. M., Hamel, E. Synthesis and cytotoxicity of 1,6,7,8-substituted 2-(4′-substituted phenyl)-4-quinolones and related compounds: identification as antimitotic agents interacting with tubulin. J. Med. Chem. 1993, 36, 1146-56; Li, L., Wang, H. K., Kuo, S. C., Wu, T. S., Mauger, A., Lin. C. M., Hamel, E. Lee, K. H. Antitumor agents. 155. Synthesis and biological evaluation of 3′,6,7-substituted 2-phenyl-4-quinolones as antimicrotubule agents. J. Med. Chem. 1994, 37, 3400-7] Later on we continued to synthesize many related analogs such as 2-phenylnaphthyridine-4-ones (B) [Chen, K., Kuo, S. C., Hsieh, M. C., Mauger, S A., Lin, C. M., Hamel, E., Lee, K. H. Antitumor agents. 174. 2′,3′,4′,5,6,7-Substituted 2-phenyl-1,8-naphthyridin-4-ones: their synthesis, cytotoxicity, and inhibition of tubulin polymerization. J. Med. Chem. 1997, 40, 2266-75], 2-phenyl-4-quinazolones (C) [Xia, Y., Yang, Z. Y., Hour, M. J., Kuo, S. C., Xia, P., Bastow, K. F., Nakanishi, Y., Namrpoothiri, P., Hackl, T., Hamel, E., Lee, K. H. Antitumor Agents. Part 204: Synthesis and Biological Evaluation of Substituted 2-Aryl Quinazolinones, Bioorg. Med. Chem. Lett. 2001, 11, 1193-6; Hour, M. J., Huang, L. J., Kuo, S. C., Xia, Y., Bastow, K. F., Nakanishi, Y., Hamel, E., Lee, K. H. 6-Alkylamino- and 2,3-dihydro-3′-methoxy-2-phenyl-4-quinazolinones and related compounds: their synthesis, cytotoxicity, and inhibition of tubulin polymerization. J. Med. Chem. 2000, 43, 4479-87] and tetrahydro-2-phenyl-4-quinolones (D) [Xia, Y., Yang, Z. Y., Xia, P., Bastow, K. F., Tachibana, Y., Kuo, S. C., Hamel, E., Hackl. T., Lee, K. H. Antitumor agents. 181. Synthesis and biological evaluation of 6,7,2′,3′,4′-substituted-1,2,3,4-tetrahydro-2-phenyl-4-quinolones as a new class of antimitotic antitumor agents. J. Med. Chem. 1998, 41. 1155-62], which enable us to establish structure and activity relationships (SAR). Among these analogs, we have discovered quite a few compounds possessing potent cytotoxicity, such as 3′,6-disubstituted 2-phenyl-4-quinolones (A-1) etc [Li, L., Wang, H. K., Kuo, S. C., Wu, T. S., Lednicer, D., Lin, C. M., Hamel, E., Lee, K. H. Antitumor agents. 150. 2′,3′,4′,5′,5,6,7-substituted 2-phenyl-4-quinolones and related compounds: their synthesis, cytotoxicity, and inhibition of tubulin polymerization. J. Med. Chem. 1994, 37, 1126-35]. However, most of the compounds with potent cytotoxicity were very lipophilic, and therefore, not suitable for in vivo and clinical studies. We thus made attempt to synthesize hydrophilic derivatives of these 2-aryl-4-quinolone skeletons in order to improve pharmacokinetic properties suitable for in vivo and clinical studies.
SUMMARY OF THE INVENTION
Preferred embodiments of the present invention include (but not limited thereto) the following items:
1. A phosphate derivative of 2-aryl-4-quinolone having the following formulas Ia, Ib or Ic:
wherein
R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, (CH 2 ) n NR 8 R 9 ,
wherein n is an integer of 0-4, Y is O or S, X is F, Cl, or Br, and R 8 and R 9 independently are H, (CH 2 ) n YH, (CH 2 ) n N(C n H 2n+1 )(C m H 2m+1 ) or (CH 2 ) n CH 3 , wherein n and Y are defined as above, and m is an integer of 0-4;
R 2 , R 3 , R 4 and R 5 independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, (CH 2 ) n NR 8 R 9 ,
or R 3 and R 4 together is —Y(CH 2 ) n Y—, wherein n, Y, X, R 8 and R 9 are defined as above; and
R 1 and R 1 ′ independently are H, Li + , Na + , K + , N + R 8 R 9 R 10 R 11 or benzyl wherein R 10 and R 11 independently are H, (CH 2 ) n YH, (CH 2 ) n N(C n H 2n+1 )(C m H 2m+1 ) or (CH 2 ) n CH 3 , n, m, R 8 and R 9 are defined as above.
2. The phosphate derivative according to Item 1, which has the formula Ia.
3. The phosphate derivative according to Item 2, wherein R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ are all H; or one of R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ is F, OCH 3 or (CH 2 ) n NR 8 R 9 , and the others thereof are H, wherein n, R 8 and R 9 are defined as in Item 1.
4. The phosphate derivative according to Item 2, wherein R 2 , R 3 , R 4 , and R 5 are all H; or one of R 2 , R 3 , R 4 , and R 5 is F, OCH 3 , Y(CH 2 ) n CH 3 or (CH 2 ) n NR 8 R 9 , and the others thereof are H; or R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 ) n O—, wherein n, Y, R 8 and R 9 are defined as in Item 1.
5. The phosphate derivative according to Item 2, wherein R 1 and R 1 ′ are both H or both Na + .
6. The phosphate derivative according to Item 5, wherein R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 )O—; and R 2 ′, R 3 ′, R 4 ′ and R 5 ′ are all H, and R 6 ′ is F.
7. The phosphate derivative according to Item 5, wherein R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 )O—; and R 2 ′, R 3 ′, R 4 ′ and R 5 ′ are all H, and R 5 ′ is F.
8. The phosphate derivative according to Item 5, wherein R 4 is F, and R 2 , R 3 and R 5 are H; and R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ are all H.
9. The phosphate derivative according to Item 5, wherein R 2 , R 3 , R 4 and R 5 are all H; and R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ are all H.
10. The phosphate derivative according to Item 5, wherein R 4 is OCH 3 , and R 2 , R 3 and R 5 are H; and R 5 ′ is F, and R 2 ′, R 3 ′, R 4 ′ and R 6 ′ are H.
11. The phosphate derivative according to Item 5, wherein R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 )O—; and R 2 ′, R 3 ′, R 4 ′ and R 6 ′ are all H, and R 5 ′ is OCH 3 .
12. The phosphate derivative according to Item 5, wherein R 4 is CH 2 N(C 2 H 5 ) 2 , and R 2 , R 3 and R 5 are H; and R 6 ′ is F, and R 2 ′, R 3 ′, R 4 ′ and R 5 ′ are H.
13. The phosphate derivative according to Item 5, wherein R 4 is CH 2 N(C 2 H 5 ) 2 , and R 2 , R 3 and R 5 are H; and R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ are all H.
14. The phosphate derivative according to Item 5, wherein R 4 is OCH 3 , and R 2 , R 3 and R 5 are H; and R 5 ′ is CH 2 N(C 2 H 5 ) 2 , and R 2 ′, R 3 ′, R 4 ′ and R 6 ′ are H.
15. The phosphate derivative according to Item 1, which has the formula Ib.
16. The phosphate derivative according to Item 15, wherein R 2 , R 3 , R 4 , and R 5 are all H; or one of R 2 , R 3 , R 4 and R 5 is F or OCH 3 , and the others thereof are H; or R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 ) n O—, wherein n is defined as in Item 1.
17. The phosphate derivative according to Item 15, wherein R 2 ′, R 3 ′ and R 4 ′ are all H; or one of R 2 ′, R 3 ′ and R 4 ′ is F or OCH 3 , and the others thereof are H.
18. The phosphate derivative according to Item 15, wherein R 1 and R 1 ′ are benzyl.
19. The phosphate derivative according to Item 18, wherein R 2 ′, R 3 ′, R 4 ′, R 2 and R 5 are all H, and R 3 and R 4 together is —O(CH 2 )O—.
20. A pharmaceutical composition for the killing of solid cancer cells, which comprises a therapeutically effective amount of a phosphate derivative of 2-aryl-4-quinolone as set forth in any one of Item 1 to Item 19 or a pharmaceutically acceptable salt thereof, as an active ingredient, in admixture with a pharmaceutically acceptable carrier or diluent for the active ingredient, wherein the solid cancer cells comprise human breast cancer, colon cancer, lung cancer, melanoma, ovarian cancer, renal cancer, stomach cancer, prostate cancer, ileocecal carcinoma, glioblastoma, bone cancer, epidermoid carcinoma of the nasopharynx, hepatoma or leukemia cancer.
21. The pharmaceutical composition according to Item 20, wherein the solid cancer cells are human breast cancer, colon cancer, lung cancer, renal cancer, hepatoma, or leukemia cancer
22. The pharmaceutical composition according to Item 21, wherein the solid cancer cells are human breast cancer or colon cancer.
23. A compound of 2-selenophene 4-quinolone having the following formulas IIb or IIc:
wherein
R 2 ′, R 3 ′ and R 4 ′ independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, or (CH 2 ) n NR 8 R 9 , wherein n is an integer of 0-4, Y is O or S, X is F, Cl, or Br, and R 8 and R 9 independently are H, (CH 2 ) n YH, (CH 2 ) n N(C n H 2n+1 )(C m H 2m+1 ) or (CH 2 ) n CH 3 , wherein n and Y are defined as above, and m is an integer of 0-4;
R 2 , R 3 , R 4 and R 5 independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, (CH 2 ) n NR 8 R 9 ,
or R 3 and R 4 together is —Y(CH 2 ) n Y—, wherein n, Y, X, R 8 and R 9 are defined as above.
24. The compound according to Item 23, wherein R 2 , R 3 , R 4 , and R 5 are all H; or one of R 2 , R 3 , R 4 and R 5 is F or OCH 3 , and the others thereof are H; or R 2 and R 5 are H, and R 3 and R 4 together is —O(CH 2 ) n O—, wherein n is defined as in Item 19.
25. The compound according to Item 24, wherein R 2 ′, R 3 ′ and R 4 ′ are all H; or one of R 2 ′, R 3 ′ and R 4 ′ is F or OCH 3 , and the others thereof are H.
26. The compound according to Item 23 which has the formula IIb.
27. The compound according to Item 26, wherein R 2 ′, R 3 ′, R 4 ′, R 2 and R 5 are all H, and R 3 and R 4 together is —O(CH 2 )O—.
28. A pharmaceutical composition for the killing of solid cancer cells, which comprises a therapeutically effective amount of a compound of 2-selenophene 4-quinolone as set forth in any one of Item 23 to Item 27 or a pharmaceutically acceptable salt thereof, as an active ingredient, in admixture with a pharmaceutically acceptable carrier or diluent for the active ingredient, wherein the solid cancer cells comprise human breast cancer, colon cancer, lung cancer, melanoma, ovarian cancer, renal cancer, stomach cancer, prostate cancer, ileocecal carcinoma, glioblastoma, bone cancer, epidermoid carcinoma of the nasopharynx, hepatoma or leukemia cancer.
29. The pharmaceutical composition according to Item 28, wherein the solid cancer cells are human breast cancer, colon cancer, lung cancer, renal cancer, hepatoma, or leukemia cancer.
30. A compound of 2-phenyl-4-quinolone having the following formula IIa:
wherein
R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, (CH 2 ) n NR 8 R 9 ,
wherein n is an integer of 0-4, Y is O or S, X is F, Cl, or Br, and R 8 and R 9 independently are H, (CH 2 ) n YH, (CH 2 ) n N(C n H 2n+1 )(C m H 2m+1 ) or (CH 2 ) n CH 3 , wherein n and Y are defined as above, and m is an integer of 0-4;
R 2 , R 3 , R 4 and R 5 independently are H, (CH 2 ) n CH 3 , (CH 2 ) n YH, Y(CH 2 ) n CH 3 , Y(CH 2 ) n YH, Y(CH 2 ) n NR 8 R 9 , X, (CH 2 ) n NR 8 R 9 ,
or R 3 and R 4 together is —Y(CH 2 ) n Y—, wherein n, Y, X, R 8 and R 9 are defined as above;
provided that one of R 2 , R 3 , R 4 and R 5 is (CH 2 ) q NR 8 R 9 , or one of R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ is (CH 2 ) q NR 8 R 9 , wherein q is an integer of 1-4, and R 8 and R 9 are defined as above.
31. The compound according to Item 30, wherein R 4 is CH 2 ) q NR 8 R 9 , and R 2 , R 3 and R 5 are H, wherein q, R 8 and R 9 are defined as in Item 30.
32. The compound according to Item 30, wherein R 5 ′ is CH 2 ) q NR 8 R 9 , and R 2 ′, R 3 ′, R 4 ′ and R 6 ′ are H, wherein q, R 8 and R 9 are defined as in Item 30.
33. The compound according to Item 31, wherein R 4 is CH 2 N(C 2 H 5 ) 2 , R 6 ′ is F, and R 2 ′, R 3 ′, R 4 ′ and R 5 ′ are H.
34. The compound according to Item 31, wherein R 4 is CH 2 N(C 2 H 5 ) 2 , R 2 ′, R 3 ′, R 4 ′, R 5 ′ and R 6 ′ are all H.
35. The compound according to Item 32, wherein R 4 is OCH 3 , and R 2 , R 3 and R 5 are H; and R 5 ′ is CH 2 N(C 2 H 5 ) 2 , and R 2 ′, R 3 ′, R 4 ′ and R 6 ′ are H.
36. A pharmaceutical composition for the killing of solid cancer cells, which comprises a therapeutically effective amount of a compound of 2-phenyl 4-quinolone as set forth in any one of Item 30 to Item 35 or a pharmaceutically acceptable salt thereof, as an active ingredient, in admixture with a pharmaceutically acceptable carrier or diluent for the active ingredient, wherein the solid cancer cells comprise human breast cancer, colon cancer, lung cancer, melanoma, ovarian cancer, renal cancer, stomach cancer, prostate cancer, ileocecal carcinoma, glioblastoma, bone cancer, epidermoid carcinoma of the nasopharynx, hepatoma or leukemia cancer.
37. The pharmaceutical composition according to Item 36, wherein the solid cancer cells are leukemia cancer.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows effects of compound I-1 and compound I-1-b on MCF7 tumor growth in a mouse xenograft model. Female SCID mice received injections of MCF7 transfectants to induce tumor xenografts. Mice were divided into five groups. The second to fifth groups were given i.p. with compounds I-1 (15 mg/kg), I-1 (30 mg/kg), I-1-b (22.5 mg/kg), and I-1-b (45 mg/kg), respectively, three times per week. Data are expressed as mean of tumor weights (g)±S.E.M.*p<0.05 compared with the control.
FIG. 2 shows effect of compound I-1-b on animal survival. BALB/c mice were intraperitoneally injected with CT-26 tumor cells for 7 days before beginning the treatments with compound I-1-b (5 mg/kg/day and 10 mg/kg/day QD×7).
FIG. 3 shows effect of quinolone derivatives on the viability of human breast cancer cells. MCF7 cells were treated with DMSO (Control) or various concentrations (0.125 μM to 10 μM) of quinolone derivative for 48 hours and subsequent cell viability was measured by MTT assay. Results from three separate experiments were averaged and are presented as mean±standard error as shown.
DETAILED DESCRIPTION OF THE INVENTION
As shown in the following Examples 1 to 6, when 2-phenyl-4-quinolones (I-1 to I-6) was reacted with tetrabenzyl pyrophosphate in the presence of alkali, the corresponding phosphoric acid dibenzyl esters (I-1-a to I-6-a) were obtained. Catalytic hydrogenation of compounds (I-1-a to I-6-a) in alcohol affords the corresponding phosphoric acid mono esters (I-1-b to I-6-b), which could be led to water soluble salts (I-1-c to I-6-c).
Example 1
Dibenzyl 2-(2′-fluorophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-1-a)
Sodium hydride (137 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-1 (64.5 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give compound I-1-a (69.1 mg, 67%)
MP 101-104° C.
1 H-NMR (CDCl 3 , 300 MHz): δ 8.01-8.02 (m, 1H, H-5′), 7.77 (s, 1H, H-5), 7.16-7.43 (m, 14H, H-3, H-3′, H-4′, H-6′, Ph), 7.05 (s, 1H, H-8), 6.12 (s, 2H, OCH 2 O), 5.26 (s, 2H, — CH 2 -Ph), 5.20 (s, 2H, — CH 2 -Ph)
MS (m/z) 544 (ES+)
Anal. calcd for C 30 H 25 FNO 6 P: C, 66.30; H, 4.27; N, 2.58. Found: C, 66.28; H, 4.35; N, 2.55.
2-(2′-Fluorophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-1-b)
A suspension of compound I-1-a (97.7 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-1-b (63.5 mg, 97.2%).
MP>300° C.
1 H-NMR (DMSO-d6, 300 MHz): δ 7.93-7.98 (m, 1H, H-5′), 7.74 (s, 1H, H-5), 7.49-7.54 (m, 1H, H-4′), 7.32-7.41 (m, 4H, H-3, H-8, H-3′, H-6′), 6.22 (s, 2H, OCH 2 O).
MS (m/z) 362 (ES−)
Anal. calcd for C 16 H 13 FNO 6 P: C, 52.91; H, 3.05; N, 3.86. Found: C, 52.73; H, 3.10; N, 3.81.
Sodium 2-(2′-fluorophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-1-c)
Compound I-1-b was added to a mixture of 20 ml Amberlite IR-120(Na + form) and 20 ml water, and then stirred for 6 h at room temperature. The mixture was then filtered to remove Amberlite, and then lyophilized to give I-1-c (49.1 mg, 69%).
1 H-NMR (D2O, 200 MHz): δ 7.48-7.66 (m, 2H, H-4′, H-6′), 7.40 (s, 1H, H-8), 7.31-7.35 (m, 1H, H-5), 7.11-7.19 (m, 2H, H-3′, H-5′), 7.03 (s, 1H, H-3), 5.92 (s, 2H, OCH 2 O).
Example 2
Dibenzyl 2-(3′-fluorophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-2-a)
Sodium hydride (13.7 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-2 (64.5 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give compound I-2-a (85.6 mg, 83%).
MP 94-96° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.61-7.78 (m, 2H, H-2′, H-4′), 7.48-7.56 (m, 1H, H-5′), 7.24-7.45 (m, 13H, H-5, H-8, H-6′, Ph), 7.10 (s, 1H, H-3), 6.21 (s, 2H, OCH 2 O), 5.29 (s, 2H, — CH 2 -Ph), 5.24 (s, 2H, — CH 2 -Ph)
MS (m/z) 544 (ES+)
Anal. calcd for C 30 H 25 FNO 6 P: C, 66.30; H, 4.27; N, 2.58. Found: C, 66.25; H, 4.34; N, 2.55.
2-(3′-Fluorophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-2-b)
A suspension of compound I-2-a (97.7 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-2-b (60.8 mg, 93.1%).
MP>300° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.91 (s, 1H, H-2′), 7.87 (s, 1H, H-4′), 7.83 (s, 1H, H-5′), 7.50-7.62 (m, 2H, H-5, H-8), 7.25-7.36 (m, 2H, H-5′, H-6′), 6.24 (s, 2H, OCH 2 O).
MS (m/z) 362 (ES−)
Anal. calcd for C 16 H 13 FNO 6 P: C, 52.91; H, 3.05; N, 3.86. Found: C, 52.86; H, 3.12; N, 3.79.
Sodium 2-(3′-fluorophenyl)-6,7-methylenedioxyquinoline 4-yl-phosphate (I-2-c)
Compound I-2-b was added to a mixture of 20 ml Amberlite IR-120(Na + form) and 20 ml water, and then stirred for 6 h at room temperature. The mixture was then filtered to remove Amberlite, and then lyophilized to give I-2-c (68.2 mg, 71%).
1 H-NMR (D2O, 200 MHz): δ 7.26-7.78 (m, 5H, H-5, H-8, H-2′, H-5′, H-6′), 6.90-6.96 (m, 2H, H-3, H-4′), 6.03 (s, 2H, OCH 2 O).
Example 3
Dibenzyl 6-fluoro-2-phenylquinolin-4-yl-phosphate (I-3-a)
Sodium hydride (13.7 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-3 (55.0 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give I-3-a as a colorless oil compound (84.4 mg, 89%).
1 H-NMR (DMSO-d6, 200 MHz): δ 8.07-8.14 (m, 1H, H-8), 7.92-7.97 (m, 2H, H-2′, H-6′), 7.67-7.77 (m, 2H, H-3′, H-5′), 7.40-7.50 (m, 10H, Ph), 5.31 (s, 2H, — CH 2 -Ph), 5.27 (s, 2H, — CH 2 -Ph)
MS (m/z) 500 (ES+)
Anal. calcd for C 29 H 23 FNO 6 P: C, 69.74; H, 4.64; N, 2.80. Found: C, 69.75; H, 4.60; N, 2.81.
6-Fluoro-2-phenylquinolin-4-yl-phosphate (I-3-b)
A suspension of compound I-3-a (89.8 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-3-b. (50.5 mg, 88%).
MP>300° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.07-8.14 (m, 3H, H-8, H-2′, H-6′), 7.95 (s, 1H, H-5), 7.70-7.74 (m, 2H, H-3′, H-5′), 7.50-7.56 (m, 3H, H-3, H-7, H-4′)
MS (m/z) 318 (ES−)
Anal. calcd for C 15 H 11 FNO 4 P: C, 56.44; H, 3.47; N, 4.39. Found: C, 56.42; H, 3.49; N, 4.30.
Sodium 6-Fluoro-2-phenylquinolin-4-yl-phosphate (I-3-c)
Compound I-3-b was added to a mixture of 20 ml Amberlite IR-120(Na + form) and 20 ml water, and then stirred for 6 h at room temperature. The mixture was then filtered to remove Amberlite, and then lyophilized to give I-3-c (41.9 mg, 73%).
1 H-NMR (D2O, 200 MHz): δ 7.20-7.83 (m, 5H, H-5, H-7, H-8, H-2′, H-6′), 7.25-7.31 (m, 4H, H-3, H-3′, H-4′, H-5′).
Example 4
Dibenzyl 2-phenylquinolin-4-yl-phosphate (I-4-a)
Sodium hydride (13.7 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-4 (50.8 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give I-4-a as a colorless oil compound (71.3 mg, 78%).
1 H-NMR (DMSO-d6, 200 MHz): δ 8.05 (d, J=8.2 Hz, 1H, H-5), 7.73-7.98 (m, 5H, H-6, H-7, H-8, H-2′, H-6′), 7.58 (d, J=8.0 Hz, 1H, H-4′), 7.48-7.51 (m, 3H, H-3, H-3′, H-5′), 7.29-7.40 (m, 10H, Ph), 5.31 (s, 2H, — CH 2 -Ph), 5.27 (s, 2H, — CH 2 -Ph)
MS (m/z) 482 (ES+)
Anal. calcd for C 29 H 24 NO 6 P: C, 72.34; H, 5.02; N, 2.90. Found: C, 71.89; H, 5.13; N, 2.88.
2-Phenylquinolin-4-yl-phosphate (I-4-b)
A suspension of compound I-4-a (86.6 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-4-b (48.9 mg, 90.3%).
MP>300° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.80-8.12 (m, 4H, H-5, H-8, H-2′, H-6′), 7.49-7.78 (m, 6H, H-3, H-6, H-7, H-3′, H-4′, H-5′), 7.78 (s, 1H, H-7), 7.66 (t, J=8.0 Hz), 7.42-7.50 (m, 4H, H-3, H-3′, H-4′, H-5′)
MS (m/z) 300 (ES−)
Anal. calcd for C 15 H 12 NO 6 P: C, 59.81; H, 4.02; N, 4.65. Found: C, 59.52; H, 4.13; N, 4.72.
Sodium 6-fluoro-2-phenylquinolin-4-yl-phosphate (I-4-c)
Compound I-4-b was added to a mixture of 20 ml Amberlite IR-120(Na + form) and 20 ml water, and then stirred for 6 h at room temperature. The mixture was then filtered to remove Amberlite, and then lyophilized to give I-4-c (41.2 mg, 74%).
1 H-NMR (D2O, 200 MHz): δ 8.21 (d, J=8.2 Hz, 1H, H-5), 7.80-7.89 (m, 3H, H-8, H-2′, H-6′), 7.78 (s, 1H, H-7), 7.66 (1, J=8.0 Hz), 7.42-7.50 (m, 4H, H-3, H-3′, H-4′, H-5′)
Example 5
Dibenzyl 6-methoxy-2(3-′fluorophenyl)-quinolin-4-yl-phosphate (I-5-a)
Sodium hydride (13.7 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-5 (61.9 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give I-5-a as a colorless oil compound (85.4 mg, 85%)
1 H-NMR (DMSO-d6, 200 MHz): δ 7.98 (d, J=9.4 Hz, 1H, H-8), 7.74-7.83 (m, 3H, H-5, H-7, H-5′), 7.43-7.54 (m, 1H, H-6′), 7.41-7.48 (m, 1H, H-2′), 7.20-7.22 (m, H-3), 5.31 (s, 2H, — CH 2 -Ph), 5.27 (s, 2H, — CH 2 -Ph), 3.78 (s, 3H, OCH 3 ).
MS (m/z) 530 (ES+)
Anal. calcd for C 30 H 25 FNO 5 P: C, 68.05; H, 4.76; N, 2.65. Found: C, 67.32; H, 4.33; N, 2.78.
6-Methoxy-2(3-′fluorophenyl)-quinolin-4-yl-phosphate (I-5-b)
A suspension of compound I-5-a (95.2 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-5-b (56.5 mg, 89.9%).
MP>300° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.93-7.89 (m, 4H, H-5, H-7, H-8, H-5′), 7.45-7.58 (m, 1H, H-6′), 7.35-7.41 (m, 2H, H-2′, H-4′), 7.20-7.32 (m, 1H, H-3), 3.81 (s, 3H, OCH 3 )
MS (m/z) 348 (ES−)
Anal. calcd for C 16 H 13 FNO 5 P: C, 55.02; H, 3.75; N, 4.01. Found: C, 54.90; H, 3.89; N, 4.35.
Example 6
Dibenzyl 2-(3′-methoxyphenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-6-a)
Sodium hydride (13.7 mg, 0.57 mmol) was added at 0° C. to a stirred solution of compound I-6 (67.9 mg, 0.23 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (100 mg, 0.19 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give to give I-6-a as a colorless oil compound (88.6 mg, 84%)
1 H-NMR (DMSO-d6, 200 MHz): δ 7.60 (s, 1H, H-6′), 7.55 (s, 1H, H-2′), 7.25-7.40 (m, 14H, H-5, H-8, H-4′, H-5′, Ph), 6.21 (s, 2H, OCH 2 O), 5.28 (s, 2H, — CH 2 -Ph), 5.24 (s, 2H, — CH 2 -Ph), 3.80 (s, 3H, OCH 3 )
MS (m/z) 556 (ES+)
Anal. calcd for C 31 H 26 NO 7 P: C, 67.02; H, 4.72; N, 2.52. Found: C, 68.15; H, 4.68; N, 2.61.
2-(3′-Methoxyphenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-6-b)
A suspension of compound I-6-a (97.74 mg, 0.18 mmol) in anhydrous MeOH (10 ml) was submitted to hydrogenation in the presence of 10% Pd/C (50 mg) at room temperature for 10 min. The catalyst and precipitates was collected and dissolved in 10% NaHCO 3 solution then filtered. The filtrate was acidified with dil HCl, the solid was then collected by filtration and washed with acetone to give compound I-6-b (63.5 mg, 94%).
MP>300° C.
MS (m/z) 374 (ES−)
Anal. calcd for C 17 H 14 NO 7 P: C, 54.41; H, 3.76; N, 3.73. Found: C, 53.86; H, 3.66; N, 3.81.
Sodium 2-(3′-methoxyphenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-6-c)
Compound I-6-b was added to a mixture of 20 ml Amberlite IR-120(Na + form) and 20 ml water, and then stirred for 6 h at room temperature. The mixture was then filtered to remove Amberlite, and then lyophilized to give I-6-c (53.9 mg, 76%).
1 H-NMR (D2O, 200 MHz): δ 7.56 (s, 1H, H-6′), 7.25-7.42 (m, 4H, H-5, H-8, H-2′, H-5′), 7.12 (s, 1H, H-4′), 6.95 (s, 1H, H-3), 6.00 (s, 2H, OCH 2 O), 3.62 (s, 3H, OCH 3 )
In the following Example 7, a novel intermediate, 2-selenophene 4-quinolone (I-7-d), was synthesized. 2-selenophene-4-quinolone (I-7-d) was reacted with tetrabenzyl pyrophosphate in the presence of alkali, the corresponding phosphoric acid dibenzyl ester (I-7-e) was obtained.
Example 7
Selenophene-2-carboxylic acid (I-7-a)
To a solution of selenophene (20 g, 1527 mmol) in (Et) 2 O (150 ml) was added TMEDA (25.5 ml, 170.0 mmol) and n-butyllithium (66.1 ml of a 2.5 M solution in hexane, 152.8 mmol). The resulting solution was heated at reflux for 1.5 h, and then cooled in an acetone/CO 2 bath, after which crushed solid carbon dioxide (40 g, 909.1 mmol) was added. The reaction mixture was allowed to return to room temperature, and quenched by addition of 10% KOH solution. The aqueous layer was acidified to pH 3 with 8 M HCl, extracted with (Et) 2 O, washed with brine, dried over MgSO 4 filtered and concentrated under vacuum to give compound I-7-a (24.6 g, 92.1%).
MP 122-124° C.
1 H-NMR (CDCl 3 -d 1 , 200 MHz): δ 8.92 (s, 1H, —COO H ), 8.37 (dd, J=1.0 Hz, 5.6 Hz, 1H, H-3), 8.13 (dd, J=0.8 Hz, 3.8 Hz, 1H, H-5), 7.37 (dd, J=3.8 Hz, 5.6 Hz, 1H, H-4).
MS (m/z) 175.0 (EI+)
Anal. calcd for C 5 H 4 O 2 Se: C, 34.31; H, 2.30. Found: C, 34.33; H, 2.28.
N-(5-acetylbenzo[d][1,3]dioxol-6-yl)selenophene-2-carboxamide (I-7-c)
I-7-a (2 g, 11.40 mmol) was taken for subsequent chlorination by refluxing with thionyl chloride (4.1 ml, 56.18 mmol) for 20 h to afford I-7-b, which, without further purification, was treated with 2-amino-(4,5-methylenedioxy)-acetophenone (1.63 g, 9.12 mmol) and triethylamine (2 ml, 14.80 mmol) in 100 ml toluene, and refluxed for 3 h. The reaction mixture was concentrated under vacuum, and the solid material is consecutively washed with ethanol and dried at 80° C. for 2 h to give crude compound I-7-c (2.7 g, 74%).
MP 198.5-198.8° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 12.85 (s, 1H, N H CO), 8.52 (d, J=5.1 Hz, 1H, H-3′), 8.16 (s, 1H, H-4), 7.93 (d, J=3.8 Hz, 1H, H-5′), 7.61 (s, 1H, H-7), 7.49-7.46 (m, 1H, H-4′), 6.13 (s, 2H, OCH 2 O), 2.58 (s, 3H, CH 3 ).
MS (m/z) 336.2 (EI+)
Anal. calcd for C14H11NO4Se: C, 50.01; H, 3.30; N, 4.17. Found: C, 50.11; H, 3.32; N, 4.15.
2-(2′-Selenophenyl)-6,7-(methylenedioxy)-4-quinolone (I-7-d)
I-7-c (2.7 g, 8.0 mmol) was suspended in 100 ml t-BuOH. Potassium tert-butoxide (4.49 g, 40 mmol) was added, and the mixture was heated at reflux for 24 h. The mixture was cooled to room temperature, and poured onto 100 ml of aqueous NH 4 Cl. The yellow-brown solid was collected and washed by distilled water to give compound I-7-d (3.1 g, 85%).
MP>300° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.27 (s, 1H, H-3′), 7.83 (s, 1H, H-5′), 7.39 (t, J=4.5 Hz, 1H, H-4′), 7.31 (s, 1H, H-5), 7.14 (s, 1H, H-8), 6.11 (s, 3H, H-3, OCH 2 O).
MS (m/z) 318.2 (EI+)
Anal. calcd for C14H9NO3Se: C, 52.85; H, 2.85; N, 4.40. Found: C, 52.87; H, 2.82; N, 4.45.
Dibenzyl 2-(2′-selenophenyl)-6,7-methylenedioxyquinolin-4-yl-phosphate (I-7-e)
Sodium hydride (30 mg, 1.25 mmol) was added at 0° C. to a stirred solution of compound I-7-d (100.0 mg, 0.32 mmol) in dry tetrahydrofuran (10 ml). After 1 h, tetrabenzyl pyrophosphate (204.6 mg, 0.38 mmol) was added and the stirring was continued for 20 min.
The mixture was filtered, and the filtrate was concentrated under vacuum at a temperature below 35° C. The residue was dissolved in dichloromethane, washed with an aqueous solution of sodium hydrogen carbonate, dried over MgSO 4 and concentrated under vacuum to give the solid which was subjected to silica gel column chromatography. Elution with CH 2 Cl 2 gave yellowish compound I-7-e (151.8 mg, 82%).
MP 110.5-110.8° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.24 (d, J=5.6 Hz, 1H, H-3′), 7.65 (d, J=3.8 Hz, 1H, H-5′), 7.57 (s, 1H, H-5), 7.05 (s, 1H, H-8), 7.39-7.26 (m, 11H, H-4′, Ph), 6.19 (s, 2H, OCH 2 O), 5.28 (s, 2H, — CH 2 -Ph), 5.24 (s, 2H, — CH 2 -Ph).
MS (m/z) 580 (ES+)
Anal. calcd for 280H 22 NO 6 PSe: C, 58.14; H, 3.83; N, 2.42. Found: C, 57.28; H, 3.56; N, 2.59.
Example 8
6-Methyl-2-phenylquinolin-4(1H)-one (I-8-a)
A mixture of p-toluidine (2.14 g, 0.02 mole), ethyl benzoylacetate (4.9 g, 0.025 mole), and polyphosphoric acid (PPA) was heated at 130° C. with stirring. After the reaction was complete, the mixture was cooled to room temperature and neutralized with 4 M NaOH. The yellow solid was filtered, washed with water, dried and recrystallized from ethanol to give compound I-8-a as white solid (2.9 g, 48.9%).
MP 290.2-291.5° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 11.55 (1H, s, H-1), 7.88 (1H, s, H-5), 7.79-7.82 (2H, m, H-2′, H-3′), 7.66 (1H, d, J=8.5 Hz, H-8), 7.54-7.57 (3H, m, H-3′, H-4′, H-5′), 7.48 (1H, d, J=8.5 Hz, H-7), 6.31 (1H, s, H-3), 2.40 (3H, s, CH 3 )
MS (m/z) 235 (EI+)
Anal. calcd for C16H13NO: C, 81.68; H, 5.57; N, 5.95. Found: C, 81.60; H, 5.63; N, 5.88.
4-(Benzyloxy)-6-methyl-2-phenylquinoline (1-B-b)
I-8-a (700 mg, 3 mmole) was dissolved in dry DMF (30 ml), and NaH (360 mg, 15 mmole) was added portionwise with stirring for 30 min at room temperature. Benzyl chloride (750 mg, 6 mmole) was then added dropwise, and stirred at room temperature overnight. The reaction mixture was poured into ice-water and extracted with CH 2 Cl 2 . The organic layer was washed with water, dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with n-hexane-EtOAc (3:1), and recrystallized from n-hexane-CH 2 Cl 2 to afford I-8-b as white crystal (536 mg, 54.9%).
MP 138.6-139.3° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.23-8.26 (2H, m, H-2′, H-6′), 7.88-7.91 (2H, m, H-5, H-8), 7.37-7.62 (9H, m, H-7, H-3′, H-4′, H-5′, Ph), 5.51 (2H, s, OCH 2 Ph), 2.48 (3H, s, CH 3 )
Anal. calcd for C23H19NO: C, 84.89; H, 5.89; N, 4.30. Found: C, 84.93; H, 5.85; N, 4.33.
N-{[4-(Benzyloxy)-2-phenylquinolin-6-yl]methyl}-N-ethyl ethanamine (I-8-d)
I-8-b (650 mg, 2 mmol), N-bromo-succinimide (NBS, 360 mg, 2 mmol), and 2,2′-azobis(isobutyronitrile) (AlBN, 30 mg, 0.19 mmol) were added to a dry round bottom flask, which was purged with argon. 50 ml of dry benzene was added to the reaction mixture in an argon atmosphere with stirring at room temperature for 30 min, and then refluxed at 80° C. for 1 h and then cooled to room temperature to give I-7-c, which, without further purification, was treated with diethylamine (3.0 ml, 29.0 mmole), and then refluxed for 1 h. After removing the solvent by evaporation, the mixture was partitioned with EtOAc and 50 ml 10% HCl, and then the acid layer was neutralized to PH 7-8 by 10% NaHCO 3 , extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with CH 2 Cl 2 -methanol (3:1), and recrystallized from n-hexane-EtOAc to afford I-8-d as light-yellow solid (120 mg, 15.1%).
MP 107.7-108.6° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.22 (2H, m, H-2′, H-6′), 8.01 (1H, s, H-5), 7.91 (1H, d, H-8), 7.33-7.69 (9H, m, H-7, H-3′, H-4′, H-5′, Ph), 5.49 (2H, s, OCH 2 Ph), 3.65 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.43 (4H, q, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ), 0.93 (6H, t, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 )
MS (m/z) 396 (EI+)
Anal. calcd for C27H28N2O: C, 81.78; H, 7.12; N, 7.06. Found: C, 81.68; H, 7.03; N, 7.15.
6-[(Diethylamino)methyl]-2-phenylquinolin-4(1H)-one (I-8-e)
I-8-d (120 mg, 0.3 mmol) was dissolved in glacial acetic acid (5 ml). HBr (3 ml) was added while the solution was heated to 60° C., and the mixture was heated to 90° C. for 3 h. After the reaction was complete, the reaction mixture was poured into water, and extracted with EtOAc. The acid layer was neutralized to pH 7-8 by adding 10% NaHCO 3 , and extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was recrystallized from n-hexane-EtOAc to afford I-8-d as gray solid (55 mg, 59.9%).
MP 227.9-229.7° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.96 (1H, s, H-5), 7.78 (2H, m, H-2′, H-6′), 7.69 (1H, d, H-8), 7.50-7.58 (4H, m, H-7, H-3′, H-4′, H-5′), 6.31 (1H, s, H-3), 3.55 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.41 (4H, q, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ), 0.92 (6H, t, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 )
MS (m/z) 306 (EI+)
Anal. calcd for C20H22N2O: C, 78.40; H, 7.24; N, 9.14. Found: C, 78.43; H, 7.35; N, 9.08.
Example 9
2-(2-Fluorophenyl)-6-methylquinolin-4(1H)-one (I-9-a)
A mixture of p-toluidine (2.14 g, 0.02 mole), 2-fluoro-ethyl benzoylacetate (5.25 g, 0.025 mole), and polyphosphoric acid (PPA) was heated at 130° C. with stirring. After the reaction was complete, the mixture was cooled to room temperature and neutralized with 4 M NaOH. The yellow solid was filtered, washed with water, dried and recrystallized from ethanol to give compound I-9-a as white solid (2.6 g, 51.3%).
MP 259.1-259.9° C.
1 H-NMR (DMSO-d6, 200 MHz): δ7.86 (1H, s, H-5), 7.64 (1H, td, J=7.58, H-4′), 7.47-7.57 (3H, m, H-7, H-8, H-6′), 7.30-7.43 (2H, d, J=7.02, dd, J=7.36, H-3′, 5′), 6.12 (1H, s, H-3), 2.36 (3H, s, CH 3 )
MS (m/z) 253 (EI+)
Anal. calcd for C16H22FNO: C, 75.88; H, 4.78; N, 5.53. Found: C, 75.94; H, 4.70; N, 5.46.
4-(Benzyloxy)-2-(2-fluorophenyl)-6-methylquinoline (I-9-b)
I-9-a (750 mg, 3 mmole) was dissolved in dry DMF (30 ml), and NaH (360 mg, 15 mmole) was added portionwise with stirring for 30 min at room temperature. Benzyl chloride (750 mg, 6 mmole) was then added dropwise, and stirred at room temperature overnight. The reaction mixture was poured into ice-water and extracted with CH 2 Cl 2 . The organic layer was washed with water, dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with n-hexane-EtOAc (3:1), and recrystallized from n-hexane-CH 2 Cl 2 to afford I-9-b as white crystal (515 mg, 50.0%).
MP 91.5-92.8° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.84-7.97 (3H, m, H-5, H-8, H-4′), 7.26-7.58 (10H, m, H-3, H-7, H-3′, H-5′, H-6′, Ph), 5.38 (2H, s, OCH 2 Ph), 2.45 (3H, s, CH 3 )
MS (m/z) 343 (EI+)
Anal. calcd for C23H18FNO: C, 80.45; H, 5.28; N, 4.08. Found: C, 80.51; H, 5.29; N, 4.17.
N-{[4-(Benzyloxy)-2-(2-fluorophenyl)quinolin-6-yl]methyl}-N— ethylethanamine (I-9-d)
I-9-b (680 mg, 2 mmol), N-bromo-succinimide (NBS, 360 mg, 2 mmol), and 2,2′-azobis(isobutyronitrile) (AlBN, 30 mg, 0.19 mmol) were added to a dry round bottom flask, which was purged with argon. 50 ml of dry benzene was added to the reaction mixture in an argon atmosphere with stirring at room temperature for 30 min, and then refluxed at 80° C. for 1 h and then cooled to room temperature to give I-9-c, which, without further purification, was treated with diethylamine (3.0 ml, 29.0 mmole), and then refluxed for 1 h. After removing the solvent by evaporation, the mixture was partitioned with EtOAc and 50 ml 10% HCl, and then the acid layer was neutralized to PH 7-8 by 10% NaHCO 3 , extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with CH 2 Cl 2 -methanol (3:1), and recrystallized from n-hexane-EtOAc to afford I-9-d as yellow solid (120 mg, 15.1%).
MP 51.2-51.5° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.04 (1H, s, H-5), 7.84-7.96 (2H, m, H-8, H-5′), 7.69 (1H, dd, H-4′), 7.28-7.54 (9H, m, H-3, H-7, H-3′, H-6′, Ph), 5.41 (2H, s, OCH 2 Ph), 3.68 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.46 (4H, q, J=7, CH 2 N(CH 2 CH 3 ) 2 ), 0.94 (6H, t, J=7, CH 2 N(CH 2 CH 3 ) 2 )
MS (m/z) 414 (EI+)
Anal. calcd for C27H27FN2O: C, 78.23; H, 6.57; N, 6.76. Found: C, 78.25; H, 6.67; N, 6.74.
6-[(Diethylamino)methyl]-2-(2-fluorophenyl)quinolin-4(1H)-one (I-9-e)
I-9-d (120 mg, 0.3 mmol) was dissolved in glacial acetic acid (5 ml). HBr (3 ml) was added while the solution was heated to 60° C., and the mixture was heated to 90° C. for 3 h. After the reaction was complete, the reaction mixture was poured into water, and extracted with EtOAc. The acid layer was neutralized to pH 7-8 by adding 10% NaHCO 3 , and extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was recrystallized from n-hexane-EtOAc to afford I-8-e as gray solid (58 mg, 59.6%).
MP 184.2-184.7° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 11.9 (1H, s, H-1), 7.97 (1H, s, H-5), 7.52-7.69 (4H, m, H-7, H-8, H-4′, H-6′), 7.31-7.43 (2H, m, H-3′, H-5′), 6.12 (1H, s, H-3), 3.57 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.40 (4H, q, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ), 0.92 (6H, t, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 )
MS (m/z) 324 (EI+)
Anal. calcd for C20H21FN2O: C, 74.05; H, 6.53; N, 8.64. Found: C, 73.94; H, 6.62; N, 8.67.
Example 10
Ethyl 3-methyl-benzoyl-acetate (I-10-a)
To a vigorously stirred suspension of NaH (564 mg, 48.5 mmol) and CO(OEt) 2 (5.73 g, 48.5 mmol) in anhydrous toluene (50 ml) was added dropwise a solution of 3-methylacetophenone (4.33 g, 32.3 mmole) in toluene under reflux. The mixture was allowed to reflux and was stirred for 30 min after the addition was complete. When cooled to room temperature, the mixture was acidified with glacial AcOH. After ice-cold water was added, the mixture was extracted with toluene. The organic layer was dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with CH 2 Cl 2 -n-haxane (3:2) to afford I-10-b as light-yellow liquid (3.13 g, 46.9%)
1 H-NMR (DMSO-d6, 200 MHz): δ 7.68-7.72 (2H, m, H-4, H-6), 7.32-7.36 (2H, m, H-2, H-3), 4.16 (2H, q, J=7, CH 2 CH 3 ), 3.94 (2H, s, H-10), 2.38 (3H, s, CH 3 ), 1.2 (3H, t, J=7, CH 2 CH 3 )
MS (m/z) 206 (EI+)
Anal. calcd for C12H14O3: C, 69.88; H, 6.84. Found: C, 69.72; H, 6.95.
6-Methoxy-2-m-tolylquinolin-4(1H)-one (I-10-b)
A mixture of p-anisidine (2.14 g, 0.02 mole), I-10-a (5.1 g, 0.025 mole), and polyphosphoric acid (PPA) was heated at 130° C. with stirring. After the reaction was complete, the mixture was cooled to room temperature and neutralized with 4 M NaOH. The yellow solid was filtered, washed with water, dried and recrystallized from ethanol to give compound I-9-a as light-purple solid (2.6 g, 25.8%).
MP 262.2-264.1° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 7.70 (1H, d, H-8), 7.55-7.60 (2H, m, H-5, 7), 7.25-7.47 (4H, m, H-2′, H-4′, H-5′, H-6′), 6.33 (1H, s, H-3), 3.80 (3H, s, OCH 3 ), 2.37 (3H, s, CH 3 )
MS (m/z) 265 (EI+)
Anal. calcd for C17H15NO: C, 76.79; H, 5.70; N, 5.28. Found: C, 76.81; H, 5.62; N, 5.34.
4-(Benzyloxy)-6-methoxy-2-m-tolylquinoline (I-10-c)
I-10-b (795 mg, 3 mmole) was dissolved in dry DMF (30 ml), and NaH (360 mg, 15 mmole) was added portionwise with stirring for 30 min at room temperature. Benzyl chloride (750 mg, 6 mmole) was then added dropwise, and stirred at room temperature overnight. The reaction mixture was poured into ice-water and extracted with CH 2 Cl 2 . The organic layer was washed with water, dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with n-hexane-EtOAc (3:1), and recrystallized from n-hexane-CH 2 Cl 2 to afford I-10-c as white crystal (530 mg, 49.7%).
MP 133.0-134° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.00 (1H, s, H-5), 7.96 (1H, d, H-8), 7.89 (1H, d, J=8 Hz, H-7), 7.32-7.58 (6H, m, H-3, H-2′, H-5′, H-6′, Ph), 7.22 (1H, d, J=7 Hz, H-4′), 5.50 (2H, s, OCH 2 Ph), 3.83 (3H, s, OCH 3 ), δ2.38 (3H, s, CH 3 )
MS (m/z) 355 (EI+)
Anal. calcd for C24H21NO2: C, 81.10; H, 5.96; N, 3.94. Found: C, 81.9; H, 5.81; N, 3.97.
N-{[3-(4-(Benzyloxy)-6-methoxyquinolin-2-yl)phenyl)methyl}-N-ethylethanamine (I-10-e)
I-10-c (530 mg, 2 mmol), N-bromo-succinimide (NBS, 360 mg, 2 mmol), and 2,2′-azobis(isobutyronitrile) (AlBN, 30 mg, 0.19 mmol) were added to a dry round bottom flask, which was purged with argon. 50 ml of dry benzene was added to the reaction mixture in an argon atmosphere with stirring at room temperature for 30 min, and then refluxed at 80° C. for 1 h and then cooled to room temperature to give I-10-d, which, without further purification, was treated with diethylamine (3.0 ml, 29.0 mmole), and then refluxed for 1 h. After removing the solvent by evaporation, the mixture was partitioned with EtOAc and 50 ml 10% HCl, and then the acid layer was neutralized to PH 7-8 by 10% NaHCO 3 , extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was further chromatographed over silica gel by elution with CH 2 Cl 2 -methanol (3:1), and recrystallized from n-hexane-EtOAc to afford I-10-e as yellow solid (25 mg, 2.9%).
MP 89.2-89.5° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 8.13 (1H, s, H-3). 7.87-8.04 (2H, m, H-7, 8), 7.34-7.43 (10H, m, H-3, H-2′, H-4′, H-5′, H-6′, Ph), 5.51 (2H, s, OCH 2 Ph), 3.84 (3H, s, OCH 3 ), 3.69 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.53 (4H, q, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ), 0.99 (6H, t, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 )
MS (m/z) 426 (EI+)
Anal. calcd for C28H30N2O2: C, 78.83; H, 7.90; N, 6.57. Found: C, 78.95; H, 7.14; N, 6.48.
2-{3-[(Diethylamino)methyl]phenyl}-6-methoxyquinolin-4(1H)-one (I-10-f)
I-10-e (42 mg, 0.1 mmol) was dissolved in glacial acetic acid (5 ml). HBr (3 ml) was added while the solution was heated to 60° C., and the mixture was heated to 90° C. for 3 h. After the reaction was complete, the reaction mixture was poured into water, and extracted with EtOAc. The acid layer was neutralized to pH 7-8 by adding 10% NaHCO 3 , and extracted with EtOAc (100 ml×5). The organic layer was dried over MgSO 4 , and evaporated. The residue was recrystallized from n-hexane-EtOAc to afford I-10-f as gray solid (20.8 mg, 61.9%).
MP 152.1-152.7° C.
1 H-NMR (DMSO-d6, 200 MHz): δ 11.76 (1H, s, H-1), 7.67-7.74 (3H, m, H-5, H-8, H-6′), 7.46-7.49 (3H, m, H-7, H-2′, H-4′), 7.27 (1H, dd, H-5′), 6.27 (1H, s, H-3), 3.80 (3H, s, OCH 3 ), 3.67 (2H, s, CH 2 N(CH 2 CH 3 ) 2 ), 2.53 (4H, q, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ), 0.97 (6H, t, J=7 Hz, CH 2 N(CH 2 CH 3 ) 2 ).
Anal. calcd for C21H24N2O2: C, 74.97; H, 7.19; N, 8.33. Found: C, 74.81; H, 7.33; N, 8.31.
Anti Cancer Activities
Effects of Compounds I-1 and I-1-b on Anti-Tumor Activity In Vivo
(I) Effects of Compounds I-1 and I-1-b on MCF-7 Tumor Xenograft Model
I-1 Materials and Methods
Female GALB/cAnN-Foxn1.E SCID mice (18-20 g; 6-8 weeks of age) were purchased from the National Animal Center and maintained in pressurized ventilated cage according to institutional regulations. The mice were implanted subcutaneously with estradiol (0.7 mg) 2 days before tumor transplantation. MCF-7 cells (2×10 6 ) were inoculated s.c. into the right flank of the mice. After appearance of a 150-mm 3 tumor nodule, 30 tumor-bearing mice were randomly divided into five groups for treatment with vehicle (PBS), I-1 or I-1-b. The first groups only received vehicle. The second to fifth groups were given i.p. the following treatments three times per week, respectively: I-1 (15 mg/kg), I-1 (30 mg/kg), I-1-b (22.5 mg/kg), and I-1-b (45 mg/kg). Mice were weighed and tumors were measured using calipers every week. Tumor size was calculated with the following formula: (L+W)/2, where L is the length and W is the width. On the final day of the treatment, mice were sacrificed; tumors were excised, weighted, and sectioned; and the tumor sections were embedded in OCT compound and frozen at −70° C.
I-2 Results
The effects of I-1 or I-1-b, were examined in vivo. Thirty female SCID mice were individually injected s.c. with MCF7 cells. The mice were divided into five groups (six mice per group) and treated with vehicle alone, I-1 (15 or 30 mg/kg), I-1-b (22.5 or 45 mg/kg). As shown in FIG. 1 , this in vivo tumor model shows a significant reduction in tumor volume in mice treated with 45 mg/kg I-1-b when compared with control mice (P<0.001). These results demonstrate that I-1-b significantly inhibited MCF7 tumor growth in a mouse xenograft model.
(II) Effects of Compounds I-1 and I-1-b on CT-26 Intraperitoneal Tumor Model
II-1 Materials and Methods
30 male 6-week-old Balb/c mice, were purchased from the National Animal cancer and maintained in pressurized ventilated cage according to institutional regulations. CT-26 (1×10 6 ) cells were injected into peritoneal cavities at day 0. Animals were randomly assigned to anti-tumoral efficacy study (n=10). Seven days after tumor inoculation, oral administration of 5 and 10 mg/kg of I-1-b (QD for seven times) to the mice was carried out. The survival rate and body weight of the animals was monitored.
II-2 Results
II-2-1 Appearance of Mice after Treatment
Mice in the excipient control group showed overt ascites, while mice receiving orally I-1-b (5 mg/kg/day, QD×7) and I-1-b (10 mg/kg/day, QD×7) exhibited reduced ascites development.
II-2-2 the Average Life Span of Mice after Treatment
As shown in FIG. 2 , all mice in the excipient control group were dead 40 days after, while those receiving compounds I-1-b (5 mg/kg/day, QD×7) and compounds I-1-b (10 mg/kg/day, QD×7) were all dead respectively by day 45 and day 50 post challenge. The average life span was prolonged by 140% at the dose of (10 mg/kg/day, QD×7) and by 120% at the dose of (5 mg/kg/day, QD×7). A maximally tolerated dose was not achieved.
Cell Viability Assay (MTT Assay)
Cells were seeded in a 24-well microtiter plate (2×10 4 cells/well) overnight, then treated with DMSO (Control) or various concentrations of test compounds, and incubated for 48 hours. The effect of test compounds on cell growth was examined by the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide) assay. Briefly, 40 μl of MTT solution (2 mg/ml, Sigma Chemical Co.) was added to each well to make a final volume of 500 μl and incubated for 1 h at 37° C. The supernatant was aspirated, and the MTT-formazan crystals formed by metabolically viable cells were dissolved in 200 μl of DMSO. Finally, the absorbance at O.D. 550 nm was detected by enzyme-linked immunosorbent assay (ELISA) reader.
Results:
Cytotoxic Effect of Compounds I-1-b, I-2-b, I-3-b, I-4-b, I-5-b, I-7-d, I-7-e Against the Human Breast Cancer MCF-7 Cells
The cytotoxic effect of compounds I-1-b, I-2-b, I-3-b, I-4-b, I-5-b, I-7-d, I-7-e were evaluated in the human breast cancer MCF-7 cells. As shown in FIG. 3 , treatment with 0.125 to 10 μM of these compounds caused a dose-dependent decrease of cell viability. These results indicate that compounds I-1-b, I-2-b, I-3-b, I-4-b, I-5-b, I-7-d, I-7-e show significant cytotoxicity against MCF-7 cells. Therefore, these new derivatives of 2-aryl-quinolines are proposed as potential therapeutic agents for the treatment of cancers.
Cytotoxic Activity of Compound I-7-d
In vitro cytotoxic activity of compound I-7-d was tested in HCT-116, Hep G2, NCI-H226, A549, A498 and HL-60 cells. As shown in Table 1, compound I-7-d demonstrates significant inhibition against most of the six cancer cell lines and most notably, is quite active against HCT-116 and HL-60 cells. Compound I-7-d shows an IC 50 of 0.9 μM against HCT-116 and an IC 50 of 0.5 μM against HL-60 cell. Compound I-7-d is an attractive candidate for development as a novel anti-cancer agent.
TABLE 1 IC 50 (μM) HCT116 Hep G2 NCI-H226 A549 A498 HL-60 I-7-d 0.9 4.1 4.9 8.1 2.7 0.5 * Six cancer cell lines were treated with compound I-7-d for 48 h. After treatment, cells were harvested and examined using MTT assay. * IC 50 value means the concentration causing 50% growth-inhibitory effect. * HCT-116, colon cancer cell line; Hep G2, hepatoma cancer cell line; NCI-H226, non-small cell lung cancer cell line; A549, lung cancer cell line; A498, renal cancer cell line; HL-60, leukemia cancer cell line.
Cytotoxic Activity of Compound I-8-e, I-9-e and I-10-f
In vitro cytotoxic activity of compound I-8-e, I-9-e and I-10-f were tested in HL-60 cells. As shown in Table 2, compound I-8-e and I-9-e demonstrated significant inhibition against HL-60 cancer cell lines. Compound I-8-e showed an IC 50 of 15 μM and compound I-9-e showed an IC 50 of 5.8 μM against HL-60 cell. Compound I-9-e is an attractive candidate for development as a novel anti-cancer agent.
TABLE 2
Compound
IC 50 (μM)
I-8-e
15
I-9-e
5.8
I-10-f
>50
HL-60 cell were treated with compound I-8-e, I-9-e and I-10-f for 48 h. After treatment, cells were harvested and examined using MTT assay.
IC50 value means the concentration causing 50% growth-inhibitory effect.
HL-60, leukemia cancer cell line.
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2-aryl-4-quinolones are converted into phosphates by reacting with tetrabenzyl pyrophosphate to form dibenzyl phosphates thereof, which are then subject to hydrogenation to replace dibenzyl groups with H, followed by reacting with Amberlite IR-120(Na + form) to form disodium salts. The results of preliminary screening revealed that these phosphates showed significant anti-cancer activity. A novel intermediate, 2-selenophene 4-quinolone and N,N-dialkylaminoalkyl derivatives of 2-phenyl-4-quinolones are also synthesized. These novel intermediates exhibited significant anticancer activities.
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FIELD OF THE INVENTION
[0001] This invention relates to novel oxetanone derivative compounds and processes for producing such derivatives which are useful as lipase inhibitors. Further the invention relates to processes for producing salts and for producing pharmaceutical compositions compounds comprising at least one such oxetanone derivative or salt, as well as methods for using such compounds and compositions for inhibiting lipases. In one aspect the invention relates to lipase inhibitors which include on the same molecule an oxetanone derivative portion capable of inhibiting a lipase and a non-absorbable moiety such a polysaccharide, which are covalently linked or are in the form of a salt. In a preferred aspect of the invention the non-absorbable moiety is lipophilic and will associate with oils or fats. An absorbable oxetanone lipase inhibitor may be rendered non-absorbable by covalent linking it directly or indirectly to a non-absorbable moiety and thereby producing a novel non-absorbable lipase inhibitor.
BACKGROUND OF THE INVENTION
[0002] Some lipase-inhibiting oxetanones and intermediates for making them are well known. See for example, U.S. Pat. Nos. 5,931,463, 5,175,186, 4,189,438 and 4,202,824. However, there is a need for improved processes for making oxetanones in commercial quantities that are have low toxicity and are essentially not absorbable by the digestive system of mammals such as dogs, cats, non-human primates and human primates.
[0003] Lipase inhibitors such as esterastin (2S, 3S, 5S) 3,5-hydroxy-2-hexadeca-7,10-dienoic 1,3-lactone), tetrahydroesterastin (2S, 3S, 5S) 3,5-di-hydroxy-2-hexylhexadecanoic 1,3-lactone, and the like (see U.S. Pat. No. 4,189,438), are well-known as lipase inhibitors and are useful as pancreatic cholesterol esterase inhibitors. While these lipase inhibitor can be obtained by cultivating microbes as described in U.S. Pat. No. 4,189,438, it is believed that examples of successful synthetic procedures for effectively making such compounds in commercially acceptable quantities from intermediates other than those obtained from microbes have not been described in the literature.
[0004] Further, esterastin and tetrahydroesterastin are excluded by proviso from the claims of the U.S. Pat. No. 5,175,186, which relates to a synthetic method for making certain analogs of esterastin and tetrahydroesteratin. The specification of that document does not illustrate the direct production of esterastin or tetrahydroesteratin or other (5S) analogs before the 2S, 3S oxetanone (lactone) ring structure is formed. Further page 6, lines 21-44, of the U.S. Pat. No. 5,175,186 points to an asymetrical hydrogenation synthesis step, which makes obtaining (2S, 3S, 5S) analog compounds before the direct closure of the oxetanone ring problematic. On page 6, when an intermediate compound having the 5 hydroxyl group in the R configuration (6R intermediate), is selectively hydrogenated only the (3S, 4S, 6R) intermediates result, which convert to a final compound having a 2S, 3S, 5R configuration. Likewise, when a only a 6S intermediate is used the (3R, 4R, 6S) hydrogenation intermediates result. The U.S. Pat. No. 5,175,186 does not illustrate a feasible and efficient solution for resolving such a synthetic difficulty prior to closure of the oxetanone ring.
[0005] Accordingly, there is a need in the art for an improved commercial process for efficiently making tetrahydroesterastin and its (2S, 3S, 5S) analogs in a enantiomeric excess of greater than 70% by the use of 2S, 3S, 5S intermediate compounds which are formed prior to the formation of the oxetanone ring structure.
SUMMARY OF THE INVENTION
[0006] In one aspect the present invention relates to novel process for making in at least 70% enantiomeric purity a (3S, 4S, 6S) oxetanone compound of the formula (I),:
[0007] or a salt thereof
[0008] wherein:
[0009] R 1 and R 3 are each independently a C 1 to C 18 straight or branched alkyl hydrocarbon chain, and
[0010] R 2 is hydrogen or an alcohol protecting group R 10 , wherein R 10 can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, comprising the steps of:
[0011] (a) selectively hydrogenating a composition comprising a compound which is a member selected from the group consisting of (6R) tetrahydro-2H-pyran-2-one compound of formula (II) and (6R) 5,6-dihydro-2H-pyran-2,4-dione of formula (IIa):
[0012] wherein
[0013] R 5 is hydrogen or an alcohol protecting group, which can be replaced by a hydrogen atom via hydrogenation, and R 1 and R 3 are defined as in formula (I), by hydrogenating the compound of formula II with a hydrogenation catalyst selected from the group consisting of PtO 2 , Raney Nichel and the like, and exchanging hydrogen atoms at the 3 and 4 ring positions or oxidizing the 4-oxo group to provide a (3S, 4S, 6R) 4-hydroxy-tetrahydro-2H-pyran-2-one compound of the formula (III):
[0014] wherein R 1 and R 3 are defined as in formula (I);
[0015] (b) re-protecting the 4-hydroxy group of the compound of formula (II) produced in (a) with an ether protecting group R 6 , which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, opening the lactone ring and esterifying the resulting free acid group to provide a (2S, 3S, 5R) [R 7 ]2-[R 3 ]-3-[R 6- oxy]-5-[hydroxy, R 1 ] pentanoic acid ester compound of the formula (IV):
[0016] wherein
[0017] R 1 and R 3 are defined as in formula (I),
[0018] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and
[0019] R 7 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation;
[0020] (c) inverting the chirality of the 5-hydroxy group of the compound of formula (IV) produced in step (b), wherein the inversion comprises a step which is a member selected from the group consisting of
[0021] (i) a Mitsunobu reaction,
[0022] (ii) esterifying the 5-hydroxy group to a carboxylic acid ester such as the trichloroacetic acid ester, and the like, and hydrolyzing the resultant ester in a water ether solvent such as 3:1 H 2 O/dioxane, and
[0023] (iii) esterifying the 5-hydroxy group to a sulfonic acid ester, such as p-toluene sulfonic acid ester and the like, and reacting the ester with an excess of an organic acid salt selected from the group consising of potassium acetate, sodium acetate, tetraethylammonium acetate, and the like, to provide an ester exchange with the organic acid,
[0024] wherein the free inverted (5S) 5-hydroxy group of (i) and (ii) is esterified with a hydroxy protecting group R 10 which can be which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, to provide a compound of the formula (V):
[0025] wherein
[0026] R 1 and R 3 are defined as in formula (I),
[0027] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation,
[0028] R 9 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation, and
[0029] R 10 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and wherein R 10 is selectively removable with respect to the R 6 alcohol protecting group; and
[0030] (d) selectively removing the R 6 alcohol protecting group and R 9 ester group of the compound of formula (V) produced in (c), and cyclizing the 3 position alcohol group with the 1 position acid group using a lactone cyclizing catalyst, such as benzene-sulphonyl chloride, in a solvent such as pyridine at a temperature of about −10 to 10° C. and optionally replacing the R 10 alcohol protecting group of formula (V) with a hydrogen atom, to yield a (3S, 4S, 6S) oxetanone compound of the formula (I):
[0031] or a salt thereof.
[0032] In a preferred aspect, the process provides a compound of formula (I) wherein R1 is undecyl, R 3 is hexyl and R 2 is hydrogen, which is (2S, 3S, 5S) tetrahydroesterastin.
[0033] In another aspect the present invention relates to coupling such compound of formula (I) to an acyl compound via an acid or base esterification procedure without inversion of the 5S hydroxy group.
[0034] In another aspect the present invention provides a novel intermediate (2S, 3 S, 5 S) compound of the formula:
[0035] wherein:
[0036] R 1 and R 3 are each independently a C 1 to C 18 straight or branched alkyl hydrocarbon chain, and
[0037] R 2 is hydrogen or an alcohol protecting group R 10 , wherein R 10 can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and R 10 is selectively removable with respect to the R 6 alcohol protecting group,
[0038] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and
[0039] R 9 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation, or, a salt thereof.
[0040] In a preferred aspect, the invention providessuch an intermediate compound wherein R 1 is undecyl or heptadecyl and R 3 is ethyl or hexyl, or a salt thereof.
DETAILED DESCRIPTION OF THE INVENTION
[0041] Definitions
[0042] In accordance with the present invention and as used herein, the following terms are defined with the following meanings, unless explicitly stated otherwise.
[0043] The term “alkenyl” refers to a trivalent straight chain or branched chain unsaturated aliphatic radical. The term “alkinyl” (or “alkynyl”) refers to a straight or branched chain aliphatic radical that includes at least two carbons joined by a triple bond. If no number of carbons is specified alkenyl and alkinyl each refer to radicals having from 2-12 carbon atoms.
[0044] The term “alkyl” refers to saturated aliphatic groups including straight-chain, branched-chain and cyclic groups having the number of carbon atoms specified, or if no number is specified, having up to 12 carbon atoms. The term “cycloalkyl” as used herein refers to a mono-, bi-, or tricyclic aliphatic ring having 3 to 14 carbon atoms and preferably 3 to 7 carbon atoms.
[0045] As used herein, the terms “carbocyclic ring structure” and “C 3-16 carbocyclic mono, bicyclic or tricyclic ring structure” or the like are each intended to mean stable ring structures having only carbon atoms as ring atoms wherein the ring structure is a substituted or unsubstituted member selected from the group consisting of: a stable monocyclic ring which is aromatic ring (“aryl”) having six ring atoms; a stable monocyclic non-aromatic ring having from 3 to 7 ring atoms in the ring; a stable bicyclic ring structure having a total of from 7 to 12 ring atoms in the two rings wherein the bicyclic ring structure is selected from the group consisting of ring structures in which both of the rings are aromatic, ring structures in which one of the rings is aromatic and ring structures in which both of the rings are non-aromatic; and a stable tricyclic ring structure having a total of from 10 to 16 atoms in the three rings wherein the tricyclic ring structure is selected from the group consisting of: ring structures in which three of the rings are aromatic, ring structures in which two of the rings are aromatic and ring structures in which three of the rings are non-aromatic. In each case, the non-aromatic rings when present in the monocyclic, bicyclic or tricyclic ring structure may independently be saturated, partially saturated or fully saturated. Examples of such carbocyclic ring structures include, but are not limited to, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, adamantyl, cyclooctyl, [3.3.0]bicyclooctane, [4.3.0]bicyclononane, [4.4.0]bicyclodecane (decalin), 2.2.2]bicyclooctane, fluorenyl, phenyl, naphthyl, indanyl, adamantyl, or tetrahydronaphthyl (tetralin). Moreover, the ring structures described herein may be attached to one or more indicated pendant groups via any carbon atom which results in a stable structure. The term “substituted” as used in conjunction with carbocyclic ring structures means that hydrogen atoms attached to the ring carbon atoms of ring structures described herein may be substituted by one or more of the substituents indicated for that structure if such substitution(s) would result in a stable compound.
[0046] The term “aryl” which is included with the term “carbocyclic ring structure” refers to an unsubstituted or substituted aromatic ring, substituted with one, two or three substituents selected from loweralkoxy, loweralkyl, loweralkylamino, hydroxy, halogen, cyano, hydroxyl, mercapto, nitro, thioalkoxy, carboxaldehyde, carboxyl, carboalkoxy and carboxamide, including but not limited to carbocyclic aryl, heterocyclic aryl, and biaryl groups and the like, all of which may be optionally substituted. Preferred aryl groups include phenyl, halophenyl, loweralkylphenyl, napthyl, biphenyl, phenanthrenyl and naphthacenyl.
[0047] The term “arylalkyl” which is included with the term “carbocyclic aryl” refers to one, two, or three aryl groups having the number of carbon atoms designated, appended to an alkyl group having the number of carbon atoms designated. Suitable arylalkyl groups include, but are not limited to, benzyl, picolyl, naphthylmethyl, phenethyl, benzyhydryl, trityl, and the like, all of which may be optionally substituted.
[0048] The terms “halo” or “halogen” as used herein refer to Cl, Br, F or I substituents. The term “haloalkyl”, and the like, refer to an aliphatic carbon radicals having at least one hydrogen atom replaced by a Cl, Br, F or I atom, including mixtures of different halo atoms. Trihaloalkyl includes trifluoromethyl and the like as preferred radicals, for example.
[0049] The term “methylene” refers to —CH 2 —.
[0050] Preferred Embodiments
[0051] In one embodiment the present invention relates to novel process for making in at least 70% enantiomeric purity a (3S, 4S, 6S) oxetanone compound of the formula (I),:
[0052] or a salt thereof
[0053] wherein:
[0054] R 1 and R 3 are each independently a C 1 to C 18 straight or branched alkyl hydrocarbon chain, and
[0055] R 2 is hydrogen or an alcohol protecting group R 10 , wherein R 10 can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, comprising the steps of:
[0056] (a) selectively hydrogenating a composition comprising a compound which is a member selected from the group consisting of (6R) tetrahydro-2H-pyran-2-one compound of formula (II) and (6R) 5,6-dihydro-2H-pyran-2,4-dione of formula (IIa):
[0057] wherein
[0058] R 5 is hydrogen or an alcohol protecting group, which can be replaced by a hydrogen atom via hydrogenation, and R 1 and R 3 are defined as in formula (I), by hydrogenating the compound of formula II with a hydrogenation catalyst selected from the group consisting of PtO 2 , Raney Nichel and the like, and exchanging hydrogen atoms at the 3 and 4 ring positions or oxidizing the 4-oxo group to provide a (3S, 4S, 6R) 4-hydroxy-tetrahydro-2H-pyran-2-one compound of the formula (III):
[0059] wherein R 1 and R 3 are defined as in formula (I);
[0060] (b) re-protecting the 4-hydroxy group of the compound of formula (II) produced in (a) with an ether protecting group R 6 , which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, opening the lactone ring and esterifying the resulting free acid group to provide a (2S, 3S, 5R) [R 7 ]2-[R 3 ]-3-[R 6- oxy]-5-[hydroxy,R 1 ] pentanoic acid ester compound of the formula (IV):
[0061] wherein
[0062] R 1 and R 3 are defined as in formula (I),
[0063] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and
[0064] R 7 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation;
[0065] (c) inverting the chirality of the 5-hydroxy group of the compound of formula (IV) produced in step (b), wherein the inversion comprises a step which is a member selected from the group consisting of
[0066] (i) a Mitsunobu reaction,
[0067] (ii) esterifying the 5-hydroxy group to a carboxylic acid ester such as the trichloroacetic acid ester, and the like, and hydrolyzing the resultant ester in a water ether solvent such as 3:1 H 2 O/dioxane, and
[0068] (iii) esterifying the 5-hydroxy group to a sulfonic acid ester, such as p-toluene sulfonic acid ester and the like, and reacting the ester with an excess of an organic acid salt selected from the group consising of potassium acetate, sodium acetate, tetraethylammonium acetate, and the like, to provide an ester exchange with the organic acid,
[0069] wherein the free inverted (5S) 5-hydroxy group of (i) and (ii) is esterified with a hydroxy protecting group R 10 which can be which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, to provide a compound of the formula (V):
[0070] wherein
[0071] R 1 and R 3 are defined as in formula (I),
[0072] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation,
[0073] R 9 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation, and
[0074] R 10 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and wherein R 10 is selectively removable with respect to the R 6 alcohol protecting group; and
[0075] (d) selectively removing the R 6 alcohol protecting group and R 9 ester group of the compound of formula (V) produced in (c), and cyclizing the 3 position alcohol group with the 1 position acid group using a lactone cyclizing catalyst, such as benzene-sulphonyl chloride, in a solvent such as pyridine at a temperature of about −10 to 10° C. and optionally replacing the R 10 alcohol protecting group of formula (V) with a hydrogen atom, to yield a (3S, 4S, 6S) oxetanone compound of the formula (I):
[0076] or a salt thereof.
[0077] In a preferred aspect, the process provides a compound of formula (I) wherein R1 is undecyl, R 3 is hexyl and R 2 is hydrogen, which is (2S, 3S, 5S) tetrahydroesterastin.
[0078] In another aspect the present invention relates to coupling such compound of formula (I) to an acyl compound via an acid or base esterification procedure without inversion of the 5S hydroxy group.
[0079] In another aspect the present invention provides a novel intermediate (2S, 3S, 5S) compound of the formula:
[0080] wherein:
[0081] R 1 and R 3 are each independently a C 1 to C 18 straight or branched alkyl hydrocarbon chain, and
[0082] R 2 is hydrogen or an alcohol protecting group R 10 , wherein R 10 can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and R 10 is selectively removable with respect to the R 6 alcohol protecting group,
[0083] R 6 is an alcohol protecting group, which can be replaced by a hydrogen atom via ester hydrolysis or hydrogenation ether degradation, and
[0084] R 9 is an ester group which can be removed by base or acid hydrolysis, or by hydrogenation, or, a salt thereof.
[0085] In a preferred aspect, the invention provide such intermediate compounds wherein R 1 is undecyl or heptadecyl and R 3 is ethyl or hexyl, or a salt thereof.
[0086] In a preferred aspect the above process comprises making a (3S, 4S, 6S) oxetanone compound of the formula (I), or a salt thereof, in at least 90% enantiomeric purity:
[0087] In another preferred aspect the present invention provides a process for making a compound wherein R 1 is undecyl or heptadecyl and R 3 is ethyl or hexyl in at least 90% enantiomeric purity:
[0088] In one aspect the invention provides a process wherein the compound of formula (II) in step (a) is present at a ratio of from 90 to 100% with respect to the corresponding (6S) enantiomer, and comprises the step of isolating such a compound of formula (II) in an enantiomeric excess of from 90 to 100% with respect to the corresponding (6S) enantiomer.
[0089] In a preferred aspect the invention provides a process wherein the compound of formula (II) in step (a) is present at a ratio of greater than 97% with respect to the corresponding (6S) enantiomer, and comprises the step of isolating such a compound of formula (II) in an enantiomeric excess of greater than 97% with respect to the corresponding (6S) enantiomer.
[0090] The present invention provides a process as described above, which further comprises isolating a compound which is a member selected from the group consisting of the 6R compound of formula (IV), or its corresponding (6R, 3RS, 4RS) racemate with an alcohol protected 3 hydroxyl group, from a compound which is a member selected from the 6S, 3R, 4R enantiomer with an alcohol protected 3 hydroxyl group corresponding to the compound in formula (IV) and a compound which is the (6S, 3RS, 4RS) racemate corresponding to the compound of formula (IV), comprising a separation step with is a member selected from the group consisting of:
[0091] (i) selectively esterifying the 6-position hydroxyl group in the presence of a lipase such as PS 30, porcine pancreas lipase, and the like, and separating the ester from the alcohol,
[0092] (ii) selectively hydrolyzing an ester an ester of the 6-position hydroxyl group via a lipase such as PS 30, porcine pancreas lipase, and the like, and separating the ester from the alcohol,
[0093] (iii) forming a chiral salt with a chiral alcohol resolving agent such as L-alaninol, D-alaninol, L-tartaric acid, D-tartaric acid, S-methylbenzyl-amine, D-methylbenzylamine in an appropriate solvent such as methyl acetate, and the like, and separating the two enantiomers by re-cyrstallization; and
[0094] (iv) other known chiral alcohol separating procedures,
[0095] and removing any ester or protecting groups from the 6R chiral hydroxyl group.
[0096] In another preferred aspect, the present invention provides such a process which further comprises the steps of
[0097] (a) inverting the 5S hydroxyl group of a (2R, 3R, 5S or 2RS, 3RS, 5S) [R 7 ]2-[R 3 ]-3-[R 6- oxy]-5-[hydroxy, R 1 ] pentanoic acid ester compound of the formula (VII):
[0098] wherein
[0099] R 1 , R 3 , R 6 and R 7 are defined as in formula IV;
[0100] wherein the inversion comprises a step which is a member selected from the group consisting of
[0101] (i) a Mitsunobu reaction, and freeing the hydroxyl group
[0102] (ii) esterifying the 5-hydroxy group to a carboxylic acid ester such as the trichloroacetic acid ester, and the like, and hydrolyzing the resultant ester in a water ether solvent such as 3:1 H 2 O/dioxane to the inverted hydroxyl group,
[0103] (iii) esterifying the 5-hydroxy group to a sulfonic acid ester, such as p-toluene sulfonic acid ester and the like, and reacting the ester with an excess of an organic acid salt selected from the group consising of potassium acetate, sodium acetate, tetraethylammonium acetate, and the like, to provide an ester exchange with the organic acid, and hydrolyzing the organic acid ester to the inverted hydroxyl group,
[0104] (iv) other known chiral alcohol inversion procedures,
[0105] (b) hydrolyzing the R 7 ester group to provide the free acid compound of the formula (VIII):
[0106] wherein
[0107] R 1 , R 3 and R 6 and R 7 are defined as in formula (VII), and
[0108] (c) cyclizing the inverted alcohol group of the compound of formula (VIII) with the 1 position acid group in the presence of a lactone cyclizing catalyst such as tonuene-4-sulfonic acid monohydrate in an alcohol at about 50-60° C. to provide a 6R tetrahydro-2H-pyran-2-one compound of formula (IX):
[0109] wherein
[0110] R 1 , R 3 , R 6 and R 7 are defined as in formula (VIII); and
[0111] (d) selectively hydrogenating the (6R) tetrahydro-2H-pyran-2-one compound of formula (IX) with a hydrogenation catalyst selected from the group consisting Of PtO 2 , Raney Nichel and the like, and exchanging hydrogen atoms at the 3 and 4 ring positions to provide a (3S, 4S, 6R) 4-hydroxy-tetrahydro-2H-pyran-2-one compound of the formula (IV):
[0112] wherein R 1 and R 3 are defined as in formula (I).
[0113] The intermediate compounds of formulae (II) and (IV) can be efficiently made from commercially feasible materials by adapting several methods known in the art and by refining the synthesis to avoid unnecessary or costly steps. Further, the following non-limiting reaction schemes, some steps of which are novel, are merely to exemplify the invention.
[0114] A process for making an intermediate compound for synthesizing a compound of the formula:
[0115] comprising the steps of:
[0116] treating dodecyl aldehyde (lauraldehyde) with a saturated aqueous solution of a bisufite such as sodium bisulfite to form a bisulfite salt of the formula:
[0117] (b) reacting the bisulfite salt with a 2-haloacetic acid R ester, such as 2 bromoacetic acid ethyl ester in a suitable solvent such as THF and water and in the presence of a catalytic amount of an acid such as HCl to produce a ketone derivative of the formula:
[0118] (c) reducing the ketone derivative with NaBH 4 , or the like, and optionally resolving the R and S enantiomer by forming an ester under chiral resolving conditions, such as esterifying the alcohol in the presence of the pseudomonas lipase PS 30 and the like, or by reducing the ketone carbonyl group with a chiral hydrogenation catalyst, at a temperature from 0° C. to 50° C. preferably at room temperature, in a suitable solvent, such as ethanol and the like, or reducing the ketone group with a chiral borane such as DIP—Cl (Aldrich) and protecting the alcohol with a protecting group (P1), such as t-butyldimethylsilyl by reaction with t-butyldimethylchlorosilane in dimethylformamide (DMF), to provide a compound of the formula:
[0119] (d) reacting the protected alcohol with at least one equivalent of a base such as NaOH followed by at least 1 equivalent of HCl to provide the free acid compound, and reacting the mono free acid with an acid reducing agent such as BF3-THF to produce the corresponding aldehyde of the formula:
[0120] (e) reacting the aldehyde with a 2-halogenoctanoate (such as ethyl 2-bromooctanoate) to produce a ketone compound of the formula:
[0121] (f) reducing the 3 ketone derivative with NaBH4, or the like, then removing the P 1 protecting group from the 5 hydroxy in a solvent such as an alcohol, e. g. , ethanol in the presence of an acid catalyst such as pyridinium-4-toluenesulphoneate or tetrabutylammonium fluoride trihydrate in THF while heating at about 50-65° C. followed by hydrogenating the ester group with hydrogen and Pd/C to yield the free acid diol as follows:
[0122] (g) and then cyclizing the 5R alcohol with the free acid to provide a 6R pyranolone ring by heating the free acid compound at a temperature from 50° C. to 60° C. in ethanol in the presence of toluene-4-sulfonic acid to provide a compound of the formula:
[0123] which may be utilized as the formula (II) compound described above.
[0124] Alternatively, the chiral ketone reducing agent utilized to reduce the beta oxo dodecanoic acid can be omitted to obtain a racemate. The racemate can be utilized as the formula (II) compound, followed by resolving the resulting (2S, 3S, 5R) formula (IV) enantiomer from its (2R, 3R, 5S) formula (VII) enantiomer.
[0125] Another process for making an intermediate compound for synthesizing a compound of the formula:
[0126] comprises the steps of:
[0127] (a) treating dodecyl halide (lauric acid chloride) with a N,O-dimethylhydroxyl-amine hydrochloride in a 1:1.5 ratio in acetonitrile, triethylamine and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and stirring at room temperature for about 5 hours to provide a compound of the formula:
[0128] (b) reacting the N-methoxymethyl amide carboxylic acid derivative with an organometallic salt of an acetic acid R ester (or a salt of a two halo acetic acid R ester), such as 2-lithium acetic acid ethyl ester in a suitable solvent such as dry THF under nitrogen or argon and the reaction is quenched with an acid such as HCl to produce a ketone derivative of the formula:
[0129] (c) forming the tetradecyl acyl halide (for example the acid chloride) of the ketone compound and reacting it with a N,O-dimethylhydroxyl-amine hydrochloride in a 1:1.5 ratio in acetonitrile, triethylamine and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and stirring at room temperature for about 5 hours to provide a compound of the formula:
[0130] (d) reacting the N-methoxymethyl amide carboxylic acid derivative with an alpha organometallic salt of an lower alkyl acid R ester (or a salt of an alpha halo lower alkyl acid R ester), such as 2-lithium octanoic acid ethyl ester in a suitable solvent such as dry THF under nitrogen or argon and quenching the reaction with an acid such as HCl, and the like to produce a 3,5 diketone derivative of the formula:
[0131] (e) reducing the 3,5 diketone acid derivative with NaBH 4 , or the like, to yield the free acid diol as follows:
[0132] and
[0133] (f) cyclizing the 5RS alcohol with the free acid to provide a 6R pyranolone ring by heating the free acid compound at a temperature from 50° C. to 60° C. in ethanol in the presence of toluene-4-sulfonic acid to provide a compound of the formula:
[0134] which may be utilized as the formula (II) compound described above.
[0135] Alternatively, the diketone reduction step of step (e) can be conducted with a chiral borane reducing to obtain a (2RS, 3R, 5R) which when cyclized provides the (3RS, 4R, 6R) compound, which can be utilized as the formula (II) compound.
[0136] A further process for making an intermediate compound for synthesizing a compound of the formula:
[0137] comprises the steps of:
[0138] (a) reacting methyl 2-acetyloctanoate (Aldrich 10887) with a organometallic base, such as butyllithium salt to deprotonate the tertiary carbon atom of the 2-acetyl group,
[0139] (b) reacting the lithium organometallic salt in a suitable solvent such as THF with a lauric acid halide (dodecoyl chloride) of the formula:
[0140] to provide a 3,5 diketone compound of the formula:
[0141] (c) reducing the 3,5 diketone acid derivative with NaBH 4 , or the like, to yield the free acid diol as follows:
[0142] and
[0143] (d) cyclizing the 5RS alcohol with the free acid to provide a 6R pyranolone ring by heating the free acid compound at a temperature from 50° C. to 60° C. in ethanol in the presence of toluene-4-sulfonic acid to provide a compound of the formula:
[0144] which may be utilized as the formula (II) compound described above.
[0145] Alternatively, the diketone reduction step of step (c) can be conducted with a chiral borane reducing agent to obtain a (2RS, 3R, 5R) which when cyclized provides the (3RS, 4R, 6R) compound, which can be utilized as the formula (II) compound.
[0146] In one aspect of the present invention, there is provided a chiral alcohol resolution process step which incorporates a lipase to hydrolyze esters of the intermediate alcohols, or to be present during an esterification step, wherein the lipase may be a lipase such as the pseudomonas PS 30, pig pancreas lipase, and the like.
[0147] The (2S, 3S, 5S) oxetanone compounds provided by the processes according to the invention may be linked to other compounds or a support by esterifying with an acyl, acyl halide, or by a transesterification process. In a preferred embodiment the lipase inhibitiors according to the invention are linked via a terminal ether/terminal ester bridge, to a oil or lipid absorbable polymer moiety. Preferably, the free 5-hydroxyl (2S, 3S, 5S) compounds are linked under acidic conditions to a polysaccharide such as chitosan, which polysaccharide has been modified to have an acyl, or acyl halide attachment group.
[0148] Non-limiting examples of preferred bridges between the lipase inhibitor oxetanone moiety produced according to the present invention and the polymer moiety includes at least one ether bridge formed from an alcohol group on the polymer moiety and at least one ester or carboxamide bond between the 5-hydroxy group of the oxetanone. Further preferred is a process for producing a compound wherein at least one amino acid derivative is located in the bridge, and is bound directly or indirectly to the 5 hydroxyl position on the 1,3 oxetanone moiety via an ester linkage.
[0149] The preferred compounds produced from such linkage with a polysaccharide also includes their pharmaceutically acceptable isomers, hydrates, solvates, salts and prodrug derivatives.
[0150] A preferred aspect of the present invention relates to a process for making novel oxetanone derivatives of the formula Ia, as follows:
[0151] wherein:
[0152] t is an integer from 0 to 1
[0153] X-O-Q is an ether linkage wherein:
[0154] X of the ether linkage is a bridging group, and
[0155] Q of the ether linkage is a polysaccharide of a sufficient molecular weight or property that such polysaccharide is not absorbed by the digestive system of a mammal such as a dog, cat, non-human primate or a human primate, which polysaccharide is further defined below;
[0156] R 1 and R 3 is defined as in formula (I) of the (2S, 3S, 5S) 5-hydroxyl oxetanone compounds, produced by a process according to the invention as described above,;
[0157] R 1a is a member selected from the group consisting of:
[0158] Hydrogen,
[0159] Ar,
[0160] Ar—C 1-5 -alkyl and
[0161] C 1-10 -alkyl interrupted by 0-3 members independently selected from the group consisting of an oxygen atom, a sulfur atom, a sulfinyl group, a sulfonyl group, a-N(—R 4a )— group, a —C(═O)—N(—R 4a )— group, and a —N(—R 4a )—C(═O)— group, wherein 0-3 carbon atoms of the C 1-10 -alkyl group can be substituted independently by a member selected from the group consisting of a hydroxy group, thiol group, C 1-10 -alkoxy group, a C 1-10 -alkylthio group, a —N(—R 5a ,—R 6a ) group, a —C(═O)—N (—R 7a , —R 8a ) group and a —N(—R 9a )—C(═O)—R 10a group;
[0162] R 2a is a member selected from the group consisting of:
[0163] hydrogen and C 1-6 -alkyl, or R 2a taken with R 1a forms a 4-6 membered saturated ring containing 0-4 nitrogen atoms wherein the ring may be substituted by 0-4 R 11 groups;
[0164] R 4a -R 10a are each independently a member selected from the group consisting of:
[0165] hydrogen and C 1-6 -alkyl;
[0166] n is an integer of 0-3;
[0167] and all pharmaceutically acceptable isomers, salts, hydrates, solvates and prodrug derivatives thereof.
[0168] A preferred compound according to formula Ia is a compound wherein X is a member selected from the group consisting of:
—(C(═O)) 0-1 —X a —,
[0169] wherein X a is a member selected from the group consisting of:
[0170] a straight or branched chained divalent C 1-17 -alkylene group which is saturated or optionally interrupted by up to eight double or triple bonds;
[0171] a straight or branched chained divalent C 1-17 -alkylene group which is saturated or optionally interrupted by one or more members selected from the group consisting of:
[0172] an oxygen atom,
[0173] a sulfur atom,
[0174] a sulfonyl group,
[0175] a sulfinyl group,
[0176] a substituted or unsubstituted 6-10 member monocyclic or bicyclic aryl or heteroaryl group having from 1-4 ring hetero atoms selected from the group consisting of O, N, S,
[0177] a —NH— group, wherein the hydrogen atom may be replaced with a C 1-10 alkyl group
[0178] a —C(═O)— group,
[0179] a —NH—C(═O)— group, wherein the hydrogen atom may be replaced with a C 1-10 alkyl group and
[0180] a —C(═O)—NH— group, wherein the hydrogen atom may be replaced with a C 1-10 alkyl group
[0181] a straight or branched chained divalent C 1-17 -alkylene group which is saturated or optionally interrupted by up to eight double or triple bonds and is interrupted in a position other than alpha to an unsaturated carbon atom by one or more members selected from the group consisting optionally interrupted by one or more members selected from the group consisting of:
[0182] an oxygen atom,
[0183] a sulfur atom,
[0184] a sulfonyl group,
[0185] a sulfinyl group,
[0186] a substituted or unsubstituted 6-10 member monocyclic or bicyclic aryl or heteroaryl group having from 1-4 ring hetero atoms selected from the group consisting of O, N, S,
[0187] a —NH— group, wherein the hydrogen atom may be replaced with a C 10 alkyl group
[0188] a —C(═O)— group,
[0189] a —NH—C(═O)— group, wherein the hydrogen atom may be replaced with a C 1-10 alkyl group and
[0190] a —C(═O)—NH— group, wherein the hydrogen atom may be replaced with a C 1-10 alkyl group
[0191] divalent phenylene or divalent naphthylene substituted on the ring structure by 0-4 members selected from the group consisting of —C 1-6 -alkyloxy-C 1-6 -alkyl, —C 1-6 -alkylthio-C 1-6 -alkyl, —C 1-6 -alkyl-OH and —C 1-6 -alkyl-SH; divalent biphenylene substituted by 0-6 members selected from the group consisting of —C 1-6 -alkyloxy-C 1-6 -alkyl, —C 1-6 -alkylthio-C 1-6 -alkyl, —C 1-6 -alkyl-OH and —C 1-6 -alkyl-SH;
[0192] phenoxyphenylene substituted by 0-6 members selected from the group consisting of —C 1-6 -alkyloxy-C 1-6 -alkyl, —C 1-6 -alkylthio-C 1-6 -alkyl, —C 1-6 -alkyl-OH and —C 1-6 -alkyl-SH;
[0193] divalent phenylthiophenylene substituted by 0-6 members selected from the group consisting of —C 1-6 -alkyloxy-C 1-6 -alkyl, —C 1-6 -alkylthio-C 1-6 -alkyl, —C 1-6 -alkyl-OH and —C 1-6 -alkyl-SH; and
[0194] and all pharmaceutically acceptable isomers, salts, hydrates, solvates and prodrug derivatives thereof.
[0195] More preferred is compound according to formula Ia wherein X is a member selected from the group consisting of:
—(C(═O))—X a —,
[0196] and X a is a member selected from the group consisting of:
[0197] a straight or branched chained divalent C 1-17 -alkylene group which is saturated or optionally interrupted by up to eight double or triple bonds.
[0198] Further preferred are compounds according to formula Ia, wherein R 1 is undecyl, R 3 is hexyl,R 1a is straight or branched chain C 1 -C 8 alkyl, R 2a is hydrogen and X is a member selected from the group consisting of:
—(C(═O))—X a —,
[0199] and Xa is a member selected from the group consisting of divalent saturated C 5 -C 18 alkylene, and more preferably, Xa is a divalent saturated pentylene or undecylene group, or a salt thereof.
[0200] Preparation of Compounds
[0201] The lipase inhibitor compounds, polymer moieties and bridging groups of the present invention may be synthesized or readily obtained from commercially available sources. Preferably, the (2S, 3S, 5S) 5-hydroxyl oxetanone lipase inhibitor compounds are obtained by a process as described above. Polymer bridging groups, bridge coupling processes and compound purification methods are described and referenced in standard textbooks, particularly the coupling of alcohol groups via diether bridges, ether/ester bridges, ether/ketone bridges and the like. Standard polymer textbooks reference typical bifunctional bridging groups and coupling procedures.
[0202] Starting materials used in any of these methods are commercially available from chemical vendors such as Aldrich, Sigma, Nova Biochemicals, Bachem Biosciences, and the like, or may be readily synthesized by known procedures.
[0203] Reactions are carried out in standard laboratory glassware and reaction vessels under reaction conditions of standard temperature and pressure, except where otherwise indicated.
[0204] During the synthesis of these compounds, the functional groups may be protected by blocking groups to prevent cross reaction during the coupling procedure. Examples of suitable blocking groups and their use are described in “The Peptides: Analysis, Synthesis, Biology”, Academic Press, Vol. 3 (Gross, et al., Eds., 1981) and Vol. 9 (1987), the disclosures of which are incorporated herein by reference. Alcohol and ester protecting group may also be utilized.
[0205] Lipase inhibitor moieties having a free hydroxy group such as the oxetanones described above, and the like, are easily coupled to a polymer moiety having free hydroxy groups such as cellulose, chitosan and other polysaccharides having free hydroxyl groups. One or both of the lipase inhibitor moiety and the polymer moiety may be derivitized to form part of the linking bridge prior to reacting with the other moiety. For example, a desired number of the hydroxy groups of the polysaccharides, such as chitosan, may be functionalized with a compound having a terminal acyl or ester group such as 6-bromohexanoic acid, 12-bromododecanoic acid, and the like, or an ester derivative of such acids, and subsequently the 5-hydroxyl group of the oxetanone lipase inhibitor molecule may be condensed with the ester group or a terminal acyl group (the acyl group may be modified with an halide group to an acyl halide group, such as the acyl chloride) to form an ester linkage with the ether bridged polymer moiety as shown in polysaccharide chemistry. In one procedure a polymer moiety such as chitosan can be reacted with a compound such as a halomethylbenzoic acid ester, loweralkyl 6-bromohexanoic acid, lower alkyl 12-bromododecanoic acid, or the like, and de-esterified to present a free acid group which may be, activated further by forming the acyl halider, and reacted with a terminal portion of the lipase inhibitor (which may have been esterified with a bridging compound which has a functional group capable of reacting with an ester or acyl group) to form an ester, ketone, or carboxamide with the optionally derivitized lipase inhibitor moiety.
[0206] In one preferred aspect of the invention, one of the two moieties is reacted with an asymmetrical halide/acyl bridging group, such as a terminal halide alkanoic acid of 1:1 to etherize a free hydroxyl group, replace a hydrogen atom on an amino group, or foom a ketone with an acid group, and the resulting intermediate can then be reacted with the an alcohol or amino moiety to form an ester group or a carboxamide group with a free alcohol group, or by replacing a nitrogen atom on a amino group. Particularly preferred polymer moieties are polysaccharides having multiple free hydroxyl group which after coupling may optionally be sulfonated to render the lipase moiety itself a lipase inhibitor compound. Etherification, amination and ketone formation procedures are well-known in the art and well within the routine skill of the ordinary practitioner. Further, other bridging groups and the techniques for binding a compound having a reactive functional group to a polymer moiety are well-known in the art. The preferred compounds also include their pharmaceutically acceptable isomers, hydrates, solvates, salts and prodrug derivatives.
[0207] The bridging group refers to a bifunctional chain or spacer group capable of reacting with one or more functional groups on a lipase inhibitor compound and then react with a second same or different functional group on a polymer compound in order to form a linked structure or conjugate between the two compounds. The bond formed between the bridging group and each of the two compounds is preferably of a type that is resistant to cleavage by the digestive environment, other than to inhibit a lipase by binding substantially irreversibly.
[0208] By appropriate selection of the type of bridging group reactant, different structural groups with various chemical properties can be incorporated into the resulting bridge and various types of lipase inhibitors can be connected to a nonabsorbable polymer moiety, such as a polysaccharide, and preferably to chitosan. Reaction temperatures and other reactions conditions, as well are reactant proportions are well within the skill of the ordinary polymer chemist practitioner. Other groups and modifications will be apparent to one of ordinary skill in the art from the above discussion.
[0209] The lipase inhibitor functionality of the coupled lipase inhibitors may be determined by well-known lipase inhibitor assays. A therapeutically effective amount of the bound lipase inhibitor may be administered to a patient. Additional fat binding polymers may optionally be added to the composition.
[0210] The following non-limiting reaction Schemes I, II, III and IV illustrate preferred embodiments of the invention with respect to making compounds according to the invention.
[0211] Such chitosan derivatives provide a lipase inhibitor with very low absorption rates, and at such rates tetrahydroesterastin is not known to be substantially toxic.
[0212] Dosage formulations of the compounds of this invention to be used for therapeutic administration must be sterile. Sterility is readily accomplished by filtration through sterile membranes such as 0.2 micron membranes, or by other conventional methods. Formulations typically will be stored in lyophilized form or as an aqueous solution. The pH of the preparations of this invention typically will be between 3 and 11, more preferably from 5 to 9 and most preferably from 7 to 8. It will be understood that use of certain of the foregoing excipients, carriers, or stabilizers will result in the formation of cyclic polypeptide salts. While the preferred route of administration is by oral tablets, capsules or other unit dose mechanisms, such as liquids, other methods of administration are also anticipated such as in food stuffs, employing a variety of dosage forms. The compounds of this invention are desirably incorporated into food articles which may include fats to prevent their absorption.
[0213] The compounds of this invention may also be coupled with suitable polymers to enhance their therapeutic effects. Such polymers can include lipophilic polymers, such as polysaccharides and the like.
[0214] Therapeutically effective dosages may be determined by either in vitro or in vivo methods. For each particular compound of the present invention, individual determinations may be made to determine the optimal dosage required. The range of therapeutically effective dosages will naturally be influenced by the route of administration, the therapeutic objectives, and the condition of the patient. For routes of administration, the lipase inhibitor activity, in view of the amount of fat consumed, must be individually determined for each inhibitor by methods well known in pharmacology. Accordingly, it may be necessary for the therapist to titer the dosage and modify the route of administration as required to obtain the optimal therapeutic effect. The determination of effective dosage levels, that is, the dosage levels necessary to achieve the desired result, will be within the ambit of one skilled in the art. Typically, applications of compound are commenced at lower dosage levels, with dosage levels being increased until the desired effect is achieved.
[0215] Typically, about 500 mg to 3 g of a lipase inhibitor compound or mixture of lipase inhibitor compounds of this invention, as the free acid or base form or as a pharmaceutically acceptable salt, is compounded with a physiologically acceptable vehicle, carrier, excipient, binder, preservative, stabilizer, dye, flavor etc., as called for by accepted pharmaceutical practice. The amount of active ingredient in these compositions is such that a suitable dosage in the range indicated is obtained. The addition, one or more other therapeutic ingredients such as a fat absorbing polysaccharide or fiber, a fat-specific lipase inhibitor or lipase, as well as other dietary agents may be utilized in therapeutically effective amounts.
[0216] Typical adjuvants which may be incorporated into tablets, capsules and the like are a binder such as acacia, corn starch or gelatin, and excipient such as microcrystalline cellulose, a disintegrating agent like corn starch or alginic acid, a lubricant such as magnesium stearate, a sweetening agent such as sucrose or lactose, or a flavoring agent. When a dosage form is a capsule, in addition to the above materials it may also contain a liquid carrier such as water, saline, a fatty oil. Other materials of various types may be used as coatings or as modifiers of the physical form of the dosage unit. Sterile compositions for injection can be formulated according to conventional pharmaceutical practice. Buffers, preservatives, antioxidants and the like can be incorporated according to accepted pharmaceutical practice.
[0217] In practicing the methods of this invention, the compounds of this invention may be used alone or in combination, or in combination with other therapeutic or diagnostic agents. In certain preferred embodiments, the compounds of this inventions may be coadministered along with other compounds typically prescribed for these conditions according to generally accepted medical practice, such as other weight control or lipase inhibitory products, cholesterol controlling drugs, and the like.
[0218] The compounds of this invention can be utilized in vivo, ordinarily in mammals such as non-human primates, humans, sheep, horses, cattle, pigs, dogs, cats, rats and mice, or in vitro.
[0219] The following non-limiting examples are provided to better illustrate the present invention.
EXAMPLE 1
Production of mixed hexyl 3-oxo-tetradecanoate esters
[0220] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, under argon is added a suspension 140 g of sodium hydride in 6 L of THF. The temperature is lowered to 0-5° C. and maintained as 1 Kg of mixed hexyl acetic acid esters (Aldrich 461253) are slowly added to this suspension with stirring. After one hour of stirring the mixture is cooled −10° C. and 1.25 Kg of 24% w/wn-Butyllithium (n-BuLi) (about 5 mol) in 3 L of hexane is added. After stirring at this temperature for 45 minutes, the flask is then cooled to below −15° C. followed by slowly adding 575 g of ethyl dodecanoate (Aldrich L4625). This solution is allowed to warm to −10° C. with stirring and is stirred at this temperature for 1 hour. The reaction solution is added under argon 1.25 L of 40% hydrochloric acid and 1.5 Kg of ice. The mixture is extracted twice with 5 L of hexane and water. The organic phases are combined, dried over magnesium sulfate, filtered, and the organic solvents are evaporated at reduced pressure to provide a solid residue (about 1.4 Kg).
EXAMPLE 2
Production of (3R) 3-hydroxy-tetradecanoic acid
[0221] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle, cooling apparatus, and vacuum system, under argon is added 8 mols (2.6 Kg) of (+)-β-chlorodiisopinocamphenylborane (“+-DIP—Cl”). To this was added 4 L of dry THF at room temperature over one hour. Once the mixture is dissolved together the temperature is lowered to −25° C. While maintaining the temperature between −20 and −25° C. the 1.4 Kg of mixed hexyl 3-oxo-tetradecanoate esters (Example 1) in 2 L of dry THF is slowly added with stirring (over a one hour period) to this solution. The reaction temperature is maintained between −10 and −20° C. for 8 hours and the reaction progress is monitored with HPLC. After the 8 hours, the temperature is allowed to gradually warm to about −5° C. and after 1 hour at this new temperature is allowed to warm to 0° C. in order to increase the rate of reaction. The reaction process is monitored by HPLC and the reaction is stopped after all the starting material is consumed. To the reaction mixture is slowly added 3 L of water (over a one hour period) while maintaining the reaction temperature below 10° C. About 4 L of methanol is then added, followed by 4 L of aqueous 5 M NaOH. The mixture is stirred at room temperature and the reaction is monitored by HPLC until it is complete (about two hours). The reaction mixture is allowed to separate and the aqueous layer is removed. The aqueous layer is extracted with hexane and the separated aqueous layer is neutralized with HCl, saturated with NaCl and extracted 3 times with 3×1 L of with warm hexane. The hexane layers are combined and concentrated by evaporation of the solvent at reduced pressure to provide a crude product which is dried over magnesium sulfate to provide about 1.3 Kg of solid.
EXAMPLE 3
Production of (3R)-3-benzoyloxy-tetradecanoyl chloride
[0222] To a 20 L 3-neck round bottom flask equipped with a mechanical stirrer, nitrogen inlet, reflux condenser, heating mantle, vacuum system, and scrubber system for efficient removal of HCl and SO 2 gases liberated during the reaction, is charged under nitrogen 15 moles of benzoic acid anhydride, 10 moles of concentrated anhydrous HCl in 4 L of THF, and 7.48 moles of the (3R)-3-hydroxy-tetradecanoic acid obtained from Example 1, above. The stirred mixture is placed under a N 2 flow, which is vented to the scrubber system. The stirred mixture is heated to reflux for 3 hours during which the reaction becomes complete. The resulting solution is neutralized with 1N NaOH and the organic layer is separated from the aqueous layer. The aqueous layer is washed with THF and the resulting organic portions are combined, placed under vacuum and THF is removed. The resulting solid is dissolved in warm hexane, cooled and worked up to provide the product (3R)-3-benzoyloxy-tetradecanoyl chloride in about 95% yield.
EXAMPLE 4
Production of 5R ethyl 5-benzoyloxy-2-hexyl-3-oxo-hexadecanoate ester
[0223] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, under argon is added a suspension 140 g of sodium hydride in 6 L of THF. The temperature is lowered to 0-5° C. and maintained as 1 Kg of ethyl octanoate (Aldrich 112321) is slowly added to this suspension with stirring. After one hour of stirring the mixture is cooled −10° C. and 1.25 Kg of 24% w/wn-Butyllithium (n-BuLi) (about 5 mol) in 3 L of hexane is added. After stirring at this temperature for 45 minutes, the flask is then cooled to below −15° C. followed by slowly adding 575 g of the (3R) 3-benzoyloxy-tetradecanoyl chloride from Example 3. This solution is allowed to warm to −10° C. with stirring and is stirred at this temperature for 1 hour. The reaction solution is added under argon 1.25 L of 40% hydrochloric acid and 1.5 Kg of ice. The mixture is extracted twice with 5 L of hexane and water. The organic phases are combined, dried over magnesium sulfate, filtered, and the organic solvents are evaporated at reduced pressure to provide a solid residue (about 1 Kg).
EXAMPLE 5
Production of 5R 3,5-dihydroxy-2-hexyl-hexadecanoic acid
[0224] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, under argon 6 L of anhydrous THF is added and 1 Kg of 5R ethyl 5-benzoyloxy-2-hexyl-3-oxo-hexadecanoate ester is dissolved while gassing with argon, treated with 250 mL of MeOH and cooled to −5° C. Then 825 g of sodium borohydride is slowly added in portions with stirring in a manner that permits the temperature to not exceed 0° C. After stirring for 3 hours the excess sodium borohydride is filtered off, the reaction mixture is hydrolyzed (to about pH 6) with cold 2N hydrochloric acid at 0° C. The mixture is allowed to warm to room temperature and the solvent was evaporated off under vacuum. The residue is extracted twice with ether and the ether phases are combined and concentrated under vaccum. The crude concentrate is added to a solution of THF and aqeuous KOH and stirred at 35° C. for three hours. The organic phase is separated, washed twice with cold water, dried over MgSO 4 and evaporated under reduced pressure. There is obtained about 1 Kg of 5R 3,5-dihydroxy-2-hexyl-hexadecanoic acid.
EXAMPLE 6
Production of (6R) 5,6-dihydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one
[0225] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, is charged under argon with 6 L of anhydrous toluene and the 1.3 Kg of product from Example 5 is slowly added to the solution with stirring pyridium para-toluenesulfonate and refluxed under argon for 2 hours to form the lactone. The reaction mixture is cooled to room temperature and washed twice with a saturated aqueous sodium carbonate solution. The organic phases are combined and evaporated under vacuum at about 40° C. to produce a product, and warm hexane is added to the product to dissolve it into a homogenous mixture. The warm hexane mixture is cooled to room temperature with stirring. The mixture is then cooled to −10° C. and stirred at that temperature for 15 hours. The crystalline solid is then filtered under suction. The filter cake is washed with cold hexane and dried over magnesium sulfate. The crystals are then dried overnight in a drier to remove any remaining solvent. About 1 Kg of (6R) 5,6-dihydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one, having a m.p. of 106-108° C. is provided.
EXAMPLE 7
Production of (3S, 4S, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one
[0226] A hydrogenator is purged twice with nitrogen and charged with the 1 Kg of product from Example 6, which is dissolved in 6 L of anhydrous ethyl acetate, and 500 g of PtO 2 is added. The hydrogenator is purged twice with hydrogen and then charged with hydrogen at 50 bar. The temperature is raised to 40° C. and hydrogen flow is maintained at 50 bar for 12 hours. The catalyst is filtered off and the solution is evaporated. After dissolving in warm hexane, the product is cooled to 0° C. overnight and recrystallized to yield 900 g of (3S, 4S, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one, having a m.p. of 108-109° C.
EXAMPLE 8
Production of (3S, 4S, 6R) tetrahydro-3-hexyl-4-[(tetrahydro-2H-pyran-2-yl)oxy]-6-undecyl-2H-pyran-2-one
[0227] The 900 g of (3S, 4S, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one of Example 7, and 500 ml of freshly distilled 3,4-dihydro-2H-pyran are dissolved in 10 L of methylene chloride and cooled to about 3° C. and 9.6 g of p-toluenesulfonic acid monohydrate are added. The temperature rises to about 8° C. and the mixture is stirred at this temperature until the reaction is finished. The reaction mixture is washed with a mixture of 4 L of saturated aqueous sodium chloride solution, 4 L of saturated aqueous sodium hydrogen carbonate solution and 8 L of water. After drying the mixture over MgSO 4 the mixture is filtered and the solvent is removed. The resulting residue is utilized in the next step without further purification of the (3S, 4S, 6R) tetrahydro-3-hexyl-4-[tetrahydro-2H-pyran-2-yl) oxy]-6-undecyl-2H-2-one.
EXAMPLE 9
Production of benzyl (2S, 3S, 5R) 2-hexyl-5-hydroxy-3-[(tetrahydro-2H-pyran-2-yl)oxy]-hexadecanoic acid ester
[0228] The product of Example 8 is dissolved in 6 L of THF under argon and anhydrous conc. sulphuric acid is added which is warmed to 30° C. and stirred for two hours. A metallic salt of benzyl alcohol (sodium salt) in an aqueous solution is slowly added in a 1:1.2 molar excess with respect to the hexadecanoic acid ester. The mixture is stirred for 4 hours at 25° C. the pH is then adjusted to 9 with NaOH, and the aqueous layer and organic layer are separated. The organic layer is extracted twice with 4 L of cold H 2 O, and the organic layer is dried over magnesium sulfate. The resulting benzyl (2S, 3S, 5R) 2-hexyl-5-hydroxy-3-[(tetrahydro-2H-pryan-2-yl)oxy] hexadecanoic acid ester is used in the next step without purification.
EXAMPLE 10
Production of benzyl (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-3-[(tetrahydro-2H-pyran-2-yl)oxy]-hexadecanoic acid ester
[0229] The product of Example 9, triphenylphosphine (1.5 Kg) and benzoic acid (600 g) are dissolved in 6 L of THF, and to the resultant solution, is added a solution of 800 g of diethyl azodicarbonate in 1 L of THF. The mixture is stirred at room temperature for 15 hours, and reaction mixture is concentrated under reduced pressure. The concentrate is dissolved in warm hexane/THF and the mixture is extracted with water and a saturated NaCl solution. The organic phase is dried over magnesium sulfate and the solvent is distilled off under vacuum to provide a concentrate containing benzyl (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-3-[(tetrahydro-2H-pyran-2-yl)oxy]-hexadecanoic acid ester which is used in the next step without purification.
EXAMPLE 11
Production of (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-3-[(tetrahydro-2H-pyran-2-yl) oxy]-hexadecanoic acid
[0230] The benzyl ester of Example 10 is dissolved in anhydrous 5 L of THF and HCl is added in an equimolar amount with respect to the benzyl ester. Under argon the ester is hydrogenated at room temperature for three hours by stirring the solution in the presence of Pd/C 10%. The solution is filtered and the catalyst is washed with THF, the washings are combined with the reaction mixture and the reaction mixture is neutralized with aqueous IN NaOH. The organic layer is separated, dried over MgSO 4 and the solvent is evaporated under vacuum to provide a crude composition of(2S, 3S, 5S) 5-benzoyloxy-2-hexyl-3-[(tetrahydro-2B-pyran-2-yl)oxy]-hexadecanoic acid, which is used in the next step without further purification.
EXAMPLE 12
Production of (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-4-hydroxyhexadecanoic 1,3 -lactone, i.e., (3S,4S) 3-hexyl-4-[(S) 2-benzoyloxytridecyl]-2-oxetanone
[0231] 500 g of the hexadecanoic acid of Example 11 is dissolved in 6 L of anhydrous ethanol and 30 g of toluene-4-sulfonic acid anhydride is added. The temperature of the reaction mixture is raised to 60° C. with stirring and maintained at 55-65° C. until the reaction is finished. The solvent is removed under vacuum and the residue is dissolved in warm hexane. The mixture is stirred for 2 hours cooled to -10° C. and allowed to stand overnight at 0° C. The crystals are removed from the solvent by filtration and washed with cold hexane to yield the compound (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-4-hydroxyhexadecanoic 1,3-lactone.
EXAMPLE 13
Production of (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone, i.e., (3S, 4S) 3hexyl-4-[(S) 2-hydroxytridecyl]-2-oxetanone
[0232] 200 g of the (2S, 3S, 5S) 5-benzoyloxy-2-hexyl-4-hydroxyhexadecanoic 1,3-lactone of Example 12 is suspended in a 4 L solution containing 0.01 N sodium hydroxide dissolved in a mixture of water-dioxane (1:1), and the resulting mixture is stirred at about 25° C. for about 12 hours to effect the hydrolysis of the benzoyloxy group to an alcohol group. The rection mixture is extracted 3 times with 2 L portions of hexane and the extracts are combined. After concentration of the extracts to dryness the solid is dissolved in warm hexane, cooled to 0° C. and stirred for 2 hours. The mixture is seeded with pure (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone crystals and the mixture is allowed to sit overnight at 0° C. The crystals are filtered, washed with cold hexane and dried to produce about 125 g of (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone, i.e., (3S, 4S) 3-hexyl-4-[(S) 2 -hydroxytridecyl]-2-oxetanone.
EXAMPLE 14
Production of ethyl 3,5-di-oxo-2-hexyl-hexadecanoate ester
[0233] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, under argon is added a suspension 140 g of sodium hydride in 6 L of THF. The temperature is lowered to 0-5° C. and maintained as 1 Kg of methyl 2-acetyloctanoate (Aldrich 10887) is slowly added to this suspension with stirring. After one hour of stirring the mixture is cooled −10° C. and 1.25 Kg of 24% w/wn-Butyllithium (n-BuLi) (about 5 mol) in 3 L of hexane is added. After stirring at this temperature for 45 minutes, the flask is then cooled to below −15° C. followed by slowly adding 575 g of ethyl dodecanoate (Aldrich L4625). This solution is allowed to warm to −10° C. with stirring and is stirred at this temperature for 1 hour. The reaction solution is added under argon 1.25 L of 40% hydrochloric acid and 1.5 Kg of ice. The mixture is extracted twice with 5 L of hexane and water. The organic phases are combined, dried over magnesium sulfate, filtered, and the organic solvents are evaporated at reduced pressure to provide a solid residue (about 1.4 Kg).
EXAMPLE 15
Production of (3R, 5R) ethyl 3,5-di-hydroxy-2-hexyl-hexadecanoate ester
[0234] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle, cooling apparatus, and vacuum system, under argon is added 8 mols (2.6 Kg) of (+)-β-chlorodiisopinocamphenylborane (“+-DIP—Cl”). To this was added 4 L of dry THF at room temperature over one hour. Once the mixture is dissolved together the temperature is lowered to −25° C. While maintaining the temperature between −20 and −25° C. the 1.4 Kg of ethyl 3,5-dioxo-tetradecanoate ester (Example 14) in 2 L of dry THF is slowly added with stirring (over a one hour period) to this solution. The reaction temperature is maintained between −10 and −20° C. for 8 hours and the reaction progress is monitored with HPLC. After the 8 hours, the temperature is allowed to gradually warm to about −5° C. and after 1 hour at this new temperature is allowed to warm to 0° C. in order to increase the rate of reaction. The reaction process is monitored by HPLC and the reaction is stopped after all the starting material is consumed. To the reaction mixture is slowly added 3 L of water (over a one hour period) while maintaining the reaction temperature below 10° C. About 4 L of methanol is then added, followed by 4 L of aqueous 5 M NaOH. The mixture is stirred at room temperature and the reaction is monitored by HPLC until it is complete (about two hours). The reaction mixture is allowed to separate and the aqueous layer is removed. The aqueous layer is extracted with hexane and the separated aqueous layer is neutralized with HCl, saturated with NaCl and extracted 3 times with 3×1 L of with warm hexane. The hexane layers are combined and concentrated by evaporation of the solvent at reduced pressure to provide a crude product which is dried over magnesium sulfate to provide about 1.3 Kg of solid.
EXAMPLE 16
Production of (4R, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one
[0235] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, is charged under argon with 6 L of anhydrous toluene and the 1.3 Kg of product from Example 15 is slowly added to the solution with stirring pyridium para-toluenesulfonate and refluxed under argon for 2 hours to form the lactone. The reaction mixture is cooled to room temperature and washed twice with a saturated aqueous sodium carbonate solution. The organic phases are combined and evaporated under vacuum at about 40° C. to produce a product, and warm hexane is added to the product to dissolve it into a homogenous mixture. The warm hexane mixture is cooled to room temperature with stirring. The mixture is then cooled to −10° C. and stirred at that temperature for 15 hours. The crystalline solid is then filtered under suction. The filter cake is washed with cold hexane and dried over magnesium sulfate. The crystals are then dried overnight in a drier to remove any remaining solvent. About 1 Kg of (4R, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one, having a m.p. of 95-96° C. is provided.
EXAMPLE 17
Production of (3S, 4S, 6R) tetrahydro-4-benzoyloxy-3-hexyl-6-undecyl-2H-pyran-2-one
[0236] A hydrogenator is purged twice with nitrogen and charged with the 1 Kg of product from Example 9 dissolved in 6 L of anhydrous ethyl acetate and 500 g of PtO 2 is added. The hydrogenator is purged twice with hydrogen and then charged with hydrogen at 50 bar. The temperature is raised to 40° C. and hydrogen flow is maintained at 50 bar for 12 hours. The catalyst is filtered off and the solution is evaporated. After dissolving in warm hexane, the product is cooled to 0° C. overnight and recrystallized to yield 900 g of (3S, 4S, 6R) tetrahydro-3-hexyl-4-hydroxy-6-undecyl-2H-pyran-2-one, having a m.p. of 108-109° C.
EXAMPLE 18
Production of (6S, 6R) 5,6 dihydro-3-hexyl-6-undecyl-2H-pyran-2,4-dione
[0237] To a 20 L 3-neck flask equipped with a mechanical stirrer, argon inlet, reflux condenser, heating mantle and vacuum system, is charged under argon with 6 L of anhydrous acetone and 1 Kg of a (6S, 6R) racemic product prepared in a similar manner to the compound of Example 6, but from a (5R, 5S) racemic mixture of the compound described in Example 5. The temperature is lowered to about 20° C. and 1 L of Jones' reagent (chromic acid/conc. H 2 SO 4 in acetone) is slowly added to the solution with stirring at an addition speed to maintain the temperature at less than 25° C. After addition of all of the Jones' reagent the mixture is stirred for 3 hours at 25° C. After completion of the reaction, the reaction mixture is poured into 15 L of H 2 O. The lactone precipitates out and is filtered off. After dissolving filter cake in a warm ether/n-hexane solvent, the mixture is cooled and recrystallized to obtain 750 g of (6R) 5,6-dihydro-3-hexyl-6-undecyl-2H-pyran-2,4-dione, having a m.p. of 112.5-113.5° C.
EXAMPLE 19
Enzymatic resolution of (6S, 6R) 5,6 dihydro-3-hexyl-6-undecyl-2H-pyran-2,4-dione
[0238] The compound of Example 18 is hydrogenated with Raney Nickil in substantially the same manner as the procedure of Example 7, and the 4 hydroxy group of the resulting compound is protected with a tetrahydro-2H-pyran-2-yl ether group substantially as described in Example 8. The lactone ring is opened substantially as described in Example 9, and the 5R, 5S hydroxy group chirality is reversed with an ester group which is sufficiently polar to render the compounds soluble in a basic aqueous solvent by using shown the general procedures shown in Example 10. The benzyl alcohol group is removed from the acid group by hydrogenation as described in Example 11 and the resulting free acid 5S and 5R enantiomers are resolved in a basic aqueous medium by using a lipase such as PS 30, pig liver lipase and the like.
[0239] After 45 to 48% of the total 5 hydroxy esters have been cleaved (about 90% of the 5S compounds) by the lipase, the insoluble 5S hydroxy compounds are separated from the reaction mixture and washed with water. Also, the remaining reaction mixture is filtered to remove the lipase, and the lipase mass is washed with water which is added to the aqueous filtrte. The aqueous filtrate is set aside for further resolution.
[0240] The separated 5S hydroxy compounds, the aqueous insoluble portion are esterified with an excess of benzoic acid using the esterification procedures in an acidic H 2 SO 4 and THF solvent. After completion of the esterification, the organic solution is washed with water, and separated from the aqueous layer. The procedures of Examples 11 and 12 are followed to yield the (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone.
EXAMPLE 20
Recycling filtrate esters (greater than 90% 2R, 3R, 5R enantiomer) from the lipase separation
[0241] The aqueous filtrate from Example 20 is obtained and stirred in 1 N NaOH at 30° C. for 3 hours, neutralized with HCl and extracted with hexane. The hexane portions are combined and the solvent is evaporated. The procedures of Example 11 are followed to provide the compound (3R, 4R, 6R) 5,6-dihydro 3-hexyl-4-[(tetrahydro-2H-pyran-2-yl)oxy ]-undecanyl-2H-pyran-2-one, which can be recycled through the processes of Examples 7-13 to produce a composition having greater than 90-95% of the yield the (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone. Combining this 1,3 lactone product with the product of Example 19 provide a composition having greater than 95 to 97% of the (2S, 3S, 5S) 3,5-dihydroxy-2-hexylhexadecanoic 1,3-lactone.
EXAMPLE 21
[0242] 10 grams of low viscosity chitosan (less than 500 cPs, readily available commercially, e.g., ChitoClear™ by Primex) which is greater than 95% deacylated chitin is dissolved in a 500 milliliter flask equipped with a stirrer thermometer and electrical heater, in a mixture of 190 g of dimethylsulfoxide and 10 g of paraformaldehyde, at 50° C. At this temperature, after the addition of 0.1 g of finely powdered sodium hydroxide, a solution of 1 g of 12-bromo-dodecanoic acid ethyl ester in 10 g of dimethylsolfoxide is added over a period of about 30 minutes. The mixture is stirred for four hours at 50° C. The reaction mixture is cooled to room temperature, then poured into ethanol while the latter is being stirred vigorously. The solid is suction filtered, suspended repeatedly in ethanol until all the soluble substances are removed to yield a crude product. The crude product is stirred in an aqueous basic 1 N sodium hydroxide ethanol solution, which is then acidified with HCl until neutral pH for chitosan. The solid is washed twice with cold ethanol and cold water, and the solid is then dried to yield about 10 grams of ether functionalized chitosan. Analysis indicates that from 1% to 3% of the free hydroxyl groups on the chitosan polymeric backbone are etherified by the entry of the 12-dodecanoic acid group.
EXAMPLE 22
[0243] A colorless power of (2S, 3S, 5S) 3,5-dihydroxy-2-hexyl-hexadecanoic 1,3-lactone (6 g), produced as in Example 13 above (or as described on pages 11 and 12 of U.S. Pat. No. 4,202,824) is dissolved in 500 mL of THF to which is added Boc-(L) 2-amino-4-methylpentanoic acid chloride (3 g, Boc-(L)-Leucine). The reaction mixture is stirred and heated to reflux until HPLC indicates that the esterification is essentially complete. The organic phase is evaporated and the residue purified by chromatography on silica gel with toluene-ethyl acetate to yield 5-[Boc-(L) 2-amido-4-methylvaleryloxy]-2-hexyl-hexadecanoic 1,3-lactone (6 g).
EXAMPLE 23
[0244] The BOC group of the product (6 mg) of Example 2 is removed by hydrogenation at room temperature in 120 mL of THF in the presence of 10% Pd/C. After hydrogenation is completed, the catalyst is filtered off and the filtrate is evaporated to yield a crude free amino group product, which is taken up in 100 mL of THF. The functionalized chitosan product produced in Example 1 which has been converted to the acyl chloride derivative is taken up in 200 mL of THF and stirred while the crude free amino product is added dropwise at room temperature under argon. The mixture is gradually heated to 40° C. with stirring until HPLC indicates the formation of the carboxamide linked product. Yielded is 5-[2-{(4-chitosan methyl ether) benzoylamido}-4-methylvaleryloxy]-2-hexyl-hexadecanoic 1,3-lactone (about 15 grams).
EXAMPLE 24
[0245] A colorless power of (2S, 3S, 5S) 3,5-dihydroxy-2-hexyl-hexadecanoic 1,3-lactone (6 g), produced as in Example 13 above (or as described on pages 11 and 12 of U.S. Pat. No. 4,202,824) is dissolved in 500 mL of THF and 25 mL of anhydrous HCl to which is added the acyl chloride derivative of the compound of Example 21 (10 g). The reaction mixture is stirred and heated to reflux until HPLC indicates that the esterification is essentially complete. The organic phase is separated from the aqueous phase and the solvent is evaporated. The resulting product is washed with warm hexane and with water to provide funtionalized chitosan linked to the (2S, 3S, 5S) 3,5-dihydroxy-2-hexyl-hexadecanoic 1,3-lactone as an ester derivative of the 5S hydroxy group (15 g).
[0246] In view of the above description it is believed that one of ordinary skill can practice the invention. The examples given above are non-limiting in that one of ordinary skill in view of the above will readily envision other permutations and variations on the invention without departing from the principal concepts. Such permutations and variations are also within the scope of the present invention.
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This invention relates to novel processes for making (2S, 3S, 5S) oxetanone derivative lipase inhibitor compounds and intermediates therefor, which processes for producing such derivatives that are useful as lipase inhibitors are capable of being scaled to commercial quantities. Further the invention relates to processes for producing salts and for producing pharmaceutical compositions compounds comprising at least one such oxetanone derivative or salt, as well as methods for using such compounds and compositions for inhibiting lipases.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of co-pending U.S. application Ser. No. 14/258,823 filed Apr. 22, 2014, which claims the benefit of and priority to U.S. application Ser. No. 12/945,353 filed Nov. 12, 2010, now U.S. Pat. No. 8,748,519, which claims the benefit of and priority to U.S. Provisional Patent Application No. 61/261,209 filed Nov. 13, 2009, the entire disclosures of which are incorporated by reference herein.
BACKGROUND
[0002] Many polymers used in packaging materials and other articles are permeable to oxygen. When oxygen permeates a polymeric composition or article, it can cause oxidative damage to the contents of the package. It is therefore desirable for certain polymer compositions and articles to have oxygen scavenging capability, such that when oxygen permeates the composition or article, oxidative damage can be mitigated.
[0003] It is known in the art to include an oxygen scavenger in the packaging structure for the protection of oxygen sensitive materials. Such scavengers are believed to react with oxygen that is trapped in the package or that permeates from outside of the package, thus extending to life of package contents. These packages include films, bottles, containers, and the like. Food, beverages (such as beer and fruit juices), cosmetics, medicines, and the like are particularly sensitive to oxygen exposure and require high barrier properties to oxygen to preserve the freshness of the package contents and avoid changes in flavor, texture and color.
[0004] Conventional polymeric materials suffer from a lack of oxygen scavenging moieties in the polymeric structures. In various aspects, the disclosed compositions provide for this need as well as other needs.
SUMMARY
[0005] In accordance with the purpose(s) of the invention, as embodied and broadly described herein, the invention, in one aspect, relates to oxygen scavenging polymers.
[0006] Disclosed are thermoplastic polymers comprising an allylic or benzylic amide compound covalently bonded thereto as a repeating unit in the polymer chain, covalently bonded thereto as a pendant group, or covalently bonded thereto as an end group of the polymer.
[0007] Also disclosed are compositions comprising the disclosed polymers.
[0008] Also disclosed are articles prepared from the disclosed polymers and compositions.
[0009] Also disclosed are methods of making oxygen scavenging polymers.
[0010] Also disclosed are the products of the disclosed methods.
[0011] Additional advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or can be learned by practice of the invention. The advantages of the invention will be realized and attained by means of the elements and combinations particularly pointed out in the appended claims. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is a plot illustrating oxygen scavenging ability of a the polymer composition prepared according to Example 2.
DETAILED DESCRIPTION
[0013] The present invention can be understood more readily by reference to the following detailed description of the invention and the Examples included therein.
[0014] Before the present compounds, compositions, articles, systems, devices, and/or methods are disclosed and described, it is to be understood that they are not limited to specific synthetic methods unless otherwise specified, or to particular reagents unless otherwise specified, as such may, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular aspects only and is not intended to be limiting. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, example methods and materials are now described.
[0015] Disclosed are the components to be used to prepare the compositions of the invention as well as the compositions themselves to be used within the methods disclosed herein. These and other materials are disclosed herein, and it is understood that when combinations, subsets, interactions, groups, etc. of these materials are disclosed that while specific reference of each various individual and collective combinations and permutation of these compounds can not be explicitly disclosed, each is specifically contemplated and described herein. For example, if a particular compound is disclosed and discussed and a number of modifications that can be made to a number of molecules including the compounds are discussed, specifically contemplated is each and every combination and permutation of the compound and the modifications that are possible unless specifically indicated to the contrary. Thus, if a class of molecules A, B, and C are disclosed as well as a class of molecules D, E, and F and an example of a combination molecule, A-D is disclosed, then even if each is not individually recited each is individually and collectively contemplated meaning combinations, A-E, A-F, B-D, B-E, B-F, C-D, C-E, and C-F are considered disclosed. Likewise, any subset or combination of these is also disclosed. Thus, for example, the sub-group of A-E, B-F, and C-E would be considered disclosed. This concept applies to all aspects of this application including steps in methods of making and using the compositions of the invention. Thus, if there are a variety of additional steps that can be performed it is understood that each of these additional steps can be performed with any specific embodiment or combination of embodiments of the methods of the invention.
[0016] As used in the specification and the appended claims, the singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to “a functional group,” “an alkyl,” or “a residue” includes mixtures of two or more such functional groups, alkyls, or residues, and the like.
[0017] Ranges can be expressed herein as from “about” one particular value, and/or to “about” another particular value. When such a range is expressed, another aspect includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent “about,” it will be understood that the particular value forms another aspect. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint. It is also understood that there are a number of values disclosed herein, and that each value is also herein disclosed as “about” that particular value in addition to the value itself. For example, if the value “10” is disclosed, then “about 10” is also disclosed. It is also understood that each unit between two particular units are also disclosed. For example, if 10 and 15 are disclosed, then 11, 12, 13, and 14 are also disclosed.
[0018] Disclosed herein are thermoplastic polymers having covalently linked thereto a benzylic or allylic amide compound which can function as an oxygen scavenger in a polymeric composition. A variety of different thermoplastic polymers can be used. Generally, polymers that exhibit at least some oxygen permeability can be used, at least inasmuch as the disclosed compositions can reduce the oxidative damage to the polymer. The polymer can be a polymer commonly used in packaging materials including most thermoplastic polymers, including polyethylene, such as low density polyethylene, very low density polyethylene, ultra-low density polyethylene, high density polyethylene, linear low density polyethylene, and polypropylene; polyesters such as (PET), (PEN) and their copolymers such as PET/IP; polyvinyl chloride (PVC); polyvinylidene chloride (PVDC); and ethylene copolymers such as ethylene/vinyl acetate copolymer, ethylene/alkyl (meth)acrylate copolymers, ethylene/(meth)acrylic acid copolymers, and ionomers. Blends of different base polymers also can be used. In a further aspect, the polymer comprises a polyester polymer or copolymer. Preferred polyesters include polymers of phthalic acids, such as polyethylene terephthalate (PET), or a copolymer thereof.
[0019] Generally, the benzylic or allylic amide compound is attached to the polymer through one or more polymer end groups or is actually part of the polymer backbone itself. In a first aspect, the polymer is a polyester or copolyester having covalently attached thereto a benzylic or allylic amide compound. Generally, the amide compound that is covalently attached to the polymer is an N-allylic amide compound or N-benzylic amide compound. The amide compound is useful as an oxygen scavenger in the composition. The oxygen scavenging ability of the amide compound can be enhanced by the transition metal.
[0020] N-allylic or N-benzylic amide compounds have the general structure shown below:
[0000]
[0000] wherein each independently denotes an optional covalent bond.
[0021] It is also appreciated that an N-allylic or N-benzylic amide compound can be further substituted and that more than one amide functionality can be present in a compound. In one aspect, an N-allylic or N-benzylic amide compound can be polymeric. In a further aspect, an N-allylic or N-benzylic amide compound can be nonpolymeric.
[0022] The benzylic amide compound or allylic amide compound can have a variety of functional groups that will enable the compound to be attached to the polymer through an endgroup of the polymer or through the polymer backbone itself.
[0023] In one aspect, the amide compound has a structure of Formula I or II:
[0000]
[0000] wherein the symbol when used in conjunction with a bond line represents a single or a double bond; wherein n is 3, 4, 5, or 6; wherein m is an integer from 0 to 6-n; wherein each X is independently selected from the group consisting of O, S, and NH; wherein each Y, each A, and each B are independently selected from the group consisting of N, CR 1 , and CR 2 ; wherein D, E, and F are independently selected from the group consisting of CH, N, O, and S; and wherein each R 1 and each R 2 is independently selected from the group consisting of carboxylic acid, amine, nitro, cyano, hydroxyl, H, alkyl, aryl, electron withdrawing groups, electron releasing groups, and a transition metal.
[0024] In one aspect, the compound of formula I or II can be represented by the following formula:
[0000]
[0025] In a further aspect, the compound has a structure of Formula III or Formula IV:
[0000]
[0000] wherein the symbol when used in conjunction with a bond line represents a single or a double bond; wherein each n is independently 1-5; wherein m is an integer from 0 to 5-n; wherein each X is independently selected from the group consisting of O, S, and NH; wherein each Y, each A, and each B are independently selected from the group consisting of N, CR 1 , and CR 2 ; wherein D, E, and F are independently selected from the group consisting of CH, N, O, and S; wherein each R 1 and each R 2 is independently selected from the group consisting of carboxylic acid, amine, nitro, cyano, hydroxyl, H, alkyl, aryl, electron withdrawing groups, electron releasing groups, and a transition metal; and wherein L is a divalent linking group selected from C2-C12 aliphatic or cyclic ether, C2-C12 aliphatic or cyclic amide, C6 to C12 aromatic amide, C2-C12 aliphatic or cyclic amine, C6-C12 aromatic amine, C2-C12 aliphatic or cyclic ester and C6 to C12 aromatic ester.
[0026] In a further aspect, the compound has a structure of Formula V or Formula VI:
[0000]
[0000] wherein the symbol when used in conjunction with a bond line represents a single or a double bond; wherein each n is independently 0-5; wherein m is an integer from 0 to 5-n; wherein each X is independently selected from the group consisting of O, S, and NH; wherein each Y, each A, and each B are independently selected from the group consisting of N, CR 1 , and CR 2 ; wherein D, E, and F are independently selected from the group consisting of CH, N, O, and S; wherein each R 1 and each R 2 is independently selected from the group consisting of carboxylic acid, amine, nitro, cyano, hydroxyl, H, alkyl, aryl, electron withdrawing groups, electron releasing groups, and a transition metal; and wherein L is a divalent linking group selected from C2-C12 aliphatic or cyclic ether, C2-C12 aliphatic or cyclic amide, C6 to C12 aromatic amide, C2-C12 aliphatic or cyclic amine, C6-C12 aromatic amine, C2-C12 aliphatic or cyclic ester and C6 to C12 aromatic ester.
[0027] Generally, linking group L is a divalent organic residue. Suitable linking groups L include divalent aliphatic chains, divalent aliphatic or cyclic ethers, divalent aliphatic or cyclic amides, divalent aromatic amide, divalent aliphatic or cyclic amines, divalent aromatic amines, divalent aliphatic or cyclic esters and divalent aromatic esters, such as those exemplified in Table 1 below. As used in the table below, the term “tether compound” refers to a difunctional organic compound capable of reactions with ring substitutents of disclosed moieties to form covalent bonds, thereby chemically connecting the ring substitutents via a divalent organic residue of the tether compound, referred to as a linking group, L. Examples of tether compounds include dielectrophilic compounds (e.g., diacyl halides, cyclic anhydrides, and bis-alkyl halides) for linking nucleophilic ring substituents (e.g., hydroxides, thiols, and amines). Further examples of tether compounds include dinucleophilic compounds (e.g., bis-hydroxides, bis-thiols, and bis-amines) for linking electrophilic ring substituents (e.g., acyl halides and alkyl halides). Selected examples are illustrated structurally in Table 1.
[0000]
TABLE 1
L
Ring Substituent
Tether Compound
[0028] In Table 1 above, R is an optionally substituted divalent organic residue; for example, R can be selected from optionally substituted alkyl or alkenyl or alkynyl, optionally substituted heteroalkyl or heteroalkenyl or heteroalkynyl, optionally substituted cycloalkyl or cycloalkenyl or cycloalkynyl, optionally substituted heterocycloalkyl or heterocycloalkenyl or heterocycloalkynyl, optionally substituted aryl, and optionally substituted heteroaryl. In further aspects, R can be linear, cyclic, or branched. Typically, R has from 1 to 48 carbons, from 1 to 24 carbons, from 1 to 12 carbons, from 1 to 8 carbons, from 1 to 6 carbon, or from 1 to 4 carbons.
[0029] In further aspects, R′ is an optionally substituted organic residue. Typically, R′ has from 1 to 12 carbons, from 1 to 8 carbons, from 1 to 6 carbon, or from 1 to 4 carbons. For example, R′ can be methyl, ethyl, propyl, butyl, pentyl, or hexyl.
[0030] It is also contemplated that the functional groups selected for use in fabricating L can be used in combinations other than those shown in the Table. For example, in a further aspect, L can be:
[0000]
[0031] Linking groups L can be readily prepared by methods known to those of skill in the art of organic synthesis.
[0032] In one aspect, the amide compound has a structure of Formula VII:
[0000]
[0000] wherein each X is selected from the group consisting of O, S, and NH; wherein each Y, each A, and each B are independently selected from the group consisting of N and CR 1 ; wherein D, E, and F are independently selected from the group consisting of CH, N, O, and S; wherein the symbol when used in conjunction with a bond line represents a single or a double bond; and wherein each R 1 is independently selected from the group consisting of H, alkyl, aryl, electron withdrawing groups, and electron releasing groups.
[0033] In a further aspect, the amide compound has a structure of Formula VIII:
[0000]
[0000] wherein each X is selected from the group consisting of O, S, and NH; wherein each Y, each A, and each B are independently selected from the group consisting of N and CR 2 ; wherein D, E, and F are independently selected from the group consisting of CH, N, O, and S; wherein the symbol when used in conjunction with a bond line represents a single or a double bond; and wherein each R 2 is independently selected from the group consisting of H, alkyl, aryl, electron withdrawing groups, and electron releasing groups.
[0034] The alkyl groups R1 or R2 of the compound of Formulae (I-VIII) can be a branched or unbranched saturated hydrocarbon group of 1 to 24 carbon atoms, e.g. 1 to 18 carbons atoms, 1 to 14 carbon atoms, 1 to 12 carbon atoms, 1 to 10 carbon atoms, 1 to 8, 1 to 6 carbon atoms, or 1 to 4 carbon atoms, such as methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, t-butyl, pentyl, hexyl, heptyl, octyl, decyl, tetradecyl, hexadecyl, eicosyl, tetracosyl and the like. The alkyl group can be substituted or unsubstituted. The alkyl group can be substituted with one or more groups including, but not limited to, alkyl, halogenated alkyl, alkoxy, alkenyl, alkynyl, aryl, heteroaryl, aldehyde, amino, carboxylic acid, ester, halide, hydroxamate, hydroxy, ketone, nitro, silyl, sulfo-oxo, sulfonyl, sulfone, sulfoxide, or thiol, as described below. The alkyl group can be halogenated, which includes an alkyl group that is substituted with one or more halide, e.g., fluorine, chlorine, bromine, or iodine. The alkyl group can also be a lower alkyl group, which is an alkyl group containing from one to six (e.g., from one to four) carbon atoms.
[0035] The aryl groups R1 or R2 of the compound of Formulae (I-VIII) can be any carbon-based aromatic group including but not limited to, benzene, naphthalene, phenyl, biphenyl, etc. The aryl group can also be heteroaryl, which is defined as an aromatic group that has at least one heteroatom incorporated within the ring of the aromatic group. Examples of heteroatoms include, but are not limited to, nitrogen, oxygen, sulfur, and phosphorus. The aryl group can be substituted or unsubstituted. The aryl group can be substituted with one or more groups including, but not limited to, alkyl, halogenated alkyl, alkoxy, alkenyl, alkynyl, aryl, heteroaryl, aldehyde, amino, carboxylic acid, ester, halide, hydroxamate, hydroxy, ketone, nitro, silyl, sulfo-oxo, sulfonyl, sulfone, sulfoxide, or thiol as described herein. A biaryl group is a specific type of aryl group and is included in the definition of aryl. Biaryl refers to two aryl groups that are bound together via a fused ring structure, as in naphthalene, or are attached via one or more carbon-carbon bonds, as in biphenyl.
[0036] Suitable electron withdrawing groups and electron releasing groups are generally known in the art. Preferred electron withdrawing groups include nitro, carboxylic acid, esters, for example loweralkyl esters, and cyano. Preferred electron releasing groups include branched and straight chain alkyl groups, for example, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, and tert-butyl. Other preferred electron releasing groups include alkoxy, for example methoxy and ethoxy. Other preferred electron releasing groups include thioalkyl. Still other preferred electron releasing groups include amines, for example —NH 2 , and NH(loweralkyl), and N(loweralkyl) 2 .
[0037] Oxygen scavenging amide compounds are disclosed in U.S. Patent Application Publication No. 20080277622, Deshpande et al. “Oxygen Scavenging Molecules, Articles Containing Same, And Methods of Their Use,” which is incorporated herein by this reference for its teaching of amide compounds, their preparation, and their use as oxygen scavenging materials. Many of the amide compounds disclosed in U.S. Patent Application Publication No. 20080277622 can be covalently attached to the end of a polymer, such as a PET polyester, or actually copolymerized with a polymer and thereby be incorporated into the polymer backbone itself.
[0038] The compound of Formulae (I-VIII) can be attached to a thermoplastic polymer through any atom and can be attached as a side-chain, end group, or as a repeating unit in the polymer backbone itself. In one aspect, amide compounds of the formulae above can be attached to a polymer, such as a polyester, through an endgroup of the polyester. Typically, this can be accomplished by reacting one of the functional groups of the amide compound, for example one or more of R 1 or R 2 groups, with the alcohol, carboxylic acid, or ester end group of the polyester. The compounds above can also be copolymerized with one or more polyester monomers, for example, if the amide compound comprises two carboxylic acid or alcohol functional groups at either end of the molecule.
[0039] To provide specific illustrations of the polymers and how to make the polymers, the following non-limiting examples are provided. As discussed above, a PET polymer can be functionalized at one or more endgroups with a benzylic amide according to Scheme 1. It will be appreciated that such a synthetic approach can be used for a variety of different benzylic or allylic amide compounds.
[0000]
[0040] According to Scheme 1, a benzylic amide compound can be prepared according to method analogous to those disclosed in U.S. Patent Application Publication No. 20080277622, discussed above. Subsequently the benzylic amide can be functionalized to a PET polymer through the carboxy terminus through a typical coupling reaction, such as a peptide coupling reaction, employing for example, a carbodiimide and a base. The resulting polymer therefore has a benzylic amide compound at its endgroup which can function as an internal oxygen scavenger in a composition comprising the polymer.
[0041] Another example of this approach is outlined in Scheme 2, wherein a different benzylic amide compound can be attached to the endgroup of a PET polymer. In this case, the amide compound is again functionalized to the PET through its carboxy terminus. The resulting polymer can be attached to yet another PET polymer through the carboxy end of the benzylic amide compound. Such a strategy can be useful, for example, when trying to alter the molecular weight of the PET polymer.
[0000]
[0042] In another aspect, as discussed above, the benzylic or allylic amide compound can be incorporated into the polymer backbone itself. Such a polymer can be made, for example, according to Scheme 3. As shown, terephthalic acid, ethylene glycol, and a benzylic amide compound can be copolymerized under typical conditions for preparing polyesters.
[0000]
[0043] In another example, a star type polymer can be produced using a trimeric or higher or benzylic or allylic amide compound. For example, as shown in Scheme 4, terephthalic acid can be copolymerized with ethylene glycol and a trimeric benzylic amide compound having three carboxylic acid groups. The resulting polymer will be a branched, star-type polymer as shown.
[0000]
[0044] Polyesters such as PET can be prepared by polymerization procedures known in the art sufficient to effect esterification and polycondensation. Polyester melt phase manufacturing processes include direct condensation of a dicarboxylic acid with a diol, optionally in the presence of one or more esterification catalysts, in the esterification zone, followed by polycondensation in the prepolymer and finishing zones in the presence of a polycondensation catalyst; or ester exchange usually in the presence of a transesterification catalyst in the ester exchange zone, followed by prepolymerization and polymerization in the presence of a polycondensation catalyst.
[0045] Also disclosed are compositions and articles made therefrom comprising the polymer having the benzylic amide or allylic amide compound covalently bonded thereto. Generally, the amide compound is present in the composition in an amount of from 0.1 to about 10 weight percent. Thus, the desired amount of amide compound to be incorporated into the polymer can be adjusted to achieve the desired amide compound weight percent in the final composition or article. In one aspect, the amide compound is present in the composition in an amount of from 1 to about 10 weight percent. In a further aspect, the amide compound is present in the composition in an amount of from 1 to about 5 weight percent. In a further aspect, the amide compound is present in the composition in an amount of from 1 to about 3 weight percent.
[0046] The amide compound can in certain aspects be complexed to the transition metal of the composition. For example, the amide compound can be complexed to the transition metal through one or more aryl groups, for example through pi-cloud complexation. The amide compound can also be polymerized via complexation to the transition metal.
[0047] The composition comprises the transition metal in a positive oxidation state. The transition metal enhances the oxygen scavenging properties of the amide compound. Amounts of transition metal in the composition can be greater than zero and can be up to 5000 ppm. Generally, the transition metal will be present in an amount of from about 10 ppm to about 400 ppm. In one aspect, about 200 ppm of the transition metal is present. In a further aspect, about 250 ppm of the transition metal is present. In wall applications (as opposed to master batch applications where more transition metal is used), it can be preferred to keep the level of metal below 300, more preferably 250 ppm. In a further aspect, the transition metal is present from 30 to 150 ppm. In a further aspect, about 50 ppm of the transition metal is present. In a further aspect, about 100 ppm of the transition metal is present. In a further aspect, about 150 ppm of the transition metal is present.
[0048] In one aspect, the transition metal can be a transition metal from the first, second, or third transition series of the Periodic Table. The metal can be Rh, Ru, or one of the elements in the series of Sc to Zn (e.g., Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, and Zn). In one aspect, the transition metal is cobalt. Cobalt can be used in +2 or +3 oxidation states. In some aspects, it is preferred to use cobalt in the +2 oxidation state. In a further aspect, the transition metal is rhodium. For example, rhodium in the +2 oxidation state can be used. The transition metal can also be a positive oxidation form of zinc.
[0049] The transition metal can be present as a salt. The cation of the salt can be the transition metal in a positive oxidation state. A variety of anions can stabilize the positively charged transition metal. Suitable anions for the salts include, but are not limited to, chloride, acetate, oleate, stearate, palmitate, 2-ethylhexanoate, carboxylates, such as neodecanoates, octanoates, acetates, lactates, naphthalates, malates, stearates, acetylacetonates, linoleates, oleates, palmitates, 2-ethylhexanoates, or ethylene glycolates; or as their oxides, borates, carbonates, dioxides, hydroxides, nitrates, phosphates, sulfates, or silicates, among others. Representative transition metal salts include cobalt (II) 2-ethylhexanoate, cobalt oleate, and cobalt (II) neodecanoate. The transition metal salt also can be an ionomer, in which case a polymeric counter ion can be present.
[0050] In one aspect, the composition can comprise a colorant in a visually effective amount. A visually effective amount refers to an amount of colorant that results in the composition or an article made therefrom appear colored to the naked eye. A composition comprising a visually effective amount of colorant can refer to a composition having at least 0.01% by weight colorant. In a further aspect, the composition can comprise at least 0.25% by weight colorant. In a still further aspect, the composition can comprise at least 0.5% by weight colorant. The compositions can also comprise up to or even exceed about 3% by weight colorant.
[0051] A visually effective amount can be determined, for example, by performing a spectrophotometric scan of the composition or article using a wavelength range from 400 to 700 nm (visible region). Specific colors can be characterized according to their spectral pattern. Every color also has its own characteristic L (lightness gradation), a (red to green) and b (yellow to blue) numbers, which can be used to characterize the compositions and articles.
[0052] The colorant can be a variety of pigments and dyes, many of which are commercially available. Examples of colorants include without limitation COLORMATRIX Dark Amber, product code: 189-10034-6, COLORMATRIX Dead Leaf Green, product codes: 284-2801-3 and 84-2801-1, AMERICHEM amber, product code: 59108-CD1, Champaigne green, and COLORMATRIX amber, product code: 189-10100-1.
[0053] The composition can include other components such as fillers, crystallization aids, impact modifiers, surface lubricants, denesting agents, stabilizers, ultraviolet light absorbing agents, metal deactivators, nucleating agents such as polyethylene and polypropylene, phosphate stabilizers and dyestuffs. Typically, the total quantity of such components will be less than about 10% by weight of the composition. In some embodiments, the amount of these optional components is less than about 5% by weight of the composition.
[0054] The composition can comprise a reheat additive. Reheat additives are commonly used in the manufacture of polyester polymer compositions used to make stretch blow molded bottles because the preforms made from the composition must be reheated prior to entering the mold for stretch blowing into a bottle. Any conventional reheat additive can be used, such as various forms of black particles, e.g., carbon black, activated carbon, black iron oxide, glassy carbon, silicon carbide, gray particles such as antimony, and other reheat additives such as silicas, red iron oxide, and the like.
[0055] The composition can also comprise an impact modifier. Examples of typical impact modifiers useful in the composition include ethylene/acrylate/glycidyl terpolymers and ethylene/acrylate copolymers in which the acrylate is a methyl or ethyl acrylate or methyl or ethyl methacrylate or the corresponding butyl acrylates, styrene based block copolymers, and various acrylic core/shell type impact modifiers. The impact modifiers can be used in conventional amounts from about 0.1 to about 25 weight percent of the overall composition and, in some aspects, in amounts from about 0.1 to about 10 weight percent of the composition.
[0056] In many applications, not only are the packaging contents sensitive to the ingress of oxygen, but the contents may also be affected by UV light. Fruit juices and pharmaceuticals are two examples of such contents. Accordingly, in some aspects, it is desirable to incorporate into the composition a UV absorbing compound in an amount effective to protect the packaged contents.
[0057] The composition or an article made therefrom preferably has an Oxygen Transmission Rate (OTR) of less than about 0.1 (units of cc/pkg/day or 1-5 cc-mm/m 2 -day-atm) under standard conditions. In a further aspect, the OTR can be less than 0.03, less than 0.01, less than 0.005, or less than 0.001. The OTR is a measure of how well the amide compound functions at scavenging oxygen that permeates the composition or article.
[0058] When OTR is expressed for a given composition or article, the units “cc/package/day” (“cc/pkg/day”) are typically employed. The term package refers to a bather between an atmosphere of relatively lower oxygen content and an atmosphere of relatively higher oxygen content. Typical barriers (e.g., packages) include bottles, thermoformed containers, and films (e.g., shrink wrap).
[0059] Oxygen Transmission Rate (oxygen permeation) can be measured, for example, as described in U.S. Pat. No. 5,021,515. A material of area A can be exposed to a partial pressure p of oxygen on the one side and to an essentially zero partial pressure of oxygen on the other side. The quantity of oxygen emerging on the latter side is measured and expressed as a volume rate dV/dt, the volume being converted to some standard condition of temperature and pressure. After a certain time of exposure (usually a period of a few days) dV/dt is generally found to stabilize, and a P W value can be calculated from equation below.
[0000] dV/dt=P W Ap (1)
[0060] P W refers to the permeance of the wall. (Analogy with magnetic permeance and electrical conductance would suggest that P W should be described as “permeance per unit area”, but we are following the nomenclature in Encyclopaedia of Polymer Science and Technology, Vol. 2, Wiley Interscience, 1985, page 178.) The standard conditions for expressing dV/dt are 0° C. and 1 atm (1 atm=101 325 Nm −2 ). If the thickness of the area of wall is substantially constant over the area A with value T and the wall is uniform through the thickness (i.e., the wall is not a laminated or coated one) then the permeability of the material in the direction normal to the wall is calculated from the equation below.
[0000] dV/dt=P M Ap/T (2)
[0061] For non-scavenging materials, P W and P M are to a reasonable approximation independent of t and p, and P M of T although they are often appreciably dependent on other conditions of the measurement such as the humidity of the atmosphere on the oxygen-rich side and the temperature of the measurement.
[0062] For oxygen-scavenging walls, P W and P M are functions of t because the concentrations and activity of scavenger vary with time (particularly as the scavenger is consumed). This typically does not prevent measurement of P W and P M reasonably accurately as a function of time, because the changes in dV/dt are relatively gradual once the normal initial equilibration period of a few days is over. After a few days' exposure to the measurement conditions, however, a non-scavenging material typically achieves a steady state in which dV/dt is equal to the rate of oxygen ingress to the wall, while a scavenging material achieves an (almost) steady state in which dV/dt is considerably less than the rate of oxygen ingress to the material. This being the case, it is likely that P W calculated from (1) is a function of p as well as of t and that P M in (2) is a function of p and T as well as of t. P W and P M for scavenging materials are, strictly speaking, not true permeances and permeabilities at all (since permeation and scavenging are occurring simultaneously) but, rather, apparent ones.
[0063] Values of P W and P M (except where stated otherwise) are to be understood to refer to conditions in which p=0.21 atm, the relative humidity on the oxygen-rich side of the wall is 50%, the temperature is 23° C. and (in the case of P M values) the thickness of the material of about 0.45 mm Conditions close to the first three of these, at least, are conventional in the packaging industry.
[0064] For example, OTR can be measured for bottles, for example, by controlling the atmosphere on both sides of a sample of bottles and measuring the rate of oxygen permeation over time. Typically, the bottles are mounted on a plate such that there are two ports for gas inlet and outlet. The interior of the bottles is separated from the exterior by an air tight seal. After sealing, the interior of the bottle is flushed with N 2 gas (or N 2 +H 2 mixture) to remove any oxygen present before mounting on plate. The bottle is then placed in a controlled environmental chamber (maintained at 23° C. and 50% RH) such that the exterior of the bottle is at standard atmosphere with ˜21% oxygen. The interior of the bottle is continuously flushed with N 2 (or N 2 +H 2 ) at a known gas flow rate. The outlet of the flushed gases contains oxygen permeating through the bottle wall. This flushed gas from the bottle interior is passed over a sensor that is calibrated to measure oxygen content of the flushed gas. Such measurements of oxygen content are made continuously over time until a steady state is reached. This steady state value is typically reported as Oxygen Transmission Rate (OTR) for that bottle in the units of cc/package/day. A preferred OTR for PET bottles is less than 0.1 cc/package/day; more preferred is less than 0.01 cc/package/day; most preferred for PET bottles is less than 0.001 cc/package/day over the shelf life of the packaged product.
[0065] In one aspect, a disclosed composition has an OTR of less than that of an otherwise identical composition in the absence of the amide compound and the transition metal. In further aspects, a disclosed composition has an OTR of less than about 75%, less than about 50%, less than about 25%, less than about 20%, less than about 10%, less than about 5%, or less than about 1% of an otherwise identical composition in the absence of the amide compound and the transition metal.
[0066] For example, measurements of oxygen permeation can be made by methods described, for example, in U.S. Pat. No. 5,639,815, which is incorporated herein by this reference for its teachings of oxygen permeability tests. Oxygen permeability tests are also discusses din U.S. Pat. Nos. 5,021,515, 5,034,252, 5,049,624, 5,159,005, 5,239,016, 5,639,815, 5,955,527, and U.S. Application Publication No. 2006/0180790, each of which is incorporated herein by this reference for its teaching of oxygen permeability tests. Oxygen permeability tests can also be carried out according to the method disclosed in WO/2006/023583 at page 10.
[0067] Various methods exist for making the composition. In one aspect, the composition can be made by mixing the polymer (comprising the amide compound), and optionally the transition metal, and optionally a colorant. In some aspects, some or part of the transition metal may already be present in the polymer prior to mixing, for example if the transition metal is used as a catalyst for making the base polymer. Other optional ingredients can be added during this mixing process or added to the mixture after the aforementioned mixing or to an individual component prior to the aforementioned mixing step.
[0068] When melt processing is desired for the composition, the composition can also be made by adding each ingredient separately and mixing the ingredients just prior to melt processing the composition to form an article. In some embodiments, the mixing can be just prior to the melt process zone. In other embodiments, one or more ingredients can be premixed in a separate step prior to bringing all of the ingredients together.
[0069] In some aspects, the transition metal can be added neat or in a carrier (such as a liquid or wax) to an extruder or other device for making the article, or the metal can be present in a concentrate or carrier with the polymer. It is desirable that the addition of the transition metal does not substantially increase the intrinsic viscosity of the melt in the melt processing zone. Thus, transition metal or metals can be added in two or more stages, such as once during the melt phase for the production of the polymer and again once more to the melting zone for making the article.
[0070] The melt blend of the polymer and any other ingredients can also be prepared by adding the components at the throat of an injection molding machine that: (i) produces a preform that can be stretch blow molded into the shape of the container, (ii) produces a film that can be oriented into a packaging film, (iii) produces a sheet that can be thermoformed into a food tray, or (iv) produces an injection molded container. The mixing section of the extruder should be of a design to produce a homogeneous blend. Such process steps work well for forming carbonated soft drink, water or beer bottles, packaging films and thermoformed trays. The present invention can be employed in any of the conventional known processes for producing a polymeric container, film, tray, or other article that would benefit from oxygen scavenging.
[0071] Various articles can be prepared from the disclosed compositions. Thus, the articles prepared from the compositions will also have the composition present in the article. Suitable articles include vessels and films, such as flexible sheet films, flexible bags, pouches, semi-rigid and rigid containers such as bottles (e.g. PET bottles) or metal cans, or combinations thereof. Typical flexible films and bags include those used to package various food items and can be made up of one or a multiplicity of layers to form the overall film or bag-like packaging material. The composition of the present invention can be used in one, some or all of the layers of such packaging material.
[0072] Specific articles include preforms, containers and films for packaging of food, beverages, cosmetics, pharmaceuticals, and personal care products where a high oxygen barrier is needed. Examples of beverage containers are bottles for holding water and carbonated soft drinks, and the invention is particularly useful in bottle applications containing juices, sport drinks, beer or any other beverage where oxygen detrimentally affects the flavor, fragrance, performance (e.g., vitamin degradation), or color of the drink. The compositions are also particularly useful as a sheet for thermoforming into rigid packages and films for flexible structures. Rigid packages include food trays and lids. Examples of food tray applications include dual ovenable food trays, or cold storage food trays, both in the base container and in the lidding (whether a thermoformed lid or a film), where the freshness of the food contents can decay with the ingress of oxygen. The compositions can also be used in the manufacture of cosmetic containers and containers for pharmaceuticals or medical devices.
[0073] Other suitable articles include rigid or semi-rigid articles including plastic, such as those utilized for juices, soft drinks, as well as thermoformed trays or cup normally having thickness in the range of from 100 to 1000 micrometers. The walls of such articles can comprise single or multiple layers of materials. The article can also take the form of a bottle or can, or a crown, cap, crown or cap liner, plastisol or gasket. The composition of the present invention can be used as an integral layer or portion of, or as an external or internal coating or liner of, the formed semi-rigid or rigid packaging article. As a liner, the composition can be extruded as a film along with the rigid article itself, e.g., by coextrusion, extrusion coating, or an extrusion lamination process, so as to form the liner in situ during article production; or alternatively can be adhered by heat and/or pressure, by adhesive, or by any other suitable method.
[0074] When the compositions are used in a wall or as a layer of a wall, the permeability of the composition for oxygen is advantageously not more than about 3.0, or about 1.7, or about 0.7, or about 0.2, or about 0.03 cm 3 -mm/(m 2 -atm-day). In some aspects, the permeability of the composition is not more than about three-quarters of that in the absence of the amide compound. In some aspects, the permeability is not more than about one half, one-tenth in certain embodiments, one twenty-fifth in other embodiments, and not more than one-hundredth of that in the absence of the amide compound.
[0075] Although it can be preferable from the standpoint of packaging convenience and/or scavenging effectiveness to employ the present invention as an integral or discrete part of the packaging wall, the invention can also be used as a non-integral component of a packaging article such as, for example, a bottle cap liner, adhesive or non-adhesive sheet insert, sealant, sachet, fibrous mat insert or the like.
[0076] Besides articles applicable for packaging food and beverage, articles for packaging other oxygen-sensitive products can also benefit from the present invention. Such products would include pharmaceuticals, oxygen sensitive medical products, corrodible metals or products, electronic devices and the like.
[0077] In a further aspect, the composition can be used as a master batch for blending with a polymer or a polymer containing component. In such compositions, the concentration of the amide compound and the transition metal will be high enough to allow for the final blended product to have suitable amounts of these components. The master batch can also contain an amount of the base polymer with which the master batch is blended.
[0078] Oxygen permeability of an article can be maintained for a longer period of time by storing the article in a sealed container or under an inert atmosphere such as nitrogen prior to use with oxygen sensitive materials.
[0079] The articles can be made by various methods known in the art. Generally, the articles are prepared by melt processing methods (i.e., a melt of the composition). Such processes generally include injection molding, stretch blow molding, extrusion, thermoforming, extrusion blow molding, and (specifically for multilayer structures) coextrusion and lamination using adhesive tie layers. Orientation, e.g., by stretch blow molding, of the polymer can be used with phthalate polyesters because of the known mechanical advantages that result.
[0080] The melt processing zone for making the article can be operated under customary conditions effective for making the intended articles, such as preforms, bottles, trays, and other articles mentioned above. In one aspect, such conditions are effective to process the melt without substantially increasing the intrinsic viscosity of the melt and which are ineffective at promoting transesterification reactions. In some preferred aspects, suitable operating conditions effective to establish a physical blend of the base polymer, oxidizable organic component, and transition metal are temperatures in the melt processing zone within a range of about 250° C. to about 300° C. at a total cycle time of less than about 6 minutes, and typically without the application of vacuum and under a positive pressure ranging from about 0 psig (pound-force per square inch gauge) to about 900 psig. In some embodiments, the residence time of the melt on the screw can range from about 1 to about 4 minutes.
EXPERIMENTAL
[0081] The following examples are put forth so as to provide those of ordinary skill in the art with a complete disclosure and description of how the compounds, compositions, articles, devices and/or methods claimed herein are made and evaluated, and are intended to be purely exemplary and are not intended to limit the disclosure. Efforts have been made to ensure accuracy with respect to numbers (e.g., amounts, temperature, etc.), but some errors and deviations should be accounted for. Unless indicated otherwise, parts are parts by weight, temperature is in ° C. or is at ambient temperature, and pressure is at or near atmospheric.
Example 1
[0082] 80 grams of bis(2-hydroxyethyl) terephthalate (BHET) (0.3147 moles) and 0.0123 g Sb 2 O 3 (132 ppm Antimony, Sb) were charged into a 250 ml 3-neck flask. The flask was equipped with a mechanical stirrer and Dean-Stark receiver was purged with nitrogen, stirred and heated to 260° C. The condensation polymerization was allowed for 1.5 hours and then was kept for another 1 hour under vacuum to remove the generated ethylene glycol. The system was then cooled down to 190° C. 6 grams of DCX-320 (half-amide) was dissolved in 50 ml DMSO and added to the flask. With reflux, the solvent—DMSO was continuously distilled out. Meanwhile, the formed ethylene glycol was also distilled off along with DMSO via the formation of an azeotrope. 4 hours after addition of DCX-320, some fresh DMSO was added into the system to dilute the polymer solution and then the polymer was precipitated into methanol. The unreacted DCX-320 and solvent DMSO were extracted by methanol under reflux. The extraction was repeated 3 times. The purified polymer was dried in vacuo at 100° C. overnight and 62 grams of dry polymer was obtained.
[0083] The resulting polymer was characterized using GPC (with polystyrene as standard). The number average molecular weight (Mn) was found to be 6300 daltons and weight average molecular weight was found to be 9300 daltons. The polydispersity index was calculated to be 1.48.
[0084] Elemental analysis of the resulting polymer showed Carbon % to be 61.1%, Hydrogen % to be 4.78% and Nitrogen % to be 0.51%. Since PET does not have any nitrogen atoms, the presence of nitrogen confirms the end-capping reaction with DCX-320. Since there are 2 nitrogen atoms in each DCX-320 molecule, it is possible to estimate the degree of end-capping in the synthesized polymer as follows:
[0000] ( X/ 6300)*100%=0.51% ( N content from elemental analysis)
[0000] The weight of nitrogen atoms in each DCX-320 end-capped PET molecule is X=32.13. Comparing to the fully double end-capped chain with nitrogen weight of 56, the actual DCX-320 end-cap degree is (32.13/56)*100=57.4%.
[0085] The reaction scheme is shown below:
[0000]
Example 2
[0086] The polymer synthesized in example 1 was used to make injection molded plaques on a BOY 22S. This polymer was vacuum dried at 110° C. for 24 hours to remove residual solvent. The PET resin used was Eastman's Vitiva™ resin. It was dried at 250° F. for ˜15 hours then dried at 350° F. for 2 hours prior to use. Cobalt catalyst was added in a PET masterbatch form, such that the cobalt levels in the final plaque is 80 ppm. A batch was prepared of the hot, dry PET, PET based Cobalt Masterbatch and 1 wt % of the dried polymer synthesized in Example 1.
[0087] Plaques were injection molded on a BOY 22S injection molding machine. The Plaques formed from Example 2 were collected and tested for oxygen scavenging ability using Oxysense™. The plaques were ground to fine powder, placed in a sealed glass vial, with a photoluminescent window on the wall. The intensity of light reflected from the photoluminescent window is proportional to the oxygen content in the vial. The Oxysense™ data for the above polymer composition and a control composition comprised of Constar International's DC-100 is shown in FIG. 1 . As seen from the data of FIG. 1 , the polymer composition of Example 2 does scavenge oxygen when melt-blended with cobalt catalyst in a PET matrix.
[0088] It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
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The disclosure relates to oxygen scavenging polymer compositions, methods of making the compositions, articles prepared from the compositions, and methods of making the articles. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present invention.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is related to the following commonly-assigned copending application: Ser. No. 12/100,294, entitled “LIGHT EMITTING DIODE BASED ILLUMINATION DEVICE”. Disclosures of the above-identified application are incorporated herein by reference.
BACKGROUND
1. Technical Field
The present invention generally relates to semiconductor solid-state light-source modules and semiconductor solid state light source assemblies having the same.
2. Discussion of Related Art
Nowadays, conventional display modules generally employ cold cathode fluorescent lamp (CCFL) as light source. A display module generally includes a lamp case, and at least one CCFL arranged therein. However, the CCFL is bulky and not environmental friendly.
Light emitting diode (LED) has been used extensively as light source for display modules due to its pollution free, high luminous efficiency and small size. A conventional display module usually includes a plurality of LEDs arranged on a printed circuit board with high density to form an LED array. According to different requirements, the LED array may have different sizes. If a portion of the LED array malfunctions, then the whole LED arrays must be replaced, this is expensive.
Therefore, what is needed is a semiconductor solid-state light-source module that overcomes the above described shortcomings.
SUMMARY
A semiconductor solid-state light-source module, in accordance with a present embodiment, is provided. The semiconductor solid-state light-source module includes a printed circuit board, at least one semiconductor solid state light source mounted on the printed circuit board and a light guide plate optically coupled to the semiconductor solid state light source. The printed circuit board includes a protrusion and a recess. The protrusion is configured for engaging with a recess of the printed circuit board of another similar semiconductor solid-state light-source module.
Detailed features of the present semiconductor solid-state light-source module will become more apparent from the following detailed description and claims, and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
Many aspects of the present semiconductor solid-state light-source module 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 present semiconductor solid-state light-source module. Moreover, in the drawings, like reference numerals designate corresponding parts throughout the several views, wherein:
FIG. 1 is a schematic isometric view of a semiconductor solid-state light-source module, according to a first exemplary embodiment;
FIG. 2 is a schematic view showing a circuit of the semiconductor solid state light sources as illustrated in FIG. 1 ;
FIG. 3 is a schematic view of a printed circuit board of the semiconductor solid-state light-source module as illustrated in FIG. 1 ;
FIG. 4 is a schematic isometric view of a semiconductor solid-state light-source module, according to a second exemplary embodiment;
FIG. 5 is a schematic view showing a circuit of the semiconductor solid state light sources as illustrated in FIG. 4 ;
FIG. 6 is a schematic isometric view of a semiconductor solid-state light-source module, according to a third exemplary embodiment;
FIG. 7 is a schematic view showing a circuit of the semiconductor solid state light sources as illustrated in FIG. 6 ;
FIG. 8 is a schematic isometric view of a semiconductor solid-state light-source module, according to a fourth exemplary embodiment; and
FIG. 9 is a schematic view showing a circuit of the semiconductor solid state light sources as illustrated in FIG. 8 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Reference will now be made to the drawings to describe the embodiments of the present semiconductor solid-state light-source module, in detail.
Referring to FIG. 1 and FIG. 2 , a semiconductor solid-state light-source module 10 according to a first exemplary embodiment is provided. The semiconductor solid-state light-source module 10 includes three semiconductor solid state light source cells 14 with the same configuration.
Each semiconductor solid state light source cell 14 includes a printed circuit board 13 , three semiconductor solid state light sources 18 and a light guide plate 16 . Each semiconductor solid state light sources 18 has a light emitting surface. The light emitting surface of each of the semiconductor solid state light sources 18 faces toward the light guide plate 16 .
Particularly referring to FIG. 3 , the printed circuit board 13 includes a power interface 131 , a first protrusion 132 , a second protrusion 133 , a first receptacle 134 opposite to the first protrusion 132 , and a second receptacle 135 opposite to the second protrusion 133 . The power interface 131 is electrically connected to an external power supply (not illustrated).
Each semiconductor solid state light source 18 includes a positive electrode 181 and a negative electrode 182 (see FIG. 2 ). The three semiconductor solid state light sources 18 are electrically connected in series and cooperatively form a light source module. The light source module is electrically connected between an external controlling unit 100 and the power interface 131 .
The semiconductor solid state light source cells 14 connect to each other by the engagement of protrusions and receptacles. The semiconductor solid state light source cells 14 can be powered on or powered off by triggers signals sent from the external controlling unit 100 so that the semiconductor solid state light source cell 14 is capable of representing different states according to the trigger signals.
Due to engagement of the protrusions 132 , 133 and the receptacles 134 , 135 , a plurality of semiconductor solid state light source cells 14 can be detachably connected together and thereby facilitate display function. When an individual semiconductor solid state light source cell 14 fails to work, it can be disassembled and replaced individually.
It is to be said that, the number of the semiconductor solid state light source cells 14 of the semiconductor solid-state light-source module 10 can also be one, two, four, five or more, and each of the semiconductor solid state light source cell 14 can also includes two, four, five, or more semiconductor solid state light sources 18 electrically connected in series.
Referring to FIG. 4 or FIG. 5 , a semiconductor solid-state light-source module 20 according to a second exemplary embodiment is provided. The semiconductor solid-state light-source module 20 has a configuration similar to the semiconductor solid-state light-source module 10 . The semiconductor solid-state light-source module 20 includes three semiconductor solid state light source cells 24 with the same configuration. Each semiconductor solid state light source cell 24 includes a printed circuit board 13 and three semiconductor solid state light sources 18 .
The difference is that, each semiconductor solid state light source cell 24 further includes three light guide plates 26 , each of which arranged on a respective light emitting surface of the three semiconductor solid state light sources 18 . The three semiconductor solid state light sources 18 are electrically connected in parallel. Each positive electrode 181 of the semiconductor solid state light sources 18 is connected to the external controlling unit 100 and each negative electrode 182 of the semiconductor solid state light sources 18 is connected to the power interface 131 .
Referring to FIG. 6 and FIG. 7 , a semiconductor solid-state light-source module 30 according to a third exemplary embodiment is provided. The semiconductor solid-state light-source module 30 has a configuration similar to the semiconductor solid-state light-source module 20 . The semiconductor solid-state light-source module 30 includes three semiconductor solid state light source cells 34 with the same configuration. Each semiconductor solid state light source cell 34 includes a printed circuit board 13 , three semiconductor solid state light sources 18 and three light guide plates 36 . Each of the three light guide plates 36 is arranged on a respective light emitting surface of the semiconductor solid state light sources 18 .
The difference is that each of the semiconductor solid state light source cells 34 further includes three controller chips 38 . Each controller chip 38 includes a signal input port 381 and a signal output port 382 . Each of the signal input port 381 is connected to a respective positive electrode 181 of the semiconductor solid state light sources 18 . Each of the signal output port 382 is connected to a respective negative electrode 182 of the semiconductor solid state light sources 18 . The negative electrodes 182 of the semiconductor solid state light sources 18 are connected to the power interface 131 .
When the signal input ports 381 receive trigger signals sent by the external controlling unit 100 , the signal output ports 382 each outputs a controlling signal to the corresponding semiconductor solid state light source 18 according to the trigger signals, thereby the semiconductor solid state light sources 18 represents different states.
Referring to FIG. 8 and FIG. 9 , a semiconductor solid-state light-source module 40 according to a fourth exemplary embodiment is provided. The semiconductor solid-state light-source module 40 has a configuration similar to the semiconductor solid-state light-source module 30 . The semiconductor solid-state light-source module 40 includes three semiconductor solid state light source cells 44 with the similar configuration.
The difference is that the three semiconductor solid state light source cells 44 include a community controller chip 48 and a community light guide plate 46 . The controller chip 48 is respectively connected to the positive electrodes 181 of the semiconductor solid state light sources 18 . The negative electrodes 182 of the semiconductor solid state light sources 18 are connected to the power interface 131 . The light emitting surface of each of the semiconductor solid state light sources 18 faces towards the light guide plate 46 .
Finally, it is to be understood that the above-described embodiments are intended to illustrate rather than limit the invention. Variations may be made to the embodiments without departing from the spirit of the invention as claimed. The above-described embodiment illustrates the scope of the invention but do not restrict the scope of the invention.
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An exemplary semiconductor solid-state light-source module includes a printed circuit board, at least one semiconductor solid state light source mounted on the printed circuit board and a light guide plate optically coupled to the semiconductor solid state light source. The printed circuit board includes a protrusion and a recess. The protrusion is configured for engaging with a recess of the printed circuit board of another similar semiconductor solid-state light-source module.
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This application is a continuation of international application number PCT/EP2009/060112 filed on Aug. 4, 2009 and claims the benefit of German application number 10 2008 038 258.2 filed on Aug. 11, 2008.
The present disclosure relates to the subject matter disclosed in international application number PCT/EP2009/060112 of Aug. 4, 2009 and German application number 10 2008 038 258.2 of Aug. 11, 2008, which are incorporated herein by reference in their entirety and for all purposes.
BACKGROUND OF THE INVENTION
The present invention relates to a projectile, comprising a gel-like or jelly-like material.
Such projectiles are used, in particular, for bird strike tests as a substitute for real birds. Bird strike tests are carried out at wind power plants, for example, and, in particular, are mandatory for the certification of aircraft and trains. To that end, projectiles are fired at a high speed by a gas gun at areas of the wind power plants, the aircraft or the trains that are to be tested. Owing to the high speeds and the resulting high air resistance during a flight phase of the projectiles, deformation and/or oscillation of the projectile occurs, particularly when artificial projectiles of the above-mentioned kind are used, which leads to distortion of the test results.
U.S. Pat. No. 5,936,190 A, FR 2 768 504 A1, EP 0 488 911 A2, U.S. Pat. No. 3,791,303 A and WO 2007/066324 A1 disclose projectiles which are fired by hand firearms at animals and/or human beings.
SUMMARY OF THE INVENTION
In accordance with the present invention, a projectile is provided, which makes reproducible and representative results in bird strike tests possible.
In accordance with an embodiment of the invention, a stabilizing device arranged in the projectile is provided for stabilizing the gel-like or jelly-like material.
A deformation of the projectile, in particular, in the flight phase is reduced, preferably completely avoided, by the stabilizing device. This leads to a reproducible shape of the projectile upon impact with a target and, therefore, to reproducible results of the bird strike tests.
In an embodiment of the invention it may be provided that the gel-like or jelly-like material comprises gelatin or consists of gelatin. As a result, the projectile is low-priced and easy to produce.
It is expedient for the gel-like or jelly-like material to be formed from a mixture of, for example, approximately four proportions of water and, for example, approximately one proportion of gelatin.
It is particularly expedient for the gel-like or jelly-like material to comprise ballistic gelatin or to consist of ballistic gelatin. The physical characteristics and the physical behavior of muscles can be recreated well by the use of ballistic gelatin.
As an alternative or supplement to this, it may be provided that the gel-like or jelly-like material comprises silicone rubber, glycerin soap, starch, polymer gel, caoutchouc, latex and/or plasticine or consists of silicone rubber, glycerin soap, starch, polymer gel, caoutchouc, latex and/or plasticine. Plasticine is a trademark registered in the name of Flair Leisure Products PLC.
It is expedient for the gel-like or jelly-like material to have a gel strength of from, for example, approximately 200 Bloom to, for example, approximately 300 Bloom. The physical characteristics and the physical behavior of muscles can then be recreated well.
Advantageously, the gelatin is a type A gelatin.
In an embodiment of the invention it may be provided that the projectile comprises hollow bodies, in particular, hollow balls.
It is expedient for at least part of the gel-like or jelly-like material to be arranged in the hollow bodies. The projectile can be stabilized in a simple way by using hollow bodies as subunits inside the projectile. Furthermore, adaptation of the density of the projectile is thereby possible.
It is also expedient for the hollow bodies to be surrounded at least partly by the gel-like or jelly-like material.
It is particularly expedient for the hollow bodies to be formed at least partly of a brittle material, in particular, from glass or polycarbonate. In this way, the shell of the hollow bodies is of stable construction, and little influence of the hollow bodies on the behavior of the projectile upon impact with a target is ensured.
It is particularly expedient for the stabilizing device to comprise hollow bodies that are connected to one another. An improved stabilization of the projectile is thus made possible by the hollow bodies present in the projectile.
In an embodiment of the invention it may be provided that the projectile has, at least in sections thereof, a substantially cylindrical shape. In this way, a bird strike can be simulated well.
As an alternative or supplement to this, it may be provided that the projectile is, at least on one side thereof, of substantially hemispherical configuration.
It is expedient for the projectile to be of substantially hemispherical configuration on either side of a middle section. As a result, the projectile has better aerodynamics and hence a reduced deformation in the flight phase.
In an embodiment of the invention it may be provided that the projectile is configured, at least in sections thereof, substantially as an ellipsoid, in particular, as an ellipsoid of revolution. In this way, the projectile has good aerodynamics and hence reduced deformation in the flight phase.
In particular, for use in single-impact tests, i.e., with only one impact per target to be tested, it is provided in an embodiment of the invention that the projectile has a mass of at least approximately 1.5 kg.
Furthermore, it is then expedient for the projectile to have a mass of at most approximately 4 kg.
It is particularly preferred for the projectile to have a mass of approximately 1.814 kg (4 lb) or of approximately 3.628 kg (8 lb).
In particular, for use in multiple-impact tests, i.e., with several impacts per target to be tested, it is advantageously provided that the mass of the projectile is preferably at least approximately 50 g and preferably at most approximately 1 kg. For example, tests with 8 projectiles, each weighing 700 g or 16 projectiles, each weighing 85 g are representative of flocks of birds.
In an embodiment of the invention it may be provided that the stabilizing device is formed, at least in sections thereof, of a material having a high brittleness. In this way, upon impact of the projectile with a target, the stabilizing device is essentially immediately destroyed and, therefore, has little, in particular, no, influence on the behavior of the projectile upon target impact.
It is advantageous for the stabilizing device to be formed, at least in sections thereof, of a material having a high stiffness. The stability of the projectile can thereby be increased.
It is expedient for the stabilizing device to be formed, at least in sections thereof, of, in particular, impregnated and/or non-absorbent, paper, or, in particular, impregnated and/or non-absorbent, cardboard. As a result, the stabilizing device can be constructed in a simple way. Moreover, the stability of the projectile can be increased by using stiff paper or stiff cardboard.
In an embodiment of the invention it may be provided that the stabilizing device comprises at least one stabilizing element. Owing to the use of at least one stabilizing element, the stabilizing device can be arranged particularly easily and flexibly in and/or on the projectile.
It is advantageous for a maximum extent of the at least one stabilizing element to be at most approximately one tenth, preferably at most approximately one fiftieth, of a maximum extent of the projectile.
It is expedient for the at least one stabilizing element to be of substantially bar-shaped configuration. In this way, in particular, a three-dimensional structure is easy to construct by means of the stabilizing elements.
It is particularly expedient for the stabilizing device to be formed, at least in sections thereof, of stabilizing elements arranged in a geometrical pattern. A particularly stable three-dimensional structure of the stabilizing device is thereby ensured.
It is advantageous for the geometrical pattern to be based on a cubic or tetrahedral basic shape. In this way, a simple construction of a stable stabilizing device is possible.
As an alternative or supplement to this, it may be provided that the stabilizing device comprises at least one, for example, spinal column-like, main support. In this way, in particular, a central section of the projectile can be easily stabilized.
As a supplement to this, it may be provided that the stabilizing device comprises a plurality of, for example, rib-shaped, stabilizing elements which are arranged, in particular, regularly, on the main support. An additional stabilization of the projectile which is already stabilized by the main support is thus possible.
In an embodiment of the invention it may be provided that a material of which at least a section of the stabilizing device is formed has substantially the same density as the gel-like or jelly-like material. In this way, an influence of the stabilizing device on the behavior of the projectile upon impact with the target can be reduced, in particular, completely avoided.
It is advantageous for the stabilizing device to comprise a material, in particular, to consist of a material which is workable by laser sintering. In this way, a user-defined shape of the stabilizing device can be easily produced, in particular, by rapid prototyping. For this purpose, a laser for sintering thermoplastic plastic powder, for example, polypropylene or polyamide, is guided, for example, in accordance with the specifications of a CAD model. A free design of the geometry of the stabilizing device is thus possible.
It is advantageous for the projectile to be surrounded, at least in sections thereof, by a substantially water-impermeable material. A drying-out of the projectile and hence a change in the physical characteristics during storage of the projectile can thereby be avoided.
It is expedient for the projectile to be provided with a water-impermeable coating. In this way, a drying-out can be prevented particularly easily.
The projectile in accordance with the invention is suited, in particular, for use in a combination of a projectile and a sabot for receiving and accelerating the projectile in an acceleration device.
The combination of projectile and sabot may have the advantages set forth above in conjunction with the projectile in accordance with the invention.
It is advantageous for the sabot to comprise a receptacle for the projectile, the shape of which, at least in sections thereof, is complementary to that of at least one section of the projectile. In this way, the projectile can be easily received, in particular, loosely held, in the sabot.
It is advantageous for the sabot to be constructed so as to be separable along a longitudinal center plane. As a result, the projectile can be easily placed in the sabot and removed from it.
The combination of projectile and sabot is suited, in particular, for use in an acceleration device configured, for example, as a gas gun.
The acceleration device with the combination of the projectile in accordance with the invention and the sabot may have the advantages set forth above in conjunction with the projectile in accordance with the invention and the combination of projectile and sabot.
The projectile in accordance with the invention, the combination of projectile and sabot, and the acceleration device with the combination of projectile and sabot may also have the following advantages:
a real bird is realistically, representatively and reproducibly simulated; and the projectile is substantially dimensionally stable in flight.
Further features of the invention are presented in the following description and the drawings of embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a diagrammatic representation of a gas gun with a first embodiment of a sabot and a first embodiment of a projectile;
FIG. 2 shows a diagrammatic representation of the projectile from FIG. 1 ;
FIG. 3 shows a diagrammatic representation of the gas gun from FIG. 1 , in which the sabot is arranged with the projectile at the end of an acceleration section of the gas gun;
FIG. 4 shows a diagrammatic representation of the gas gun from FIG. 3 , with the projectile deformed by the air resistance;
FIG. 5 shows a diagrammatic representation of the gas gun from FIG. 3 , with the projectile deformed by the air resistance;
FIG. 6 shows a diagrammatic representation of the gas gun from FIG. 3 , with the projectile striking a target;
FIG. 7 shows a diagrammatic representation of the gas gun from FIG. 3 , with a second embodiment of a projectile;
FIG. 8 shows a diagrammatic representation of a third embodiment of a projectile;
FIG. 9 shows a diagrammatic perspective representation of a stabilizing device with a cubic basic shape of a fourth embodiment of a projectile;
FIG. 10 shows a diagrammatic perspective representation of a stabilizing device with a tetrahedral basic shape of a fifth embodiment of a projectile;
FIG. 11 shows a diagrammatic perspective representation of a stabilizing device of a sixth embodiment of a projectile;
FIG. 12 shows a diagrammatic perspective representation of a seventh embodiment of a projectile;
FIG. 13 shows a diagrammatic representation of an eighth embodiment of a projectile; and
FIG. 14 shows a diagrammatic representation of a ninth embodiment of a projectile.
DETAILED DESCRIPTION OF THE INVENTION
Identical or functionally equivalent elements are given the same reference numerals in all Figures.
A gas gun shown in FIGS. 1 and 3 to 6 and designated in its entirety by 100 comprises a main body 102 , a sabot 104 and a projectile 106 arranged in the sabot 104 .
The gas gun 100 is an acceleration device and serves to accelerate the projectile 106 by means of the sabot 104 in a direction of acceleration 108 .
The main body 102 is of cylindrical and hollow construction and comprises a rear end 110 in the direction of acceleration 108 , a barrel 112 and a front outlet 114 in the direction of acceleration 108 .
Arranged at the rear end 110 of the main body 102 is a propellant chamber 116 , which in the direction of acceleration 108 borders at the front on a rear wall 118 of the sabot 104 when the sabot 104 is arranged in an initial position (see FIG. 1 ).
Stops 120 against which the sabot 104 bears in the initial position with the rear wall 118 are provided on the main body 102 to lock the sabot 104 in the direction opposite to the direction of acceleration 108 .
The sabot 104 is of substantially cylindrical and solid construction.
An outer diameter 122 of the sabot 104 is selected so that an outer lateral surface 124 of the sabot 104 can slide along an inner lateral surface 126 of the barrel 112 .
An inner diameter 128 of the barrel 112 of the main body 102 is, therefore, slightly larger than the outer diameter 122 of the sabot 104 .
Sabot stoppers 132 are provided at a front end 130 of the main body 102 in the direction of acceleration 108 for restricting movement of the sabot 104 in the direction of acceleration 108 .
The barrel 112 of the main body 102 of the gas gun 100 extends from the stops 120 to the sabot stoppers 132 .
The sabot 104 comprises a receptacle 134 for receiving the projectile 106 .
The receptacle 134 is of complementary construction to a section of the projectile 106 so as to be able to easily receive this section.
The projectile 106 is of rotationally symmetrical construction with respect to an axis of rotation 137 and comprises a front hemispherical section 136 , a cylindrical section 138 located centrally and a rear hemispherical section 140 , the hemispherical sections 136 and 140 having, for example, a substantially identical radius 142 (see FIG. 2 ).
The radius 142 of the front hemispherical section 136 and of the rear hemispherical section 140 corresponds, for example, approximately to a radius 144 of the cylindrical section 138 of the projectile 106 and, for example, approximately to half of a length 146 of the cylindrical section 138 .
A length 148 of the projectile 106 therefore corresponds, for example, approximately to four times the radius 142 of the front hemispherical section 136 and of the rear hemispherical section 140 .
In the initial position, the projectile 106 is arranged in the receptacle 134 of the sabot 104 so that the receptacle 134 surrounds the rear hemispherical section 140 and, for example, approximately half of the cylindrical section 138 of the projectile 106 (see FIG. 1 ).
In an embodiment (not shown) of the sabot 104 , the projectile 106 is substantially completely received in the sabot 104 .
The gas gun 100 described above with the sabot 104 and the projectile 106 operates in the following way:
A compressed gas or gas mixture is introduced into the propellant chamber 116 of the main body 102 of the gas gun 100 .
The resulting rise in pressure in the propellant chamber 116 causes a force to be applied to the rear wall 118 of the sabot 104 and hence the sabot 104 including the projectile 106 to be accelerated in the direction of acceleration 108 to, for example, approximately 70 m/s to simulate an impact on rotor blades (not shown) of a wind power plant.
The sabot 104 of the projectile 106 is thus brought in the direction of acceleration 108 from the initial position to an end position at the front end 130 of the main body 102 (see FIG. 3 ).
The sabot 104 is braked by the sabot stoppers 132 .
The projectile 106 held loosely in the sabot 104 separates from the sabot 104 on account of its inertia and flies in the direction of acceleration 108 towards a target 150 .
During the flight phase the projectile 106 is deformed by the air resistance (see FIGS. 4 and 5 ).
The deformations shown in FIGS. 4 and 5 result in an inaccuracy in the reproducibility of the impact of the projectile 106 on the target 150 shown in FIG. 6 .
A second embodiment of the projectile 106 shown in FIG. 7 comprises, in particular, for stabilization of the projectile 106 in the flight phase a stabilizing device 152 .
The deformations of the projectile 106 caused by the air resistance can be reduced, in particular, avoided altogether by means of the stabilizing device 152 .
The stabilizing device 152 is formed by square honeycombs and extends in both the radial and the axial direction over the entire extent of the projectile 106 .
To produce the projectile 106 , the stabilizing device 152 is placed in a mold into which, for example, a mixture of gelatin and water is subsequently introduced.
Apart from that, the embodiment of the gas gun 100 shown in FIG. 7 with the sabot 104 and the projectile 106 corresponds with respect to construction and operation to the embodiment of the gas gun 100 shown in FIGS. 1 and 3 to 6 with the sabot 104 and the projectile 106 , to the above description of which reference is made in this respect.
The third embodiment of the projectile 106 shown in FIG. 8 differs from the embodiment shown in FIG. 7 in that instead of a square honeycomb pattern, the stabilizing device 152 has a triangular honeycomb pattern.
Apart from that, the third embodiment of the projectile 106 shown in FIG. 8 corresponds with respect to construction and operation to the second embodiment shown in FIG. 7 , to the above description of which reference is made in this respect.
In an embodiment (not shown) of the projectile 106 corresponding substantially to the third embodiment shown in FIG. 8 , the honeycomb pattern is a hexagonal honeycomb pattern.
A fourth embodiment of the projectile 106 shown in FIG. 9 differs from the second embodiment shown in FIG. 7 in that the stabilizing device 152 comprises a cubic lattice formed by stabilizing elements 156 .
The stabilizing elements 156 are connected to one another by connecting elements 158 .
Lamellae 160 which are, for example, rectangular, are provided on the stabilizing elements 156 for further stabilization of the projectile 106 . Such lamellae 160 can be provided on individual stabilizing elements 156 or also on all stabilizing elements 156 .
Apart from that, the fourth embodiment of the projectile 106 shown in FIG. 9 corresponds with respect to construction and operation to the second embodiment shown in FIG. 7 , to the above description of which reference is made in this respect.
A fifth embodiment of the projectile 106 shown in FIG. 10 differs from the fourth embodiment shown in FIG. 9 in that instead of a cubic lattice, a tetrahedral lattice is provided, which is formed by a plurality of stabilizing elements 156 .
Apart from that, the fifth embodiment of the projectile 106 shown in FIG. 10 corresponds with respect to construction and operation to the fourth embodiment shown in FIG. 9 , to the above description of which reference is made in this respect.
A stabilizing device 152 of a sixth embodiment of the projectile 106 shown in FIG. 11 differs from the second embodiment shown in FIG. 7 in that the stabilizing device 152 is formed by four substantially identical plate-shaped stabilizing elements 156 .
Two of the plate-shaped stabilizing elements 156 are arranged parallel to each other, parallel to the axis of rotation 137 of the projectile 106 and at a distance from each other which corresponds, for example, approximately to the radius 142 of the hemispherical sections 136 and 140 of the projectile 106 .
The two stabilizing elements 156 are arranged in mirror-symmetrical relation to each other with respect to the axis of rotation 137 of the projectile 106 and extend along the largest extent of the projectile 106 and in a direction transverse thereto as far as a surface 161 of the projectile 106 in each case.
The two further plate-shaped stabilizing elements 156 correspond in their extent, their position relative to each other and their arrangement on the projectile 106 to the previously described plate-shaped stabilizing elements 156 , but are arranged at, for example, approximately 90° to the previously described two plate-shaped stabilizing elements 156 with respect to the axis of rotation 137 of the projectile 106 .
In a viewing direction along the axis of rotation 137 of the projectile 106 , an arrangement of the plate-shaped stabilizing elements 156 thus corresponds substantially to a hash sign.
One or more stabilizing plates (not shown) aligned substantially perpendicularly to the axis of rotation 137 may also be provided for further reinforcement of the stabilizing device 152 .
Apart from that, the sixth embodiment of the projectile 106 shown in FIG. 11 corresponds with respect to construction and operation to the second embodiment shown in FIG. 7 , to the above description of which reference is made in this respect.
A seventh embodiment of the projectile 106 shown in FIG. 12 differs from the second embodiment shown in FIG. 7 in that the stabilizing device 152 is formed by a plurality of hollow bodies in the form of hollow balls 162 .
The hollow balls 162 are filled with the gel-like or jelly-like material and are arranged on one another and connected to one another in such a way that the projectile 106 has substantially the same outer contour as the second embodiment of the projectile 106 shown in FIG. 7 .
Apart from that, the seventh embodiment of the projectile 106 shown in FIG. 12 corresponds with respect to construction and operation to the second embodiment shown in FIG. 7 , to the above description of which reference is made in this respect.
An eighth embodiment of the projectile 106 shown in FIG. 13 differs from the first embodiment shown in FIGS. 1 to 6 in that the projectile 106 is of cylindrical configuration and has no hemispherical sections.
The length 146 of the cylindrical section 138 in this embodiment is, for example, approximately four times the radius 144 of the cylindrical section 138 .
One, or a combination of several, of the stabilizing devices 152 shown in FIGS. 7 to 12 may be provided in the eighth embodiment of the projectile 106 .
Apart from that, the eighth embodiment of the projectile 106 shown in FIG. 13 corresponds with respect to construction and operation to the first embodiment shown in FIGS. 1 to 6 , to the above description of which reference is made in this respect.
A ninth embodiment of the projectile 106 shown in FIG. 14 differs from the first embodiment shown in FIGS. 1 to 6 in that the shape of the projectile 106 is an ellipsoid.
A length 164 of the first semiaxis of the ellipsoid in this embodiment is, for example, approximately half of a length 166 of the second semiaxis of the ellipsoid.
The length of the third semiaxis is identical to the length of the first semiaxis, so that the projectile 106 has the shape of an ellipsoid of revolution.
In the ninth embodiment of the projectile 106 , one, or a combination of several, of the stabilizing devices 152 shown in FIGS. 7 to 12 may be provided.
Apart from that, the ninth embodiment of the projectile 106 shown in FIG. 14 corresponds with respect to construction and operation to the first embodiment shown in FIGS. 1 to 6 , to the above description of which reference is made in this respect.
In principle, each of the projectiles described above may be provided with one of the stabilizing devices described above or with a combination of several of the stabilizing devices described above.
Bird strike tests can be carried out with reproducible and representative results by using projectiles with a stabilizing device.
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To provide a projectile for bird strike tests, comprising a gel-like or jelly-like material, which makes reproducible and representative results in bird strike tests possible, it is proposed that the projectile comprise a stabilizing device arranged in the projectile for stabilizing the gel-like or jelly-like material.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. patent application Ser. No. 12/507,684, filed Jul. 22, 2009, which claims the benefit of U.S. provisional patent application No. 61/082,653, filed Jul. 22, 2008 (now expired).
TECHNICAL FIELD
[0002] Embodiments of the subject matter described herein relate generally to video game technology. More particularly, embodiments of the subject matter relate to massively multiplayer online video game technology.
BACKGROUND
[0003] Massively multiplayer online (“MMO”) games enjoy tremendous popularity, with some games numbering players in the hundreds of thousands or even millions. Such games' players typically control one or more player characters, and these player characters interact with other player characters as well as with non-player characters, i.e., characters controlled by the system, and further interact with the game environment itself.
[0004] A central design goal for an MMO is to bring the world and characters of the game environment to life. Giving the game environment believable characters and features requires that the experience be engaging, deep, and immersive.
[0005] Typical cut scenes or narrative voice overs (VO) are used to enliven characters in a game. However, players have certain expectations of properties with well-known or iconic characters, e.g., licensed superheroes, and in a game setting, the game environment should make each iconic character feel rounded and real. The environment should connect players with such characters personally and socially, creating an illusion that the characters have lives and ambitions beyond any one interaction a player may have with them.
[0006] In other words, part of the immersion experience for a player is to have realistic and/or engaging responses from non-player characters and the environment. In prior systems, such responses have had little or no reliance on a player character's prior actions or on game (or world) events. To the extent they did, they were based on prior quests completed, or other such generic game variables.
BRIEF SUMMARY
[0007] Implementations of the system and method enhance the realism of a simulation such as an MIO by enhancing the relationship of non-player characters to player characters, using, e.g., personal contact, social communication, and shared history. Personal contact means that the player character acts alongside the non-player character, in many cases fighting with or against the player character. Quests, tasks, or the like, are arranged such that the non-player character purposely encounters the player character. Social communication is described in more detail below and pertains to acts and speech which communicate information from the non-player character to a player character. For personal contact and social communication, a given non-player character may have a range of responses, based on, e.g.: variety (to avoid repetition), relationship with the player character, and framing (to give context to what the player character is doing). Another category, shared history, provides a way for a player character to learn more about a non-player character. For example, the player character may find a newsreel with footage about the origin of the non-player character. The level of depth for which information about a non-player character may be available may depend on the category of non-player character, e.g., primary, secondary, global, or generic.
[0008] In the social communication aspect, the system and method provide ways to make a non-player character act and communicate in a more realistic fashion, in particular, by using historical events such as prior interactions to make the non-player character's acts and communications more relevant to player characters (and thus players). In particular, the response of a non-player character to a player character action may be via one or more of various actions: a verbal response, an emotive response such as a frown, grin, or smile, or a physical response such as running away, attacking, a clap on the back, or the like. The non-player character's responses, whether actions or communications, are based on more than just standard game variables. The responses are based on the experiences of the player character, including milestones, actions, communications, as well as on in-game or world events, or in-game interpretations of world events. In essence, non-player characters are made to act and communicate as if their personalities were persistent and dynamic. This may be particularly important in the MIO environment because of its persistent nature. Non-player characters are made to appear to react to player character actions over time. They appear to form an opinion of a player character over time and this opinion can be made to affect and modify the player's experience.
[0009] To accomplish the above, data is tracked pertaining to the interaction(s) of a subject player character with other player characters and non-player characters. Non-player character responses may be based not only on interactions with the subject player character, but also on the subject player character's interactions with other player characters and non-player characters, as well as the player character's interactions with the environment, e.g., tasks attempted and subsequent results. Tracked data may also pertain to events that are relevant with or to a subject player character. In any case, tracked data may be stored on a game server.
[0010] In one aspect, the invention is directed toward a computer-readable medium, comprising instructions for causing a processor in an electronic device to perform a method of generating responses of a non-player character in a simulation. The method includes steps of: receiving a first signal from a client computing device, the first signal indicating that a player character has initiated a communication with a non-player character; calculating a response to the first signal, where the calculating includes calculating a response based on one or more acts performed by the player character prior to the receiving; and transmitting a second signal, corresponding to the response, to the client computing device, the response in part causing a video renderer or sound renderer in the client computing device to render an indication of the response on a video or audio device, respectively, or both.
[0011] Implementations of the invention may include one or more of the following. The calculating a response based on one or more acts performed by the player character prior to the receiving may include calculating a response based on one or more quests or tasks accomplished or attempted by the player character, one or more prior communications or interactions between the player character and the non-player character, or one or more prior communications or interactions between the player character and other player characters or non-player characters. The calculating a response may further include choosing one of a plurality of responses at random, or calculating a response based on one or more in-game events.
[0012] In another aspect, the invention is directed toward a computer-readable medium, comprising instructions for causing a processor in an electronic device to perform a method of enabling interactions of player characters with non-player characters in a simulation. The method includes steps of receiving a first signal, the first signal indicating that a player character is within a predetermined distance from a personal contact spawning point; and upon the receiving, transmitting a second signal to the client computing device, the second signal indicative of a contact between the player character and a non-player character. The second signal causes one or more of the following: a rendering of a communication of the non-player character addressing the player character, the rendering performed by a video renderer or a sound renderer, the rendering indicating the initiated contact on a video or an audio device, respectively, or both; a locating and rendering of the non-player character in a vicinity of the player character, the rendering performed by a video renderer or a sound renderer on a video or an audio device, respectively, or both; or an arranging and rendering of the non-player character in a situation with the player character such that the non-player character is working with or against the player character to accomplish a common task, objective, or goal, the rendering performed by a video renderer or a sound renderer on a video or an audio device, respectively, or both.
[0013] Implementations of the invention may include one or more of the following. The rendering a communication may be based on one or more acts performed by the player character prior to the receiving, including one or more quests or tasks accomplished or attempted by the player character, one or more prior communications or interactions between the player character and the non-player character, or one or more prior communications or interactions between the player character and other player characters or non-player characters. The rendering a communication may include a step of choosing one of several potential communications at random, or may be based on one or more in-game events.
[0014] In yet another aspect, the invention is directed toward a computer-readable medium, comprising instructions for causing a processor in an electronic device to perform a method of providing information about a non-player character to a player character in a simulation. The method includes: receiving a first signal, the first signal indicating that a player character is within a predetermined distance from a shared history spawning point; upon receipt of the first signal, transmitting a second signal to the client computing device, the second signal causing the client computing device to display an activatable element corresponding to information about a non-player character; and upon receipt of a third signal corresponding to an activation of the displayed element, transmitting a fourth signal to the client computing device, the fourth signal causing the client computing device to play back a media file corresponding to the information about the non-player character.
[0015] Implementations of the invention may include one or more of the following. The causing the client computing device to play back a media file may include choosing a media file to play, wherein the choosing includes choosing a media file based on one or more quests or tasks accomplished or attempted by the player character, one or more prior communications or interactions between the player character and the non-player character, or one or more prior communications or interactions between the player character and other player characters or non-player characters. The choosing a media file to play may further include choosing one of a plurality of media files at random. The causing the client computing device to play back a media file may include causing the client computing device to play back a cinematic sequence or a cut scene. The causing the client computing device to play back a media file may include choosing a media file to play, and the choosing may be based on an in-game event.
[0016] In a further aspect, the invention is directed toward a computer-readable medium comprising a system for enhancing responses of a non-player character in a multiplayer game. The medium including the following modules: a database module for storing data about a plurality of player characters, a plurality of non-player characters, and a plurality of features in a game environment; and a response calculating module for calculating responses of non-player characters to player character interactions, where the response calculating module is configured to calculate a response based on one or more acts performed by the player character, or to alternatively calculate a response based on one or more in-game events.
[0017] Implementations of the invention may include one or more of the following. The calculating module may be configured to calculate a response based on one or more quests or tasks accomplished or attempted by the player character, one or more prior communications or interactions between the player character and the non-player character, or one or more prior communications or interactions between the player character and other player characters or non-player characters.
[0018] In another aspect, the invention is directed toward a computer-readable medium comprising a system for enabling interactions of player characters with non-player characters in a multiplayer game. The medium includes the following modules: a database module for storing data about a plurality of player characters, a plurality of non-player characters, and a plurality of features in a game environment; and a response calculating module for calculating responses to player character interactions, where the response calculating module is configured to, upon receipt of a first signal indicating that a player character is within a predetermined distance from a personal contact spawning point, transmit a second signal to the client computing device, where the second signal causes one or more of the following: a rendering of a communication of the non-player character addressing the player character, the rendering performed by a video renderer or a sound renderer, the rendering indicating the initiated contact on a video or an audio device, respectively, or both; a locating and rendering of the non-player character in a vicinity of the player character, the rendering performed by a video renderer or a sound renderer on a video or an audio device, respectively, or both; or an arranging and rendering of the non-player character in a situation with the player character such that the non-player character is working with or against the player character to accomplish a common task, objective, or goal, the rendering performed by a video renderer or a sound renderer on a video or an audio device, respectively, or both.
[0019] Implementations of the invention may include one or more of the following. The communication may be based on one or more acts performed by the player character prior to the receiving, which may include one or more quests or tasks accomplished or attempted by the player character, one or more prior communications or interactions between the player character and the non-player character, or one or more prior communications or interactions between the player character and other player characters or non-player characters.
[0020] In another aspect, the invention is directed toward a computer-readable medium, comprising a system for providing information about a non-player character to a player character in a multiplayer game. The medium includes the following modules: a database module for storing data about a plurality of player characters, a plurality of non-player characters, and a plurality of features in a game environment; and a response calculating module for calculating responses to player character interactions. The response calculating module is configured to, upon receipt of a first signal indicating that a player character is within a predetermined distance from a shared history spawning point, transmit a second signal to the client computing device, where the second signal causes a client computing device to display an activatable element corresponding to information about a non-player character. The response calculating module is configured to, upon receipt of a third signal corresponding to an activation of the displayed element, transmit a fourth signal to the client computing device, the fourth signal causing the client computing device to play back a media file corresponding to the information about the non-player character.
[0021] Implementations of the invention may include that the media file is selected based on an occurrence of an in-game event, and may be a cinematic.
[0022] Advantages of the invention may include one or more of the following non-limiting examples. Non-player character responses are made so as to be more realistic by choosing or developing the responses, for a given player character, based on tracking data reflecting that player character's interactions with the non-player character, with other non-player characters and player characters, on characteristics of the player character or an associated player or user, on in-game events, on real-world events, or the like. Non-player characters may be made more realistic by having the same act alongside or against player characters in scenarios, as well as by revealing non-player character backstories by having player characters find, watch, listen to, or otherwise consume clues about the same. Other advantages will be apparent from the following description, including the figures and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] FIG. 1 illustrates an exemplary environment of the simulation, e.g., a multiplayer game, and further illustrates how proximity to certain locations (or characters) may be employed to enhance the level of a player's immersion by providing scenarios and responses that are relevant to that player.
[0024] FIG. 2 illustrates a logical diagram of a system that may be employed to implement a simulation such as a multiplayer game, including a client-server architecture.
[0025] FIG. 3 is a flowchart of a method for implementing one embodiment of the invention, in particular employing social communication.
[0026] FIG. 4 is a flowchart of a method for implementing another embodiment of the invention, in particular employing personal contact.
[0027] FIG. 5 is a flowchart of a method for implementing yet another embodiment of the invention, in particular employing shared history.
DETAILED DESCRIPTION
[0028] Referring to FIG. 1 , an exemplary environment of the simulation, e.g., a multiplayer game, is illustrated. The environment may vary widely, and may be, e.g., a fantasy simulation, a science fiction simulation, a space simulation, a real world simulation, a city simulation, an apocalyptic simulation, a superhero simulation, and so on. The exemplary simulation of FIG. 1 shows a number of characters 32 , 33 , 34 , and 36 , and the same are shown traversing various streets 30 and 31 within a game environment 20 . In FIG. 1 , the characters 32 , 33 , and 34 are intended to portray player characters, controlled by players. The same interact with other players' player characters as well as with computer-controlled characters, termed non-player characters. The character 36 is intended to portray a non-player character, controlled by the simulation or game engine. That is, a non-player character is controlled by the simulation, either at the server level or by the client software, and the same acts in a way dictated by the software instructions and data set for that non-player character. A player may interact with the non-player character 36 by clicking on or otherwise activating icon 38 , this icon associated with the non-player character 36 . In some implementations, the player may also click directly on the non-player character.
[0029] A number of city features are also shown, such as a bank 22 , a city hall 24 , a convenience store 26 , and a private home 28 . The features will vary according to the applicable game environment. An icon 42 is also indicated adjacent the private home 28 . The user may click on such an icon 42 to, e.g., direct their focus to the private home 28 to perform any number of associated tasks, e.g., to rescue an occupant, prevent a crime, or the like. Each structure may have such an activatable element, according to the degree of interaction intended between player characters and the given structure.
[0030] A number of radii and circles, both full and partial, are illustrated, indicating how proximity to certain locations (or characters) may be employed to enhance the level of a player's immersion by providing scenarios and responses that are relevant to that player. For example, the center of the intersection of streets 30 and 31 serves as the locus of a circular zone of radius R player character or R personaContact . Similarly, the private home 28 serves as the locus of a circular zone of radius R SH or R SharedHistory . And in the same way, the bank 22 serves as the locus of a circular zone of radius R 1 .
[0031] Proximity to certain locations is just one way to initiate interactions that provide enhanced scenarios and responses. Other ways may include providing an activatable object that tells a player character about a non-player character, initiating an interaction where a non-player character plays alongside a player character, having a non-player character respond in a way that takes account of a player character's prior actions and exploits, or the like. Non-player characters within the game react to players, and their associated player characters, with a range of emotional responses cued by real-world events, player milestones, and player actions. They act as if their personalities are persistent and dynamic based on their personal history with a player character. This is not necessarily only a factional response, e.g., based on the player's reputation with a particular group for which the non-player character has a response set. Rather, it may be a deep series of verbal reactions, stories, and attitudes that convey the relationship status between the player and the character.
[0032] These and other aspects are discussed below in connection with FIGS. 3-5 .
[0033] FIG. 2 illustrates a logical diagram of a system 30 that may be employed to implement a simulation such as a multiplayer game. The system 30 includes an MMO or simulation client computing device 49 and an MMO or simulation server 45 which communicate by way of a network 48 . The client computing device 49 includes one or more processors 44 which communicates with the network 48 via a network card 46 or via a network-enabled processor (not shown). The client computing device 49 has client software running which enables communication with the network 48 and server 45 .
[0034] The client computing device 49 includes at least one input device 62 , which may include a keyboard, mouse, game controller, haptic controller, touchscreen, or other devices which may provide an input to a computer. The client 49 further includes a computer-readable medium 52 , such as a hard drive, flash memory, solid state drive, or the like, which stores instructions 54 for the processor 44 , including calculating module 56 . The computer-readable medium 52 may also store media files 58 , including graphics files, cinematics files, and media files for cut scenes. These media files may also be streamed when needed from the server 45 . In some implementations, certain media files may be downloaded to the client, especially those that are often used, and others may be kept at the server for later streaming, to avoid cluttering the client system. Certain media files are may also be cached at the client system, such as those pertaining to the immediate game locale of the player character.
[0035] The system 30 also includes a sound renderer 64 , such as a sound card, by which signals pertaining to game sounds may be put in a form suitable for playing on a sound device 68 , e.g., computer speakers. Moreover, the system 30 also includes a video renderer 66 , such as one or more GPUs or video cards, or both, by which signals pertaining to game video may be put in a form suitable for playing on a video device 72 , e.g., a computer display.
[0036] The simulation server 45 controls the game, and may be a game server having a processor 47 and running a game engine 61 and other components, including a physics engine 59 , user interface, input/output components, a database 57 , and the like. Certain of these components or modules may be implemented on a computer-readable medium 51 , which includes instruction 53 for carrying out these and other processes, including module 55 for calculating responses of non-player characters to player character actions. The computer-readable medium 51 may also include media files, including cinematics and cut scenes, for downloading or streaming to client computing devices 49 .
[0037] FIGS. 3-5 are flowcharts that illustrate certain ways to increase player immersion, primarily by enhancing the relationship of non-player characters to player characters. In particular, ways to enhance the relationship of non-player characters to player characters may include social communication, personal contact, and shared history.
[0038] The first way, an implementation of which is shown in FIG. 3 , is via social communication, which pertains to acts and speech which communicate information from the non-player character to a player character. In this aspect, the system and method provide ways to make a non-player character act and communicate in a more realistic fashion, in particular, by using historical events such as prior interactions, to make the non-player character's acts and communications more relevant to player characters (and thus players). In particular, the response of a non-player character to a player character action may be via one or more of various actions: a verbal response, an emotive response such as a frown, grin, or smile, or a physical response such as running away, attacking, a clap on the back, or the like. By way of the implementations of the system and method, the non-player character's responses, whether actions or communications, are based on more than just standard game variables. The responses are based on the player character, including milestones, actions, communications, as well as on in-game or world events, or in-game interpretations of world events. The responses may also be based on the player associated with the player character, including birthdays, anniversaries, and the like.
[0039] In the exemplary method 40 of FIG. 3 , a first step is to receive a first signal from a client computing device, the first signal indicating that a player character has initiated a communication with a non-player character (step 74 ). For example, and referring back to FIG. 1 , a player character may click on an activatable element or icon 38 associated with the non-player character 36 . Step 74 may include a step of receiving the first signal via the client computing device receiving a signal from an input device, e.g., from a game controller, keyboard, mouse, touchscreen, haptic controller, or via any other input device (step 82 ). The player may activate the element, icon, or non-player character for any number of reasons, including a request to converse, transact business such as to buy or sell items or trade skills, attack, subdue, protect, observe, rescue, transport to or away from a target location, and others.
[0040] This activating step, while sometimes employed, is not required in many implementations. That is, a non-player character may provide a response to a player with no activation step—the non-player character may provide the response, e.g., if the player character is within a certain proximity of the non-player character or a predetermined landmark. For example, as indicated in FIG. 1 , the player character 32 is shown within a radius R 1 from the bank 22 , and this proximity may be employed as a response trigger for a nearby non-player character. In the case where a response is triggered if a player character comes within a certain proximity or radius of a non-player character, then this radius may move if the non-player character moves.
[0041] Another way for a non-player character to interact with a player character is by way of a communication screen, or “communicator”. This is a pop-up display in the player's user interface that simulates a video phone call from the non-player character to the player character. Other aspects of such a response are described below in connection with ally personalization.
[0042] An optional step is to provide some indication to the player that they have activated, “clicked on”, or otherwise initiated a communication with the non-player character. This step may be accomplished by, e.g., highlighting or otherwise distinguishing the non-player character.
[0043] A second step is to calculate a response to the first signal, and transmitting a second signal back to the client computing device (step 78 ). The second signal, or another signal based thereon, is transmitted to a renderer and a rendering step is performed; this step may be accomplished, for example, by transmitting a second or corresponding signal to a GPU or video card or sound card (step 84 ) to render an indication of the response. The indication may be, e.g., an audio playback of words spoken by the non-player character, a textual indication of words so spoken, both, or the like.
[0044] The step 78 of calculating a response to the communication may be accomplished in a number of ways. For example, a response may be calculated based on prior acts of the player character (step 86 ). In other words, responses may be based on quests or tasks performed by the player character, prior communications between the player character and the non-player character, or prior communications between the player character and other characters, e.g., player characters or non-player characters, or combinations of these (step 92 ). Responses may also be given a degree of randomness (step 94 ). For example, a number of potential responses may be calculated using step 92 , and a random choice may then be made between the potential responses. The random choice ensures some degree of variety, variability and believability in the non-player character's response.
[0045] Another way to calculate a response is based on in-game events (step 88 ). For example, an in-game event may give rise to all player characters being offered certain quests or tasks related to the event. A calculated response may incorporate a mention of the in-game event or a mention of the related quests or tasks. As is known, in-game events may often be related to real life events or holidays.
[0046] In one implementation, responses may depend on player histories in the following way. Player activities across all play sessions are logged and metrics created. This metrics constitutes metadata which is then employed to drive the non-player character's state in relation to the player character. By playing the game and interacting with the non-player character, the player may skew this base state into a variety of alternate conditions. Thus there is an overall range of reactionary states in which a non-player character can be, and the player's behavior determines where on this spectrum the non-player character's responses fall.
[0047] Generally, not all non-player characters will be provided with a rich backstory. In some cases, only iconic characters are provided with such, or other characters which the developer desires to have a deeper level of communication with a player character. The amount and kind of characterization may depend primarily on the status of the player's relationship with the non-player character.
[0048] Non-player character responses for social communication may be categorized in the following non-limiting way. A first is “ally personalization” responses, e.g., voice-overs. These are responses that a non-player character sends directly to the player based on actions the player has taken, and may range from congratulations for quests successfully accomplished to admonishments for failure. Such responses may also include personal events in a player's life, such as birthdays or other important dates. Other types of ally personalization, often provided via text or voice-over, include: requests, where a non-player character requests that a player character undertake an action, and there may be variants of these requests depending on relationship or location; affirmation anchors, where a non-player character affirms actions a player character has taken; admonishment anchors, where a non-player character admonishes a player character for taking certain actions; temporal responses, where a non-player character responds to a player character in such a way as to make the player feel that the non-player character is aware of temporal events and their connection to the player, and may include past events such as anniversaries of accomplishments the non-player character and player character shared, present events such as the time of day or season, future events such as prompts or holidays established in-game or out-of-game, or personal events such as a birthday, the anniversary of the date the player began playing the game, accomplishments, or the like (assuming the same is in-character and appropriate for the non-player character to acknowledge).
[0049] Another type of response is “enemy personalization” responses, e.g., voice-overs. These are responses that a non-player character targets at a player character with a negative connotation, such as mocking or the like. These responses may also include memorable anniversaries, such as the non-player character reminding a player character of a previous battle or the like. Other types of enemy personalization, often provided via text or voice-over, include: challenge responses, where an enemy non-player character desires to challenge the player character to a face-to-face confrontation or to trick them into an action, and there may be variants of this based on relationship or location; curse or critical responses, which are negative versions of affirmations, where a non-player character curses or otherwise criticizes actions a player character has taken; temporal responses, which are similar to those described above in connection with ally personalization, but where the non-player character responds to a player character in a negative way.
[0050] Yet another type of response is related to in-game events, e.g., a non-player character's response reacting to events in-game. Such responses may include commands to players, e.g., missions, commentary, or opinions. Such responses may also include responses about group accomplishments.
[0051] Yet another type of response is a framing response, which may include the responses that a non-player character will employ to frame any content they are concerned about but not directly involved with. For example, a superhero may use a voice-over to let a player character know of an event at a given location, and that the superhero wants the player character to investigate. Such responses may be generally based on the content the character is involved in, and may be further divided into scenario type and location.
[0052] Another way to enhance the relationship of non-player characters to player characters, an implementation of which is shown in FIG. 4 , is via personal contact. Personal contact, also termed “action characterization,” means that the player character acts alongside the non-player character, in many cases fighting with or against him or her. In this implementation, quests, tasks, or the like, are arranged such that the non-player character purposely encounters the player character.
[0053] Referring to a method 50 depicted in the flowchart of FIG. 4 , a first step may include receiving a first signal indicating that a player character is within a predetermined distance from a personal contact spawning point (step 96 ). For example, in the implementation of FIG. 1 , player characters 33 and 34 are within a distance R player character from a personal contact spawning point, but player character 32 is not. This first step may include a step of receiving the first signal from the game engine (step 102 ), as the game engine may be the best source of data about where characters are in relation to each other and in relation to events of interest. Besides proximity to predefined locations, other triggers may be employed, including character mentions of keywords, proximity to certain non-player characters, and the like.
[0054] A second step is to initiate contact between a non-player character and the player character (step 98 ). The second step may be accomplished in a number of ways; in each way, generally, a second signal is transmitted to the client computing device (step 99 ). For example, a communication may be made from the non-player character to the player character, and the communication may then be rendered on the client computing device by a video or audio renderer (step 104 ). The communication may be a response that is calculated based on prior acts of the player character (step 112 ), such as quests or tasks performed by the player character, prior communications between the player character and the non-player character, or prior communications between the player character and other characters, e.g., player characters or non-player characters, or combinations of these. Responses may have a degree of randomness (step 114 ), for the same reasons and by the same techniques as indicated above in connection with steps 92 and 94 .
[0055] Another type of contact that may be initiated is to locate the non-player character in the vicinity of the player character (step 106 ). For example, the system may situate an iconic non-player character in the same vicinity as the player character, and the player character may then take the opportunity to play alongside, or against, the non-player character. In this case, the second signal causes the rendering of the non-player character in the vicinity of the player character.
[0056] In another example, the system may arrange a non-player character in a situation with the subject player character such that there is a common goal the two must accomplish, or alternatively work against each other to accomplish (step 108 ). In this case, the second signal causes the rendering of the non-player character in the vicinity of the player character and the notification of the player of the goal or goals the non-player character and player character are striving toward.
[0057] Generally, only non-player characters that are or will be part of actual gameplay scenarios may have this type of personal contact. The depth and scope of the personal contact may depend on the number of times the content calls for the non-player character to interact directly with players.
[0058] Non-player character responses for personal contact may be categorized in the following non-limiting way. Non-player characters may be provided with ally scenario responses, e.g., ally scenario voice-overs, for situations where the player character being addressed is an ally. Ally scenario responses may include: greetings, used at the beginning of a scenario, and which may include variants based on location or relationship to a player character, as well as variants based on the urgency of the scenario; objective responses, which are used to direct the player to accomplish specific tasks in an encounter, and which may include attacking, securing, protecting, transporting, destroying, or collecting a target; affirmation responses, which may be used to have the non-player character affirm the player character for successes, and different degrees of affirmation may be provided based on a player's qualitative or quantitative completion of an objective; admonishment responses, which are used to admonish the player character for mistakes, and as with affirmations different degrees of admonition may be provided; call-out responses, which are used by the non-player character as quick commands, such as “look out”, “over there”, or “stay back”; and culmination responses, employed at the completion of a scenario, and which may include variants based on location or relationship to a player character, as well as variants based on the scenario.
[0059] Similarly, non-player characters may be provided with enemy scenario responses, e.g., enemy scenario voice-overs, for situations where the player character being addressed is an enemy. Enemy scenario responses may include: interaction responses, which are generic responses employed to establish a non-player character or player character within the scenario; curse responses, which are employed when a player character is successful at a task, and there may be variants of this depending on the player character's degree of success; criticism responses, which are employed when a player character fails at a task, and there may be variants of this depending on the player character's degree of failure; call out responses, which are used by the non-player character as quick commands to his or her minions; and culmination responses, employed at the completion of a scenario, and which may include variants based on location or relationship to a player character, as well as variants based on the scenario.
[0060] Other potential personal contact responses include social responses, which again may be voice-overs or the like, and which may be the generic responses used by a non-player character in social settings. Social responses may include: greetings, used to greet player characters, and which may include variants based on location or relationship to a player character; affirmation anchor responses, which may have scenario and relationship variants and which may be used to have the non-player character affirm the player character for actions they have taken, which may be particularly relevant when a player character encounters an iconic non-player character after just playing through a scenario with them; admonishment anchor responses, which are used to admonish the player character for actions they have taken, which may have scenario and relationship variants; and redirection responses, which are employed to redirect a player to another general area or character, thus reinforcing the content line the player character is already on, emphasizing its importance.
[0061] Another potential personal contact response includes key moments responses, which again may be voice-overs or the like, and constitute specific responses non-player characters will use in corresponding specific scenarios.
[0062] As above, these responses may be in the form of voice-overs, visual effects, or a combination of the same.
[0063] For both personal contact and social communication, a given non-player character may have a range of responses, based on, e.g.: variety (to avoid repetition), relationship with the player character, and framing (to give context to what the player character is doing). For variety, i.e., in order to prevent too much repetition in phrases, each personal contact element may have, e.g., three variations, while social communication may vary as needed. Generally, shared history elements need not vary. To accommodate and account for differences in relationship with the non-player character, there may be provided a number of tiers of relationship: trusted, liked, neutral, disliked, or hated. Both personal contact and social communication may vary based on the tier. For framing, i.e., in order to frame the content users are playing, there may be location and scenario variants that allow the non-player character to give context to what the user is doing without specifically stating the same.
[0064] Yet another way to enhance the relationship of non-player characters to player characters, an implementation of which is shown in FIG. 5 , is via shared history, which provides a way for a player character to learn more about a non-player character. In this way, the player character may become aware of information about a non-player character's past history or exploits, and in this way receive an impression of the non-player character beyond just what they hear from the non-player character. For example, the player character may find a newsreel with footage about the origin of the non-player character. Other examples may include family videos, audio recordings, press clippings, personal diaries, photographs, writings or artworks, or the like. These items may be collected in the player character's inventory, and replayed whenever the user desires.
[0065] Referring to a method 60 depicted by the flowchart of FIG. 5 , a first step may include receiving a first signal indicating that a player character is within a predetermined distance from a shared history spawning point (step 116 ). This first step may include a step of receiving the first signal from the game engine (step 124 ), and/or the game database, as noted above in connection with FIG. 4 .
[0066] A second step is to choose a media file to play (step 128 ). This step may also occur after a user clicks on an activatable element as described below in connection with step 118 . The choice of media file may be by default or may be based on prior acts of the player character (step 134 ), as well as by other criteria. If prior acts are employed, the choice of media file may be based on quests or tasks performed by the player character, prior communications between the player character and the non-player character, or prior communications between the player character and other characters, e.g., player characters or non-player characters, or combinations of these. Also in this aspect, the choice of media file may have a degree of randomness (step 136 ), similar to steps 92 and 94 above. The choice of media file may also generally depend on whether the player has previously seen the media file, or whether the player has seen other shared history files which give a given media file context, e.g., “prerequisite” media files.
[0067] A next step is to transmit a second signal to the client computing device, the second signal in part causing the rendering of an activatable element pertaining to the non-player character (step 118 ). A part of this step may be accomplished, for example, by transmitting the second signal to a GPU or video card (step 126 ). This step provides an indication to the player that an opportunity for a shared history or background characterization has been offered.
[0068] As an example, in FIG. 1 , a shared history spawning point is illustrated as the private home 28 , and player characters within a proximity R SH may be enabled to see the activatable element 42 , such as an icon. For example, the player character 34 may see the element 42 , but not the player characters 32 and 33 .
[0069] By activating or clicking on the activatable element, the next step is initiated, that of rendering and playing back a media file corresponding to the non-player character (step 122 ).
[0070] In one implementation, the step 122 may include a step of playing back a cinematic sequence or cut scene (step 132 ). “Playing back” steps, such as step 132 , may include steps of sending the file to a renderer and performing a rendering step. Following playback, if appropriate, an item giving rise to the media file, e.g., a newsreel, may be placed in the player character's inventory and played back again at a subsequent time. Of course, not all shared history need be passive, e.g., watching media files. The same may involve dialogue with a non-player character or any other type of interaction in which history may be shared.
[0071] Whether social communication, personal contact, or shared history, the level of depth for which information about a non-player character is available may depend on the category of non-player character: primary, secondary, global, or generic. Primary characters, e.g., iconic non-player characters, may be provided with significant levels of all characterization types. Secondary characters serve a supporting role, and may be provided with more of one type of characterization than another, e.g., personal contact. Their social communication and shared history may be more limited, and may serve to support the primary characters. Global characters are similar to secondary ones, but have somewhat greater depth. These characters may be useful as information and content sources for player characters. Global characters may have some shared history and personal contact, but their focus may be social communication. Generic characters are ones that support the reality of a given scenario, and include firemen, policemen, thugs, and ordinary citizens. Such characters may have minimal personal contact, virtually no shared history, and their social communication may often be limited to specific scenarios. For example, a fireman may call for heroes to help fight a fire.
[0072] What have been described are systems and methods for managing the actions or responses of a digital entity in a simulation to reflect its interaction with a player character over time.
[0073] One implementation of the system and method includes one or more programmable processors and corresponding computer system components to store and execute computer instructions, such as to provide the server and client systems to operate the game environment and to monitor and control the data and interaction of non-player character's and player characters in the game environment. The modules, components, or portions thereof, may also be stored on one or more other servers, i.e., there is no requirement that all components be located on a common server, and in some cases certain components will be located on client computing devices.
[0074] Data may be tracked in various ways. In one implementation, the server stores data for a non-player character reflecting the past interactions with each player character and of events that are defined as relevant to the non-player character. For example, the system could store information about the state of the relationship between the two characters based on their last conversation and whether the player character helped the non-player character or not. Similarly, the system could store data reflecting significant events in the real world, such as the election of a president or the player's birthday, or in the game world, such as the player character's success or failure in a prominent mission or their joining a new organization. As part of maintaining the player character's data, various data about the player character will also be available to manage the non-player character reactions. For example, data such as the player's occupation, rank in an organization, age, and address could be used to form the non-player character's reaction. In this way, the non-player character will treat the player character more like a real person and, in turn, feel more like a real person to the player through its responses and reactions. Additional variations may be used depending on the nature of the game or system.
EXAMPLES
[0075] In one implementation, a server computer system in conjunction with one or more client computer systems provide an MMO that has a superhero theme where players create and use player characters which may be heroes or villains. The same may interact with superheroes or iconic villains. The following non-limiting examples are set in this milieu.
Example 1
Personal Contact
[0076] The player character, playing as a hero, may enter a dilapidated warehouse and find himself surrounded by enemies. He may go on the offensive, attempting to attack the group. An iconic non-player character superhero may then appear, defeating the group and calling the player character to follow the superhero deeper into the building.
Example 2
Social Communication
[0077] The player may be controlling a player character that is a minor villain. The player character may have pulled a few minor capers in the city. The player character's communicator may suddenly receive a communication from an iconic non-player character superhero, telling the player character that she has gone too far, and that the superhero will soon bring her to justice.
Example 3
Shared History
[0078] A hero or villain may find a newsreel depicting an important moment in the history of an iconic superhero. For example, in a grainy black-and-white picture it portrays a crime scene in an ally, with two victims lying prone and detectives taking photographs of the scene. The camera may pan to the superhero as a youth, watching the scene with emotion and being taken away to a new life.
[0079] It will be apparent to one of ordinary skill in the art, given this teaching, that variations in the above description will be encompassed by the scope of the claims. For example, the development system could be applied to other types of games, e.g., fantasy and science fiction games, or offline games. The event tracking could also apply to events that are defined in the game but do not directly involve the non-player character, e.g., a natural disaster that occurred in another location and causes the non-player character to have a new goal or request. In another example, a non-player character may use data reflecting indirect relationships as well, e.g., if the player character has done something beneficial for a friend of the non-player character, the non-player character may react favorably towards or mention the favor to the player character. Accordingly the scope of the invention is to be limited only by the claims appended hereto, and equivalents thereof.
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Apparatus and methods are provided to implement a technique for managing the response of a digital entity in a simulation to reflect its interaction with one or more players over time, such as managing a non-player character's responses to player characters in an online computer game. In the system, a computer system tracks the interaction of the digital entity with other entities and the occurrence or status of internal and external events to control how the digital entity reacts to current events and interactions.
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BACKGROUND OF THE INVENTION
The present invention is related to a signal display lamp which is suitable for signaling a warning or alerting to a particular condition.
The number of display lamps for signaling a warning or condition are legion in number. The use of LED's as the illuminating source has greatly increased the number of such lights since LED's require lower energy and generate less heat than incandescent bulbs and LED's do not expire as readily. While LED's have major advantages over conventional incandescent lights they require a different light design since LED's emit a light cone as opposed to the radiant light typically observed with incandescent lights.
Various designs have been presented to convert the light cone of an LED into a light globe as required in many applications.
One such example is provided in U.S. Pat. No. 5,769,532 wherein a series of reflectors are used to diffuse the light. This particular design is an improvement yet the light is still difficult to observe at steep angles from above and below the lamp.
A simple design which allows for a wide viewing area has been lacking in the art. The present invention provides a display lamp with an improved field of view.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a display light with a superior field of view.
It is another object to provide a display light which takes advantage of the superior qualities available with LED's while still providing a superior field of view.
These and other advantages are provided in a signal lamp comprising a base and at least one hollow cylindrical light transmitting column attached to the base. A light source is contained in the column wherein the light source comprises: a mounting plate; a globe reflector element attached to the mounting plate; and at least one LED directed toward the reflector element.
A preferred embodiment is provided in a signal lamp comprising a base and at least one hollow cylindrical transmitting column attached to said base. A light socket is contained within the column. Also within the column is a light source comprising: a mounting plate; a globe reflector attached to the mounting plate; and at least one LED attached to the mounting plate and directed towards the globe reflector. A light socket base is electrically connected to said LED and the light socket base is receivable within the light socket.
A particularly preferred embodiment is provided in a light source comprising a mounting plate and a globe reflector attached to the light mounting plate. A first LED is attached to the mounting plate and directed towards the globe reflector. The light source further comprises a light socket base electrically connected to the first LED.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a perspective view of the exterior of a fully assembled display lamp.
FIG. 2 is an exploded view of an embodiment of the present invention.
FIG. 3 is an exploded view of a preferred embodiment of the present invention.
FIGS. 4, 5 and 6 illustrate different embodiments of the LED configuration in the present invention.
FIG. 7 is an explanatory diagram illustrating optimal LED reflector separation.
FIG. 8 is a perspective view of a cylindrical parallel convex magnifier as employed in the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Throughout the following description similar elements are numbered accordingly.
FIG. 1 illustrates a signal light generally represented at 1. The signal light comprises a mounting bracket, 2, which is standard in the art for attaching a signal light to a piece of equipment or the like. An optional mounting pole, 3, may separate the mounting bracket from a base, 4, if desired. The electrical power source, not shown, is preferably enclosed in the mounting pole. The base, 4, is optional but preferred as a convenient location for wiring connections, control boards, if present, and as an attachment means for the elements necessary to form operating portions of the signal light. The design, appearance and function of the mounting bracket, mounting pole and base may be broadly interpreted as well known in the art.
The illuminating portion of the signal light comprises at least one cylindrical transmitting column, 5, which diffuses light. Between cylindrical transmitting columns are optional but preferred covers, 6, to isolate light to a single column. A cap, 7, attached with a mounting means, 8, covers the uppermost cylindrical transmitting column and eliminates, or reduces, light leak from the uppermost column.
FIG. 2 is an exploded view of an embodiment of the present invention. In FIG. 2, an optional mounting pole, 3, and base, 4, are as described previously. A mounting bracket assembly, 9, attaches to the base, 4, by engaging a pair of tubes, 12, over a pair of lugs, 10, which are integral to the base. The tube can attach to the lug by a variety of methods as known in the art including snap-fit, or a threaded rod interior to the tube. The mounting bracket assembly, 9, comprises a bracket plate, 11, and a top plate 19, both rigidly attached to the tubes. A support, 21, attached to the bracket plate, 11, provides support for the light source which will be described in further detail below. The mounting bracket assembly, and attached light source are received within the cylindrical transmitting column, 5, which is in turn secured in place by a cap, 7. The cap, 7, is secured to the top plate, 19, by an attachment means, 8, such as a screw or rivet, which is inserted through a hole, 20, in the cap.
The light source comprises at least one LED, 18, attached to a mounting plate, 16. Each LED is directed toward a globe reflector, 17. Light is emitted from the LED which reflects off of the globe reflector and is emitted through the cylindrical transmitting column.
FIG. 3 comprises a preferred embodiment of the present invention. In FIG. 3 the bracket plate, 11, comprises a light socket, 14, and the light source comprises a light socket base, 15. The light socket and light socket base preferably comprise complementary threads, as common in an AC light bulb, or complementary protrusions and slots, as common in a DC automobile, such that the light source can be easily removed and replaced in the event of a LED burnout or the like. This embodiment also allows for the replacement of the light source with a light source of more, or fewer, LED's.
FIGS. 4, 5 and 6 illustrate various configurations of the light source. FIG. 4 illustrates the preferred orientation when four LED's are used. The four LED's are arranged in a square with the globe reflector in the center of the square. The four LED's and the globe reflector form a plane. The mounting plate is illustrated as a square for convenience, however, any shape is considered within the teachings of the present invention. FIG. 5 illustrates a linear arrangement which is the preferred orientation with two LED's. In this arrangement the two LED's and the globe reflector form a line. In FIG. 6 three LED's are arranged in an equilateral triangle with the globe reflector contained in the center. The number of LED's is not particularly limiting. It is most preferable for the LED's to be symmetrically arranged.
The optimal spacing between the LED and the reflector is determined by the light cone of the LED. The optimal spacing is illustrated in FIG. 7. As shown in FIG. 7 the LED, 18, emits directed light in a cone the boundaries of which are represented by ray lines, 24. The optimal distance between the LED and the reflector is that which allows the ray lines to be tangential to the reflector as shown in FIG. 7. If the distance between the reflector and LED is greater than the optimal distance some of the light emitted from the LED bypasses the reflector resulting in a shadow on the opposite side of the light source. If the distance is too short then the maximum reflective cone is compromised.
A preferred cylindrical transmitting column is illustrated in FIG. 8. In FIG. 8 a cylindrical parallel convex magnifier, 22, is illustrated. The cylindrical parallel convex magnifier, 22, comprises a multiplicity of linear convex lens, 23, arranged in parallel on the surface of a cylinder. The cylindrical parallel convex magnifier is extremely efficient at reflecting light and diffuses the light source sufficiently that the entire cylinder appears to be illuminated.
The globe reflector is most preferably a polished sphere or an ellipse. If an ellipse is used the ratio of the major axis to the minor axis is preferably no more than 2 to 1. Most preferably the globe does not contain facets. Facets can be employed with small facets being preferred. As the size of the facet increases the light becomes more anisotropic which is not desirable. The size of the globe reflector is chosen to optimize the distance from the LED and the cone required for adequate lighting.
The present invention has been illustrated and described and the preferred embodiments thereof have been provided. It would be apparent that a skilled artisan could employ other embodiments without departing from the scope of the invention as described herein and illustrated with the examples.
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The present invention is directed to an improved signal light. The signal lamp comprising a base and at least one hollow cylindrical light transmitting column attached to the base. A light source in contained in the column wherein the light source comprises: a mounting plate; a globe reflector element attached to the mounting plate; and at least one LED directed toward the reflector element.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is related to concurrently filed application Ser. No. ______, titled GAS TURBINE COMPRESSOR INLET PRESSURIZATION AND FLOW CONTROL SYSTEM, filed jointly in the names of John Anthony Conchieri, Robert Thomas Thatcher, and Andrew Mitchell Rodwell and application Ser. No. ______, titled GAS TURBINE COMPRESSOR INLET PRESSURIZATION HAVING A TORQUE CONVERTER SYSTEM, filed jointly in the names of Sanji Ekanayake and Alston I. Scipio, each assigned to General Electric Company, the assignee of the present invention.
TECHNICAL FIELD
[0002] The subject matter disclosed herein relates to combined cycle power systems and more particularly to supercharged combined cycle systems with air flow bypass.
BACKGROUND
[0003] Combined cycle power systems and cogeneration facilities utilize gas turbines to generate power. These gas turbines typically generate high temperature exhaust gases that are conveyed into a heat recovery steam generator (HRSG) that produces steam. The steam may be used to drive a steam turbine to generate more power and/or to provide steam for use in other processes.
[0004] Operating power systems at maximum efficiency is a high priority for any generation facility. Factors including load conditions, equipment degradation, and ambient conditions may cause the generation unit to operate under less than optimal conditions. Supercharging (causing the inlet pressure to exceed the exhaust pressure) turbine systems as a way to increase the capacity of gas-turbine is known. Supercharged turbine systems typically include a variable speed supercharging fan located at the gas turbine inlet that is driven by steam energy derived from converting exhaust waste heat into steam. The supercharging fan is used to increase the air mass flow rate into the gas turbine so that the gas turbine shaft horsepower can be augmented.
[0005] A problem with conventional supercharged combined cycle systems is that they are uneconomical due primarily to the prevailing “spark spread.” Spark spread is the gross margin of a gas-fired power plant from selling a given amount of electricity minus the cost of fuel required to produce that given amount of electricity. Operational, maintenance, capital and other financial costs must be covered from the spark spread. Another problem with conventional supercharged systems is that controlling the inlet fan is difficult. In many cases, the return on investment of such systems is not attractive. Conventional supercharged combined cycle systems do not provide customers with sufficient system flexibility, output and efficiency over the system life cycle. Additionally, those systems require significant modifications and are sometimes not compatible with legacy systems.
BRIEF DESCRIPTION OF THE INVENTION
[0006] In accordance with one exemplary non-limiting embodiment, the invention relates to a combined cycle system including a gas turbine subsystem having a compressor and an output side that provides an exhaust, and a heat recovery steam generation subsystem having an inlet. An exhaust duct is coupled to the gas turbine system and the inlet for transporting the exhaust to the heat recovery steam generation system. The system also includes a controllable air stream source that produces an air flow and a ducting assembly coupled to the controllable air stream source that conveys at least a portion of the air flow to the compressor. A bypass coupled to the controllable air stream source and the exhaust duct adapted to selectively convey at least a portion of the air flow to the inlet is also provided.
[0007] In another embodiment, a supercharging system is provided, the system including a forced draft fan providing a variable air flow. A duct that directs at least a portion of the air flow to a compressor and a bypass subsystem that diverts at least a portion of the air flow to a heat recovery steam generator are also provided. The system includes a control system coupled to the bypass subsystem and the forced draft fan.
[0008] In another embodiment, a method of operating a combined cycle system includes determining a first operating state and determining a desired operating state. The method includes determining a first mass flow quantity of air to be provided to a compressor and a second mass flow quantity of air to be provided to a heat recovery steam generator to achieve the desired operating state. The method includes providing source of controllable air flow, selectively conveying the first mass flow quantity of air into the compressor; and selectively conveying the second mass flow quantity of air to the heat recovery steam generator.
[0009] Other features and advantages of the present invention will be apparent from the following more detailed description of the preferred embodiment, taken in conjunction with the accompanying drawings which illustrate, by way of example, the principles of certain aspects of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a schematic illustration of an embodiment of a supercharged combined cycle system with air bypass.
[0011] FIG. 2 is a schematic illustration of another embodiment of a supercharged combined cycle system with air bypass.
[0012] FIG. 3 is a flow chart of an embodiment of a method implemented by a supercharged combined cycle system with air bypass.
[0013] FIG. 4 is a chart illustrating a result accomplished by a supercharged combined cycle system with air bypass.
[0014] FIG. 5 is a flow chart of an embodiment of a method implemented by a supercharged combined cycle system with air bypass.
[0015] FIG. 6 is a chart illustrating a result accomplished by a supercharged combined cycle system with air bypass.
[0016] FIG. 7 is a chart illustrating a result accomplished by a supercharged combined cycle system with air bypass.
DETAILED DESCRIPTION OF THE INVENTION
[0017] Illustrated in FIG. 1 is a schematic illustration of a supercharged combined cycle system with air bypass (SCCAB system 11 ) in accordance with one embodiment of the present invention. The SCCAB system 11 includes a gas turbine subsystem 13 that in turn includes a compressor 15 , having a compressor inlet 16 , a combustor 17 and a turbine 19 . An exhaust duct 21 may be coupled to the turbine 19 and a heat recovery steam generator subsystem (HRSG 23 ). The HRSG 23 recovers heat from exhaust gases from the turbine 19 that are conveyed through HRSG inlet 24 to generate steam. The HRSG 23 may also include a secondary burner 25 to provide additional energy to the HRSG 23 . Some of the steam and exhaust from the HRSG 23 may be vented to stack 27 or used to drive a steam turbine 27 and provide additional power. Some of the steam from the HRSG 23 may be transported through process steam outlet header 28 to be used for other processes. The SCCAB system 11 may also include an inlet house and cooling system 29 . The inlet house and cooling system 29 is used to cool and filter the air entering the compressor inlet 16 to increase power and avoid damage to the compressor 15 .
[0018] The SCCAB system 11 also includes a forced draft fan 30 used to create a positive pressure forcing air into the compressor 15 . Forced draft fan 30 may have a fixed or variable blade fan (not shown) and an electric motor (not shown) to drive the blades. Forced draft fan 30 may be driven by a variable frequency drive (VFD 31 ) that controls the rotational speed of the electric motor by controlling the frequency of the electrical power supplied to the motor. VFD 31 provides a number of advantages, including energy savings from operating at lower than nominal speeds. Another advantage is that VFD 31 may be gradually ramped up to speed lessening the stress on the equipment. The forced draft fan 30 provides a controllable air stream source though a duct assembly 32 and may be used to increase the mass flow rate of air into the compressor 15 . The quantity of air going into the compressor is controlled by the VFD 31 . The compressor inlet 16 may be configured to accommodate slight positive pressure as compared to the slight negative pressure conventional design.
[0019] The SCCAB system 11 may also include a bypass 33 (which may include external ducting) that diverts a portion of the air flow from forced draft fan 30 into the exhaust duct 21 . This increased air flow provides additional oxygen to the secondary burner 25 to avoid flame out or less than optimal combustion. Bypass 33 may be provided with a flow sensor 35 and a damper valve 37 to control the airflow through the bypass 33 . A control system 39 may be provided to receive data from flow sensor 35 and to control the damper valve 37 and the VFD 31 . Control system 39 may be integrated into the larger control system used for operation control of SCCAB system 11 . The airflow from the bypass is conveyed to the exhaust duct 21 where the temperature of the combined air and exhaust entering the HRSG 23 may be modulated.
[0020] Illustrated in FIG. 2 is another embodiment of a SCCAB system 11 that includes a pair of gas turbine subsystems 13 . In this embodiment, the exhaust of the pair of gas turbine subsystems 13 is used to drive a single steam turbine 27 . In this embodiment, an inlet house 41 is positioned upstream of the forced draft fan 30 , and a cooling system 43 , where the airflow from the fan may be cooled, is positioned downstream of the forced draft fan 30 . The bypass 33 is coupled to the cooling system 43 . One of ordinary skill in the art will recognize that although in this embodiment two gas turbine systems 13 are described, any number of gas turbine systems 13 in combination with any number of steam turbine(s) 27 may be used.
[0021] In operation, the SCCAB system 11 provides increased air flow into the HRSG 23 resulting in a number of benefits. The SCCAB system 11 may provide an operator with the ability to optimize combined cycle plant flexibility, efficiency and lifecycle economics. For example, boosting the inlet pressure of the gas turbine subsystem 13 improves output and heat rate performance. The output performance of the SCCAB system 11 may be maintained flat (zero degradation) throughout the life cycle of SCCAB system 11 by increasing the level of supercharging (and parasitic load to drive the forced draft fan 30 ) over time commensurate with the degradation of SCCAB system 11 . The use of the VFD 31 to power the forced draft fan 30 enables and substantially improves system efficiencies under partial-supercharge conditions. Another benefit that may be derived from the SCCAB system 11 is the expansion of the power generation to steam production ratio envelope. This may be accomplished by modulating the exhaust gas temperature at HRSG inlet 24 with air from the forced draft fan 30 . Another benefit that may be derived from the SCCAB system 11 is an improved start up rate as a result of the reduction in the purge cycle (removal of built up gas). The SCCAB system 11 may also provide an improved load ramp rate resulting from the modulation of the exhaust temperature at the exhaust duct 21 with air from the forced draft fan 30 provided through the bypass 33 . The forced draft fan 30 of the SCCAB system 11 also provides an effective means to force-cool the gas turbine subsystem 13 and HRSG 23 , reducing maintenance outage time and improves system availability. The forced draft fan 30 provides comparable benefit for simple cycle and combined-cycle configurations for all heavy-duty gas turbine systems 13 delivering in the range of 20% output improvement under hot ambient conditions with modest capital cost.
[0022] The SCCAB system 11 may implement a method of maintaining the output of a combined cycle plant over time (method 50 ) as illustrated with reference to FIGS. 3-4 . In FIG. 3 the method 50 may determine the current state (method element 51 ), and may determine a desired state (method element 53 ). The desired state may be to maintain a nominal output over time to compensate for performance losses. Performance losses typically arise as a result of wear of components in the gas turbine over time. These losses may be measured or calculated. The method 50 may determine the required increased air mass flow to maintain the desired output (method element 55 ). Based on that determination, the method 50 may adjust the air mass flow into the compressor inlet 16 (method element 57 ). The method 50 may adjust the combined air and exhaust mass flow into the HRSG inlet 24 (method element 59 ).
[0023] FIG. 4 illustrates the loss of output and heat rate over time (expressed in percentages) of a conventional combined cycle system and a SCCAB system 11 . Gas turbines suffer a loss in output over time, as a result of wear of components in the gas turbine. This loss is due in part to increased turbine and compressor clearances and changes in surface finish and airfoil contour. Typically maintenance or compressor cleaning cannot recover this loss, rather the solution is the replacement of affected parts at recommended inspection intervals. However, by increasing the level of supercharging using forced draft fan 30 output performance may be maintained, although at a cost due to the parasitic load to drive the forced draft fan 30 . The top curve (unbroken double line) illustrates the typical output loss of a conventional combined cycle system. The second curve (broken double lines) illustrates the expected output loss with periodic inspections and routine maintenance. The lower curve (broken triple line) shows that the output loss of an SCCAB system 11 may be maintained at near 0%. Similarly, the heat rate degradation of a conventional combined cycle system (single solid curve) may be significantly improved with an SCCAB system 11 .
[0024] FIG. 5 illustrates a method of controlling the steam output of a SCCAB system 11 (method 60 ). Method 60 may initially determine the current state (method element 61 ). The method 60 may also determine the desired output and steam flow (method element 63 ). The method 60 may determine the required increased air flow (method element 65 ) to the compressor inlet 16 and the HRSG inlet 24 . Method 60 may then adjust the air flow into the compressor inlet 16 (method element 67 ) and the combined exhaust and air flow into the HRSG inlet 24 (method element 69 ), to provide the desired steam output.
[0025] FIG. 6 illustrates expanded operating envelope to maintain constant steam flow. The vertical axis measures output in MW and horizontal axes measures steam mass flow. The interior area (light vertical cross hatch) shows the envelope of a conventional combined cycle system. The envelope of an SCCA 11 is shown in diagonal cross hatching, and a larger area illustrates the performance of an SCCA 11 combined with secondary firing in the HRSG 23 .
[0026] FIG. 7 is a chart that illustrates the improved operational performance of an SCCAB system 11 at a specific ambient temperature in comparison with conventional combined cycle systems at minimum and base loads. The horizontal axis measures output in MW and the vertical axis measures heat rate (the thermal energy (BTU's) from fuel required to produce one kWh of electricity). The chart illustrates the improved efficiency delivered by the SCCAB system 11 .
[0027] The foregoing detailed description has set forth various embodiments of the systems and/or methods via the use of block diagrams, flowcharts, and/or examples. Insofar as such block diagrams, flowcharts, and/or examples contain one or more functions and/or operations, it will be understood by those within the art that each function and/or operation within such block diagrams, flowcharts, or examples can be implemented, individually and/or collectively, by a wide range of hardware. It will further be understood that method steps may be presented in a particular order in flowcharts, and/or examples herein, but are not necessarily limited to being performed in the presented order. For example, steps may be performed simultaneously, or in a different order than presented herein, and such variations will be apparent to one of skill in the art in light of this disclosure.
[0028] This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any incorporated methods. The patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims.
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A system and method for supercharging a combined cycle system includes a forced draft fan providing a variable air flow. At least a first portion of the air flow is directed to a compressor and a second portion of the airflow is diverted to a heat recovery steam generator. A control system controls the airflows provided to the compressor and the heat recovery steam generator. The system allows a combined cycle system to be operated at a desired operating state by controlling the flow of air from the forced draft fan to the compressor and the heat recovery steam generator.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an imaging apparatus for electronic endoscopes.
2. Description of the Prior Art
The conventional electronic endoscope is mostly configured so as to form a image of an object by a circular lens system 32 on a nearly square image pickup device 31, process this image by an image processing circuit 33 and project a processed image 36 onto a display unit 35 of a TV monitor 34 as illustrated in FIG. 16.
The display unit 15 of the TV monitor 14 has a screen which is designed for an aspect ratio of H:V=4:3 in accordance with the current TV code (NTSC standard). Therefore, only a narrow screen area of the display unit 35 is used wastelessly when the image is projected to a partial area of the screen of the display unit 35 as shown in FIG. 16.
However, the high quality TV set adopts a display unit which has a screen designed for an aspect ratio of H:V=16:9, or is horizontally elongated. In case of an endoscope for the high quality TV set, a large screen area is utilized wastelessly when the square image formed by the electronic endoscope shown in FIG. 16 is projected onto the horizontally elongated screen of the display unit 15.
The problem of such wasteless use of the screen of the display unit can be solved by using a horizontally elongated solid-state image pickup device, but such a solid-state image pickup device will undesirably enlarge an outside diameter of an endoscope.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide an imaging apparatus configured so as to permit observing images which are made strongly appealing or highly impressive by effectively utilizing the horizontally elongated screen of the display unit of the high quality TV set.
The imaging apparatus according to the present invention comprises a nearly square solid-state image pick-up device, composed, for example, of CCD's, an objective lens system using at least one aspherical surface which is asymmetrical with regard to an optical axis and electrically elongating means.
A composition of the imaging apparatus according to the present invention is illustrated in FIG. 1, wherein the reference numeral 1 represents the solid-state image pickup device, the reference numeral 2 designates the objective lens system, the reference numeral 3 denotes a sampling circuit, the reference numeral 4 represents a hold circuit, the reference numeral 5 designates a video signal generating circuit, the reference numeral 6 denotes a TV monitor, the reference numeral 7 represents a display unit having a horizontally elongated screen, the reference numeral 8 designates a light source and the reference numeral 9 denotes a light guide fiber bundle.
In the imaging apparatus according to the present invention, the objective lens system having at least one aspherical surface which is revolutionally asymmetrical with regard to the optical axis functions to form an image of a rectangular range of an object on the solid-state image pickup device 1 which is nearly square.
Further, signals provided from the solid-state image pickup device 1 are read out by the sampling circuit 3 at a readout speed in the horizontal direction (a horizontal scanning direction) on the solid-state image pickup device 1 which is set at a level lower than the ordinary horizontal readout speed for elongating the image of the object in the horizontal direction.
Let us represent a vertical size and a horizontal size of the image of the object by B V and B H respectively, designate a vertical size and a horizontal size of the solid-state image pickup device 1 by C V and C H respectively, and denote numbers of picture elements of CCD's disposed in the horizontal direction and the vertical direction on the solid-state image pickup device 1 by N H and N V respectively. Then, the objective lens system 2 forms, on the solid-state image pickup device 1, an image which is contracted at a ratio multiplied by k expressed by the following formula (1):
(C.sub.H /B.sub.H)/(C.sub.V /B.sub.V).tbd.k (1)
C V /C H is larger than V/H.
It is therefore possible to obtain a horizontally elongated image by selecting the readout speed 1/k times as high as the ordinary readout speed for reading out the signals provided from the solid-state image pickup device 1.
The image is not elongated in the horizontal direction when a number of the picture elements disposed in the vertical direction on the solid-state image pickup device 1 corresponds to a number N V of the scanning lines at a given average scanning times T H (≈33 microseconds) on the high quality TV set and a given aspect ratio A (≈16/9) of the display unit of the high quality TV set. That is to say, the picture elements disposed on the solid-state image pickup device 1 which is used in the ordinary manner are read out at a time interval t H expressed by the following formula (2):
t.sub.H ≈N.sub.V /N.sub.HD ·C.sub.H /C.sub.V ·1/A·T.sub.H /N.sub.H ( 2)
This formula is obtained on an assumption that blanking periods are sufficiently short in both the horizontal direction and the vertical direction.
In the formula mentioned above, the reference symbol N HD represents a number of scanning lines in the vertical direction on the high quality TV set (1,125 in Japanese standard).
An image which is elongated k times as large in the horizontal direction can be obtained by reading out the signals provided from the solid-state image pickup device at intervals of 1/k·t H per picture element.
Signals which are sampled by the sampling circuit 3 are held by the hold circuit 4, then converted into luminance signals and color difference signals by the video signal generating circuit 5, and displayed on the display unit 7.
FIG. 2 shows another example of the imaging apparatus for magnifying, at a ratio 1/k times as high, an image which is contracted k times as large in one direction.
In this example, the video signals provided from the solid-state image pickup device 1 are stored once in a memory 10 and magnified 1/k times as large by a computerized image processing circuit 11.
This imaging apparatus can perform not only the magnification of an image 1/k times as large by the image processing circuit 11 but also correction of distortion produced by a lens system, thereby providing an image which is more correct than the image available with the imaging apparatus shown in FIG. 1. Further, the imaging apparatus shown in FIG. 2 can provide an image which is deformed as desired. In case of this imaging apparatus, signals of R.G.B. code which are generated by a video signal generating circuit 12 are displayed on a TV monitor.
Now, description will be made of an objective lens system which is to be used in the imaging apparatus according to the present invention.
The objective lens system to be used in the imaging apparatus according to the present invention has magnifications which are different between the horizontal direction and the vertical direction, and satisfies the following condition (4):
β.sub.z /β.sub.y ≈k (4)
wherein the reference symbol β z represents the magnification in the horizontal direction and the reference symbol β y designates the magnification in the vertical direction.
The objective lens system is an anamorphic lens system which is shown in FIG. 3A and FIG. 3B, or a retrofocus type lens system having a composition in which at least one revolutionally asymmetrical aspherical surface (A S ) is disposed in each of sections located before and after an aperture stop. This aspherical surface (A S ) has a small radius of curvature in FIG. 3A which shows a sectional view taken in the horizontal direction (horizontal sectional view) but a large radius of curvature in FIG. 3B which shows a sectional view taken in the vertical direction (vertical sectional view) of the objective lens system.
The aspherical lens system having the aspherical surfaces A S described above has a form similar to that of a rugby ball as illustrated in FIG. 4 and is expressed by the following formula (5): ##EQU1## wherein the reference symbol i represents an ordinal number of a surface, the reference symbols x, y and z designate values on x, y and z axes respectively on an coordinates system on which the direction of the optical axis is taken as the x axis and a vertex of an aspherical surface is taken as an origin, the reference symbol R i denotes a radius of a reference sphere of the aspherical surface, the reference symbols B yi , B zi , . . . represent aspherical surface coefficients, and the reference symbols E 1i , E 2i , . . . designate aspherical surface coefficients.
This formula does not contain y and z of odd orders because the aspherical surface is symmetrical with regard to a horizontal section and a vertical section respectively. Further, the first term of the formula expresses a component of a centered spherical surface. The origin shown in FIG. 4 corresponds to the vertex of the aspherical surface. Further, radii of curvature R y and R z in the y and z directions on an elliptic parabaloid which is in contact with the vertex of the aspherical surface are given by the following formulae (6) and (7):
1/R.sub.y =2B.sub.y ( 6)
1/R.sub.z =2B.sub.z ( 7)
At least one aspherical surface expressed by the above-mentioned formula (5) need be disposed in the objective lens system and it is advantageous to use two or more aspherical surfaces on both the sides of the stop as shown in FIG. 3 for correcting astigmatism, curvature of field and on-axis astigmatism Δ.
The on-axis astigmatism Δ means a distance as measured between a paraxial image point in the horizontal direction and another image point in the vertical direction, and an image will be blurred when the on-axis astigmatism Δ has a value which is not sufficiently small.
Conditions which are required for imparting a small value to the on-axis astigmatism Δ and enabling to contract an image in the horizontal direction will be described below:
Let us assume that anamorphic surfaces (toric surfaces) i and j, such as that shown in FIG. 4, are disposed before and after the stop respectively, represent refractive indices of media disposed before and after the surface i by n i-1 and n i respectively, and designates refractive indices of media disposed before and after the surface k by n j-1 and n j respectively. Then, the surfaces i and j have refractive powers in the horizontal direction (z direction) and vertical direction (v direction) which are defined as follows:
φ.sub.yi =2(n.sub.i -n.sub.i-1)B.sub.yi ( 10)
φ.sub.zi =2(n.sub.i -n.sub.i-1)B.sub.zi ( 11)
φ.sub.yj =2(n.sub.j -n.sub.j-1)B.sub.yj ( 12)
φ.sub.zj =2(n.sub.j -n.sub.j-1)B.sub.zj ( 13)
wherein the reference symbol φ yi represents a refractive power of the surface i in the vertical direction, the reference symbol φ zi designates a refractive power of the surface i in the horizontal direction, the reference symbol φ yi denotes a refractive power of the surface j in the vertical direction and the reference symbol φ zj represents a refractive power of the surface j in the horizontal direction.
For contracting an image in the horizontal direction, it is sufficient that the anamorphic surface disposed before the stop satisfies the condition (14) and that the anamorphic surface disposed after the stop satisfies the condition (15):
φ.sub.yi >φ.sub.zi ( 14)
φ.sub.yj <φ.sub.zj ( 15)
The anamorphic surfaces should be disposed in the vicinities of an object side lens component and an image side lens component respectively on which a principal ray is higher than a marginal ray.
For correcting the on-axis astigmatism Δ until it has a value of 0 in the objective lens system, on the other hand, it is necessary, from a viewpoint of its function to converge paraxial rays, to satisfy the following condition (16):
(φ.sub.zi -φ.sub.yi)(φ.sub.zj -φ.sub.yj)<0 (16)
The relationship expressed by the condition (16) establishes when the conditions (14) and (15) are satisfied.
By disposing the anamorphic surfaces satisfying the conditions (14) and (15) before and after the aperture stop respectively, it is therefore possible to obtain an objective lens system which forms an image contracted in the horizontal direction in which the on-axis astigmatism Δ has a small value.
When the objective lens system is to use three or more anamorphic surfaces including at least two which are to be disposed before and after the aperture stop respectively, it is necessary for contracting an iamge in the horizontal direction that any one of the anamorphic surfaces satisfies the condition (14) or (15).
For correcting the on-axis astigmatism Δ until it has a value of 0, at least a pair of surfaces m and n must satisfy the following condition (17):
(φ.sub.zm -φ.sub.ym)(φ.sub.zn -φ.sub.yn)<0 (17)
wherein the reference symbol φ zm represents a refractive power in the z direction of the surface m, the reference symbol φ ym designate a refractive power in the y direction of the surface m, the reference symbol φ zn denotes a refractive power in the z direction of the surface n and the reference symbol φ yn represents a refractive power in the y direction of the surface n.
For correcting the on-axis astigmatism Δ until it has a value of 0 in a lens system comprising anamorphic surfaces, it is necessary to satisfy in place of the conditions (14) and (15), the following conditions (18) and (19): ##EQU2##
Alternately, it is possible for reducing the on-axis astigmatism Δ to a value of 0 to replace the condition (17) with the following condition (20): ##EQU3## wherein the reference symbols h zn and h yn represent the height of paraxial rays on the surface n in the z direction and the y direction respectively.
The condition (20) means that a total sum of angles of refraction for the paraxial rays in the z direction is equal to that in the y direction, and is required for reducing the on-axis astigmatism Δ until it has a value of 0. In practice, however, it is sufficient to satisfy the following condition (21) shown below in place of the condition (20): ##EQU4## wherein the reference symbol φ z represents a reverse number of f z which is a focal length in the z direction, the reference symbol φ y designates an inverse number of f y which is a focal length in the y direction, and the reference symbols h z0 and h y0 denote heights of incidence of the paraxial rays on the first surface in the z direction and the y direction respectively.
A lens system which uses an anamorphic surface disposed only before or after the aperture stop cannot have both the functions to contract an image in the horizontal direction and reduce the on-axis astigmatism Δ to 0, but can exhibit an effect which is rather satisfactory since it can reduce the on-axis astigmatism Δ nearly to 0 when the marginal ray is lower than the principal ray on the anamorphic surface. For obtaining such an effect, the anamorphic surface should be disposed in the vicinity of a surface which is apart from the stop, i.e., an object side surface or an image side surface. The condition (14) should be satisfied when the anamorphic surface is disposed before the stop or the condition (15) should be satisfied when the anamorphic surface is disposed after the aperture stop.
When two or more anamorphic surfaces are to be disposed only before or after the aperture stop, it is possible to obtain the functions to contract an image in the horizontal direction and reduce the on-axis astigmatism Δ to 0 by configuring at least one of the anamorphic surfaces to be disposed before the aperture stop so that it satisfies the condition (14) or configuring at least one of the anamorphic surfaces to be disposed after the aperture stop so that it satisfies the condition (15).
For reducing the on-axis astigmatism Δ until it has a value of 0, it is necessary that at least a pair of surfaces k and l satisfy the following condition (22):
(φ.sub.zk -φ.sub.yk)(φ.sub.z1 -φ.sub.z1)<0 (22)
The anamorphic surfaces should desirably have shapes which are not circular at least in a horizontal section or a vertical section thereof so that optional shapes of aspherical surface can be selected for favorable correction of astigmatism.
A range allowable for the on-axis astigmatism selected for the examples described above is defined by the following formula (23): ##EQU5## wherein the reference symbols F Noy and F Noz represent F numbers in the y direction and the z direction respectively, and the reference symbols P V and P H designate lengths in the horizontal direction and the vertical direction respectively of a single picture element of the CCD disposed on the solid-state image pickup device 1.
The solid-state image pickup device 1 should be disposed on the optical axis at a location in the middle of a paraxial image point in the horizontal direction and a paraxial image point in the vertical direction or a location slightly shifted from the middle location toward the lens system when curvature of field is taken into consideration.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a sectional view illustrating a composition of the imaging apparatus according to the present invention;
FIG. 2 shows a sectional view illustrating a composition of another example of the imaging apparatus according to the present invention;
FIG. 3A and FIG. 3B show diagrams compositions of lens systems to be used in the imaging apparatus according to the present invention;
FIG. 4 shows a view illustrating a shape of an aspherical surface to be used in the lens systems shown in FIG. 3A and FIG. 3B;
FIG. 5 shows a horizontal sectional view illustrating a composition of a first embodiment of the lens system to be used in the imaging apparatus according to the present invention;
FIG. 6 shows a vertical sectional view illustrating the first embodiment of the lens system;
FIG. 7 shows a horizontal sectional view illustrating a second embodiment of the lens system to be used in the iamging apparatus according to the present invention;
FIG. 8 shows a vertical sectional view illustrating the second embodiment of the lens system;
FIG. 9A, FIG. 9B and FIG. 9C show graphs illustrating aberration characteristics in the horizontal direction of the second embodiment of the lens system;
FIG. 10A, FIG. 10B and FIG. 10C show graphs visualizing aberration characteristics in the vertical direction of the first embodiment of the lens system;
FIG. 11A, FIG. 11B and FIG. 11C show curves illustrating aberration characteristics in the horizontal direction of the second embodiment of the lens system;
FIG. 12A, FIG. 12B and FIG. 12C show curves visualizing aberration characteristics in the vertical direction of the second embodiment of the lens system;
FIG. 13 shows a sectional view illustrating a composition of an illumination optical system to be used for an electronic endoscope which comprises the imaging apparatus according to the present invention;
FIG. 14 shows a perspective view of another example of the illumination optical system to be used in the electronic endoscope;
FIG. 15A and FIG. 15B show a horizontal sectional view and a vertical sectional view respectively of the illumination optical system shown in FIG. 14; and
FIG. 16 shows a view schematically illustrating a configuration of the conventional imaging apparatus.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Now, the imaging apparatus according to the present invention will be described in more detail below with reference to the preferred embodiments illustrated in the accompanying drawings and given in a form of the following numerical data:
Embodiment 1
(z direction)
f z =1.000, F Noz =4.218, NA=-0.0105, ω=43.874°, IH=0.7280, β z =-0.08859, φ z =1.0, object distance=-10.8696
______________________________________r.sub.1 = ∞ d.sub.1 = 0.3304 n.sub.1 = 1.88300 ν.sub.1 = 40.78r.sub.2 = 0.6783 d.sub.2 = 0.6000r.sub.3 = 3.5348 d.sub.3 = 1.3652 n.sub.2 = 1.72916 ν.sub.2 = 54.68r.sub.4 = -1.3600 d.sub.4 = 0.0870r.sub.5 = ∞ (stop) d.sub.5 = 0.3478 n.sub.3 = 1.52287 ν.sub.3 = 59.89r.sub.6 = ∞ d.sub.6 = 0.0261r.sub.7 = ∞ d.sub.7 = 0.5391 n.sub.4 = 1.52000 ν.sub.4 = 74.00r.sub.8 = ∞ d.sub.8 = 0.1391r.sub.9 = 2.9104 d.sub.9 = 1.2609 n.sub.5 = 1.69680 ν.sub.5 = 55.52r.sub.10 = -0.9191 d.sub.10 = 0.2609 n.sub.6 = 1.84666 ν.sub.6 = 23.78r.sub.11 = -3.8252 d.sub.11 = 0.0870r.sub.12 = ∞ d.sub.12 = 0.3478 n.sub.7 = 1.52287 ν.sub.7 = 59.89r.sub.13 = ∞ d.sub.13 = 0.5739r.sub.14 = ∞ d.sub.14 = 0.8696 n.sub.8 = 1.51633 ν.sub.8 = 64.15r.sub.15 = ∞hight of paraxial rayk Y1 0.114130 d.sub.4 = 0.0870r.sub.5 = ∞ (stop) d.sub.5 = 0.3478 n.sub.3 = 1.52287 ν.sub.3 = 59.89r.sub.6 = ∞ d.sub.6 = 0.0261r.sub.7 = ∞ d.sub.7 = 0.5391 n.sub.4 = 1.52000 ν.sub.4 = 74.00r.sub.8 = ∞ d.sub.8 = 0.1391r.sub.9 = 2.9104 d.sub.9 = 1.2609 n.sub.5 = 1.69680 ν.sub.5 = 55.52r.sub.10 = -0.9191 d.sub.10 = 0.2609 n.sub.6 = 1.84666 ν.sub.6 = 23.78r.sub.11 = -3.8252 d.sub.11 = 0.0870r.sub.12 = ∞ d.sub.12 = 0.3478 n.sub.7 = 1.52287 ν.sub.7 = 59.89r.sub.13 = ∞(aspherical surface) d.sub.13 = 0.5739r.sub.14 = ∞ d.sub.14 = 0.8696 n.sub.8 = 1.51633 ν.sub.8 = 64.15r.sub.15 = ∞______________________________________
(y direction)
f y =1.404, F Noy =6.100, NA=-0.0105, ω=27.596°, IH=0.7280, β y =-0.12852, φ y =0.7122, Δ=0.003, object distance=-10.8696
______________________________________r.sub.1 = ∞(aspherical surface) d.sub.1 = 0.3304 n.sub.1 = 1.88300 ν.sub.1 = 40.78r.sub.2 = 0.6783 d.sub.2 = 0.6000r.sub.3 = 3.5348 d.sub.3 = 1.3652 n.sub.2 = 1.72916 ν.sub.2 = 54.68r.sub.4 = -1.3600 d.sub.4 = 0.0870r.sub.5 = ∞ (stop) d.sub.5 = 0.3478 n.sub.3 = 1.52287 ν.sub.3 = 59.89r.sub.6 = ∞ d.sub.6 = 0.0261r.sub.7 = ∞ d.sub.7 = 0.5391 n.sub.4 = 1.52000 ν.sub.4 = 74.00r.sub.8 = ∞ d.sub.8 = 0.1391r.sub.9 = 2.9104 d.sub.9 = 1.2609 n.sub.5 = 1.69680 ν.sub.5 = 55.52r.sub.10 = -0.9191 d.sub.10 = 0.2609 n.sub.6 = 1.84666 ν.sub.6 = 23.78r.sub.11 = -3.8252 d.sub.11 = 0.0870r.sub.12 = ∞ d.sub.12 = 0.3478 n.sub.7 = 1.52287 ν.sub.7 = 59.89r.sub.13 = ∞(aspherical surface) d.sub.13 = 0.5739r.sub.14 = ∞ d.sub.14 = 0.8696 n.sub.8 = 1.51633 ν.sub.8 = 64.15r.sub.15 = ∞______________________________________
aspherical surface coefficients
(1st surface) B=0.14670, (13th surface) B=0.25000 hight of paraxial ray
______________________________________ k Y______________________________________ 1 0.114503 2 0.111146 3 0.186486 4 0.255252 5 0.250925 6 0.239561 7 0.238263 8 0.220616 9 0.213693 10 0.138704 11 0.127643 12 0.118377 13 0.094040 14 0.046998 15 -0.000008______________________________________
E i =0, F i =0, G i =0, φ y1 =0.25907, φ y14 =-0.2614, φ z1 =0, φ z14 =0 (φ zi -φ yi )·(φ zj -φ yj )=(-φ 1 )·(-φ 14 )=-0.06772<0 Σ(φ zn h zn -φ yn h yn )=0.00508, 1/3(φ z h zo +φ yhyo )=0.0653, φ y1 h y1 =0.02966, φ z1 h z1 =0, φ y14 h y14 =-0.02458, φ z14 h z14 =0, h yo =h zo =0.114503, φ y h yo =0.08155, φ z h zo =0.1145
Embodiment 2
(z direction)
f z 1.000, F Noz =5.906, NA=-0.0075, ω=57.282°, IH=0.8948, β z =-0.08859, object distance=-10.8696
______________________________________r.sub.1 = ∞ d.sub.1 = 0.3304 n.sub.1 = 1.88300 ν.sub.1 = 40.78r.sub.2 = 0.6783 d.sub.2 = 0.6000r.sub.3 = 3.5348 d.sub.3 = 1.3652 n.sub.2 = 1.72916 ν.sub.2 = 54.68r.sub.4 = -1.3600 d.sub.4 = 0.0870r.sub.5 = ∞ (stop) d.sub.5 = 0.3478 n.sub.3 = 1.52287 ν.sub.3 = 59.89r.sub.6 = ∞ d.sub.6 = 0.0261r.sub.7 = ∞ d.sub.7 = 0.5391 n.sub.4 = 1.52000 ν.sub.4 = 74.00r.sub.8 = ∞ d.sub.8 = 0.1391r.sub.9 = 2.9104 d.sub.9 = 1.2609 n.sub.5 = 1.69680 ν.sub.5 = 55.52r.sub.10 = -0.9191 d.sub.10 = 0.2609 n.sub.6 = 1.84666 ν.sub.6 = 23.78r.sub.11 = -3.8252 d.sub.11 = 0.0870r.sub.12 = ∞ d.sub.12 = 0.3478 n.sub.7 = 1.52287 ν.sub.7 = 59.89r.sub.13 = ∞ d.sub.13 = 0.5739r.sub.14 = ∞ d.sub.14 = 0.8696 n.sub.8 = 1.51633 ν.sub.8 = 64.15r.sub.15 = ∞______________________________________
hight of paraxial ray
______________________________________ k Y______________________________________ 1 0.081522 2 0.082838 3 0.152044 4 0.218348 5 0.215471 6 0.207913 7 0.207050 8 0.195315 9 0.190711 10 0.132196 11 0.124117 12 0.116755 13 0.097417 14 0.048828 15 0.000276______________________________________
(y direction)
f y =1.000, F Noy =5.924, NA=-0.0075, ω=41.248°, IH=0.8948, β y =-0.08859, Δ=0, object distance=-10.8696
______________________________________r.sub.1 = ∞(aspherical surface) d.sub.1 = 0.3304 n.sub.1 = 1.88300 ν.sub.1 = 40.78r.sub.2 = 0.6783 d.sub.2 = 0.6000r.sub.3 = 3.5348 d.sub.3 = 1.3652 n.sub.2 = 1.72916 ν.sub.2 = 54.68r.sub.4 = -1.3600 d.sub.4 = 0.0870r.sub.5 = ∞ (stop) d.sub.5 = 0.3478 n.sub.3 = 1.52287 ν.sub.3 = 59.89r.sub.6 = ∞ d.sub.6 = 0.0261r.sub.7 = ∞ d.sub.7 = 0.5391 n.sub.4 = 1.52000 ν.sub.4 = 74.00r.sub.8 = ∞ d.sub.8 = 0.1391r.sub.9 = 2.9104 d.sub.9 = 1.2609 n.sub.5 = 1.69680 ν.sub.5 = 55.52r.sub.10 = -0.9191 d.sub.10 = 0.2609 n.sub.6 = 1.84666 ν.sub.6 = 23.78r.sub.11 = -3.8252(aspherical surface) d.sub.11 = 0.0870r.sub.12 = ∞ d.sub.12 = 0.3478 n.sub.7 = 1.52287 ν.sub.7 = 59.89r.sub.13 = ∞ d.sub.13 = 0.5739r.sub.14 = ∞ d.sub.14 = 0.8696 n.sub.8 = 1.51633 ν.sub.8 = 64.15r.sub.15 = ∞______________________________________
aspherical surface coefficients
(1st surface) E=0.13000, (11th surface) E=0.18000 hight of paraxial ray
______________________________________ k Y______________________________________ 1 0.081275 2 0.082587 3 0.151583 4 0.217686 5 0.214818 6 0.207284 7 0.206423 8 0.194723 9 0.190134 10 0.131796 11 0.123741 12 0.116401 13 0.097122 14 0.048680 15 0.000275______________________________________
B y1 =B z1 =F j1 =G j1 . . . =0, E 11 =0.13, E 21 =0.065, E 31 =0, E 114 =0.18, E 214 =0.09, E 314 =0, B y14 =B z14 =F j14 =G j14 . . . =0 (j=1,2,3, . . . )
wherein the reference symbols r 1 , r 2 , . . . represent radii of curvature on surfaces of respective lens elements, the reference symbols d 1 , d 2 , . . . designate thicknesses of the respective lens elements and airspaces reserved therebetween, the reference symbols n 1 , n 2 , . . . denote refractive indices of the respective lens element, and the reference symbols ν 1 , ν 2 , . . . represent Abbe's numbers of the respective lens elements.
The first embodiment of the present invention has the composition which is illustrated in the sectional view in the z direction shown in FIG. 5 and the sectional view in the y direction shown in FIG. 6. The first embodiment uses two cylindrical lens components which are disposed before and after an aperture stop respectively so that it can form an image of a rectangular range of an object on a square solid-state image pickup device.
β H has a value which is the same as that of β z and β V has a value which is the same as that of β y .
The lens system used in the first embodiment is specified for β z =-0.08859, β y =-0.12852 or β z /β y =0.6893≈9/16≈0.5625.
Though the value of β z /β y seems to be different from 9/19, the half field angle ω H in the horizontal direction is -43°87 and the half field angle ω V in the vertical direction is -27°596, whereby an image of a rectangular range of an object has an aspect ratio defined below:
tan 27°596/tan 43°87=0.5437≈9/16
Therefore, the aspect ratio of the image obtained is matched with the aspect ratio of the display unit screen of the high quality TV set.
The difference between the value of β z /β y and 9/16 is produced due to distortion.
Therefore, β z /β y may practically have a value which is rather different from 9/16. Even when possibility to use the display unit for displaying data such as characters together with an image, it is sufficient that β z /β y has a value within a range defined by the following condition (24):
0.25<β.sub.z /β.sub.y <0.97 (24)
FIG. 7 and FIG. 8 show sectional views in the y direction and the z direction respectively illustrating the composition of the second embodiment of the lens system which is to be used in the imaging apparatus according to the present invention.
The second embodiment has a vertical paraxial magnification which is equal to a horizontal paraxial magnification thereof and produces distortion in the z direction in an amount modified so as to form an image of a rectangular range of an object which is contracted in the horizontal direction.
In the second embodiment, an aspherical surface which has a revolutionally asymmetrical component in the term of the fourth order is disposed in each of the sections before and after the stop.
When the aspherical surface disposed before the aperture stop is represented by an ordinal number p and the aspherical surface disposed after the aperture stop is designated by an ordinal number q, we obtain:
E.sub.1p (n.sub.p -n.sub.p-1)=φ.sub.yp (25)
E.sub.3p (n.sub.p -n.sub.p-1)=φ.sub.zp (26)
(For formula (25) and (26) can be defined similarily for the surface q by replacing p with q.) It is desirable for reducing curvature of field in each of the y and z directions to satisfy the conditions (27) and (28):
φ.sub.yp ·φ.sub.yq <0 (27)
φ.sub.zp ·φ.sub.zq <0 (28)
This is because the fourth order term E ap (a=1 or 3) of the formula expressing aspherical surfaces influences on the third order astigmatism A p to be produced by the surface p as expressed below:
A.sub.p =8h.sub.ap.sup.2 ·h.sub.bp.sup.2 ·φ.sub.yp (29)
Similarly, the surface q produces third order astigmatism A q as expressed below:
A.sub.q =8h.sub.aq.sup.2 ·h.sub.bq ·φ.sub.yp (30)
The reference symbols h ap and h bp used in the above-mentioned formula (29) represent heights of the paraxial marginal ray and paraxial principal ray respectively on the surface p. Similarly, the reference symbols h aq and h bq used in the formula (30) represent heights of the paraxial marginal ray and the paraxial principal ray on the surface q.
Form the formulae (29) and (30), φ yp and φ yq must have signs different from each other for obtaining A p +A q ≈0.
Similarly, φ zp and φ zq in the z direction must have signs which are also different from each other.
The second embodiment is specified for β y =β z and f y =f z so as to reduce the on-axis astigmatism Δ to 0, and has a half field angle ω H in the horizontal direction=57°282 and a field angle ω V in the vertical direction=41°248.
As a result, the second embodiment provides an aspect ratio defined below:
(tan ω.sub.H /tan ω.sub.V).sup.-1 =0.5634≈9/16
That is to say, the second embodiment is an example for controlling field angles in the horizontal direction and the vertical direction by controlling distortion.
The second embodiment reduces the on-axis astigmatism Δ to 0 and features high resolution at a center of a visual field which is important for observation.
Though the foregoing description has been made of the present invention for its applicability to the imaging apparatus which is used for observing images on TV monitors using solid-state image pickup device, the present invention is also applicable to electronic endoscopes or similar instruments which are to be used for observing images on TV monitors by utilizing solid-state image pickup devices.
FIG. 13 shows a sectional view illustrating an illumination optical system to be used with the imaging apparatus according to the present invention when it is combined with an electronic endoscope. Since the imaging apparatus according to the present invention forms a horizontally elongated image, the illumination optical system must illuminate a rectangular range of an object. FIG. 13 exemplifies such an illumination system wherein a concave lens component 22 disposed before a light guide fiber bundle 21 is eccentric in the z direction with regard to the light guide fiber bundle for broadening an illumination light bundle in the z direction. For obtaining such a function, it is desirable to shift the concave lens component 22 inward with regard to the light guide fiber bundle, or in the z direction as shown in FIG. 13.
FIG. 14 shows another example of an illumination optical system which is to be used with the imaging apparatus according to the present invention and comprises an anamorphic concave lens component disposed before a light guide fiber buundle having a circular end surface. FIG. 15A and FIG. 15B show a horizontal sectional view and a vertical sectional view respectively of the illumination optical system shown in FIG. 14. As is seen from FIG. 15A and FIG. 15B, the anamorphic concave lens component has a refractive power in the vertical direction which is weaker than that in the horizontal direction. A shape of this lens component is also expressed by the formula (5). An illumination light bundle which is broadened in the horizontal direction can be obtained also by using a light guide fiber bundle which has a circular sectional shape as shown in these drawings.
When a vertical focal length of an illumination lens is represented by f VL and a horizontal focal length of the illumination lens is designated by f HL , it is desirable to satisfy the relationship expressed by the following formula (36):
H:V≈f.sub.HL :f.sub.VL (36)
The relationship expressed by the formula (36) is satisfied even when the illumination lens is anamorphic.
The imaging apparatus according to the present invention can be combined not only with electronic endoscopes but also TV cameras and electronic cameras. Further, the imaging apparatus according to the present invention does not always require correction of image shapes or permits modifying image shapes as occasion demands. Furthermore, the imaging apparatus according to the present invention is applicable not only to the high quality TV sets but also to TV sets which are designed in accordance with the NTSC standard and the PAL standard, and compatible with display screens which are not square.
The imaging apparatus according to the present invention is applicable even when solid-state image pickup devices have shapes similar to those of display units of TV monitors or when images to be displayed are modified for displaying data such as characters additionally.
In addition, the imaging apparatus according to the present invention can be configured so as to form an image, at a ratio modified between two obliquely intersecting directions instead of the aspect ratio, which is to be deformed by an electronic circuit and then displayed on a TV monitor. In such a case, magnifications in the two obliquely intersecting directions correspond to β H and β V used in the foregoing description, and these two directions correspond to the y and z directions.
It is desirable for the imaging apparatus according to the present invention to use a solid-state image pickup device having picture elements each of which has a horizontal size longer than a vertical size thereof since picture elements disposed at a high density in the horizontal direction are preferable for the imaging apparatus which forms a horizontally elongated image. A solid-state image pickup device using such picture elements will find a hopeful future since the NTSC standard is to be modified for adopting such a solid-state image pickup device. Since such a solid-state image pickup device has an aspect ratio of 4/3, the formulae adopted by the present invention are applicable with a simple modification to A=4/3 as well as modifications of the formulae (29) and (30) into (31) and (32) respectively:
β.sub.z /β.sub.y ≈1/A=0.75 (31)
(tan ω.sub.H /tan ω.sub.V).sup.-1 ≈1/A=0.75 (32)
The present invention provides a compact imaging apparatus which permits displaying strongly appealing or highly impressive image on a TV monitor.
Further, anamorphic lens components may be used to form images having different ratios between vertical sizes and horizontal sizes on rectangular solid-state image pickup devices. Anamorphic lens components may be used, for example, to form images of objects at a ratio of approximately 9:16 between vertical sizes and horizontal sizes on solid-state image pickup devices in accordance with the NTSC standard which generally have rectangular shapes having a ratio of 3:4 between vertical sizes and horizontal sizes and are available rather easily. In this case, a ratio between a magnification in the z direction and a magnification in the y direction will be as calculated by the following equation (33): ##EQU6##
Considering possibilities that images are not displayed over entire ranges of screens of display units to reserve some areas for displaying characters and other data, that images are influenced due to distortion, and that allowances of actual magnification errors are rather large for images of objects of certain kinds, the ranges defined by the formulae (31) and (32) may be replaced with that specified by the formula (34) shown below, and the range defined by the formula (32) may be replaced with that defined by the following formula (35): ##EQU7##
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An imaging apparatus includes an objective lens system for forming an image of an object, a solid-state image pickup device, a signal processor and a display device. The objective lens system includes at least one revolutionally asymmetrical refractive surface for deforming the image formed by the objective lens system and is configured so as to deform further the image which is deformed by the signal processor.
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FIELD OF THE INVENTION
The field of this invention is valves for subterranean use that are actuated with an indexing mechanism and more particularly flapper type valves actuated with pressure cycles on a plug that can be removed after use.
BACKGROUND OF THE INVENTION
Various valve designs used in the past have incorporated sleeves indexed by j-slot devices to selectively align and misalign ports. In one example the ball that lands on a seat to allow application of pressure cycles to operate the j-slot is blown through the seat after a change in valve position. This is illustrated in U.S. Pat. No. 7,416,029. Another device is in essence a sliding sleeve that allows flow uphole and the sleeve, which is mounted to a j-slot, can be cycled from uphole as flow from uphole acts to close a flapper on top of the sleeve for pressure cycling. This is shown in US Publication 2008/0196898.
Other designs use a j-slot to unlock a lock in conjunction with a plug that can then disappear as illustrated in U.S. Pat. Nos. 5,765,641; 6,119,783 and 6,026,903. Other designs use relatively movable mandrel components where cycles of picking up and setting down weight actuate a j-slot to operate a flapper, as shown in U.S. Pat. No. 4,458,762. Some designs use a j-slot to unlock a lock so that a flapper can then operate. A plug is landed on a seat which then is dissolved. Some examples of combinations of some of these features are U.S. Pat. Nos. 7,270,191; 6,904,975 and US Publication 2009/0242199.
Other designs provide a flowpath constriction to create differential pressure on a flow tube to open a flapper. These designs such as the MC Injection Valves from Halliburton and the A Series Injection Valve from Schlumberger restrict access through the valve for advancing other tools. The Model J Wireline Retrievable Injection Valve from Baker Hughes opens on a predetermined flow through a restriction. Some hydraulically operated safety valves had a feature to lock a flapper open after the flapper was displaced with a flow tube driven by a hydraulic piston. In this design shown in U.S. Pat. No. 6,902,006 the flame holding the flapper was itself shifted when the flapper was open to catch the edge of the flapper in a top groove of a sleeve below. Yet a few other applications that use flow bore restrictions to create a force to move a tube to open a flapper are U.S. Ser. Nos. 12/433,134, filed on Apr. 30, 2009 entitled Innovative Flow Tube, 12/469,310, filed on May 20, 2009, entitled Flow-Actuated Actuator, and 12/469,272, filed on May 20, 2009, entitled Flow-Actuated Actuator and Method.
The present invention deals with flapper type valves with a preferred use in injection service. The design provides a way of operating the flapper without control lines. In deep applications there will be high hydrostatic pressure in the control line that would have to be offset with a very large return spring. While a dual control line system can offset this hydrostatic effect in deep applications there is additional expense and operational issues from doubling up the control lines and running them with a string into the subterranean location. In the preferred embodiment there is no need for control lines. A flapper is operated by a sleeve that responds to pressure cycles against a seated ball or plug to push the flapper open after a predetermined number of cycles. The ball, plug or other object is removed from its blocking position on a seat preferably by dissolving it so that flow can commence. The preferred application is injection service where water, salt water, chemicals, CO 2 or steam can be the flowing fluid. When it is desired to close the flapper another object can be landed in the same seat and the cycling with pressure repeated to allow a return spring to raise the flow tube so that a torsion spring on the flapper pivot can move the flapper to the closed position against its seat. As few as a single application and removal of pressure cycle can be used to change the flapper position between open and closed.
In an alternative embodiment an actuation sleeve pushes the flapper open as well as engaging or contacting a counter sleeve below that is engaged to a j-slot. On release of pressure a return spring on the counter sleeve raises it to retain the flapper in the open position while a separate return spring biases the actuation sleeve up. A second ball or other object landed in the seat of the actuation sleeve once again displaces the actuation sleeve against the counter sleeve. This time the counter sleeve is held against its return spring by the j-slot so that on release of pressure the torsion spring on the flapper allows the flapper to pivot closed when the actuation sleeve is also pushed up by its return spring. After a use of either the first or the second object, either is removed preferably by dissolving to get either object out of the flow path.
The dissolving of the object can occur by fluids such as water, saltwater in the wellbore, acid added to the wellbore, or by other reactive or dissolving agents present or added to the wellbore. Other ways to fail the object to get it out of the flow path are also contemplated.
Those skilled in the art will better appreciate the scope of the invention from a review of the description of the preferred embodiment and the associated drawings while recognizing that the full scope of the invention is determined by the appended claims.
SUMMARY OF THE INVENTION
A flapper valve preferably used in injection application in deep subterranean locations has an actuating sleeve with a seat to accept an object. A j-slot connects the actuation sleeve movement to the housing so that with an object on the seat and an applied pressure cycle the sleeve moves the flapper to the open position. The plug is dissolved and the injection begins. The plug can have an opening so as to allow continuous injection flow as the flapper is operated. Closing the flapper involves a second object on the same seat and a pressure cycle so that a spring can push the sleeve away from the flapper to allow a torsion spring on the flapper to close it. In an alternative embodiment an actuation sleeve pushes a counter sleeve that is movable through a j-slot. The first object on the actuation sleeve pushes both sleeves such that removal of pressure allows the now open flapper to be retained in the open position and the object to be dissolved or otherwise removed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a section view with the flapper closed;
FIG. 2 is the view of FIG. 1 after the object is landed on the actuation sleeve and the sleeve is displaced to compress the return spring;
FIG. 3 shows the object dissolved and the passage through the sleeve cleared;
FIG. 4 is an unrolled view of the track for the j-slot for the actuation sleeve;
FIG. 5 is the flapper closed view for run in using an alternative embodiment that moves an actuation sleeve against a counting sleeve where the counting sleeve is on a j-slot;
FIG. 6 is the view of FIG. 5 with an object on the seat on the actuation sleeve and both sleeves displaced as pressure is applied;
FIG. 7 is the view of FIG. 6 with applied pressure removed and the object dissolved showing the counting sleeve holding the flapper open;
FIG. 8 is an unrolled version of the counting sleeve j-slot track showing a straight lower end; and
FIG. 9 is an alternative embodiment to FIG. 8 where the lower end of the counting sleeve is scalloped to enhance the amount of protrusion over the flapper when the flapper is retained in the open position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 has a housing 10 with a passage 12 and a flapper 14 that pivots on a pin 16 . A torsion spring 18 biases the flapper 14 toward the closed position against the seat 20 . An actuating sleeve 24 is slidably mounted in the passage 12 to move against the bias of a return spring 26 when an object such as a ball or plug 28 lands and obstructs the passage 12 at seat 30 as shown in FIG. 2 . A pin or screw 32 extends into a j-slot track 34 that is shown rolled open in FIG. 4 . The j-slot track 34 has a series of long passages 36 and short passages 38 that alternate. In the FIG. 1 position, the actuating sleeve 24 is at its highest location where spring 26 is extended and the flapper 14 is biased by spring 18 against the seat 20 . This can happen because the actuating sleeve 24 in FIG. 1 is not in contact with the flapper 14 . In essence the spring 26 advances the actuating sleeve 24 until the long passage 36 hits the pin 32 , as shown in FIG. 1 .
Dropping the object 28 onto seat 30 and applying pressure moves the sleeve 24 axially and initially without rotation as the long passage 36 with pin 32 extending into it guides the axial movement. When the pin advances to passage 40 there is rotation of the sleeve 24 as the pin enters passage 42 and remains there as long as pressure is held against the object 28 . When the pressure is removed in passage 12 on the object 28 the sleeve 24 reverses direction and resumes rotation as the pin 32 rides in passage 44 on the way to passage 38 . This is the FIG. 2 position.
The object 28 is then removed from the seat 30 in one of a variety of ways such as dissolving, chemical reaction, melting, or being ejected through the seat 30 . Note that the sleeve 24 has been pushed down to contact the flapper 14 and rotate it 90 degrees so that in FIG. 2 it is behind the sleeve 24 with the spring 26 being compressed. The position of FIG. 2 is held because the pin 32 in short passage 38 is at the end of that passage with the sleeve 24 under a spring force. FIG. 3 is the view of FIG. 2 after the object 28 is no longer on the seat 30 . Injection of fluid down passage 12 or production in the opposite direction can now take place as indicated by arrow 46 .
Those skilled in the art will appreciate that a single application and removal of pressure cycle has gotten the flapper 14 to go from closed to open and that the landing of a second object (not shown) on seat 30 followed by a pressure cycle of application and removal of pressure will get the pin 32 into the next long passage 36 to allow the sleeve 24 to rise up and away from the flapper 14 so that the torsion spring 18 can close the flapper 14 against its seat 20 . While the j-slot 34 is designed for a single cycle of pressure application and removal to move the flapper 14 the j-slot 34 can be designed for multiple cycles before the flapper moves. Since the second object (not shown) lands on the same seat 30 , it can have the same shape as the object 28 .
As an option to avoid stopping injection when trying to close the flapper while landing a second object (not shown) on seat 30 , a small passage 46 (illustratively shown on object 28 but is actually used in the second object that is not shown) is put in so that there is some injection flow through it but the pressure difference across the object is sufficient to move the sleeve 24 so that it can be raised when pressure is removed so that the flapper 14 can close. If such a passage is used it is preferred that the object shape not be round but instead be a cylindrical plug for example so that the passage 46 is in fluid communication with the passage 12 when the object (not shown) lands on seat 30 as the second landed object.
FIGS. 4-9 show an alternative embodiment. Here there is an actuating sleeve 124 biased by a spring 126 but with no j-slot mechanism. As before there is a flapper 114 on a pivot 116 that has a torsion spring 118 . The flapper seats on seat 120 . Below the flapper 114 there is a counting sleeve 50 biased by a spring 52 . A pin 54 extends into a j-slot 56 that is shown rolled out in FIGS. 8 and 9 . When the first object 128 lands on seat 130 and pressure is applied in passage 112 the actuating sleeve 124 is pushed down to compress the spring 126 and to push the flapper 114 90 degrees to the open position behind the sleeve 124 as shown in FIG. 6 . That same movement of sleeve 124 that opened the flapper 114 has resulted in the lower end 58 hitting the upper end 60 of the counting sleeve 50 and pushing it in tandem with sleeve 124 while compressing the spring 52 . In the FIG. 5 position the pin 54 is in the short passage 62 . As pressure is applied to the object 128 the sleeve 50 initially moves axially without rotation as pin 54 guides the passage 62 until passage 64 is reached at which time there is translation and rotation followed by translation only as the passage 66 runs past the pin 54 . Once the pressure in passage 112 is let off the object 128 , the spring 126 pushes up sleeve 124 , while the spring 52 pushes up sleeve 50 . Sleeve 50 initially only translates down as pin 54 tracks path 66 in the opposite direction before going into path 68 which causes the sleeve 50 to advance axially while rotating until pin 54 reaches path 70 where there is only axial motion of sleeve 50 without rotation. The upper end 60 of sleeve 50 , while initially moving in tandem with sleeve 124 , stops moving when the upper end 60 is in front of the flapper 114 so that rotation of the flapper from the open position is prevented. The sleeve 124 moves away from the now stationary sleeve 50 until the sleeve 124 resumes its original position. These movements are illustrated in FIG. 7 which also shows that the initial object 128 has been removed using any of the techniques described before. Flow in passage 112 can now occur as indicated by arrow 72 . As before, dropping a second object on seat 130 and another pressure cycle gets the device back to the FIG. 5 position and the second object (not shown) can then be removed using the previously described techniques.
FIGS. 8 and 9 are identical except for the variation of FIG. 9 having a scalloped end 74 having peaks 76 and alternating valleys 78 . This feature extends the reach of the sleeve 50 toward the flapper 114 when the pin 54 is in the long slots 70 .
Those skilled in the art will appreciate that the device eliminated the need for a hydraulic control system including control lines and a piston to move the sleeves for operating the flapper. The springs in the design simply offset the weight of the sleeve that they bias independent of the depth of the application. The passage is cleared after the operation of the flapper so that preferably injection can take place with the flapper held open. A second object can be used to release the flapper so it can close. A passage in the object can be optionally provided to continue injection flow with the object being seated. Dissolving the object with an introduced fluid is the preferred way to reopen the flowpath.
The above description is illustrative of the preferred embodiment and many modifications may be made by those skilled in the art without departing from the invention whose scope is to be determined from the literal and equivalent scope of the claims below:
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A flapper valve preferably used in injection application in deep subterranean locations has an actuating sleeve with a seat to accept an object. A j-slot connects the actuation sleeve movement to the housing so that with an object on the seat and an applied pressure cycle the sleeve moves the flapper to the open position. The plug is dissolved and the injection begins. The plug can have an opening so as to allow continuous injection flow as the flapper is operated. Closing the flapper involves a second object on the same seat and a pressure cycle so that a spring can push the sleeve away from the flapper to allow a torsion spring on the flapper to close it.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to solar heaters wherein sunlight and its heat energy is absorbed and transferred to moving air in an enclosure.
2. Description of the Prior Art
Prior solar heaters have utilized transparent and translucent panels for heating air within an enclosure formed thereof. See for example U.S. Pat. Nos. 2,998,005 and 3,244,486. Other solar heating proposals have included utilizing the attic space in a dwelling as in U.S. Pat. No. 2,780,415 and still other patents arrange heat exchangers in boxes exposed to the sunlight as in U.S. Pat. No. 3,902,474.
Pyramidal structures not heretofore considered as useful solar heaters may be seen in U.S. Pat. Nos. 2,982,054 and 3,577,691. A thermoplastic heat responsive fire venting apparatus includes a modified pyramidal structure, the surfaces being bowed as disclosed in U.S. Pat. No. 3,918,226.
This invention provides a double hollow pyramidal shape exposed to the sunlight and incorporates air moving means for moving heated air from the inner surface of the outer one of the double pyramidal shaped structures so as to heat a room in association therewith.
SUMMARY OF THE INVENTION
A pyramidal solar heater is formed of translucent heat absorbing plastic material or the like provided with a spaced, smaller pyramidal structure and air moving means whereby heated air may be moved out of the pyramidal solar heater downwardly into a room or enclosure therebelow.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a vertical section through a portion of a roof and a pyramidal solar heater positioned in an opening therein;
FIG. 2 is an enlarged detail of the upper portion of the pyramidal solar heater seen in FIG. 1
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the form of the invention chosen for illustration herein, the pyramidal solar heater may be seen in FIG. 1 to comprise a pyramid formed of four triangular shaped panels 10, having a common peak 11 and an open square bottom 12. The pyramidal solar heater may be of any desired size and as disclosed in FIG. 1 of the drawings it is positioned in registry with an opening 13 in a roof structure 14 of a building. The roof structure includes joists 15, roofing boards 16, roofing material 17 and a ceiling 18. A grille 19 is positioned on the ceiling 18 so as to register with the opening 13 in the roof structure 14. A bracket 20 is positioned adjacent the peak 11 of the pyramidal solar heater and an air moving device such as an electric motor 21 and a fan 22 driven thereby are mounted on the bracket 20 as best seen in FIG. 2 of the drawings. The triangular panels 10 of the pyramidal solar heater are formed of heat absorbing shaded or translucent plastic material or the like characterized by its ability to convert light energy to heat energy. The panels 10 may accordingly be tinted plastic such as Lucite or alternately tinted window glass, both of which products will be familar to those skilled in the art, and both of which convert light energy to heat energy.
Still referring to FIG. 1 of the drawings, it will be seen that there is a smaller pyramidal structure 23 positioned inwardly in spaced relation to the four triangular panels 10 of the pyramidal solar heater. The apex of the inner pyramidal structure 23 is cut off to form a small square opening 24 and the bottom of the secondary pyramidal structure 23 is open as at 25. The smaller pyramidal structure 23 may be formed of any suitable material and it is supported adjacent its uppermost and lowermost ends by a plurality of small individual arms 26.
By referring now to FIG. 2 of the drawings it will be seen that the rotating shaft of the electric motor 21 on which the fan 22 is carried also supports a deflector cone 27. The electric motor 21 is provided with an energizing circuit 28 and by referring to FIG. 1 it will be seen that this extends downwardly through the roof structure 14 and to a thermostatic control 29 which in turn is connected with a suitable power source.
A tubular heat exchanger 30 is seen arranged in a substantially square configuration and positioned around the outer edges of the opening 13 in the roof structure and pipes 31 extend from the heat exchanger as desired.
In operation the pyramidal solar heater acts to receive sunlight regardless of the direction of the sun with respect to the heater and the inclination of the suns rays engaging the same as the four triangular panels 10 of the solar heater provide almost universal directional alignment with the sun at all times. The suns rays engaging the four triangular panels 10 create heat on the inner side thereof due to the characteristic of the panel material and this may be enhanced by heat absorption qualities of the smaller pyramidal structure 23 positioned within the solar heater. The energization of the electric motor 10 revolves the fan 22 and moves the air downwardly between the pyramidal solar heater and the smaller pyramidal structure in a wiping action which moves the warmed air downwardly and is in turn heated by convection. The warm air moves downwardly as indicated by the arrows in FIG. 1 of the drawings and through the opening 13 in the roof structure 14 through the grille 19 and into the room or other enclosure. If supplemental heating at a distance is desired, the tubular heat exchanger 30 is supplied with a fluid such as water circulated slowly therethrough and the same is heated by the warm air flowing downwardly thereover. Cool air enters the solar heater through the center section of the grille 19 and moves upwardly through the interior of the smaller pyramidal structure 23 and out of the small square opening in the upper end thereof where it is directed downardly by the fan and the directional cone 27 heretofore described. It will thus be seen that a solar heater has been disclosed which has the novel ability of presenting a relatively large surface area to the sun regardless of the time of day and the positioning of the sun relative to the solar heater.
Experiments with a solar heater the height of the triangular panels 10 being 12 inches, has determined that it will raise the temperature in a 30 × 30 room approximately 25° over a period of 6 hours.
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A pyramidal solar heater for a dwelling house or other building takes the form of a pyramidal structure formed of translucent plastic or like material having heat absorbing properties and includes a second pyramidal structure spaced inwardly thereof together with an air moving device for circulating air from the dwelling house or other building against the solar heated translucent plastic pyramidal device.
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FIELD OF THE INVENTION
Embodiments of the present invention relate to data network analysis and, more particularly, to methods of presenting views of network traffic and content.
BACKGROUND OF THE INVENTION
Computers on a network send information to each other as part of a communication session. The data for a communication session is broken up by the network and transferred from a source address to a destination address. This is analogous to the mail postal system, which uses zip codes, addresses, and known routes of travel to ship packages. If one were to ship the entire contents of a home to another location, it would not be cost effective or an efficient use of resources to package everything into one container for shipping. Instead, smaller containers would be used for the transportation and assembled after delivery. Computer networks work in a similar fashion by taking data and packaging it into smaller pieces for transmitting across a network. Each of these packets is governed by a set of rules that defines its structure and the service it provides. For example, the World Wide Web has a standard protocol defined for it, the Hyper Text Transport Protocol (HTTP). This standard protocol dictates how packets are constructed and how data is presented to web servers and how these web servers return data to client web browsers.
Any application that transmits data over a computer network uses one or more protocols. There are many layers of protocols in use between computers on a network. Not only do web browsers have protocols they use to communicate, but the network has underlying protocols as well. The use of multiple nested protocols is sometimes referred to as “data encapsulation.” For example, when a request is made to a web site, the data request is encapsulated by the HTTP protocol used by the browser. The data is then encapsulated by the computer's network stack before it is put onto the network. The network may encapsulate the packet into another packet using another protocol for transmission to another network. Each layer of the protocol helps provide routing information to get the packets to their target destination.
In order for a network administrator or other entity to analyze or monitor its users' traffic effectively, tools may be deployed to: “sniff” or capture the packets traversing the network of interest; understand the protocol(s) being used in the communication; analyze the data packets used in the communication; and draw conclusions based on information gained from this analysis. Conventional tools for analyzing network traffic include protocol analyzers, intrusion detection systems, application monitors, log consolidators, and combinations of these tools.
A conventional protocol analyzer can provide insight into the type of protocols being used on a network. The analysis tools within such an analyzer enable the analyzer to decode protocols and examine individual packets. By examining individual packets, conventional protocol analyzers can determine where the packet came from, where it is going, and the data that it is carrying. However, it is virtually impossible to look at every packet on a network by hand to see if security or other concerns exist. Consequently, more specialized analysis products were created.
One example of a more specialized but conventional analysis tool is an Intrusion Detection System (IDS), which validates network packets based on a series of known signatures. If the IDS determines that certain packets are invalid or suspicious, the IDS provides an alert. Analysts, in some cases using additional analysis tools, must then analyze most of these alerts. This analysis can require extensive manpower and resources.
Another example of a more specialized but conventional analysis tool is an application monitor. Application monitors focus on specific application layer protocols to decide if illegal or suspicious activity is being performed. Such conventional application monitors may focus, for example, on the Hyper Text Transfer Protocol (HTTP) to monitor accesses to websites. As such, when a network user visits a website, the analyst can monitor the packets transmitted and received between the network user's computer and the web server. These packets can be analyzed by parsing the HTTP protocol to determine the website's hostname, the name of the file requested, and the associated content that was retrieved. Thus, this HTTP analyzer could be used to decide if a network user is visiting inappropriate web sites and alert appropriate personnel of this activity. This type of analysis tool monitors the actions of web browsers, but falls short for other types of communications.
Another conventional application monitor can monitor the Simple Mail Transport Protocol (SMTP). This system can be used to, e.g., record and track e-mails sent outside of a company to ensure employees were not sending trade secrets or intellectual property owned by the company. It can also ensure e-mails entering into a company do not contain malicious attachments or viruses. Employees could, however, use other means of communication such as instant messaging, chat rooms, and website-based e-mail systems to circumvent detection. Because this application monitor only monitors SMTP communications, companies must also use many other security and analytical tools to monitor network activity.
Another example of a more specialized but conventional analysis tool is a log consolidator system (LCS). An LCS processes log-based output from network applications or devices. These data inputs can include firewall logs, router logs, application logs such as web server or mail server logs, host system logs, and/or IDS alerts. LCS analysis tools aggregate and correlate each different log format. However high level log data often lacks detail needed for effective analysis.
While these and other conventional network analysis systems analyze communications of a particular protocol or format, they fail to analyze a broad breadth of protocols and formats, and provide true context. Thus, an entity wishing to ensure security of its network currently must purchase and maintain multiple network analysis systems. Further, with each new protocol or protocol change, companies must create, rewrite, upgrade, or repurchase at least one of their systems. The conventional method of using a patch-work of multiple analyzers is expensive and complex to maintain.
In addition, because of the many ways to communicate over a network and the many different analysis tools needed to perform deep content and context analysis, the conventional network analysis methods make it difficult to answer even simple questions such as “What is happening on my network?,” “Who is talking to whom?,” and “What resources are being accessed?” Answering these questions is difficult because there is virtually no limit to which applications one can use. Each application introduced onto a network brings new protocols and new analytical tools to audit those applications. For example, there are many ways to send a file to another person using a network: E-mailing the document as an attachment using the SMTP protocol; transmitting the file using an Instant Messenger like MSN, AOL IM™, or Yahoo™ IM; uploading the file to a shared file server using the FTP protocol; web sharing the document using the HTTP protocol; or uploading the file directly using an intranet protocol like SMB or CIFS. All of these protocols are implemented differently and special analysis tools are required to interpret them—a complex and expensive system.
In sum, the ever-increasing amount and different possible types of network traffic is forcing network administrators, Internet service providers (ISPs), corporate information technology (IT) managers, and law enforcement personnel, among others, to re-evaluate how best to effectively monitor the types and nature of data traffic that traverses the networks for which they have oversight.
One system that provides significant insight into network traffic is described in U.S. patent application Ser. No. 10/133,392, entitled “Apparatus and Method for Network Analysis,” and filed Apr. 29, 2002 (“the '392 application”). The methodology described in the '392 application includes capturing network traffic in its native format, and converting the same into a common language, or event-based language. Records of the data can then be organized around the common language. The disclosure of the '392 application is incorporated by reference herein in its entirety.
Notwithstanding the advances and advantages of the systems and methods described in the '392 application, there is nevertheless a need for improved systems and methodologies for monitoring network traffic.
SUMMARY OF THE INVENTION
Embodiments of the present invention provide systems and methods that translate network packet streams into easily interpretable information. The system and methodology may be used for network intrusion analysis, incident response, network investigations, ediscovery, anti-data leakage, threat and malware analysis, and compliance verification.
The system and methodologies provided by embodiments of the invention operate as a collection, transformation, correlation, and analysis solution providing insight into electronic data networks. The embodiments act as a sort of “video camera” on the network, recording all activities (in some embodiments), and transforming data into a dense transactional model describing the network, application, and content levels of those activities. This information enables users to quickly and effectively investigate the model for patterns of concern.
Embodiments of the present invention provide analysis in an intuitive fashion, without complicated “network-speak.” The system allows for the analysis of multiple protocols and applications including, for example, email, instant messaging, file transfers, and even Voice-over-IP. With the data presentation techniques provided by embodiments of the present invention, both analysts and business users can easily interpret raw packet data associated with enterprise user transactions.
Features of embodiments of the present invention may allow users to:
Isolate I/T asset misuse and external threats;
Manage insider threats and data leakage;
Speed incident response, security audits and investigations; and
Verify policy and regulatory compliance, among many other benefits.
Embodiments of the present invention may be provided as software or as a network appliance. The invention may be used to collect live network traffic or process pre-collected packets from other collection systems. Features of the invention may also be integrated to augment existing network infrastructure components. For example, triggers from intrusion detection, log consolidators, network behavior and content monitoring systems can be used to guide user inspection of data.
More specifically, an embodiment of the present invention provides a method of visualizing and displaying a representation of data that has traversed a network. The method includes the steps of:
Storing a collection of packets retrieved from an electronic network;
Displaying a list of categories related to characteristics of the collection of packets, the categories including listings of categorical elements, wherein at least some of the categorical elements are selectable by a user;
Receiving an indication that one of the categorical elements has been selected, and filtering the categorical elements in accordance with the selected categorical element; and
Displaying a selectable count value adjacent each of the categorical elements, the selectable count value being indicative of the number of times an adjacent categorical element is present in the collection of packets, or byte volume of that categorical element.
The method may also include storing a plurality of collections of packets, and selecting one of the plurality of collections of packets for display.
In a preferred embodiment, the method provides for receiving successive indications that categorical elements have been selected, and successively filtering the categorical elements in accordance with respective ones of the selected categorical elements. In connection with this feature, the method may further display a “breadcrumb” path indicative of the successive selected categorical elements. Preferably, each of the components of the path is selectable by user such that an earlier view of the data can be easily and quickly accessed.
The visualization method may further include displaying a session view of selected packets in the collection of packets, and doing so in response to a receipt of an indication that the selectable count value has been selected. The session view may display a time a given session occurred, a service type of the given session, a size of the session, and a plurality of events associated with the session. The session view preferably further displays pairs of network layer entities such as Internet Protocol (IP) addresses associated with the given session, or application layer entities such as user or filename. An arrow icon is preferably incorporated into the session view to indicate which way a particular communication within a given session is directed. The session may still further include a selectable view content icon, which, when selected, causes a display to show the content of the given session.
In another embodiment, a method of visualizing network data includes:
Presenting to a user, on a display, a plurality of categories that represent characteristics of network data, each category having listed thereunder a series of listings corresponding to respective categories, each listing having associated therewith a count value that indicates the number of times an associated listing is present in the network data, wherein both the listings and respective count values associated therewith are user selectable;
Receiving an indication that one of the listings has been selected, and in response thereto re-presenting to the user, on the display, the plurality of categories but only with respective listings that have been filtered in accordance with the one of the selected listings; and
Receiving an indication that one of the count values has been selected, and in response thereto presenting to the user, on the display, a session view of network data associated with the listing with which the selected count view is associated.
These and other features of embodiments of the present invention, and their attendant advantages, will be more fully appreciated upon a reading of the following detailed description in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a network in which embodiments of the present invention may operate.
FIG. 2 is a schematic diagram of a data store or database that stores packet collections that are made available for display in several different possible views in accordance with embodiments of the present invention.
FIG. 3 shows an exemplary packet collection display view in accordance with an embodiment of the present invention.
FIGS. 4-6 show exemplary navigation views including successive drill down views in accordance with an embodiment of the present invention.
FIG. 7 shows an exemplary event view in accordance with an embodiment of the present invention.
FIG. 8 shows an exemplary content view in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
FIG. 1 depicts a typical network environment in which embodiments of the present invention may operate. A given electronic data network 100 comprises a plurality of computers 110 that are interconnected with one another, often times, via a local area network (LAN) operating in accordance with, e.g., the Ethernet standard. Respective networks 100 can likewise be connected to each other, such that any given computer 110 , which is physically connected within a given network 100 , can communicate with virtually any other computer 110 , which is physically or wireless sly connected within the any other network. Conventionally, digital information flows among networks using the Internet Protocol (IP). Such digital information is broken up into individual packets in accordance with the protocol and addressed with unique IP addresses in order to be passed from one node (such as a computer 110 ) to another node (such as another computer 110 ).
According to TeleGeography, a division of PriMetrica, Inc. (Carlsbad, Calif.), as of mid-2005, the volume of data that traversed cross-border internet backbones stood at just under 1 Terabit per second (Tbps). While any single given network does not carry that much traffic, it is not uncommon for Terabytes of data to traverse a sub-network over any given period of days or weeks. Analyzing this amount of data in a meaningful and efficient way is a significant challenge. To address this challenge, the present invention provides a unique set of views into this vast amount of data, including providing intuitive representations of relationships among various data categories and elements.
FIG. 2 shows a simple representation of a data store or database 200 that is connected to a computer 110 on which executable program code is running, which code provides or generates the network data views described more fully below. In an actual implementation of the invention, the code is written using C++, C# and Java. However, those skilled in the art will appreciate that other software development environments, programming languages, etc., may be used to implement the systems and processes for network data visualization in accordance with the instant invention. For instance, the systems and processes described herein may be web-based and operate via a web browser, or may be client based. Database 200 may be implemented as files, object-oriented databases, SQL databases, or any other suitable database architecture that allows for access to individual data packets that have been captured from network(s) 100 .
Data packets can be captured in one of two ways. First, data may be captured in real-time (“Real-Time Network Capture Mode”). In this mode, traffic may be captured from a given network 100 by connecting to a network “wire” using, e.g., the well-known libpcap capture driver, or variants thereof. To capture data, the driver preferably monitors a hub, a port-spanned switch or a passive network tap in the network. In one possible implementation, monitoring may be established between a corporate firewall and the corporate intranet, thereby allowing monitoring of outbound and inbound Internet traffic.
Ideally, if the system is capturing real-time traffic from a network, the point of collection is preferably logically invisible to would-be hackers or other targets. To achieve invisibility, the network card used for collection may be configured to operate without a TCP/IP or other network stack. Without a TCP/IP stack, a network card will neither respond to probes from the network nor broadcast data from the card. However, the card can still collect data transmitted or traversing over the network. Such a configuration may be referred to as a “stealth mode.” Of course, where invisibility is not a necessity, the network card may operate in a conventional manner.
A second way to obtain a collection of network traffic is from a third party source that has previously recorded a collection of traffic. For example, TCPDump files, previously collected from a UNIX-based machine, can be loaded and stored in database 200 . This mode may be referred to as “Filed Based Network Capture Mode.” In either case, Real-Time Network Capture Mode or Filed Based Network Capture Mode, a collection of packets is stored for further processing and user controlled presentation.
FIG. 3 shows an exemplary screen shot 300 of a plurality of packet collections 310 that have been respectively named and stored in respective databases 200 , or the same database 200 . Individual ones of these packet collections 310 may have been collected as described above. It is inconsequential to the instant invention how any given packet collection comes to be stored in a database 200 .
By clicking on a given one of the collections of packets 310 —in this case “Investigation IP”—screen 400 of FIG. 4 is preferably displayed. Screen 400 represents a first of a series of displays or screens that allows a user to view ever-increasing details about network data, and in particular, details about the selected packet collection 310 . Stated alternatively, using the several screens and views described herein, a user can quickly “drill down” into network data to look for specific details, as desired. As shown, screen 400 (as well as screens 500 and 600 of FIGS. 5 , 6 A, 6 B) includes a plurality of bolded categories that describe the plurality of packets in the selected collection of packets 310 . Categories include:
410 —Applications—applications verified within the traffic may include, e.g., HTTP, RTP, SNMP, HTTPS, POP3, FTP, GNUTELLA, and SMTP, among others.
412 —Time—this category includes a time period such as a given year, month, week, day, hour span, etc. This category helps to identify traffic that occurred at a specific time.
414 —Protocol—the protocol category identifies the Ethernet protocol in accordance with which a given session is configured. For example, protocols might include, IP, ARP, IPX, PPPoE, etc.
416 —Size—this category represents the total session size.
418 —IP Addresses—this category lists the IP addresses associated with the collection of sessions.
420 —Port Numbers—this category identifies port numbers associated with the collection of sessions.
422 —Content—this category shows what content type given sessions carry as their payloads. For example, as shown in screen 400 , content may include text/html, image/gif, image/jpeg, etc.
424 —HostNames—this category provides the domain name present in given sessions. For example, for an HTTP session, the domain name for that transaction could be registered as www.samplecorporation.com.
426 —Properties—the properties category provides a listing of properties for each session. This list may include the existence of passwords, encryption, querystring, referrer, attachment, and many other descriptors.
428 —Action—the action category describes a specific action such as get, login, logoff, put, delete, send, etc.
430 —UserNames—this category identifies names of users.
432 —Email Addresses—this category includes the email addresses of users.
434 —Files—this category describes names of files.
Those skilled in the art will appreciate that other categories of information associated with network traffic may also be included and used to help categorize discrete elements of captured data at the network and application layer. For instance, categories may be broken down into more granular representations to include, e.g., source IP, destination IP, source MAC Address, destination MAC Address, IP Protocol, and many others.
Screen 400 also shows several additional features. For instance, at the end of the listings for several of the categories, there is, preferably, a “clickable link” named “show more” 460 . By clicking on this link, more items or listings under the particular category are provided for presentation. In connection with this, elements listed under most of the categories include a parenthetical “count” value 480 that represents how many sessions, packets, or byte count the given element represents in the collection of packets. Further, the elements under each category are arranged in descending count order. However, the view may be configured to display in, e.g., ascending count order. Alternatively, the items under categories may be arranged in alphanumeric order. The user preferably has control over the ordering method used.
Moreover, each element listed in the several categories is also preferably a clickable link. Thus, in order to further drill down into the collection of packet data 310 , a user merely needs to click (with a mouse or other pointing device) on, or select, a desired element under a given category. For purposes of discussion, element 475 , which corresponds to IP address 192.168.1.147, may be clicked, which causes screen 500 of FIG. 5 to be displayed. Screen 500 includes substantially the same categories as screen 400 , but now only data that is associated with IP address 192.168.1.147 is displayed. As shown, that IP address is also now listed first under the IP address category. Thus, by a single click of a mouse (or other known selection method), a user can capture from the collection of packets 310 all network information having to do with the selected IP address. As can be seen, the number of different application types 410 is fewer, as are the elements of the time and protocol categories 412 , 414 . In other words, by selecting an element from screen 400 , the collection of packets is filtered based on the selected element—in this case a selected IP address.
Noteworthy in screen 500 is the beginning of a “breadcrumb” 510 that delineates a drill down or query path. In a preferred embodiment, each element in breadcrumb 510 is a clickable link enabling the user to quickly move back up the path (and display an earlier screen). To still further drill down, a user may, for example, click on element “HTTP” under the applications category 410 , thereby further filtering the data to be presented. Screen 600 of FIGS. 6A and 6B shows the result of the further filtering and a further expanded breadcrumb path 510 . By then clicking on, e.g., a selected email address (e.g., “mikeyj52@hotmail.com”) 675 ( FIG. 6B ), screen 700 of FIG. 7 is displayed to a user.
Screen 700 is another unique visual display of network data in accordance with the present invention. This view may be referred to as an “event view” or “session description” in that network data filtered in accordance with an IP address, a selected application (or service), and a particular email account and shown via screens 400 , 500 and 600 , is now depicted by session. Session 710 , for example, is arranged in five general columns: a view select button/icon 730 , time, service (or application), size and events. The time, service and size columns correspond to the same categories on screens 400 , 500 , and 600 . By clicking on view button/icon 710 , screen 800 of FIG. 8 is displayed to the user. In addition, by hovering a mouse over the shown image, a quick preview of the content screen 800 of FIG. 8 may also be shown. FIG. 8 is described later herein.
The events column of screen 700 is of particular interest. The first line of this column identifies two entities (192.168.1.147 and 64.4.48.250) that are part of the session being “depicted” in this view. Further down the column are several actions such as “put,” “send from” and “send to” along with destination or source locations associated with the specific event. Thus, by quickly scanning screen 700 , it is possible to obtain a simple view of a session that includes, in this case, IP address 192.168.1.147 and the mickeyj52@hotmail.com email address. Referring back to FIG. 6B , it can be seen that the count associated with element 675 is four. Thus, although not all are shown in screen 700 of FIG. 7 , four separate sessions could be viewed by scrolling down on screen 700 .
Actions that may be listed under the events column of screen 700 may include, but are not limited to:
login logoff sendfrom sendto get put delete attach print
Also shown in screen 700 of FIG. 7 are arrows 755 that designate which way communication between the identified nodes is directed. As shown, most of the communication is directed from IP address 192.168.1.147 to IP address 64.4.48.250. Further, as shown, next to each of the arrows 755 , is preferably a description or the nature of the data that is being passed from one node to the other in the session. Thus, for instance, the subject of an email is listed, or the notation “text/html” is listed showing information passing from the node on the right to the node on the left.
Finally, to keep views manageable, clickable elements “collapse events” 780 and “expand events” 782 are provided to enable a user to minimize or maximize the list of events for a given session 710 .
If a user desires to view more definitively the actual content of a given session, the user may click on view element 730 , which leads to screen 800 of FIG. 8 . In this case, a web page is seen as the content. This is consistent with the last listed event in the top session 710 on screen 700 —text/html.
From the forgoing it can be appreciated that embodiments of the present invention provide an intuitive and efficient view into network data, and particularly network data that has been stored and is now being analyzed. A user can select a given collection of packet data, and then quickly “drill down” through that data using an intuitive graphical user interface and mouse (or other pointing device). Many of the views allow a user to move back and forth between different types of views, thus enabling a user to quickly find connections between network users, patterns in network use, and obtain insight into general network operations, among other things.
The systems and methods described herein may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The foregoing embodiments are therefore to be considered in all respects illustrative and not meant to be limiting.
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A method of visualizing network data includes parsing a collection of packets in accordance with a set of categories related to characteristics of the collection of packets, the categories including listings of categorical elements, wherein at least some of the categorical elements are selectable by a user. When a categorical element is selected by a user, the collection of packets is filtered in accordance with the selected categorical element. Alongside each categorical element is a selectable count value that is indicative of the number of discrete communications sessions in which an associated categorical element is present in the collection of packets. When the count value is selected, a session view or views is/are created for each respective session, with content payload available for review and viewing.
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BACKGROUND OF THE INVENTION
The invention relates to a method for testing cigarette heads, at least one region of a cigarette head being irradiated with light, and light reflected by the cigarette head being received by a detector in such a way that irradiating and received reflected light run at an angle to one another, the irradiated region is imaged on the detector and a signal generated by the detector is evaluated. The invention also relates to an apparatus for testing cigarette heads, having a light source and an optical system for producing at least one region, irradiated with light, on a cigarette head, and having a detector, for receiving light reflected by the cigarette head, which is arranged in such a way that irradiating and received reflected light run at an angle to one another and the irradiated region can be imaged on the detector.
A test method or a testing apparatus is known for contactless testing of cigarette heads, in the case of which a straight line is radiated onto a tobacco-end cigarette head. If the cigarette is not properly filled with tobacco, the line no longer appears as a straight line—if it is observed from a different viewing angle—, but as a wavy line or as a broken wavy line. This image is detected by a sensor. Finally, the image points which lie inside and outside a narrow region around an imaginary, theoretical straight line are counted and their ratio is formed. If this ratio exceeds a limiting value, this is formed to indicate that a cigarette is not properly filled.
This type of testing has the disadvantage that it is inaccurate and does not permit exact statements on the state of a cigarette. The invention is therefore based on the problem of improving the testing of cigarettes and permitting more accurate statements on the state of a cigarette.
SUMMARY OF THE INVENTION
For the purpose of solving this problem, the method according to the invention is characterized in that, when evaluating, a possible deviation, in particular a distance, of the position of the image of the irradiated region from an expected position of an image of a corresponding region of an ideal cigarette head on the detector is determined, the deviation being used to determine the distance of the irradiated region from a desired position of this region. Furthermore, the problem is solved by an apparatus according to the invention which is characterized by an evaluation device which evaluates a signal generated by the detector in order to determine a possible deviation, in particular a distance, in the position of the image of the irradiated region from an expected position of an image of a corresponding region of an ideal cigarette head, in order to determine from the deviation the distance of the irradiated region from a desired position of this region.
A cigarette head can be measured in a contactless fashion by means of the invention. In this case, it is preferred for the light beam of a laser or another bright light source to be used and focused onto a cigarette head via a lens. One or more image points are thereby illuminated essentially at the test distance. A lens focuses the reflected light on a position-sensitive detector. If the illuminated region is not located in its desired position, this leads to a deviation in the image point on the position-sensitive detector, or to a deviation in the image of the illuminated region with reference to an expected position of the image on the detector. On the basis of the geometrical arrangement of the cigarette head or the desired position of the cigarette head, the direction of incidence of the light and direction of the reflected light, as well as of the distances of these positions from the lens or from the optical system and from the detector, this deviation, which may be expressed as a distance, yields the distance of the irradiated region in relation to a desired position of this region.
The invention achieves a very high measuring accuracy. Furthermore, an instantaneous exposure of the cigarette head suffices for determining these distances. Consequently, a cigarette head can be measured as it moves and in a contactless fashion. This permits a high operating speed of the cigarette packaging or cigarette producing machine.
It is preferred to irradiate and evaluate a plurality of regions of a cigarette head. It is possible in this way to judge the correct construction, in particular of recess filter or Russian cigarettes and, in particular, to measure the length of a hollow section of a tip sleeve of such cigarettes. Furthermore, the correct, in particular round construction of such tip sleeves can be monitored by irradiating a plurality of points or relatively small regions onto the end region of a tip sleeve.
BRIEF DESCRIPTION OF THE DRAWING
Further preferred embodiments of the invention follow from the subclaims and with the aid of the exemplary embodiments illustrated in the drawing, in which:
FIG. 1 shows a testing apparatus according to the invention for testing the heads of a cigarette formation, having a light source arranged directly upstream of a lens-stop system;
FIG. 2 shows a further testing apparatus according to the invention, having a glass fibre line for guiding light from a remote light source to a lens-stop system;
FIG. 3 shows a further testing apparatus according to the invention, having a glass fibre bundle for guiding light of a light source into the region of the cigarette ends;
FIG. 4 shows a stop or arrangement of the glass fibre ends of the glass fibre bundle of FIG. 3, in accordance with a section along the line IV—IV in FIG. 1;
FIG. 5 shows the light pattern, yielded by the use of a stop or an arrangement of glass fibres in accordance with FIG. 4, on a 7/6/7 formation of 20 cigarettes, in accordance with a section along the line V—V in FIG. 1;
FIG. 5 a shows the geometrical structure of an image of a correctly constructed cigarette on a detector;
FIG. 5 b shows the image resulting on the detector in the case of a geometrical arrangement in accordance with FIG. 5 a , in the case of a section in accordance with the plane of section Vb—Vb;
FIG. 6 a shows the geometrical structure of an image of a cigarette which is too short on a detector;
FIG. 6 b shows the image resulting on the detector in the case of a geometrical arrangement in accordance with FIG. 6 a , in the case of a section in accordance with the plane of section VIb—VIb;
FIG. 7 a shows the geometrical structure of an image of a cigarette of correct length but defective filling on a detector;
FIG. 7 b shows the image resulting on the detector in the case of a geometrical arrangement in accordance with FIG. 7 a , in the case of a section in accordance with the plane of section VIIb—VIIb;
FIG. 8 a shows the geometrical structure of an image of a recess filter cigarette of correct construction, on a detector; and
FIG. 8 b shows the image resulting on the detector in the case of a geometrical arrangement in accordance with FIG. 8 a , in the case of a section in accordance with the plane of section VIIIb—VIIIb.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a testing apparatus 10 for testing cigarette heads, having a light source in the form of a laser 11 . In addition or alternatively, it is also possible to use other light sources having bright light which is monochromatic or non-monochromatic and non-coherent such as, for example, bright LEDs. The light source can shine permanently or be operated in a pulsed fashion in order to produce individual light flashes.
A light beam 12 emanating from the laser 11 strikes a lens-stop system 13 which has a lens 14 and a stop (diaphragm) 15 or mask. This lens-stop system 13 converts the light beam 12 into light 18 irradiating cigarette heads 16 of a cigarette formation 17 . The irradiating light 18 is reflected by the cigarette heads 16 . Located in a direction of reflecting is a detector 19 , for example a CCD camera, that is to say a camera having a CCD chip, comprising a plurality of two-dimensionally arranged CCD elements, for producing a two-dimensional image with a multiplicity of pixels.
Reflected light 20 received by the detector 19 is arranged at a non-vanishing angle to the irradiating light 18 , that is to say the light beams incident on the cigarette heads 16 are reflected to the detector 19 in a direction deviating from the direction of incidence. In addition to the CCD chip, the detector 19 also has an optical system 21 , in particular a lens located therein. This optical system 21 serves the purpose of focusing the reflected light beams 20 onto the CCD chip. The detector 19 is connected via a cable 22 to an evaluation device in which the received image or images of the irradiated regions of the cigarette heads 16 are evaluated.
The cigarette formation 17 is tested in accordance with FIG. 1 as an overall, three-layer formation. Consequently, the detector 19 also detects the cigarette heads 16 of all cigarettes located inside the cigarette formation 17 . The evaluation device must therefore evaluate an image comprising a number of partial images, specifically 20 , corresponding to the number of cigarettes in the formation 17 . This testing of the cigarette formation 17 preferably takes place on the cigarette turret of a cigarette packaging machine. If a defective cigarette is detected in this testing method, this leads to ejection of the corresponding defective cigarette formation 17 .
Furthermore, it is also possible to investigate only a single cigarette. Such testing can also take place in the cigarette magazine of a cigarette packaging machine, in which case it is only individual cigarettes which are ejected, and not an entire cigarette formation 17 . The ejection of individual cigarettes is then performed in accordance with the way described in the German Laid-Open Patent Application DE 36 20 735 A1, in particular with the aid of an apparatus explained there.
FIG. 2 shows a further testing apparatus 23 , which corresponds to the testing apparatus 10 illustrated in FIG. 1, with the following exception: the light beam 12 does not pass directly to the lens-stop system 13 , but is firstly guided via an optical system 24 , in particular having a lens 25 . This optical system 24 focuses the light beam 12 onto a glass fibre line 26 which has at its ends a section 27 for entry of the light coming from the optical system 24 , and a section 28 for exit of the light coming from the glass fibre line 26 . The light coming from the exit section 28 passes to the lens-stop system 13 . The testing apparatus 23 corresponds otherwise to the testing apparatus 10 in accordance with FIG. 1, to the description of which reference is hereby made.
The glass fibre line 26 serves the purpose of enabling a light source 11 also to be arranged at a different location than in the immediate vicinity of the lens-stop system 13 . This has the advantage that it is possible for some of the components of the testing apparatus 23 to be arranged where enough space is available. Other components, such as the lens-stop system 13 , can then be accommodated in the immediate vicinity of the cigarette or cigarette formation 17 . The detector 19 can be accommodated at a different location as appropriate. For this purpose, the detector 19 is likewise connected optically to the site of the cigarette testing, likewise via a glass fibre line. The reflected light 20 is then focused into an appropriate glass fibre line via a small optical system. This produces further space in the region of the cigarette or cigarette formation to be tested.
Alternatively, instead of the stops 15 illustrated in FIGS. 1 and 2, it is also possible to use a hologram in order to produce a structured light pattern on the cigarette heads 16 of the cigarette formation 17 .
FIG. 3 shows a further testing apparatus 29 , which likewise has a light source 11 . The light beam 12 emanating from the light source 11 is guided, in a fashion similar to FIG. 2, onto an optical system 24 having a lens 25 . This lens 25 serves to focus the light beam 12 onto a bundle of glass fibre lines, or onto the individual fibres of a glass fibre line. The term glass fibre bundle 30 is used below generically for both variants, that is to say both for a bundle of individual glass fibre lines and for a glass fibre line having a multiplicity of individual glass fibres.
The glass fibre bundle 30 likewise has an entry section 31 for the entry of the light coming from the optical system 24 , and an exit section 32 for the exit of the light originating from the glass fibre bundle 30 . An apparatus 33 guides the light coming from the exit section 32 in the direction of the cigarette heads 16 . The apparatus 33 serves either only to hold the exit section 32 , or else only to arrange the fibres or glass fibre lines of the glass fibre bundle 30 , in order to produce a specific structured light pattern on the cigarette heads 16 . This is, in particular, an arrangement in accordance with the way illustrated in FIG. 4, the regions illustrated as relatively large circles respectively illustrating a bundle of glass fibres, while the regions illustrated as relatively small circles illustrate only a few or individual glass fibres.
Otherwise, the testing apparatus 29 illustrated in FIG. 3 corresponds to the testing apparatuses 10 and 23 , to which reference is made, illustrated in FIG. 1 or 2 . This holds, in particular, for the embodiment (not illustrated) of an additional glass fibre line from the cigarette heads 16 to the detector 19 , that is to say for transporting the reflected light 20 .
FIG. 4 shows the stop 15 in accordance with a section along the line IV—IV in FIG. 1 . This stop 15 has three rows of relatively large openings 34 , and a number of relatively small openings 35 arranged around the openings 34 . This stop produces a structured light pattern on the cigarette heads. Each relatively large opening 34 corresponds to the central region of a cigarette located in a cigarette formation 17 . This opening 34 serves the purpose of illuminating a large portion of the cigarette head, in particular essentially 40% to 90% of the surface of the end face of a cigarette head. This relatively large opening 34 serves the purpose of producing a light spot for testing the tobacco or the filter at the cigarette head 16 . It has a diameter of 5 mm to 6 mm, for example, when the cigarette diameter is 8 mm, that is to say the ratio of the relatively large opening 34 to the cigarette diameter is 5{fraction (6/8)}. Alternatively, the relatively large opening 34 can also be of polygonal or irregular construction.
In the example in accordance with FIG. 4, six relatively small circular openings 35 are provided in a fashion arranged circularly and concentrically with reference to the relatively large opening 34 . They are located essentially at a distance from the centre of the relatively large opening 34 which corresponds to the cigarette radius, that is to say at a distance of approximately 4 mm from the centre of the relatively large opening 34 in the case of a cigarette having a diameter of 8 mm. These relatively small openings 35 serve the purpose of illuminating the end face of the cigarette paper or the external cigarette wrapping. This is either the cigarette paper itself, or else a paper-like section surrounding a cigarette filter.
Furthermore, however, it can also be a tip sleeve of a recess filter cigarette or a Russian cigarette. A recess filter cigarette is a filter cigarette in which the cigarette filter does not terminate with the cigarette paper, the filter being situated set back instead, with the result that a hollow tip is formed. A Russian cigarette is a similar cigarette, but without a filter, that is to say a filterless cigarette likewise has a hollow tip. The construction of this hollow tip can be tested with the aid of the apparatus according to the invention and the method according to the invention. In particular, it is possible according to the invention to scan and test the contour, that is to say the circular construction of the tip, in particular. However, it is also possible to determine the depth of the tip, specifically owing to the advantageous arrangement of at least one illuminated region of the centre of a cigarette head (specifically through the relatively large opening 34 ) and owing to the arrangement of one or more illuminated regions on the edge of the tip sleeve. A depth measurement is likewise performed using the distance-measuring method described here.
However, FIG. 4 also serves the purpose of the explanation, already mentioned above, of the apparatus 33 , specifically of explaining the geometrical arrangement of individual glass fibres of the glass fibre bundle 30 for a testing apparatus 29 in accordance with the exemplary embodiment in accordance with FIG. 3 . Here, a plurality of glass fibres are respectively combined to produce relatively large formations, arranged in three layers, in accordance with the relatively large opening 34 . A smaller number of glass fibres are correspondingly arranged to produce a multiplicity of relatively small formations in accordance with the relatively small opening 35 . Such a bundling or combination of glass fibres serves the purpose of producing a structured light pattern which corresponds to the light pattern produced by a stop 15 in accordance with FIG. 4 .
FIG. 5 is an illustration of the light pattern 36 resulting on the cigarette heads 16 of a cigarette formation 17 , in an illustration of a section along the line V—V in FIG. 1 . The light pattern 36 comprises a total of 20 relatively large, circular light spots 37 arranged in three layers, specifically in a 7/6/7 formation. Six relatively small light spots 38 are respectively arranged around these relatively large light spots 37 and are located on the outer wrapping 39 of the cigarette. The relatively large light spots 37 serve as evaluation surfaces for testing the tobacco-end or filter-end ends of the cigarette heads 16 . By contrast, the relatively small light spots 38 serve as evaluation surfaces for the paper ends of the tip sleeves in the case of recess filter cigarettes and/or Russian cigarettes.
FIG. 5 a shows the geometrical structure of light 18 which irradiates a cigarette head 16 and passes as reflected light 20 onto a CCD chip 41 via a lens 40 . The cigarette head 16 is located at its correct position in the position illustrated in FIG. 5 a , and is also correctly constructed. In the case of such a correct cigarette, the result on the CCD chip 41 is a display 42 in accordance with FIG. 5 b corresponding to a section along the line Vb—Vb in FIG. 5 a . The display 42 shows a plurality of irradiated regions 43 , specifically a relatively large region 44 and six relatively small regions 45 in a concentric arrangement therewith. The circular double line is an imaginary line for orientating and indicating the cigarette wrapping 47 . All regions 43 or 44 and 45 respectively illuminate a multiplicity of CCD elements displayed in small squares. These CCD elements form an image, comprising a multiplicity of pixels, of the cigarette heads or of an entire cigarette formation.
The display 42 shown by way of example in FIG. 5 b is arranged symmetrically with the CCD chip. Furthermore, the relatively small regions 45 are also arranged symmetrically or concentrically with the relatively large region 44 . This symmetry indicates a correctly constructed cigarette of correct length. All images of irradiated regions of a cigarette head 16 are located at their expected position, since the correct cigarette head 16 is located at its desired position.
By contrast, FIGS. 6 a and 6 b show the display 48 of a cigarette which is constructed too short by the length A. The display 48 corresponds essentially to the display 42 . It is however, located in a different position, that is to say the regions 43 or 44 and 45 of the display 42 from FIG. 5 b , specifically the images of the irradiated regions of tobacco and cigarette wrapping are no longer situated in the middle of the CCD chip 41 , but are displaced upwards by comparison with the display 42 from FIG. 5 b . This deviation, that is to say displacement, in particular the distance of this displacement is detected according to the invention by the evaluation device connected to the CCD chip. A desired position of these regions at the distance of the irradiated regions can then be determined from this deviation.
FIGS. 7 a and 7 b correspondingly show the resulting display 49 of a cigarette of correct length and having a defective filling. As shown in FIG. 7 a , at the cigarette head 16 the cigarette is not filled with tobacco 50 up to the end of the cigarette wrapping 47 . This defective filling changes the display 49 by comparison with the displays 42 and 48 from FIGS. 5 b and 6 b , respectively. To be precise, the relatively large region 44 of FIG. 7 b is now no longer arranged concentrically with the relatively small regions 45 . The images of the irradiated regions, that is to say the relatively small and relatively large regions 45 and 44 , are now no longer arranged symmetrically relative to one another. It is thereby possible to infer a defective cigarette. The depth of the hole, that is to say the absence of tobacco, can be concluded from the deviation of the relatively large region 44 , that is to say from the displacement of this region by comparison with the display in FIG. 5 b . The evaluation is performed in such a way that a cigarette is detected as defective in the case of overshooting predetermined limiting values of the deviation, or in the case of asymmetries, and this leads to the ejection of the cigarette or of the cigarette group containing this cigarette.
Finally, FIGS. 8 a and 8 b show a recess filter cigarette 51 of correct construction. This recess filter cigarette 51 has a hollow tip 50 and a recessed filter 53 . The centrally irradiated region of the recessed filter 53 is imaged as a relatively large region 44 on the CCD chip. By contrast, the relatively small regions 45 , which result from illumination of the tip at six sites, do not form at sites situated concentrically with the relatively large region 44 . This asymmetry of relatively small and relatively large regions 44 and 45 is a normal phenomenon in the case of recess filter cigarettes, but also in the case of Russian cigarettes, and is taken into account when evaluating the display 54 of the evaluation device.
A deviation in the display 54 from this expected position shown in FIG. 8 b results in the case of defectively constructed recess filter cigarettes and/or Russian cigarettes. Such a deviation can likewise be tolerated within specific limiting values. Only upon overshooting of predetermined limiting values is the corresponding cigarette or an entire cigarette formation ejected.
In the case of a variant which is not illustrated, two of the previously explained testing apparatuses are provided at both ends of the cigarettes. It is possible in this way to detect the correct construction of a correctly constructed cigarette even in the case of an axial displacement thereof, since the overall length of a cigarette can be inferred on the basis of the determined distance of an end of the cigarette from its desired position at either end, respectively. It is thereby possible advantageously to prevent the ejection of inherently correct cigarettes which are, however, slightly displaced axially.
The invention opens up a multiplicity of possibilities in testing cigarette heads, with the result that it is possible to detect not only defective tobacco locations, but also the depth of tips in the case of recess filter cigarettes and/or Russian cigarettes, as well as the construction of the tip itself, that is to say whether the latter is really circular or deformed. Finally, the invention can also be used to determine the length of a cigarette exactly.
LIST OF REFERENCE SYMBOLS
10
Testing apparatus
11
Laser
12
Light beam
13
Lens-stop system
14
Lens
15
Stop
16
Cigarette head
17
Cigarette formation
18
Irradiating light
19
Detector
20
Reflected light
21
Optical system
22
Cable
23
Testing apparatus
24
Optical system
25
Lens
26
Glass fibre line
27
Entry section
28
Exit section
29
Testing apparatus
30
Glass fibre bundle
31
Entry section
32
Exit section
33
Apparatus
34
Relatively large opening
35
Relatively small opening
36
Light pattern
37
Relatively large light spot
38
Relatively small light spot
39
Outer wrapping
40
Lens
41
CCD chip
42
Display
43
Region
44
Relatively large region
45
Relatively small region
46
Circular double line
47
Cigarette wrapping
48
Display
49
Display
50
Tobacco
51
Recess filter cigarette
52
Hollow tip
53
Recessed filter
54
Image
A
Length
|
The invention relates to a method for testing cigarette heads, at least one region of a cigarette head being irradiated with light, and light reflected by the cigarette head being received by a detector in such a way that irradiating and received reflected light run at an angle to one another, the irradiated region is imaged on the detector and a signal generated by the detector is evaluated. Such known methods have the disadvantage that they are inaccurate and do not permit exact statements on the state of cigarettes. The invention is therefore based on the problem of improving the testing of cigarettes. It solves this problem by virtue of the fact that, when evaluating, a possible deviation, in particular a distance, of the position of the image of the irradiated region from an expected position of an image of a corresponding region of an ideal cigarette head onto the detector is determined, the deviation being used to determine the distance of the irradiated region from a desired position of this region. The invention also relates to an apparatus for carrying out this method.
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RELATED APPLICATION
This application claims priority to U.S. Provisional Application No. 60/699,621, filed Jul. 15, 2005, the subject matter thereof incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
This application relates generally to radar systems, and more particularly to cylindrical phased array radar antennas useful for airborne applications.
BACKGROUND OF THE INVENTION
In both military and civilian terrain mapping and object tracking there exists a need to enable coverage of an earth-fixed azimuth sector from high-altitude airships whose orientation continuously changes. The high-altitude airships are generally gas filled dirigibles or blimps that have shapes designed for maximizing their aerodynamic performance such as lift, maneuverability and stationary or forward movements. The airship's distinctive skin materials and craft shape often challenge equipment designers in their efforts to effectively mount information gathering instrumentation, such as radar systems. Still, high-altitude airships are receiving increased attention for use as radar sensor platforms because of the inherent capability of an unobstructed view of large segments of the earth's surface as well the large volume of available space within and/or around the airship.
Information gathering missions tend to require radar coverage over a broad azimuth sector that is fixed with respect to the earth's surface. However, various factors such as the airship's need to face into the wind, the variable direction of high altitude winds, and the airship's need to maintain a minimum airspeed for waste heat convection, forces airship orientation to constantly change with respect to the desired coverage sector. These factors require radar systems that can adapt to the changing attitudes in pitch, elevation, yaw and roll movements.
As a result, such high altitude airship radar sensors should not only be capable of providing coverage over the desired sector width, but should also be capable of continually reorienting the position of this sector coverage with respect to the airship. Consequently, radar orientation with respect to the airship provides few satisfactory options.
One option illustrated in FIG. 1 a is to mount a planar phased-array radar flat antenna 110 inside an airship 102 , such that it maintains coverage in a fixed direction by slowly rotating with respect to the airship as the airship orientation changes with respect to the earth. In this configuration, array normal is approximately centered in the desired coverage sector. Electronic steering is then used to position the beam within the sector. Such an internal planar phased array as shown in FIG. 1 a provides a beam output that is restricted to about sixty degrees (60°) relative to array normal. Disadvantages associated with such an approach include the undesirable requirements for heavy mechanical components, including a rotary joint and coupler that are incompatible with lightweight airship applications. Furthermore, such a solution would require an increased propulsion power to compensate for a rotating radar antenna's angular momentum. Still further, the aforementioned planar phased array cannot provide instantaneous coverage over 360°. Moreover, such a solution would suffer significant beamsteering gain loss (e.g. >9 dB) near coverage limits, thus, severely compromising overall operational performance.
Another option illustrated in FIG. 1 b is to install a non-planar radar antenna phased array 110 on an airship's doubly-curved surface as opposed to internally to airship 102 (see FIG. 1 a ), such that the phased-array conforms to a large fraction of the airship's outer surface 105 . In such a surface-conformal phased array radar system, a portion of the array whose normal approximately matches the center of the desired coverage sector is activated and then used to form and electronically position the beam within the desired sector. Numerous problems exist with this approach as well.
As is known in the art, a collimated beam of radio frequency energy may be formed and steered by controlling the phase of the energy radiated from each one of a plurality of antenna elements in an array thereof. A portion of the array whose normal approximately matches the center of the coverage sector might then be activated and used to form and electronically position the beam within a geographic sector.
For example, the curvature of surface 105 varies as a function of position on the airship surface (which is made larger or smaller due to gas expansion and contraction) so that antenna radiator element-to-element separations must also change as a function of position in order to maintain conformality. In addition, non-uniform element-to-element separations degrade the shape, gain, and sidelobes of the electronically scanned beam. Furthermore, range coverage and azimuth beamwidth are non-uniform in azimuth, as the projected aperture changes significantly as a function of azimuth. Accurate beamforming and shaping is therefore difficult because the airship surface expands and contracts significantly due to air density and temperature variations and tends to undulate or flutter due to airflow.
Still further, manufacturing and construction costs associated with the above approaches are high, due at least in part because the variable surface curvature requires the sub-panels constituting the array be of many different shapes and designs, creating adherence problems analogous to the well publicized space shuttle tiling problem.
Time-varying aperture shape associated with the conformal array approach also causes pulse-to-pulse variations that limit clutter cancellation. Other problems associated with the aforementioned approaches include complicated power and signal distribution, as different parts of the array may be hundreds of meters apart. Changing airship shapes also make calibration difficult, particularly with regard to the difficulty or inability to inject test signals into the antenna elements in the above surface-conformal approach.
An alternative mechanism for a radar system useful in a vessel such as a high altitude airship, and which overcomes one or more of the above-identified problems, is highly desired.
SUMMARY OF THE INVENTION
According to an aspect of the present invention, a radar antenna in the form of a right regular polygonal cylinder has multiple generally flat rectangular panels, each capable of operating as an autonomous electronically scanned radar, and each capable of independently forming, steering, and shaping transmit and receive beams. The flat rectangular panels are joined along vertical edges and tangent to a virtual right circular cylinder such that the panels form a right polygonal cylinder having M panels along the circumference of the cylinder and N panels along the axis of the cylinder, where M is an integer greater than or equal to three and N is an integer greater than or equal to one. A signal switching distribution network allows transmit power and requisite radar and control signals to be sent to and received from selected subsets of the panels. A processor coherently combines the outputs of the selected subsets of the panels to provide an output signal indicative of the requested coverage area.
According to another aspect of the present invention, a polygonal cylindrically shaped antenna radar array has an active aperture that focuses in one or more angular azimuth directions without inertia. The array further includes M (M≧3) adjacent, flat rectangular staves of like shape and joined to form a right regular polygonal cylinder. Each of the M staves is further decomposed into N (N≧) identical flat rectangular panels joined along their horizontal edges wherein each panel includes a plurality of antenna elements positioned in rectangular, triangular or hexagonal tessellation of the plane or lattice. Each panel contains a beam forming network that electronically forms and steers an electromagnetic beam for purposes of transmission and subsequent reception. The panels optionally may operate as autonomous radars or coherently, which when electronically combined form multiple larger antenna apertures, each capable of operating autonomously. A switching network allows transmit power and all requisite radar and control signals to be sent to and received from a selected set of panels anywhere on the polygonal cylinder.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is best understood from the following detailed description when read in connection with the accompanying drawing. The various features of the drawings are not specified exhaustively. On the contrary, the various features may be arbitrarily expanded or reduced for clarity. Included in the drawing are the following figures:
FIG. 1 a illustrates mounting a trainable planar phased-array radar antenna internal to an airship.
FIG. 1 b illustrates the conformal mounting of a phased-array radar antenna on the doubly-curved surface of an airship.
FIG. 2 a illustrates mounting a polygonal cylindrical antenna array internal to the airship in accordance with an exemplary embodiment of the present invention.
FIG. 2 b illustrates a cut-away view of a polygonal cylindrical antenna array mounted within an airship in accordance with an exemplary embodiment of the present invention.
FIG. 2 c illustrates a cut-away end view of a polygonal cylindrical antenna array mounted within airship in accordance with an exemplary embodiment of the present invention.
FIG. 3 illustrates a polygonal cylindrical antenna array mounted on the surface of and supported by an inflatable pressure vessel in accordance with an exemplary embodiment of the present invention.
FIG. 4 is a functional block diagram of a phased-array radar based on the polygonal cylinder antenna in accordance with an exemplary embodiment of the present invention.
FIG. 5 illustrates a plan view of a phased-array radar antenna having staves along the circumference of the cylindrical surface.
FIG. 6 a illustrates a perspective view of a polygonal cylindrical antenna array having active and inactive staves in accordance with an exemplary embodiment of the present invention.
FIG. 6 b illustrates a plane view of a polygonal cylindrical antenna array having sets of active and inactive staves in accordance with one embodiment of the present invention.
FIG. 7 a illustrates a perspective view of a polygonal cylindrical antenna array having sets of staggered active and inactive staves in accordance with one embodiment of the present invention.
FIG. 7 b illustrates a plane view of a polygonal cylindrical antenna array having sets of staggered active and inactive staves in accordance with one embodiment of the present invention.
FIG. 8 is a graphical plot of constant-SNR contour against range, height, and elevation for pencil beam performance of an antenna of the present invention.
FIG. 9 is a graphical plot of constant-SNR contour against range, height, and elevation for GMTI performance of an antenna of the present invention.
FIG. 10 is a graphical comparison of transmit beams with and without phase shaping of an antenna of the present invention.
FIG. 11 is a graphical comparison of receive beams with & without amplitude and phase shaping of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
In the figures to be discussed, the circuits and associated blocks and arrows represent functions of the process according to the present invention which may be implemented as electrical circuits and associated wires or data busses, which transport electrical signals. Alternatively, one or more associated arrows may represent communication (e.g., data flow) between software routines, particularly when the present method or apparatus of the present invention is a digital process. In the embodiments of the invention disclosed herein, the airships are gas filled dirigibles, however, the invention as disclosed is not limited in its application to dirigibles, but may be employed in other types of aircraft, satellites or stationary ground radar systems.
As previously discussed with regard to FIG. 1 a and FIG. 1 b , an airship 102 surface curvature 117 changes continuously over an entire surface 115 , and an antenna array 110 on such a doubly-curved surface must continuously change its antenna radiating element-to-element spacings to maintain conformality. Variable element 119 spacings and changing surface curvature 117 also degrade the quality of the electronically formed beam and corresponding sidelobe structure. Radars mounted as illustrated in FIG. 1 b typically produce non-uniform azimuth beamwidth coverage, with the changing surface curvature 117 being particularly severe near the nose 107 or tail 109 of the vessel. Manufacturing and construction costs for the above designs are high because the variable surface curvature 117 requires that the sub-panels 119 constituting the conformal array be different shapes and designs. Air pressure variations due to changes in air density and/or temperature also cause the (non-rigid) airship outer surface to change shape as the airship 102 expands and contracts. Air flowing past the surface 115 also induces localized shape changes, essentially causing the surface 115 to undulate or flutter. Each of these variables contributes to making it virtually impossible to perform accurate beamforming. Additionally, an unpredictable varying surface shape 117 whose variations change as a function of time also induces pulse-to-pulse errors that limit the radar's ability to cancel severe mainlobe surface clutter. Power and signal distribution is also a problem, particularly for an airship-surface-conformal array, due to the severe spacing (e.g., hundreds of meters apart) between different parts of the array.
Referring now to FIG. 2 a , there is shown a schematic representation of a polygonal cylinder array 210 according to an exemplary embodiment of the present invention. Antenna 210 may be mounted either internal to the airship 102 (as shown in FIG. 2 a ) or beneath or above its exterior surface 115 or hull, and provides virtually instantaneous scan capability over a full 360° azimuth without inertia and without scan loss. Such mounting avoids problems associated with the surface-conformal array's shape change, since the polygonal cylinder array 210 structure is independent of the airship surface 115 . The decoupling from the airship 102 surface 115 and decomposition of antenna panel 206 elements into flat vertical staves 207 simplifies electronic calibration, as the ability to inject test signals into the antenna elements is not impeded by changing physical relationships. Furthermore, such a configuration provides for complete modular maintenance, replacement and repair of the antenna and radar components at the line or depot repair level.
FIG. 2 a shows the airship 102 having a hull in which is housed polygonal cylindrical antenna array 210 comprising a right cylinder 203 having mounted upon its outer surface 205 antenna element panels 206 arranged in columns of staves 207 . The panels 206 may be formed from various shapes such as a triangle, hexagon or rectangle, however, each panel's outer surface is flat and perpendicular to the axis of the right cylinder. The panels 206 as mounted form the polygonal structure of the cylindrical antenna array 210 . It will be recognized by those skilled in the pertinent arts that the location and manner of mounting the cylindrical antenna array 210 will depend on various factors, including the design and choice of the particular application (e.g. particular vessel or airship), and other design choices including weight, balance, and performance of the radar system to meet its intended objectives, for example.
FIG. 2 b illustrates a cut-away view of the polygonal cylindrical antenna array 210 mounted within an airship 102 . The cylindrical antenna array 210 is shown mounted through support members 320 . FIG. 2 b illustrates a cut-away end view of antenna array 210 mounted within the airship 102 . In this embodiment of the invention, the supported support members 320 that attach the outer housing of the cylindrical antenna array 210 , also attach to the inner structure of the airship 102 .
FIG. 3 illustrates cut-a-way view of the polygonal cylindrical antenna array 210 mounted on the outer surface of an inflatable pressure vessel 310 whose purpose is to keep the antenna rigid with minimum weight. The pressure vessel and antenna are then mounted inside the airship 102 . The antenna array 210 and pressure vessel 310 are supported by support members 320 that attach the outer surface or housing of the pressure-vessel-mounted cylindrical antenna array 210 , which contains electronic processing circuitry and power systems 325 , to the structure of the inflatable pressure vessel 310 . The inflatable pressure vessel provides lift to the airship 102 , but its primary purpose is to provide a lightweight and rigid support for the cylindrical array 210 . In fact through additional partial inflation pressures over the interior pressure of airship the novel configuration of the rigid cylinder shape achieves a relatively lightweight formation. In addition the antenna cylinder shape is highly scalable in terms of radar frequency, cylinder height, cylinder diameter, panel size, number of staves, and number of rows.
The antenna array 210 and supporting electronics may be jointly or separately mounted internally or beneath the airship to permit the radar coverage sector to be instantaneously repositioned to any desired azimuth, thus maintaining coverage of an earth-fixed azimuth sector as the airship changes its orientation with respect to the earth. The invention can also be used as a ground-based radar, independent of its airship application, where instantaneous inertial-less 360° azimuth coverage is desirable.
FIG. 4 shows a functional block diagram of a cylindrical polygonal antenna array 500 a and an electronic radar processing system 500 b for controlling and processing signals to/from the antenna array according to an exemplary embodiment of the present invention. The processing system includes an analog beamforming portion and a digital beamforming portion, in accordance with an embodiment of the present invention. Each panel 206 11 - 206 mn of the antenna 210 has a corresponding set of transmit-receive subsystems (“T/R subsystems”) 208 11 - 208 nm . Each set of transmit-receive subsystems (“T/R subsystems”) 208 11 -208 nm comprises individual T/R modules a 513 1 - 513 r , having optional phase shifters with amplitude control, generate multiple independent and simultaneous beams distributed to one of an associated panels 2061 , of the entire set of panel elements 206 11 - 206 nm . In a receive mode the T/R modules 513 1 - 513 r are synchronized to the previous transmissions. In one configuration, e.g., the multiple simultaneous Ground Moving Target Indicator (GMTI) radars, the multiple simultaneous transmissions emanate from separate radars or panels 206 11 - 206 nm on the cylinder 205 . The amplitude of panel 206 11 - 206 mn , both in transmission and reception, may be variably controlled depending on the mission and the need to improve the reliability of signal capture. Amplitude control typically is used to maintain low sidelobes on transmit and receive and in some cases is used in combination with phase control to shape the transmit beam. In another embodiment, the system 500 b broadens the GMTI radar transmit beams in azimuth using phase spoiling. Each broad transmit beam is filled with multiple simultaneous and narrow receive beams to provide more time on target than would be typically be available with a single transmit-receive beam pair. Each flat rectangular panel 206 may be operated as an independent sub-radar, wherein each panel individual T/R modules a 513 1 - 513 r has a corresponding element 509 . In some cases these sub-radars are grouped and coherently combined to form multiple special-purpose radars, such as the multiple staggered rows, which serve as multiple independent GMTI radars or are coherently combined to form a single pencil-beam radar for track.
Still referring to FIG. 4 and FIG. 5 , the antenna 210 array may also optionally utilize a variety of beam shapes during operation. For example, the GMTI search radars use a non-linear phase progression across all element columns on transmit and vector or complex (amplitude and phase) weighting on receive to shape the two-way beam gain in elevation. This shaping is such that signal-to-noise ratio (“SNR”) against a reference surface target at a fixed azimuth is approximately constant for any target range from the horizon into some pre-determined minimum range. The transmit beam is further broadened in azimuth by applying a non-linear phase progression across the horizontal dimension of the transmit aperture. Multiple simultaneous receive beams, each with identical elevation shape and each steered to a different azimuth then fill the broadened transmit beam. Each of the resulting simultaneous two-way beams then has the desired constant SNR property. In GMTI track, however, more panels 206 are combined and the element 206 weighting is chosen to produce a beam that is very narrow in both azimuth and elevation, as for example what is commonly referred to as a pencil beam.
FIG. 5 illustrates a plan view of a portion of the cylinder array 210 shown in FIG. 4 as an 18-stave set, having six rows. The multiple stave beams such as the six staves 560 a - 560 f are coherently shaped and steered by element level analog beamforming, and then combined by stave-level digital beamforming to form pencil beam 580 . In the illustrated example, each stave offsets 20° relative to its adjacent neighbors, 20° being characteristic of an 18-stave design. In coherently combining the multiple staves via a digital beaming system to be more fully described below, the example pencil beam 580 has been steered to 10°, the maximum electronic steering angle employed by this particular set of staves. The net beam has a higher gain than the individual stave beams 560 a - 560 f and a narrower beamwidth consistent with the projection of the total 6-stave aperture 585 as projected in the direction of the beam 580 .
The panel or stave near-field pattern of the antenna 210 is approximately a projection of the stave or shape 206 in a direction perpendicular to the plane of the panel 206 . The panel beam begins to collimate and diverge at a distance approximately given by D 2 /λ were D is the aperture width in meters and λ is the wavelength in meters. The far-field phase front is planar and subtends an angle with respect to the antenna array 210 face which is a function of the beam steering direction.
MIMO (Multiple Input Multiple Output) radar applications may also optionally be employed, where multiple sub-radars each transmit different signals, which are then received by multiple sub-radars. The outputs of these radars are combined depending upon mission assigned to the MIMO radar such as by way of example and not limitation, achieving high probability of detection or resolving targets from background or electronic countermeasures.
Again referring to FIG. 4 , the cylindrical polygon array 500 a circumscribes the outer periphery of the cylindrical surface 205 of the phased array antenna 210 , panels 206 and for purposes of illustration, comprise a subset of flat active panels 515 and a subset of inactive panels 517 in accordance with one embodiment of the present invention. The panels 206 are arranged as adjacent staves in a generally square matrix around the circumference of the cylinder 203 and along the operational length of the cylinder. The number of matrix elements will be a function of the physical dimensions of the operational circumference, length of the cylinder 205 and size of the panel 206 . The electronic system 500 b may optionally adjust each antenna 210 panel element 206 amplitude and phase independent of all other elements. This “phase-phase” capability enables each of the panel 206 elements to shape and steer its beam in two dimensions. This in turn enables configuring different radars from sets of sub-radars. Panels 206 are typically broadband, but broadband is not a limitation of the basic invention in that any bandwidth falls within the scope of the invention as disclosed. With regard to beamforming, the beam created by each flat rectangular panel 206 can be individually shaped in azimuth and elevation for very low sidelobes. When the beams from multiple panels 206 are coherently combined by digital beamforming the net beam reliably has low sidelobes. This is in contrast to pure cylinder arrays, which suffer from sidelobe blooming where cylinder curvature blocks some elements from view at wide scan angles so the sidelobes at these angles increase dramatically. In addition, the use of flat panels 206 greatly simplifies and improves calibration, sidelobe control, and beam-pointing accuracy. It also reduces SNR loss at the peak of the beam.
As further illustrated in FIG. 4 , the system 500 b receives an RF signal from panel 206 having elements 509 , which are digitized and later combined. Depending upon the radar frequency, it may be desirable to decompose each panel 206 into sub-panels, each with its own manifold. Each sub-panel would then have its own manifold and transceiver (transmitter and receiver), such that the transceiver outputs would be in-phase (I) and quadrature-phase (Q) signals. More specifically, the phased array antenna array 210 receives RF energy forming a desired beam pattern by imparting a prescribed amplitude-phase distribution over the wave field emanating from its aperture or panels 206 , each containing a radiating element 509 . An analog portion 547 of system 500 comprises a plurality of a T/R modules 513 1 - 513 r , a plurality of panel RF manifolds 516 1 - 516 r (one manifold per panel or sub-panel if there are sub-panels) that feed and receive T/R modules 513 1 - 513 r signals, a plurality of transceivers comprising wave form generators and up conversion apparatuses 514 1 - 514 r , that feed the panel RF manifolds 516 1 - 516 r , and a plurality of receiver and digital demodulators 519 1 - 519 r that receive radar signals from the panel RF manifolds 516 1 - 516 r .
The plurality of T/R modules 513 1 - 513 r amplify the transmit signals on transmission of the radar signal and amplify the received radar signal during reception. The T/R modules 513 1 - 513 r also serve to provide an element 509 phase and amplitude control. The panel RF manifolds 516 1 - 516 r receive amplified element 509 signals and feed the signals to the plurality of receiver and digital demodulators 519 1 - 519 r . The panel RF manifolds 516 1 - 516 r distribute element 509 signals on transmit and coherently combine element signals on receive.
A digital portion 549 of system 500 b comprises a digital fiber link 507 having to feed the plurality of wave form generators and up conversion apparatuses 514 1 - 514 r and to receive the plurality of receiver and digital demodulators 519 1 - 519 r radar return signals. The demodulators within the receiver and digital demodulators 519 1 - 519 r receive radar return signals which are mixed with a local oscillator 510 to produce a demodulated radar signal. Essentially, the receiver and digital demodulators 519 1 - 519 r and later associated beamforming networks electronically combine the panel 206 elements 509 to amplify the beamformer RF output and associated downconverters into digitized in-phase (I) and quadrature-phase (Q) signal that are then passed on to a signal processor.
A panel selector and distributor 520 both feeds and receives transmission signals from a fiber link 507 . Fiber link 507 receives analog signals and converts the analog signals to a digital signal so as panel selector and distributor 520 receives radar return signals from the fiber link 507 for further processing. The waveform generators and up conversion apparatuses 514 1 - 514 r and associated downconverters digitize an in-phase (I) and quadrature-phase (Q) signal that is then passed on to the panel selector and distributor 520 . The panel selector and distributor 520 receives input data from the radar controller 530 to select the panels 206 that array as a group determined by the mission. Controller 530 also inputs data directly to the T/R modules 513 1 - 513 r to establish the element 509 phase and gain control commands.
A subsystem 535 receives in-phase (I) and quadrature-phase (Q) signal from the panel selector 520 . The subsystem 535 selects the number of panels 206 and the number of radars configured and sets up the multi-radar in-phase (I) and quadrature-phase (Q) output signals. The digital data from sub system 535 feeds a multi-radar signal and data processing system 534 to achieve proper pulse compression and to choose selected processing modes to overcome the effects of clutter or electronic countermeasures. The multi-radar signal and data processing system 534 output provides input to the radar controller 530 for among other things multi-radar detections and mapping data. Radar controller 530 also receives appropriate input from an air ground command 540 , which in turn is dependent on human-machine interface 550 that allows human intelligence through an air ground link 555 to establish various mission operating parameters.
It is understood that the processor, memory and operating system with functionality selection capabilities can be implemented in hardware, software, firmware, or combinations thereof. In a preferred embodiment, the processor functionality selection, threshold processing, panel selection and mode configuration may be implemented in software stored in the memory. It is to be appreciated that, where the functionality selection is implemented in either software, firmware, or both, the processing instructions can be stored and transported on any computer-readable medium for use by or in connection with an instruction execution system, apparatus, or device, such as a computer-based system, processor-containing system, or other system that can fetch the instructions from the instruction execution system, apparatus, or device and execute the instructions.
Further, it is understood that the subject invention may reside in the program storage medium that constrains operation of the associated processors(s), and in the method steps that are undertaken by cooperative operation of the processor(s) on the messages within the signal and data processing network. These processes may exist in a variety of forms having elements that are more or less active or passive. For example, they exist as software program(s) comprised of program instructions in source code or object code, executable code or other formats. Any of the above may be embodied on a computer readable medium, which include storage devices and signals, in compressed or uncompressed form. Exemplary computer readable storage devices include conventional computer system RAM (random access memory), ROM (read only memory), EPROM (erasable, programmable ROM), EEPROM (electrically erasable, programmable ROM), flash memory, and magnetic or optical disks or tapes. Exemplary computer readable signals, whether modulated using a carrier or not, are signals that a computer system hosting or running the computer program may be configured to access, including signals downloaded through the Internet or other networks. Examples of the foregoing include distribution of the program(s) on a CD ROM or via Internet download.
The same is true of computer networks in general. In the form of processes and apparatus implemented by digital processors, the associated programming medium and computer program code is loaded into and executed by a processor, or may be referenced by a processor that is otherwise programmed, so as to constrain operations of the processor and/or other peripheral elements that cooperate with the processor. Due to such programming, the processor or computer becomes an apparatus that practices the method of the invention as well as an embodiment thereof. When implemented on a general-purpose processor, the computer program code segments configure the processor to create specific logic circuits. Such variations in the nature of the program carrying medium, and in the different configurations by which computational and control and switching elements can be coupled operationally, are all within the scope of the present invention.
Referring now to FIG. 6 a , there is shown a perspective view of the polygonal cylindrical antenna 210 array having selective sets of active staves 515 in accordance with one embodiment of the present invention. Selected sets of panels or staves means that signals and power are sent to various subsets of panels 206 a - 206 n to form one or more active radars. As previously indicated the polygonal 205 cylinder is mounted inside or beneath the airship with the staves oriented vertically and to form a beam at a given azimuth, a subset of panels or staves 206 whose average normal is closest in azimuth to the desired beam azimuth are electronically identified. Staves 206 or sub-panels whose individual normal deviate from the desired azimuth direction by more than some pre-selected threshold angle are electronically excluded. The FIG. 5 a panel selector 520 in combination with panel-level multi-radar 535 then configures the selected staves or sub-panels as a radar whose outputs are coherently combined, and if necessary, appropriate phase progressions are applied to electronically steer the net beam to the desired angle. Since the staves 206 or sub-panels are selected to point approximately in the desired direction, electronic steering need not steer the beam by more than 180/N degrees, where N is the number of staves. As the airship changes orientation with respect the desired earth-fixed azimuth to be probed, an updated set of staves 206 or sub-panels is selected whose average normal is closest in angle to the desired beam position. Electronic steering is then applied again to provide a fine beam correction to position the beam exactly at the desired azimuth. Even if the airship rotates through a full 360 degrees, the selected set of staves or sub-panels moves around the polygonal cylinder to maintain its near-normal orientation with respect to the desired beam direction. As a result, the radar beam can continually probe a given earth-fixed azimuth independent of the airship 102 orientation.
In an example of active staves dedicated to single pencil-beam radar, FIG. 6 b illustrates a plane view of an antenna array 210 having sets of active staves 515 and inactive staves 517 . In the exemplary embodiment shown for purposes of illustration and not limitation, the 16 rows of 48 panels 206 a - 206 n , each arranged in 48 columns (staves) of 16 panels each, for a total 768 panels. In this example, 16 horizontally adjacent staves 605 are activated to electronically form the steered pencil beam, wherein the bulk of azimuth beamsteering is achieved by selecting a set of 16 horizontally adjacent staves 610 whose local normal is closest to the desired pencil beam azimuth. The final position of the pencil beam is achieved via electronic steering of stave set in azimuth and elevation. Note that no set of 16 staves need steer in azimuth more than 3.75° (½ of 7.5°) from its own local normal. The azimuth sector 610 is covered by staves numbered 6 through 21. When operating in a pencil beam mode the 3 dB beamwidth is given approximately by λ/Dp where λ is the wavelength in meters and Dp is the projected width of the aperture onto a plane perpendicular to the beam steering direction. The beam will broaden from this width if aperture weighting is applied to reduce sidelobes.
Referring now to FIG. 7 a , there is shown a perspective view of a cylindrical antenna array 210 having sets of staggered active panels 515 and inactive panels 517 in accordance with one embodiment of the present invention. Instantaneous coverage of a broad azimuth sector does not suffer a significant gain loss as the beam is electronically steered toward the limits of the coverage sector due the ability to stagger each row of active panels 515 .
FIG. 7 b illustrates a plane view of the antenna array 210 having selected sets of panels which are staggered active panels 515 and inactive panels 517 in accordance with one embodiment of the present invention. The cylinder 210 has N staves and M panels 206 per stave for a total of N*M panels. Selected sets of panels means that signals and power are sent to various subsets of these N*M panels 206 to form one or more active radars. The specific selected sets of panels are chosen dependent upon the radar mission (search, track, fire control, etc.), as by way of example and not limitation, the orientation of the airship with respect to the azimuth covered, and a predetermined radar configuration for satisfying the mission. Panels that are not selected remain neither transmit nor receive. The antenna 210 optionally positions nulls in the sidelobes and mainlobes of the beam to reduce interference and jamming. The nulls in the directions of jammers will be formed adaptively on receive, while nulls in the direction of severe surface clutter are formed deterministically.
FIG. 8 is a graphical plot of constant-SNR contour against range, height, and elevation for a pencil beam performance of the antenna 210 of the present invention. The example illustrates the performance of the antenna 210 having dimensions eight (8) meters vertical height aperture arrayed in a pencil beam 815 configuration steered to −5.09° and 300 km located at an exemplar elevation of 22,000 meters above earth's surface along the ordinate and constant ground range 810 from the antenna 210 along the abscissa. From the location of the antenna 210 are indicated constant elevation angles 820 relative to the antenna 210 and contours of constant SNR that are referenced to the SNR at the horizon. In the illustrative example, shown in FIG. 8 , the transmit aperture is uniformly weighted in amplitude and the receive aperture of 30 dB Taylor weights are applied to each element column.
FIG. 9 is a graphical plot of constant-SNR contour against range, height, and elevation for GMTI performance of an antenna of the present invention, further illustrating the antenna 210 having dimensions eight (8) meters vertical height. The result of beam shaping is plotted against contours of constant SNR 825 referenced to the SNR at the horizon. The lines 810 indicate the constant range from the antenna 210 . The GMTI beam in this example is designed to maintain constant reference-target SNR along earth's surface from −5.09° (300 km) to −60° (24.6 km). In FIG. 9 the transmit aperture is again uniformly weighted in amplitude and an exponential phase tapers down columns to broaden and shape the elevation response. The receive aperture has an amplitude and phase which tapers down columns designed to shape the response, while countering deficiencies in the transmit pattern.
FIG. 10 is a graphical comparison of transmit beams in the elevation plane with and without phase shaping of an antenna of the present plotted against a normalized gain along the ordinate and elevation angles along the abscissa. The line 830 shows the shaped transmit beam from the phase-weighted aperture, and the line 835 shows the transmit beam from a uniformly weighted aperture steered to −5.09° elevation. The transmit phase taper is chosen to complement the complex receive taper such that constant SNR is maintained along earth's surface from −5.09° to −60° elevation.
FIG. 11 is a graphical comparison of receive beams in the elevation plane with and without amplitude and phase shaping of the present plotted against a normalized gain along the ordinate and elevation angles along the abscissa. The line 850 shows the shaped receive beam from the amplitude and phase weighted aperture, and the line 840 shows the receive beam from a 30 dB Taylor-weighted aperture steered to −5.09° elevation. The receive amplitude and phase tapers are chosen to complement the transmit phase taper such that constant SNR is maintained along the earth's surface from −5.09° to −60° elevation.
While the present invention has been described with reference to the illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications of the illustrative embodiments, as well as other embodiments of the invention, will be apparent to those skilled in the art on reference to this description. It is expressly intended that all combinations of those elements that perform substantially the same function in substantially the same way to achieve the same results are within the scope of the invention. Substitutions of elements from one described embodiment to another are also fully intended and contemplated.
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A polygonal cylindrically shaped phased array antenna forming a radar has an active aperture that focuses in any of one or more angular azimuth directions without inertia. It further includes adjacent multiple similar polygonal staves joined along their vertical edges to form a right regular polygonal cylinder. Each stave is further decomposed into flat panels, wherein each panel has a plurality of antenna elements positioned in a regular rectangular or triangular lattice. Each panel contains a beam forming network that electronically forms and steers an electromagnetic beam for purposes of transmission and subsequent reception. The panels optionally may operate as autonomous radars which when coherently combined form multiple larger antenna apertures, each capable of operating autonomously. A switching network allows transmit power and all requisite radar and control signals to be sent to and received from a selected set of panels anywhere on the polygonal cylinder.
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This application is a 371 of PCT/US98/20877, filed Oct. 2, 1998 which claims benefit to U.S. provisional application Ser. No. 60/061,085, filed Oct. 3, 1997.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a locking assembly for portable firearms such as semiautomatic pistols or automatic machine pistols and, more particularly, to a locking assembly which safely houses the firearm in either a loaded or unloaded status and provides for drawing and automatically loading and cocking the firearm with only the action of the user's shooting hand.
2. Discussion of Prior Art
Locking assemblies for portable firearms are already known from U.S. Pat. No. 5,611,164. Such an assembly includes a body plate designed to center around the wearer's hip with openings to accommodate a belt for wearing, and an action locking assembly, which is attached to the body plate and exactly dimensioned for the specific pistol to be secured.
The action locking assembly includes a flat support member, and an action locking arm extending from a first upper end of the support member and a retainer arm extending from a second lower end of the support member. The action locking arm carries an action locking lug. This locking lug is received in the firing chamber and barrel face of a firearm and prevents cartridges from entering the firing chamber. When the firearm is removed from the locking assembly, the firearm is automatically loaded and cocked, ready to shoot.
A drawback of such locking assemblies is that they are made for firearms of only one length. Another drawback is that once the firearm is pulled, it has to be unloaded before it can be put back into the locking assembly. This can create problems when the user must attend to other matters before the firearm can be returned to the locking assembly.
The user may want to lock the firearm such that it can only be taken out of the assembly with a key. However, when suddenly the firearm is needed, it takes too long to unlock the firearm.
It is an object of the present invention to eliminate the above-mentioned drawbacks.
SUMMARY OF THE INVENTION
This object is reached by several improvements, according to the present invention, as follows. First, several mounting positions are provided for the action locking arm. Thus, firearms of different lengths can be locked in the locking assembly.
Second, an elastic band or “retention loop” is provided on the locking assembly in order to suspend the firearm in a loaded position within the locking assembly.
Third, for carrying the gun locked in the assembly, while still being able to remove it quickly from the assembly, the present invention provides a locking pin which has a compressible ball bearing at one end and a finger ring at the other.
Fourth, the present invention provides an enclosing holster to protect the firearm against environmental influences.
Fifth, the present invention provides several slots in the body plate in order to accommodate belts of different widths.
Finally, a spacer is interposed between the body plate and the locking assembly to facilitate mounting the enclosing holster and to enable carrying large firearms comfortably.
These and other advantages of the present invention will become more apparent from the following description, taken in conjunction with the accompanying drawings wherein like reference numerals represent like parts.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a perspective side view of a locking assembly having an adjustable locking arm according to the present invention;
FIG. 2 shows a sectional view of the locking assembly of FIG. 1;
FIG. 3 shows a firearm suspended in a locking assembly with an elastic band according to the present invention;
FIGS. 4 A, B and C show, respectively, a firearm brought into the locking assembly, the firearm suspended by an elastic band in the locking assembly, and the firearm being released out of the locking assembly according to the present invention;
FIG. 5 shows a sectional view of the attachment of the elastic band to the locking assembly;
FIG. 6 shows a groove for receiving an elastic band according to the invention;
FIG. 7 is a perspective view showing a locking assembly having an elastic band and a body plate according to a further embodiment of the present invention;
FIG. 8 is a side view showing the locking assembly of FIG. 7;
FIG. 9 is a side view showing the embodiment in FIG. 7, excluding the body plate;
FIG. 10 is a perspective view showing an enclosing holster according to the invention;
FIG. 11 is a side view of the holster of FIG. 10;
FIG. 12 shows a locking pin as known in the prior art;
FIGS. 13A and B show a locking pin according to the present invention;
FIG. 14 shows a sectional view of a locking assembly, a body plate and a spacer according to a further embodiment of the present invention;
FIG. 15 is a perspective view of the spacer and body plate of FIG. 14;
FIG. 16 shows a side view in partial section of the embodiment according to FIG. 14;
FIG. 17 shows an elevated view of a body plate having added belt slots according to a further embodiment of the present invention; and
FIG. 18 shows a top view of the embodiment of FIG. 17 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1 and 2 show a slide shield 10 of a locking assembly for portable firearms. Shield 10 has an opening 12 on the bottom and a first end 14 , which is also open. Shield 10 has a sight slot 16 to provide clearance for the forward sight of a firearm. Further details respecting the slide shield 10 may be seen in U.S. patent application Ser. No. 08/743,797, filed Nov. 5, 1996, incorporated herein by reference.
Action locking arm 18 is secured to a top wall 20 by a bolt 22 . Mounting plate 24 allows for removability of the action locking arm 18 . It may be desired to replace arm 18 with another arm more suitable for a different pistol model, or to move the action locking arm 18 to accommodate firearms with different length slides. Holes 26 are provided for this purpose.
The second end 28 of the slide shield 10 has an integral slide block 30 which provides a bearing surface for the slide of a firearm.
FIG. 3 shows a further embodiment of the locking assembly according to the present invention, including a slide shield 10 mounted to a body plate 32 and a rubber retention loop 34 .
The function of this rubber loop 34 is to allow, for example, an officer to re-holster his already loaded and cocked pistol momentarily in a secure manner while he attends to other requirements. Once the situation has stabilized, the pistol may be returned to the holster with an empty chamber and with no magazine within its grip while holstering. A loaded magazine is inserted into the grip of the pistol after the pistol's action is locked.
FIGS. 4A-4C show the use of rubber retention loop 34 . This loop 34 is retained in a stowed mode by a retention loop post 38 . A machined groove 40 is provided at an angle on the slide shield 10 to align the retention loop 34 when it is under compression against the back strap 42 of the hand gun grip. Retention loop restraining bracket 44 is so dimensioned as to allow the retention loop 34 to rotate freely within its diameter.
In FIG. 4A, the rubber retention loop 34 is secured by the post 38 on one end, with its other end secured by bracket 44 . This is the stowed position of the retention loop.
In FIG. 4B, the rubber retention loop has been manually rolled off the post 38 at which point the retention loop 34 is extended over the top of the slide shield 10 whereby the retention loop 34 is positioned into the machined grooves 40 on either side of the slide shield. The top end of the loop is extended back over the handgun's slide and into the crotch of the back strap 42 of the handgun's grip. The expanded tension of the retention loop exerts sufficient pressure to keep the hand gun locked in the slide shield 10 , without the necessity of the action locking arm 18 entering the chamber of the pistol which may be occupied by a cartridge.
FIG. 4C shows that upon gripping the handgun's handle and rolling the loop 34 up over the back strap 42 of the handgun grip, the retention loop 34 will collapse forward, releasing its tension from the handgun. At that point, the pistol can be easily withdrawn in a loaded or unloaded condition.
FIG. 5 shows another type of rubber retention method. A rubber cord 46 has on opposing ends indented nubs 48 , which are so dimensioned as to press fit into appropriately positioned holes on either side of the slide shield 10 , so as to securely lock within said holes.
As shown in FIG. 6, the locking assembly according to the present invention does not interfere with frame-mounted laser devices or high intensity flashlights 50 mounted to the underside of the handgun's frame, forward of the trigger guard. These devices 50 are being increasingly used for proper target acquisition in police and military action. In contrast with the locking assembly according to the present invention, conventional holsters are not appropriately designed to accommodate the various sizes and positions of these devices to the handgun's frame. Placement of a handgun so equipped into an inappropriate holster has often caused the on/off switch to be activated expending the battery life of the devices so that they are inoperative when the handgun is withdrawn.
The locking assembly according to present invention has no contact at any angle of its use with the frame and grip portion of the handgun while it is in its primary unloaded, locked and unlocked position, or in its loaded and cocked position restrained by the action of the rubber retention loop 34 .
FIGS. 7, 8 and 9 show an alternative embodiment of a retention loop according to the present invention. FIG. 7 shows a handgun 36 holstered in a locking assembly including a slide shield 10 and a body plate 32 . A first strap 52 consisting of stiff nylon fabric or plastic is attached to the outside of the body plate 32 . The length of this first strap 52 is proportioned and designed to be rigidly maintained within the center of the back strap 42 of the handgun's grip. A second strap 54 of like material is affixed to the slide shield 10 by means of, for example, a removable bolt and nut 56 . The length of the second strap 54 is proportioned to have it meet at the center of the back strap 42 , whereby a corresponding male snap 58 is received in the affixed rigid female snap release 60 on the first strap 52 .
The function of these snaps 58 and 60 is to exert a closing pressure at the yoke of the back strap 42 , as seen in FIG. 9 . This will allow a handgun to be carried within the locking assembly with its chamber closed with either a round in battery or with a closed empty chamber.
The muzzle end 62 of the handgun 36 is contained within the forward portion of the slide shield 10 near the slide block 30 . In order to prevent the muzzle end 62 from moving out of the slide shield 10 , a configuration of the slide shield 10 is provided having an angulation 64 . Angulation 64 shrouds a significant additional portion of the handgun's slide and lower receiver so that pressure is constant when the pistol is in this position.
So locked within the holster, the weapon cannot be withdrawn unless the snaps 58 and 60 on the straps 52 and 54 are released by unsnapping. The action locking arm 18 is in contact with the closed bolt of the chamber. The handgun 36 cannot be rocked out of the holster because of the restraint of the coupled snaps 58 and 60 nor can it be rocked away from the slide and lower receiver containment within the muzzle end of the shield 10 .
FIGS. 10 and 11 show an enclosing holster 70 , which is so fabricated to securely contain within it the slide shield 10 which is securely affixed to the body plate 32 . The enclosing holster 70 has a flap 72 which is hinged to the body 74 at flap pivot point B. The flap 72 is closely attached to the body 74 by male snap portion 76 . Female snap portion 78 has a thumb release part 80 . This release part 80 can be disengaged by a user's thumb to allow the flap 72 to swing outward and down along arrow P, exposing the handgun 36 loaded within the slide shield 10 .
In the closed position, the flap 72 secures the trigger guard of the handgun in its loaded and cocked position as shown in FIG. 3, and also protects the handgun from rain, snow, mud, etcetra.
The space 82 between the enclosing holster 70 and the slide shield 10 is provided to accommodate the downward action of the grip of the handgun allowing the muzzle end of the barrel to pass through the slide shield during the loading, cocking and withdrawal of the pistol from the holster.
The enclosing holster 70 is preferably made of leather, zytel, kydex, plastic or nylon.
FIG. 12 shows a locking pin 90 known in the art. The pin 90 includes a rod 92 which extends through hole 94 in the slide shield 10 , shown in FIGS. 1 and 2. A combination lock 96 prevents the pin from being taken out of the slide shield 10 . The pin 90 blocks the downward motion of the muzzle end of the barrel, preventing the withdrawal of the handgun.
FIGS. 13A and B show an alternative pin 98 designed with a compressible ball bearing 100 at one end to allow the pin to pass through the hole 94 and to retain the pin therein. On the other end of the pin 98 , a ring 102 is provided to pull the pin 98 out of the hole 94 .
The safety function of pin 98 is to block the downward motion of the muzzle end of the barrel if downward pressure is applied. As the muzzle cannot exit the barrel port 104 of the slide shield 10 , the weapon cannot be actioned or withdrawn. The advantage of pin 98 over the locking pin 90 is that a felon cannot snatch the weapon from the rear, but with a single pull, an officer can withdraw his handgun when he wants, loaded and cocked. The ring 102 is so sized to accommodate the index finger of the drawing hand so that the pin can easily be withdrawn with the same hand which subsequently withdraws the pistol from the slide shield 10 .
FIGS. 14, 15 and 16 show a body plate spacer 108 interposed between the body plate 32 and the slide shield 10 . The body plate spacer 108 is attached to the body plate 32 by bolts 110 . The slots 112 in the spacer 108 function to accommodate mounting an enclosing holster 70 to the spacer, as described above.
The body plate 32 and spacer 108 can be produced separately, but can also be produced as one monolithic piece, or be molded in high density polymer, or be cast as one piece in aluminum or other metal.
FIGS. 17 and 18 show again the locking assembly according to the present invention. The body plate 32 has belt slots 114 of different sizes to accommodate belts of different widths. The holster can thus be carried in perfect upright position without sliding or rotating relative to the belt.
It will be understood by those of ordinary skill in the art that modifications to the above described preferred embodiments may be made without departing from the spirit and scope of the present invention.
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Several improvements to a locking assembly for a firearm are disclosed. The locking assembly may be provided with means for adjusting a mounting position of an action locking arm ( 18 ) and lug within the locking assembly. A retention loop ( 34 ) may be attached to a slide shield ( 10 ) on the locking assembly, which retention loop ( 34 ) may be removably secured behind a firearm to retain the firearm in the slide shield ( 10 ) when the firing chamber is closed. The locking assembly may be provided with an enclosing holster ( 70 ) which receives the slide shield ( 10 ) and the firearm. The enclosing holster ( 70 ) may have a hinged flap with means for securing the flap in a closed position. Finally, a locking pin may be provided, which is insertable in a slide lock ( 30 ) of the slide shield ( 10 ) to prevent passage of the firearm's barrel through the slide block. The locking pin ( 90 ) may have at one end a grip means an at an opposite end at least one compressible ball bearing.
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TECHNICAL FIELD
[0001] The present invention relates to novel branched fluorescent materials having a α-cyanostilbene core structure, which can variously tune the fluorescent colors of red, green and blue.
Background Art
[0002] Recently, the organic EL element has been attracted considerable attention as a most suitable material for the flat panel display (FPD) having high brightness. Under this trend, a lot of the researches and developments have been carried out vigorously. The organic EL element has a structure wherein the luminescent layer is inserted between the two electrodes. The hole streaming in the anode positively charged recombines with the electron flowing in from the cathode negatively charged in the luminescent layer to become finally luminescent. The both materials of high molecular and low molecular can all be utilized to the production of the organic EL element. The both of them are proved to provide the organic EL element having high brightness.
[0003] The organic EL element is divided broadly into the two types. The one forms the luminescent layer by the use of the materials comprising the fluorescence dye to transporting the charges (See Journal of the Applied Physics, 65, 3610, 1989). The other utilizes the luminescence dye per se as the luminescent layer (See Japanese Journal of the Applied Physics, 27, L269, 1988).
[0004] The organic EL element utilizing the luminescence dye per se as the luminescent layer is further divided into the following three types. The first one is the three layers element wherein the luminescent layer is inserted between the hole transporting layer and the electron transporting layer, the second one is the two layers element wherein the hole transporting layer and the luminescent layer are laminated to the other one, and the third one is the two layers element wherein the electron transporting layer and the luminescent layer are laminated to the other one. So, the organic EL element has been known as exhibiting the improved luminescence efficiency in case that it consists of two or three layers.
[0005] In said organic EL element, the electron transporting layer comprises an electron transporting compound to function as transporting the electron from the cathode to the luminescent layer. Both of the hole injection layer and the hole transporting layer comprise the hole transporting substance to function as transporting the hole from the anode to the luminescent layer. When the hole injection layer is inserted between the anode and the luminescent layer, a number of increased holes can be flowed into the luminescent layer from the low electric field and the electrons streamed in from the cathode or the electron injection layer can be preserved restrictedly in the luminescent layer. Accordingly, the luminescent efficiency can be improved and thus the organic EL element with an excellent efficiency of the luminescence can be realized.
[0006] The various kinds of materials concentrated on triphenylamine derivatives used usually have been known widely as the materials used for such organic EL element. However, only very small number of materials are suitable for the practical use. N,N′-diphenyl-N,N′di(3-methylphenyl)-4,4′-diaminophenyl(TPD), for instance, has been informed (Applied Physics Letter, Vol. 57, No. 6, 531, 1990). However, this compound is thermally unstable and has a problem in respect to the life of element produced. Though lots of triphenylamine derivatives have been known (U.S. Pat. Nos. 5,047,686, 4,047,948 and 4,536,457, Japanese Patent Publication No. 6-32307 and Japanese Laid Open Patent Application Nos. 234681, 5-239455, 8-87122 and 8-259940), the most of them are not satisfactory at the aspect of the feature.
[0007] Neither the star-burst amine derivatives disclosed either in Japanese Laid Open Patent Application No. 4-308688 or 6-1972, or in the literature of Advanced Material, Vol. 6, 577, 1994 satisfy neither the essential requirement for the organic EL element, i.e., the high luminous efficiency and the long life, nor satisfy it the respective compounds disclosed in Japanese Laid Open Patent Application Nos. 7-126226, 7-126615, 7-331238, 7-97355, 8-48656 and 8-100172 and the literature of Journal of the Chemical Society Chemical Communication, p2175, 1996.
[0008] The compound having thiophene-ring disclosed in the literature of Advanced Material Vol. 9, 720, 1997 has a defect to emit the long wavelength beam.
[0009] As set forth hereinabove, the materials used for the usual organic EL element has still been required the improved efficiency. Accordingly, an excellent material capable of improving the luminous efficiency has been desired.
SUMMARY OF THE INVENTION
[0010] Under those circumstances, the inventors made an attempt to solve the problems in respect to the usual organic EL element and to render a new efficacy, and then synthesized a novel branched stilbene compound, whereby the inventors have discovered that the efficiency required for the organic EL element can be realized at last and possibly completed the present invention.
[0011] Accordingly, the object of the invention is directed to provide a new material with the organic fluorescent materials.
[0012] An other object of the invention is to provide a new material with the organic fluorescent materials, which can tune the fluorescent colors of red, green and blue.
DETAILED DESCRIPTION OF THE INVENTION
[0013] The invention is explained in detail herein below.
[0014] The branched α-cyanostilbene derivatives of the invention are polyphenyl derivatives of the formula 1, which can be prepared by the method showing in Examples 1 to 13.
R 2 and R 3 denotes respectively C 1 -C 6 alkyl, C 1 -C 6 alkoxy, substituted or unsubstituted amino, substituted or unsubstituted aryl, or substituted or unsubstituted heterocycle, and the substituted or unsubstituted aryl, or substituted or unsubstituted heterocycle can be condensed at the optional site of the corresponding two benzene rings.
[0015] The branched α-cyanostilbene derivatives of the formula 1 of the invention are used in the composition in the amount of 1 to 99% by weight based on the total weight of the organic electro-luminescent composition.
[0016] On the other hand, the branched stilbene fluorescent materials produced show the ultraviolet ray absorption appeared in FIG. 1 and exhibit the fluorescent emission feature shown in FIG. 2 and the electro-luminescent feature shown in FIG. 3 . Particularly, all the luminescent colors of the materials in the present invention are emitted throughout the whole color area (red, green, blue) to change the core structure in the branched basic structure. Accordingly, the present invention is considered as an invention capable of color tuning.
[0017] Further, most materials of the invention display the early decomposition temperature of 350 to 400° C. as shown in FIG. 4 to exert the high thermal stability.
BRIEF DESCRIPTION OF DRAWINGS
[0018] FIG. 1 is a diagram showing the ultraviolet absorption spectrum of the synthesized organic fluorescent materials.
[0019] FIG. 2 is a diagram showing the fluorescent emission spectrum of the synthesized organic fluorescent materials in the solid state.
[0020] FIG. 3 is a diagram showing the electro-luminescent spectrum of the synthesized organic fluorescent materials in the solid state.
[0021] FIG. 4 is a diagram indicating the result of the thermogravimetry analysis (TGA) of the organic fluorescent materials synthesized.
[0022] FIG. 5 is a scheme presenting the basic structure of the new branched α-cyanostilbene organic fluorescent materials exhibiting the luminescent feature.
EXAMPLES
[0023] The present invention will be understood more readily with reference to the following examples, however, those examples are not to be construed to limit the scope of the invention. The modification and application thereof usually acceptable in the pertinent art fall within the scope of the invention.
[0024] The process for producing branched α-cyanostilbene derivatives of formula 1 is explained herein below.
Examples 1 to 8
Preparation of a Compound for Producing Branched α-cyanostilbene Derivatives of Formula 1
Example 1
Preparation of 4,4′-dimethylbiphenyl
[0025]
[0026] 10 g(79 mmol) of 4-chlorotoluene was added into the solution of purified dimethylformamide together with 0.51 g(3.9 mmol) of nickel chloride(II), 0.617 g(3.9 mmol) of 2,2′-bipyridine, 4.14 g(15.7 mmol) of triphenylphosphine and 122.3 mmol of zinc to be agitated at 90° C. for 5 hours. When the reaction was completed, the reaction mix was poured in 1N aqueous solution of hydrogen chloride to break the complex structure. The reactant was extracted with methylene chloride and the solvent was distilled off under reduced pressure. The resulted product was washed around twice with methanol and suction-filtrated to dryness. Yield; 75%.
[0027] 1 H-NMR(CDCl 3 , ppm): 7.49(d, 4H, Ar—H), 7.25(d, 4H, Ar—H), 2.38(s, 6H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2900, 1500, 1110, 800. MS (EI) (Calculated for C 14 H 14 , 182.26 ; Found, 182).
Example 2
Preparation of 4′-methylbipheny-4-carboaldehyde
[0028]
[0029] Into CCl 4 solvent, 2.4 g(13.3 mmol) of the compound produced in Example 1 (Compound 1) and 0.536 g(3.0 mmol) of N-bromosuccinimide were added and refluxed for 24 hours. After cooled down, the reactant was suction-filtrated and the resultant solution was washed with distilled water and then was dried with anhydrous magnesium sulfate. The dried product was dissolved again in chloroform together with 5.34 g(51.2 mmol) of hexamethylenetetraamine and refluxed for 5 hours. After the reactant was cooled down, the solvent was distilled off under reduced pressure and the residue was refluxed severely in acetic acid/H 2 O(17 mL/17 mL) at 120° C. for 2 hours. Finally, 7 mL of HCl was added to be refluxed. After cooled down, the reactant was extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:3) to be dried. Yield; 24%.
[0030] 1 H-NMR(CDCl 3 ): 10.0(s, 1H, —CHO), 7.95(d, 2H, Ar—H), 7.75(d, 2H, Ar—H), 7.55(d, 2H, Ar—H), 7.28(d, 2H, Ar—H), 2.42(s, 3H, —CH 3 ).
Example 3
Preparation of 1,3,5-tris(4-methyl-phenyl)-benzene
[0031]
[0032] 20 g(149.1 mmol) of 4-methylacetophenone was added to ethanol and agitated at low temperature (5-10° C.) while introducing gradually 17.08 mL(149.1 mmol) of SiCl 4 through a syringe. After the agitation for 24 hours, the product was suction-filtrated. The resulted solid product was washed several times with ethanol and then was dried under a vacuum. Yield; 82%.
[0033] 1 H-NMR(CDCl 3 , ppm): 7.72(s, 3H, Ar—H), 7.60(d, 6H, Ar—H), 7.29(d, 6H, Ar—H), 2.41(s, 9H, —CH 3 ). IR(KBr, cm −1 ): 3010, 2950, 1600, 1500, 1410, 1390, 800. MS (EI) (Calculated for C 27 H 24 , 348.38 ; Found, 348).
Example 4
Preparation of [1,3-bis(4-methyl-phenyl)-5-(4-cyanomethyl-phenyl)]-benzene
[0034]
[0035] 5 g(14.4 mmol) of the compound produced in Example 3 (Compound 4) and 2.56 g(14.4 mmol) of N-bromosuccinimide were added in CCl 4 solvent and refluxed for 24 hours. The reactant was cooled down and suction-filtrated. The filtrate was washed with distilled water and dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The resulted product was dissolved again in THF and the solution was mixed with ethanol wherein 2.35 g(48 mmol) of NaCN was dissolved to be agitated for 5 hours. After the completion of the reaction, the solvent was distilled off under reduced pressure and the residue was washed with water to be extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:3) to be dried. Yield; 39% (Compound 5 was obtained as the byproduct. Yield; 17%).
[0036] 1 H-NMR(CDCl 3 , ppm): 7.76(s, 1H, Ar—H), 7.72(d, 4H, Ar—H), 7.60(d, 4H, Ar—H), 7.45(d, 2H, Ar—H), 7.30(d, 4H, Ar—H), 3.81(s, 2H, —CH 2 CN), 2.46(s, 6H, (—CH 3 ) 2 ). IR(KBr, cm −1 ): 3010, 2950, 2250, 1600, 1500, 1410, 800. MS (EI) (Calculated for C 28 H 23 N, 373.49 ; Found, 373).
Example 5
Preparation of [1,3-bis(4-methyl-phenyl)-5-(4-formyl)-phenyl]-benzene
[0037]
[0038] 4.67 g(13.4 mmol) of the compound 4 and 3.58 g(20.0 mmol) of N-bromosuccinimide were added in CCl 4 solvent and refluxed for 24 hours. The reactant was cooled down and suction-filtrated. The filtrate was washed with distilled water and dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:5) to be dried. The resulted product was dissolved again in chloroform together with 4.4 g(42.7 mmol) of hexamethylenetetraamine and the solution was refluxed for 5 hours. After the reactant was cooled down, the solvent was distilled off under reduced pressure and the residue was refluxed intensely in acetic acid/H 2 O(25 mL/25 mL) at 120° C. for 2 hours. Finally, 10 mL of HCl was added to be refluxed. After cooled down, the reactant was extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/ n-hexane=1:3) to be dried. Yield 17%.
[0039] 1 H-NMR(CDCl 3 , ppm): 10.0(s, 1H, —CHO), 8.0(d, 2H, Ar—H), 7.87-7.77(m, 5H, Ar—H), 7.60(d, 4H, Ar—H), 7.28(d, 4H, Ar—H), 2.42(s, 6H, (—CH 3 ) 2 ).
Example 6
Preparation of Biphenyl-4,4′-dicarboaldehyde
[0040]
[0041] 2.5 g(13.7 mmol) of the compound 1 and 6.1 g(34.3 mmol) of N-bromosuccinimide were added in CCl 4 solvent and refluxed for 24 hours. The reactant was cooled down and suction-filtrated. The filtrate was washed with distilled water and dried with anhydrous magnesium sulfate. The resulted product was dissolved again in chloroform together with 6.6 g(47.1 mmol) of hexamethylenetetraamine and the solution was refluxed for 5 hours. After the reactant was cooled down, the solvent was distilled off under reduced pressure and the residue was refluxed intensely in acetic acid/H 2 O(17 mL/17 mL) at 120° C. for 2 hours. Finally, 7 mL of HCl was added to be refluxed. After cooled down, the reactant was extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:3) to be dried. Yield ; 69%.
[0042] 1 H-NMR(CDCl 3 ): 10.1(s, 2H, —CHO), 7.99(d, 4H, Ar—H), 7.79(d, 4H, Ar—H).
Example 7
Preparation of 4,4′-dimethyl-stilbene
[0043]
[0044] 2.4 g(5.37 mmol) of (4-methylbenzyl)triphenylphosphonium bromide and 0.98 g(60%, 24.4 mmol) of NaH were refluxed in toluene for 6 hours. After cooled down, 0.586 g(4.88 mmol) of 4-methylbenzaldehyde was introduced gradually to the solution to be refluxed again for 6 hours. The resulted product was treated with water to be extracted with ethyl acetate. The solvent was distilled off and the residue was recrystallized in ethanol. Yield; 71%.
[0045] 1 H-NMR(CDCl 3 ): 7.64(d, 4H, Ar—H), 7.16(d, 4H, Ar—H), 6.90(s, 2H, vinyl).
Example 8
[0046]
Preparation of 4,4′-diformyl-stilbene
[0047] Into CCl 4 solvent, 2 g(9.6 mmol) of the compound produced in Example 7 (Compound 9) and 4.27 g(24.0 mmol) of N-bromosuccinimide were added and refluxed for 24 hours. After cooled down, the reactant was suction-filtrated and the resultant solution was washed with distilled water and then was dried with anhydrous magnesium sulfate. The dried product was dissolved again in chloroform together with 4.0 g(38.4 mmol) of hexamethylenetetraamine and refluxed for 5 hours. After the reactant was cooled down, the solvent was distilled off under reduced pressure and the residue was refluxed severely in acetic acid/H 2 O(17 mL/17 mL) at 120° C. for 2 hours. Finally, 7 mL of HCl was added to be refluxed. After cooled down, the reactant was extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:3) to be dried. Yield; 20%.
[0048] 1 H-NMR(CDCl 3 ): 10.03(s, 2H), 7.92(d, 4H, Ar—H), 7.71(d, 4H, Ar—H), 7.30(s, 2H, vinyl).
Examples 9 to 13
Preparation of Branched α-cyanostilbene Derivatives of Formula 1
Example 9
Preparation of 2,3-bis-[3,5-(4-methyl-phenyl)-biphenyl-4-yl]-acrylonitrile (Model 1)
[0049]
[0050] 0.31 g(0.8 mmol) of the compound produced in Example 4 (Compound 5) and 0.2 g(0.8 mmol) of the compound produced in Example 5 (Compound 6) were dissolved in tert-butylalcohol and purified THF solvent at 50° C. and 0.08 mL of tetrabutylammoniumhydroxide (1M solution in methanol) was gradually introduced to the solution to be agitated at 50° C. for 20 minutes. The precipitate was suction-filtered to be dried. Yield; 93%.
[0051] 1 H-NMR(CDCl 3 , ppm): 8.06(d, 2H, Ar—H), 7.80(m, 12H, Ar—H), 7.66(s, 1H, vinyl proton), 7.62(d, 8H, Ar—H), 7.32(d, 8H, Ar—H), 2.43(s, 12H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2950, 2230, 1600, 1510, 800. MS (EI) (Calculated for C 55 H 43 N, 717.94 ; Found, 718).
Example 10
Preparation of Model 2
[0052]
[0053] The same synthesizing method of Knoevenage 1 as the method for Model 1 was carried out. Yield; 74%.
[0054] 1 H-NMR(CDCl 3 , ppm): 8.06(s, 4H, Ar—H), 7.80(m, 14H, Ar—H), 7.64(m, 10H, Ar—H), 7.30(d, 8H, Ar—H), 2.43(s, 12H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2950, 2222, 1600, 1500, 1280, 800, 750. MS (EI) (Calculated for C 55 H 43 N, 845.08 ; Found, 845).
Example 11
Preparation of Model 3
[0055]
[0056] The same synthesizing method of Knoevenage 1 as the method for Model 1 was carried out. Yield; 97%.
[0057] 1 H-NMR(CDCl 3 , ppm): 8.06(d, 4H, Ar—H), 7.85(m, 18H, Ar—H), 7.66(m, 10H, Ar—H), 7.62(d, 8H, Ar—H), 2.43(s, 12H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2950, 2222, 1600, 1500, 1280, 810, 750. MS (EI) (Calculated for C 55 H 43 N, 921.18; Found, 921).
Example 12
Preparation of Model 4
[0058]
[0059] The same synthesizing method of Knoevenage 1 as the method for Model 1 was carried out. Yield; 83%.
[0060] 1 H-NMR(CDCl 3 , ppm): 8.10(s, 1H, Ar—H), 7.96(s, 1H, Ar—H), 7.80(m, 14H, Ar—H), 7.62(m, 10H, Ar—H), 7.26(d, 8H, Ar—H), 4.00(s, 6H, —OCH 3 ), 2.43(s, 12H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2950, 2220, 1600, 1510, 1230, 800, 750. MS (EI) (Calculated for C 55 H 43 N, 905.13 ; Found, 905).
Example 13
Preparation of Model 5
[0061]
[0062] The same synthesizing method of Knoevenage 1 as the method for Model 1 was carried out. Yield; 93%.
[0063] 1 H-NMR(CDCl 3 , ppm): 7.98(d, 4H, Ar—H), 7.78(m, 14H, Ar—H), 7.62(m, 15H, Ar—H), 7.32(d, 9H, Ar—H), 2.43(s, 12H, —CH 3 ). IR(KBr, cm −1 ): 3040, 2950, 2222, 1600, 1500, 1380, 800, 750. MS (EI) (Calculated for C 55 H 43 N, 947.21; Found, 947).
INDUSTRIAL APPLICABILITY
[0064] The branched α-cyanostilbene fluorescent materials with a new structure of the formula 1 of the present invention can be called an organic electro-luminescent material greatly useful to the production of the organic EL element, which exhibit the luminescent feature in all the state of powder, liquid and film.
[0065] Particularly, it is the initiative substance which can regulate the colors of red, green and blue by means of changing the core structure such as the substituent RI and can produce the high efficient display device capable of the whole color display. Furthermore, all the said materials exhibit the excellent heat stability and thus exert the excellent stability in the manufacturing process of the organic EL element.
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A branched α-cyanostilbene fluorescent materials with a new structure useful to the organic electroluminescence display (OELD), which includes the organic substance in the state of powder, liquid and film with the stilbene core structure and the terminal branched phenyl structure. The fluorescent materials of the invention exhibits the high luminescent efficiency and is capable of tuning the fluorescent colors of red, green and blue according to the core structure in the molecular, i.e., the structure of stilbene radical, particularly it exhibits the higher luminescent efficiency in the state of solid more than solution.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a radial piston engine with roller guides for axial guidance of the rollers, via which the pistons are braced against the cam ring.
2. Discussion of the Background
From British Patent GB B 2238086 there is known a radial piston engine corresponding to the preamble of claim 1 , wherein the object was to reduce the manufacturing complexity previously associated with axial positioning of the rollers and thus to lower the manufacturing and assembly costs. This object was supposedly achieved in that, in each of the spaces between the roller end faces and the cylindrical inside face as the roller guide, there is disposed a wedge piece, whose cross section viewed in piston displacement direction is a circular segment, and which positions the roller axially in the cylinder relative to the cam. ring. The wedge pieces disclosed in the cited patent can be divided substantially into three different designs.
In a first design, each wedge piece has on the side facing the roller a plane surface which bears on the end face of the roller and on the side facing away from the roller a cylindrical surface which is in contact with the inside face of the cylinder. In addition, this wedge piece is accommodated in the space between roller, piston and cylindrical inside face, without being rigidly connected to any of these components. By virtue of the fact that the wedge piece is freely movable in piston displacement direction relative to the roller, the piston urges the wedge pieces toward the cam ring during a load stroke. In the process, the wedge pieces do not yet come into contact with the cams formed on the cam ring. In the ensuing idle stroke of the piston, however, the wedge pieces strike the cams formed on the cam ring. This recurring striking contact between the cams and the wedge pieces as well as the friction occurring therebetween can lead to severe wear of the wedge pieces. A further disadvantage of this design is that the width of the cam ring must be at least sufficiently large that the cam ring in addition to the roller also provides a contact face for the two laterally disposed wedge pieces. Aside from large total weight of the radial piston engine, a broad cam ring results in high manufacturing costs due to the greater manufacturing complexity associated with precision machining of the cam ring.
In a second design, each of the two wedge pieces has on the side facing the roller a driver-like projection, which extends toward the other wedge piece in an opening provided in the piston between piston and roller. Since in this case the wedge pieces are driven back into the cylinder by the roller during an idle stroke of the piston, striking contact between the wedge pieces and the cams basically cannot occur. Due to the high relative velocity between the roller and the driver-like projections of the wedge pieces in contact with the outside circumference of the roller, however, severe abrasion can take place on the driver-like projections. With increasing abrasion of the driver-like projections, the space available for play of the wedge pieces in piston displacement direction could ultimately increase to the point that striking contact could occur between the wedge pieces and the cams. A further disadvantage of this design is that driver-like projections must be formed on the roller guides and recesses must be formed on the piston, thus increasing the manufacturing complexity and thus the manufacturing costs.
In addition, the friction between the roller and the wedge pieces in the two foregoing designs occurs over the entire end face of the roller. This relatively large-area frictional contact necessitates precision machining of the friction faces of both components, once again resulting in high manufacturing costs.
At that time a further assumption was that, by virtue of the recurring contact of the rollers with the cam ring, the rollers and thus the respective piston automatically assume a particular angular position in the cylinder or relative to the cam ring, which is critical for reliable operation of the radial piston engine. In certain cases, however, for example during initial operation of the radial piston engine, when hydraulic fluid is fed to the cylinders for the first time, it is conceivable that the pistons and thus the rollers may be inserted so far into the respective piston that contact between roller and curved path does not yet occur. To ensure the necessary angular position of the piston in the cylinder in those cases, one of the two wedge pieces has, in a third design, on the side facing the cylindrical inside face, an elongated slot, into which a bolt, clamp or the like extending through the cylinder wall engages and in this way prevents turning of the piston in the cylinder and thus of the roller relative to the cam ring. The presence of the slot leads to weakening of the wedge piece in question, however, and thus to shortening of the useful life of the wedge piece, which is subjected to severe stresses and strains during operation of the radial piston engine. In addition, sliding contact takes place between the wedge piece and the bolt or clamp, which appears disadvantageous as regards good roller guidance. Furthermore, such a structural feature means high manufacturing complexity.
BRIEF SUMMARY OF THE INVENTION
In view of the disadvantages encountered in conventional radial piston engines, the object of the present invention is therefore to provide an optimally engineered radial piston engine, which is characterized by greater manufacturing simplicity and at the same time functionally reliable operation.
This object is achieved by the inventive subject matter according to the features of claim 1 , which is characterized in particular in that the roller guides disposed on the front sides of the rollers are rigidly connected to the respective roller with respect to sliding in piston displacement direction.
Since the respective roller urges the roller guides in piston displacement direction, in other words both during the load stroke and during the idle stroke, the roller guides can be dimensioned such that they do not project beyond the outside circumference of the respective roller, thus ensuring that striking contact does not take place between the roller guides and the cam ring. This ultimately leads to longer useful life of the roller guides and thus to functionally reliable operation of the radial piston engine on the whole. In addition, material economies are achieved in the manufacture of the roller guides.
If the roller guides do not come into contact with the cam ring, the width of the cam ring can be further reduced to a width which corresponds at most to the width of the rollers. In this way, not only is the total weight of the radial piston engine lessened, but also manufacturing complexity and thus the manufacturing costs are considerably reduced with regard to precision machining of the curved paths of the cam ring.
By suitable structural measures, such as by formation of a cylindrical projection on the roller guide, which projection is inserted in a corresponding recess on the front side of the roller, the relative velocities at the friction faces of roller and roller guides and thus the wear of the two components can also be reduced. Because of the reduced wear, the play developed between roller and roller guides is kept to a minimum, even after prolonged operating time. This contributes to functionally reliable and dependable operation of the radial piston engine on the whole.
Further advantageous features of the inventive radial piston engine are subject matter of the dependent claims.
The roller and roller guides can be rigidly connected with respect to sliding in displacement direction by simple manufacturing techniques. For example, the roller guides can be provided on the side facing the end face of the roller with a cylindrical projection, which is insertable into a central cylindrical recess formed on the end face of the roller. Likewise, it would naturally also be conceivable for the roller guides to be provided on the side facing the front side of the roller with a recess into which a projection formed on the front side of the roller is insertable. Of course, the opening and the projection engaged therewith could also have conical shape. If the diameter of the openings and projections are dimensioned such that they are small compared with the outside diameter of the roller, or in other words such that the projections and the openings are concentrated on a central region around the axis of rotation of the roller, and if the projections are engaged with the respective openings in such a way that play is present between the annular face of the roller around the opening and of the face around the projection of the roller guide, the circumferential velocities present at the outside circumference of the projection and at the inside circumferential wall of the opening during operation of the radial piston engine are reduced, as is therefore the relative velocity between roller and roller guides. Moreover, since no friction occurs at the two spaced-apart faces of roller and roller guide, reduction of frictional abrasion of both components is achieved.
The surfaces of the roller guides in contact with the cylindrical inside face preferably have cylindrical shape for simplicity, thus achieving optimal guidance of the piston-roller system in the cylinder. Since the roller is normally not subjected to compressive loads in axial direction, it would also be conceivable, however, to give the surface of the roller guide bearing on the cylindrical inside face rotationally symmetric shape or to construct it as a spherical segment relative to the axis of rotation of the roller. In this case, rigid connection between roller guide and roller would even be possible both in piston displacement direction and in the direction of rotation of the roller. This would have the advantage that, during operation of the radial piston engine, friction between roller and roller guides would no longer take place and the friction occurring between roller guide and cylindrical inside face would be considerably reduced.
Heretofore it has been assumed that the roller is constantly in contact with the curved paths of the cam ring, whereby the angular position of the piston in the cylinder and accordingly the orientation of the roller relative to the curved path is automatically predetermined. As already explained in the introduction, however, it is possible for the contact between roller and cam ring to be separated. In this case it is possible according to the present invention to prevent turning of the piston in the cylinder by means of an antirotation device disposed separately from the roller guide and thus to maintain a particular orientation of the roller relative to the cam ring.
For this purpose, the piston can be provided on the end portion facing away from the roller with a flattened part oriented perpendicular relative to the axis of rotation of the cylinder block, which flattened part bears on a corresponding contact face of the antirotation device, thus unambiguously predetermining the angular position of the piston in the cylinder and of the roller relative to the curved path. Another effective expedient has proved to be providing the cylinder with at least two cylinder portions of different inside diameters and the piston accordingly with at least two piston portions of different diameters matching the corresponding cylinder diameters. In this case, the antirotation device is provided in the cylinder portion with the smaller inside diameter and the flattened part is provided accordingly on the piston portion with the smaller diameter. By this expedient, on the one hand a large face for admission of pressure is retained on the piston and on the other hand only little material is removed from the piston in order to form the flattened part. The additional antirotation device creates better guidance of the piston in the cylinder compared with the conventional antirotation device mentioned in the introduction, since according to the present invention large-area sliding contact takes place between piston and antirotation device.
The antirotation device preferably has a cross section which, viewed in piston displacement direction, is a circular segment, with an arc corresponding to the cylindrical inside face and a chord corresponding to the flattened part.
Since the cylinder block in any case is normally provided with axial inlet ports, through which the hydraulic fluid enters the respective cylinder spaces, the manufacturing complexity with regard to fixing the antirotation device in the cylinder can be reduced in that the antirotation device is fixed in the cylinder by means of a pin, which is inserted through the inlet port into a blind hole in the cylinder block aligned with the inlet port.
BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS
Further features and advantageous embodiments of the present invention will become clear from the description hereinafter of preferred embodiments with reference to the drawing, wherein
FIG. 1 shows a longitudinal section of a preferred embodiment of the inventive radial piston engine;
FIG. 2 shows a cross section through the cylinder block in FIG. 1 along line II—II;
FIG. 3 a shows a section on larger scale through the cylinder block in FIG. 2 along line III—III;
FIG. 3 b shows a perspective view of the piston;
FIG. 4 shows a section through the cylinder block along line IV—IV in FIG. 1;
FIG. 5 shows a perspective view of the roller guide;
FIG. 6 shows a section through the cylinder block along line VI—VI in FIG. 1;
FIG. 7 shows a perspective view of the antirotation device;
FIGS. 8 a and 8 b show modifications of the roller guide in FIG. 5;
FIGS. 9 a and 9 b show modifications of the connection between roller guide and roller in FIG. 5; and
FIGS. 10 a and 10 b show modifications of the cylinder block in FIG. 3 a.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIGS. 1 to 6 there will be described a preferred embodiment of the inventive radial piston engine. Radial piston engine 2 comprises, as illustrated in FIG. 1, substantially two housing parts 4 and 6 as well as a cam ring 8 disposed between the two housing parts 4 and 6 . The two housing parts 4 and 6 and cam ring 8 are coaxially connected to one another in fluid-tight manner by means of bolts 10 . On the inside face of cam ring 8 there is formed a curved path 12 with a plurality of cams 14 , as can be seen in particular in FIG. 2 .
Inside cam ring 8 there is disposed a cylinder block 18 which can rotate around a longitudinal axis of rotation 16 . As is evident in FIGS. 1 and 2, cylinder block 18 is provided with a central opening 20 having an internal toothing. In this opening 20 there is accommodated in axial sliding relationship an end portion 22 of a driven shaft 24 , which is equipped with an external toothing corresponding to the internal toothing of opening 20 . By means of a bearing assembly 30 , driven shaft 24 is mounted to rotate relative to the two housing parts 4 and 6 and to cam ring 8 . Bearing assembly 30 comprises two tapered roller bearings 32 and 34 , which are mounted in housing part 4 and can transmit large axial and radial forces. The other end portion 26 of driven shaft 24 projects out of housing part 4 and is provided with a shaft flange 28 for fastening to a drive element (not shown) of a device to be driven, such as a gear of a loader.
In cylinder block 18 there is also formed a plurality of cylinders 36 directed radially outward in a star pattern relative to axis of rotation 16 , which cylinders have cylinder axis 37 perpendicular relative to axis of rotation 16 . As is evident in the enlarged illustration in FIG. 3 a , cylinder 36 has a cylinder portion 38 of large inside diameter disposed radially outward relative to axis of rotation 16 , as well as a cylinder portion 40 with small inside diameter disposed radially inward. Cylinder portion 38 is open at the substantially cylindrical outside circumferential face 42 of cylinder block 18 . Furthermore, there is formed in cylinder block 18 an inlet port 43 , which is parallel to longitudinal axis of rotation 16 and opens into cylinder portion 40 , and via which hydraulic fluid is supplied and removed during operation of radial piston engine 2 .
In cylinder 36 there is accommodated a piston 44 which, as shown in FIG. 3 b , has piston portions 46 and 48 . Piston portion 46 has a diameter corresponding substantially to the inside diameter of cylinder portion 38 . Piston portion 48 has on its outside circumference two flattened parts 48 a and 48 b which, as is evident in FIG. 6, are oriented perpendicular to axis of rotation 16 . The diameter of the outside circumference of piston portion 48 corresponds to the inside diameter of cylinder portion 40 . Flattened part 48 b defines a contact face, which bears on a correspondingly provided contact face 50 b of an antirotation device 50 , to be described in more detail hereinafter. Flattened portion 48 a faces inlet port 43 .
When cylinder 36 is supplied with hydraulic fluid via inlet ports 43 during operation of radial piston engine 2 , pistons 44 are pressurized selectively to the effect that they execute a displacement movement toward cam ring 8 . In the process they are each braced via a corresponding roller 54 against curved path 12 formed on cam ring 8 . As shown in FIG. 1, axial width B of the cam ring in this embodiment of radial piston engine 2 corresponds substantially to the axial length of rollers 54 . On the end portion of each piston portion 46 facing cam ring 8 there is formed a bearing 56 , in which there is accommodated the respective roller 54 , mounted to rotate relative to piston 44 around an axis of rotation 58 .
As shown in FIGS. 1, 3 a , 4 and 5 , a roller guide 60 is disposed at each of the two front sides 54 a and 54 b of roller 54 , whereby the axial position of roller 54 in cylinder 36 and thus relative to piston 44 and curved path 12 is predetermined. Roller guides 60 are each disposed in a space formed between end faces 54 a and 54 b of roller 54 , piston 44 and the cylindrical inside face of cylinder 36 . FIG. 5 shows a perspective view of roller guide 60 which, viewed in piston displacement direction, has a cross section substantially in the form of a circular segment. On the chord side facing front side 54 a or 54 b of roller 54 , each roller guide 60 has a cylindrical projection 62 which is axial relative to axis of rotation 58 and which is engaged with a corresponding central recess 54 c or 54 d on front sides 54 a and 54 b of roller 54 . Cylindrical arc side 63 of each roller guide 60 bears on the cylindrical inside face of cylinder 36 . The length of axial projection 62 is somewhat greater than the depth of recess 54 c and 54 d , and so play exists between the face of roller guide 60 around central projection 62 and each annular face on front sides 54 a and 54 b of roller 54 around central recess 54 c and 54 d.
By virtue of the type of connection of roller guides 60 with roller 54 described hereinabove, roller guides 60 are driven in piston displacement direction by respective roller 54 during operation of radial piston engine 2 , or in other words during a displacement movement of the piston. Since, as described hereinabove, the width of the cam ring corresponds to the length of the rollers, striking contact between the roller guides and the cam ring does not occur during operation of the radial piston engine according to this embodiment, regardless of whether the roller guides project beyond the roller in piston displacement direction. In addition, the wear of both components due to the relative velocity that occurs between roller guides and roller during operation of the radial piston engine can be reduced considerably, since the friction between the two components occurs in a range in which the relative velocity is quite low.
As is evident in FIG. 6 and has already been mentioned hereinabove, there is provided at the cylindrical inside face of cylinder portion 40 opposite inlet port 52 a so-called antirotation device 50 , which has the function of preventing turning of piston 44 in cylinder 38 around a cylinder axis 37 . The critical factor here is that a particular angular position of piston 44 relative to cylinder axis 37 and thus of roller 54 relative to curved path 12 is maintained. Antirotation device 50 is fastened to cylinder block 18 by means of a pin 76 , such as a tapered pin, straight pin or grooved pin in the manner shown in FIG. 3 a or FIG. 6 . FIG. 7 shows a perspective view of antirotation device 50 which, viewed in piston displacement direction, has in common with roller guide 60 a cross section in the form of a circular arc, wherein cylindrical arc side 50 a bears on the cylindrical inside face of cylinder portion 40 and chord side 50 b bears on flattened part 48 b formed on piston portion 48 of piston 44 . In contrast to roller guide 60 , which in this embodiment of the radial piston engine is provided with a projection 62 , there is formed in antirotation device 50 a cylindrical opening 78 , in which there is seated the part of pin 76 which projects out of blind hole 84 , disposed in cylinder block 18 in such a way as to be aligned with inlet port 43 .
Reference symbol 66 denotes a fluid-control unit, by means of which, via inlet ports 43 , hydraulic fluid is supplied to the respective cylinder spaces or removed from the respective cylinder spaces during operation of radial piston engine 2 . Fluid-control unit 66 is disposed in fluid-tight relationship in housing part 6 such as to rotate therewith. In order to be able to distribute hydraulic fluid to the respective cylinder spaces, fluid-control unit 66 is provided with two separate circumferential grooves 68 and 70 , which are in communication with fluid channels 72 and 74 respectively. During operation of radial piston engine 2 , fluid channels 72 and 74 come alternately into communication with axial inlet ports 43 , which are formed in cylinder block 18 and each of which communicates with one of the cylinder spaces.
During operation of radial piston engine 2 , pistons 44 are actuated by means of hydraulic fluid via fluid channels 68 , 70 , 72 and 74 , inlet ports 43 and the cylinder spaces in such a way that they are urged radially outward relative to axis of rotation 16 . In the process they are braced via the respective roller 54 against curved path 12 of cam ring 8 , whereby cylinder block 18 is ultimately caused to perform a rotary movement around axis of rotation 16 . The direction of rotation is selected by the mode of actuation. Because of the positive connection of driven shaft 24 to cylinder block 18 , a torque is transmitted to driven shaft 24 . This shaft is braced via tapered roller bearings 32 and 34 of bearing assembly 30 . A drive element such as a gear of a loader (not illustrated in more detail here), which is connected via flange portion 28 to drive shaft 24 , therefore receives a torque.
FIGS. 8 a and 8 b show modifications of the roller guides described in connection with the foregoing embodiment of the inventive radial piston engine.
Roller guide 90 illustrated in FIG. 8 a differs from roller guide 60 shown in FIG. 5 in that, at the upper outside face facing cam ring 8 , it is rounded in a manner corresponding to the outside circumference of roller 54 and is designed to ensure that it does not project beyond the outside circumference of the roller in piston displacement direction. Since roller guide 90 in this case does not project beyond the outside circumference of roller 54 , and since in addition it is rigidly connected to roller 54 with respect to sliding in piston displacement direction, roller guide 90 could also be used—of course, only together with inventive roller 54 —for a conventional radial piston engine with a cam ring, in which the cam ring has a width which is greater than the length of roller 54 .
Whereas surfaces 63 of roller guides 60 in contact with the cylindrical inside face were of cylindrical structure hereinabove for the sake of simplicity, roller guide 92 shown in FIG. 8 b is provided on the side facing the cylinder face with a surface 93 which is rotationally symmetric or has the form of a spherical segment relative to axis of rotation 58 of roller 54 . Since the roller and thus also the roller guides normally do not experience particularly large axial loads during operation of the radial piston engine, the service life of the roller guides should not be shortened by giving the structure of the roller guides the form of a spherical segment. In order constantly to achieve reliable axial positioning of the rollers in this case, however, it is necessary that the extent to which the pistons are displaced during operation of the radial piston engine is sufficiently limited that axis of rotation 58 of each roller 54 is still disposed inside the cylinder even at maximum piston displacement. This restriction is not necessary in the roller guides mentioned hereinabove, however, because they are in contact over a large area.
In the special case shown in FIG. 8 b , roller guides 92 could be connected positively and nonpositively to roller 54 not only in piston displacement direction but also in the direction of rotation of roller 54 , so that friction no longer develops between roller and roller guide. Because of the small, substantially only linear contact of roller guide 92 on the cylindrical inside face, the friction occurring between roller guide 92 and cylindrical inside face would also be considerably reduced. Since roller guides 90 and roller 54 then can no longer turn relative to one another, the positive and/or nonpositive connection between roller guide and roller could also be achieved in any other manner. It would even be conceivable to construct the roller and the roller guides in one piece, or in other words to provide the roller guides on the roller.
FIGS. 9 a and 9 b show further options for connecting the roller guides to the roller.
Whereas in the preferred practical example of inventive radial piston engine 2 described hereinabove there were formed on each roller guide a projection 62 and on the roller corresponding recesses 54 c and 54 d , roller guide 94 according to FIG. 9 a is provided with a recess 95 and roller 96 with a corresponding projection 97 . In this example also, play is present between the oppositely disposed faces on roller guide and roller around the recess or around the projection, whereby the friction developed between these components occurs in a range in which small relative velocities exist between roller and roller guides. However, the present invention is not limited merely to this arrangement; it would naturally also be conceivable for the roller guides to be directly in contact with the roller in the conventional sense, or in other words without play.
Roller guide 98 in FIG. 9 b is characterized by a conical projection 99 , which is engaged with a corresponding central recess 101 of conical shape on roller 100 . In this case the roller guide is engaged with the roller without play but, as is also the case in the foregoing examples, the area of contact between roller 100 and roller guides 98 is relocated into a central region relative to axis of rotation 58 .
In the preferred embodiment there is provided an antirotation device 50 , which prevents turning of piston 44 in cylinder 36 and thus turning of roller 54 relative to curved path 12 . Since the rollers are normally constantly in contact with the curved path, however, whereby the angular position of the roller and thus of the piston is automatically determined, it is not absolutely necessary to provide an antirotation device. This case is shown in FIG. 10 a . Here the structure of the cylinder and piston is simplified substantially, since special manufacturing steps do not have to be performed either for piston 102 or for the cylinder block.
It is also possible by another relatively simple structural modification to the piston and cylinder block, however, as shown for example in FIG. 10 b , to provide an antirotation device 106 for piston 104 without having to form the piston and cylinder as stepped structures.
At this juncture it should be pointed out that all features described hereinabove, especially in connection with the geometry of the roller guide, the connection between roller guides and rollers, and also the antirotation device for the pistons, can be combined with one another to the extent technically possible.
The present invention therefore creates a technically optimized radial piston engine with a cam ring and a cylinder block, which is disposed to rotate relative to the cam ring around an axis of rotation and which has a plurality of cylinders aligned in the radial direction of the cylinder block. In each cylinder there is disposed a piston which can be displaced in radial direction, and which is braced via a roller against the cam ring. The roller is mounted in a bearing provided on the piston such that it can rotate around an axis of rotation parallel to the axis of rotation of the cylinder block while being braced axially in the cylinder relative to its axis of rotation via roller guides disposed at its front sides. The inventive radial piston engine is characterized in particular in that the roller guides are rigidly connected with the respective roller with respect to sliding in piston displacement direction and accordingly are urged in piston displacement direction by the respective roller both during a load stroke and during an idle stroke of the piston, whereby the roller guides do not come into contact with the cam ring.
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The invention concerns a technically optimized radial piston engine comprising a cam ring and a cylinder block arranged so as to rotate about an axis of rotation relative to the cam ring and having a plurality of cylinders oriented in the radial direction of the cylinder block. A piston capable of being radially displaced is located in each cylinder, resting on the cam ring via a roller. Said roller is mounted on the piston so as to rotate about an axis parallel to that of the cylinder block and rests axially, relative to its axis of rotation in the cylinder, against roller guides arranged on its surfaces. Said radial piston engine is characterized in that the roller guides are integrally mobile with the roller associated with them, in the piston stroke direction, and thereby driven by the roller both when the piston performs a loaded stroke and an idle stroke, without any contact occurring between the roller guides and the cam ring. The pistons are rotationally fixed by a torsional stop which is separate from the roller guide.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a divisional application of U.S. patent application Ser. No. 10/943,772, filed Sep. 16, 2004, which is based upon co-pending, commonly assigned U.S. provisional patent application Ser. No. 60/503,745, filed Sep. 16, 2003, incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
[0002] The application is directed to an implantable wireless sensor. More particularly, this invention is directed to a wireless, unpowered, micromechanical sensor that can be delivered using endovascular techniques, to measure a corporeal parameter such as pressure or temperature.
BACKGROUND OF THE INVENTION
[0003] Abdominal aortic aneurysms represent a dilatation and weakening of the abdominal aorta which can lead to aortic rupture and sudden death. Previously, the medical treatment of abdominal aortic aneurysms required complicated surgery with an associated high risk of injury to the patient. More recently, endografts (combining stents and grafts into a single device) have been developed that can be inserted through small incisions in the groin. Once in place, these endografts seal off the weakened section of the aorta. The aneurysms can then heal, eliminating the risk of sudden rupture. This less invasive form of treatment for abdominal aortic aneurysms has rapidly become the standard of care for this disease. An example of an endograft device is disclosed in Kornberg, U.S. Pat. No. 4,617,932.
[0004] A significant problem with endografts is that, due to inadequate sealing of the graft with the aorta, leaks can develop that allow blood to continue to fill the aneurysmal sac. Left undiscovered, the sac will continue to expand and potentially rupture. To address this situation, patients who have received endograft treatment for their abdominal aortic aneurysms are subjected to complex procedures that rely on injection of contrast agents to visualize the interior of the aneurysm sac. These procedures are expensive, not sensitive, and painful. In addition, they subject the patient to additional risk of injury. See, for example, Baum R A et al., “Aneurysm sac pressure measurements after endovascular repair of abdominal aortic aneurysms”, The Journal of Vascular Surgery , January 2001, and Schurink G W et al., “Endoleakage after stent-graft treatment of abdominal aneurysm: implications on pressure and imaging—an in vitro study”, The Journal of Vascular Surgery , August 1998. These articles provide further confirmation of the problem of endograft leakage and the value of intra-sac pressure measurements for monitoring of this condition.
[0005] Thus, there is a need for a method of monitor the pressure within an aneurysm sac that has undergone repair by implantation of an endograft to be able to identify the potential presence of endoleaks. Furthermore, this method should be accurate, reliable, safe, simple to use, inexpensive to manufacture, convenient to implant and comfortable to the patient.
[0006] An ideal method of accomplishing all of the above objectives would be to place a device capable of measuring pressure within the aneurysm sac at the time of endograft insertion. By utilizing an external device to display the pressure being measured by the sensor, the physician will obtain an immediate assessment of the success of the endograft at time of the procedure, and outpatient follow-up visits will allow simple monitoring of the success of the endograft implantation.
[0007] An example of an implantable pressure sensor designed to monitor pressure increases within an aneurysmal sac is shown in Van Bockel, U.S. Pat. No. 6,159,156. While some of the above objectives are accomplished, this device has multiple problems that would make its use impractical. For example, the sensor system disclosed in the Van Bockel patent relies on a mechanical sensing element that cannot be practically manufactured in dimensions that would allow for endovascular introduction. In addition, this type of pressure sensor would be subject to many problems in use that would limit its accuracy, stability and reliability. One example would be the interconnection of transponder and sensor as taught by Van Bockel, such interconnection being exposed to body fluids which could disrupt its function. This would impact the device's ability to maintain accurate pressure reading over long periods of time. A fundamental problem with sensors is their tendency to drift over time. A sensor described in the Van Bockel patent would be subject to drift as a result of its failure to seal the pressure sensing circuit from the external environment. Also, by failing to take advantage of specific approaches to electronic component fabrication, allowing for extensive miniaturization, the Van Bockel device requires a complex system for acquiring data from the sensor necessary for the physician to make an accurate determination of intra-aneurysmal pressure.
OBJECTS OF THE INVENTION
[0008] It is an object of this invention to provide an implantable wireless sensor.
[0009] It is also an object of this invention to provide a wireless, unpowered, micromechanical sensor that can be delivered endovascularly.
[0010] It is a further object of this invention to provide an implantable, wireless, unpowered sensor that can be delivered endovascularly to measure pressure and/or temperature.
[0011] It is a yet further object of this invention to provide a method of preparing a micromechanical implantable sensor.
[0012] It is a yet further object of this invention to provide a micromechanical sensor with a hermetically sealed, unbreached pressure reference for enhanced stability.
[0013] These and other objects of the invention will become more apparent from the discussion below.
SUMMARY OF THE INVENTION
[0014] The present invention comprises a method for manufacturing a device that can be implanted into the human body using non-surgical techniques to measure a corporeal parameter such as pressure, temperature, or both. Specific target locations could include the interior of an abdominal aneurysm or a chamber of the heart. This sensor is fabricated using MicroElectroMechanical Systems (MEMS) technology, which allows the creation of a device that is small, accurate, precise, durable, robust, biocompatible, radiopaque and insensitive to changes in body chemistry, biology or external pressure. This device will not require the use of wires to relay pressure information externally nor need an internal power supply to perform its function.
[0015] Stated somewhat more specifically, according to the disclosed method, a cavity is etched in one side of a first substrate. A conductive central plate and surrounding conductive coil is formed on the base of the cavity. A second conductive central plate and surrounding conductive coil is formed on a surface of a second substrate, and the two substrates are mutually imposed such that the two conductive plates and coils are disposed in opposed, spaced-apart relation. A laser is then used to cut away perimeter portions of the imposed substrates and simultaneously to heat bond the two substrates together such that the cavity in the first substrate is hermetically sealed.
[0016] According to one embodiment of the invention, the second conductive plate and coil are formed on the upper surface of the second substrate. According to another embodiment, the second substrate has a cavity etched into its upper side, and the conductive plate and coil are formed on the base of the cavity. According to this second embodiment, when the two substrates are mutually imposed, the cavities in the respective substrates communicate to form a hollow. The subsequent laser operation hermetically seals the hollow within the sensor body.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is an oblique perspective view of an embodiment of the invention;
[0018] FIG. 2 is a top, partly cross-sectional view of the embodiment of the invention shown in FIG. 1 ;
[0019] FIG. 3 is a top, partly cross-sectional view of another embodiment of the invention;
[0020] FIG. 4 is an oblique, cross-sectional view of the embodiment of the invention shown in FIG. 2 ;
[0021] FIG. 5 is an oblique, cross-sectional view of the embodiment of the invention shown in FIG. 3 ;
[0022] FIG. 6 is a exposed cross-sectional view of the embodiment of the invention shown in FIG. 5 ;
[0023] FIG. 7 shows part of the sensor tethering system;
[0024] FIG. 8 shows the further details of the tethering system;
[0025] FIGS. 9 to 12 show additional details of the tethering system;
[0026] FIGS. 13 to 15 show details of the delivery system;
[0027] FIGS. 16 to 26 show details of the manufacturing process used to fabricate the invention;
[0028] FIG. 27 represents an additional embodiment of the invention; and
[0029] FIG. 28 is a schematic of a control system.
DETAILED DESCRIPTION OF THE INVENTION
[0030] The invention can perhaps be better understood by referring to the drawings. FIG. 1 is an oblique, perspective view of a sensor 2 , an embodiment of the invention. Sensor 2 preferably has an outer coating of biocompatible silicone.
[0031] FIG. 2 is a top, partial cross-section of a schematic representation of sensor 2 where a wire spiral inductor coil 4 is positioned in planar fashion in a substrate 6 . Optionally sensor 2 may have recesses 8 , each with a hole 10 , to receive a tether wire (not shown here) for delivery of the device into a human patient, as described below.
[0032] In the embodiment of the invention shown in FIG. 3 , a wire 12 connects coil 4 to a capacitor plate 14 positioned within coil 4 .
[0033] FIG. 4 is a slightly oblique cross-section across its width of the embodiment of the invention shown in FIG. 2 , where it can be seen that sensor 2 is comprised of a lower substrate 20 and an upper substrate 22 . Lower substrate 20 and upper substrate 22 are constructed from a suitable material, such as glass, fused silica, sapphire, quartz, or silicon. Fused silica is the preferred material of construction. Lower substrate 20 has on its upper surface 24 an induction coil 26 , and upper substrate 22 has a recess 28 with a surface 30 having an induction coil 32 thereon. The top surface of upper substrate 22 forms a membrane 34 capable of mechanically responding to changes in a patient's physical property, such as pressure. The end 36 of sensor 2 has a notch or recess 38 .
[0034] In similar fashion, FIG. 5 is a slightly oblique cross-section across its width of the embodiment of the invention shown in FIG. 3 . The primary difference between FIGS. 4 and 5 is the presence of upper capacitor plate 42 and lower capacitor plate 44 on surfaces 24 and 30 , respectively. In the embodiment of FIG. 4 , the spiral coil 4 itself acts as the capacitive element of the LC circuit that describes the operation of the sensor.
[0035] FIG. 6 is a variation of FIG. 5 where the outline of upper substrate 22 is shown but the details of lower substrate 20 can be seen more clearly, including individual coils of inductor coil 26 . A wire 46 connects lower capacitor plate 44 to induction coil 26 .
[0036] The size of the sensors of the invention will vary according to factors such as the intended application, the delivery system, etc. The oval sensors are intended to be from about 0.5 in. to about 1 in. in length and from about 0.1 in. to about 0.5 in. in width, with a thickness of from about 0.05 in. to about 0.30 in.
[0037] As shown in FIGS. 4 and 5 , upper substrate 22 can be significantly thinner than lower substrate 20 . By way of example, upper substrate 22 may be from about 100 to about 300 microns thick, whereas lower substrate 20 may be from about 500 to about 1500 microns thick. In an alternate embodiment of the invention, both substrates may be of the same thickness ranging from about 100 to about 1000 microns.
[0038] In the embodiment of the invention shown in FIG. 7 , a sensor 50 is attached to a hollow tube 52 that has a flexible tip 54 .
[0039] FIG. 8 shows the sensor 50 and specific features of the tethering system, namely proximal holes 56 and distal holes 58 disposed in a hollow tube 52 .
[0040] FIG. 9 shows a tether wire 60 that is attached to sensor 50 at sensor holes 62 and hollow tube holes 56 and 58 , and a tether wire 60 is positioned slidably within a hollow tube 52 .
[0041] A better appreciation of certain aspects of the invention, especially of a delivery system, can be obtained from FIG. 10 which shows a vessel introducer 66 and the delivery system 68 .
[0042] Further details of the delivery system are shown in FIG. 11 . A double lumen tube 70 has one channel that accepts a guidewire 72 and a second channel that accepts the sensor tether wire. The guidewire 72 can be advanced through hub 74 . A rigid delivery capsule 78 is disposed at the far end of the delivery catheter and flexible tip 80 is connected to the catheter via a hollow tube 81 extending through the delivery capsule 78 . A sensor 82 is positioned inside a slot in the delivery capsule 78 proximal to flexible tip 80 .
[0043] FIG. 12 shows a lateral, cross-sectional view of this arrangement where the sensor 82 is inside the slot of delivery capsule 78 and the flexible tip 84 of the tether wire is disposed between the end of delivery capsule 78 and flexible tip 80 .
[0044] FIG. 13 shows delivery catheter 68 loaded into the previously placed vessel introducer 66 prior to introduction of the sensor into the body.
[0045] FIG. 14 shows that the sensor 82 on tether tube 52 has been advanced out of delivery capsule 78 and the delivery catheter has been removed.
[0046] In FIG. 15 , the tether wire has been retracted into the hollow tether tube, releasing the sensor. The tether wire, tether tube and vessel introducer 66 are then all removed.
[0047] The pressure sensor of the invention can be manufactured using Micro-machining techniques that were developed for the integrated circuit industry. An example of this type of sensor features an inductive-capacitive (LC) resonant circuit with a variable capacitor, as is described in Allen et al., U.S. Pat. Nos. 6,111,520 and 6,278,379, all of which are incorporated herein by reference. The sensor contains two types of passive electrical components, namely, an inductor and a capacitor. The sensor is constructed so that the fluid pressure at the sensor's surface changes the distance between the capacitor's substantially parallel plates and causes a variation of the sensor's capacitance.
[0048] In a preferred embodiment the sensor of the invention is constructed through a series of steps that use standard MEMS manufacturing techniques.
[0049] FIG. 16 shows the first step of this process in which a thin layer of metal (Protective mask) 90 is deposited onto the top and bottom surface of a fused silica substrate 92 (alternative materials would be glass, quartz, silicon or ceramic). Substrate diameters can range from about 3 to about 6 in. Substrate thickness can range from about 100 to about 1500 microns. A pattern mask is then created on one side of the substrate to define the location of cavities that need to be etched into the surface.
[0050] FIG. 17 shows trenches or cavities 94 are etched into one surface of the substrate 92 to depths ranging from about 20 to about 200 microns. This etching is accomplished using any combination of standard wet and dry etching techniques (acid etch, plasma etch, reactive ion etching) that are well known in the MEMS industry. The protective metal mask is removed using standard metal etching techniques
[0051] In FIG. 18 , a thin metal seed layer 96 (typically chromium) is deposited on the etched side of the substrate using standard metal deposition techniques such as sputtering, plating or metal evaporation.
[0052] In FIG. 19 a layer of photo-resistive material 98 is applied to the etched surface of the substrate using standard spin coating procedures.
[0053] FIG. 20 shows that a mask aligner and UV light 102 is used in a photolithographic processes to transfer a pattern from a mask 104 to the photoresist coating on the substrate.
[0054] In FIG. 21 , the non-masked portions of the Photoresist are removed chemically creating a mold 106 of the desired coil pattern.
[0055] FIG. 22 shows copper 108 electroplated into the mold to the desired height, typically from about 5 to about 35 microns.
[0056] In FIG. 23 , the Photoresist 110 and seed layer 112 are etched away leaving the plated copper coils 114 .
[0057] This process is then repeated with a second substrate.
[0058] In FIG. 24 , the two processed substrates 118 and 120 are aligned such that the cavities 122 and 124 with plated coils are precisely orientated in over one another and temporarily bonded to each other.
[0059] FIGS. 25 and 26 show that by using a CO 2 laser 126 (or other appropriate laser type), the individual sensors 130 are cut from the glass substrate. The laser cutting process results in a permanent, hermetic seal between the two glass substrates. The laser energy is confined to a precise heat effect zone 128 in which the hermetic seal is created.
[0060] FIG. 27 represents an embodiment of the invention wherein a sensor 132 attached to a delivery catheter 134 has a stabilizer or basket 136 . The stabilizer can be any appropriate device or structure that can be fixedly attached to a sensor of the invention to assist the sensor in maintaining position, location, and/or orientation after the sensor is delivered to an intended site. The stabilizer can comprise any appropriate physiologically acceptable rigid or slightly flexible material, such as stainless steel, nitinol, or a radiopaque metal or alloy.
[0061] This sensor design provides many important benefits to sensor performance. The hermetic seal created during the laser cutting process, coupled with the design feature that the conductor lines of the sensor are sealed within the hermetic cavity, allows the sensor to remain stable and drift free during long time exposures to body fluids. In the past, this has been a significant issue to the development of sensors designed for use in the human body. The manufacturing methodology described above allows many variations of sensor geometry and electrical properties. By varying the width of the coils, the number of turns and the gap between the upper and lower coils the resonant frequency that the device operates at and the pressure sensitivity (i.e., the change in frequency as a result of membrane deflection) can be optimized for different applications. In general, the design allows for a very small gap between the coils (typically between about 3 and about 35 microns) that in turn provides a high degree of sensitivity while requiring only a minute movement of the coils to sense pressure changes. This is important for long term durability, where large membrane deflection could result in mechanical fatigue of the pressure sensing element.
[0062] The thickness of the sensor used can also be varied to alter mechanical properties. Thicker substrates are more durable for manufacturing. Thinner substrates allow for creating of thin pressure sensitive membranes for added sensitivity. In order to optimize both properties the sensors may be manufactured using substrates of different thicknesses. For example, one side of the sensor may be constructed from a substrate of approximate thickness of 200 microns. This substrate is manufactured using the steps outlined above. Following etching, the thickness of the pressure sensitive membrane (i.e., the bottom of the etched trench) is in the range of from about 85 to about 120 microns.
[0063] The matching substrate is from about 500 to about 1000 microns thick. In this substrate, the trench etching step is eliminated and the coils are plated directly onto the flat surface of the substrate extending above the substrate surface a height of from about 20 to about 40 microns. When aligned and bonded, the appropriate gap between the top and bottom coils is created to allow operation preferably in a frequency range of from 30 to 45 MHz and have sensitivity preferably in the range of from 5 to 15 kHz per millimeter of mercury. Due to the presence of the from about 500 to about 1000 micron thick substrate, this sensor will have added durability for endovascular delivery and for use within the human body.
[0064] The sensor exhibits the electrical characteristics associated with a standard LC circuit. An LC circuit can be described as a closed loop with two major elements, a capacitor and an inductor. If a current is induced in the LC loop, the energy in the circuit is shared back and forth between the inductor and capacitor. The result is an energy oscillation that will vary at a specific frequency. This is termed the resonant frequency of the circuit and it can be easily calculated as its value is dependent on the circuit's inductance and capacitance. Therefore, a change in capacitance will cause the frequency to shift higher or lower depending upon the change in the value of capacitance.
[0065] As noted above, the capacitor in the assembled pressure sensor consists of the two circular conductive segments separated by an air gap. If a pressure force is exerted on these segments it will act to move the two conductive segments closer together. This will have the effect of reducing the air gap between them which will consequently change the capacitance of the circuit. The result will be a shift in the circuit's resonant frequency that will be in direct proportion to the force applied to the sensor's surface.
[0066] Because of the presence of the inductor, it is possible to electromagnetically couple to the sensor and induce a current in the circuit. This allows for wireless communication with the sensor and the ability to operate it without the need for an internal source of energy such as a battery. Thus, if the sensor is located within the sac of an aortic aneurysm, it will be possible to determine the pressure within the sac in a simple, non-invasive procedure by remotely interrogating the sensor, recording the resonant frequency and converting this value to a pressure measurement. The readout device generates electromagnetic energy that penetrates through the body's tissues to the sensor's implanted location. The sensor's electrical components absorb a fraction of the electromagnetic energy that is generated by the readout device via inductive coupling. This coupling induces a current in the sensor's circuit that oscillates at the same frequency as the applied electromagnetic energy. Due to the nature of the sensor's electromechanical system there exists a frequency of alternating current at which the absorption of energy from the readout device is at a maximum. This frequency is a function of the capacitance of the device. Therefore, if the sensor's capacitance changes, so will the optimal frequency at which it absorbs energy from the readout device. Since the sensor's capacitance is mechanically linked to the fluid pressure at the sensor's surface, a measurement of this frequency by the readout device gives a relative measurement of the fluid pressure. If calibration of the device is performed, then an absolute measurement of pressure can be made. See, for example, the extensive discussion in the Allen et al. patent, again incorporated herein by reference, as well as Gershenfeld et al., U.S. Pat. No. 6,025,725, incorporated herein by reference. Alternative readout schemes, such as phase-correlation approaches to detect the resonant frequency of the sensor, may also be employed.
[0067] The pressure sensor is made of completely passive components having no active circuitry or power sources such as batteries. The pressure sensor is completely self-contained having no leads to connect to an external circuit or power source. Furthermore, these same manufacturing techniques can be used to add additional sensing capabilities, such as the ability to measure temperature by the addition of a resistor to the basic LC circuit or by utilizing changes in the back pressure of gas intentionally sealed within the hermetic pressure reference to change the diaphragm position and therefore the capacitance of the LC circuit.
[0068] It is within the scope of the invention that the frequency response to the sensor will be in the range of from about 1 to about 200 MHz, preferably from about 1 to about 100 MHz, and more preferably from about 2 to about 90 MHz, and even more preferably from about 30 to about 45 MHz, with a Q factor of from about 5 to about 150, optimally from about 5 to about 80, preferably from about 40 to about 100, more preferably from about 50 to about 90.
[0069] In a further embodiment of the invention there is no direct conductor-based electrical connection between the two sides of the LC circuit. Referring again to the sensor described in the Allen et al. patents, the device is constructed using multiple layers upon lie the necessary circuit elements. Disposed on the top and bottom layer are metal patterns constructed using micro-machining techniques which define a top and bottom conductor and a spiral inductor coil. To provide for an electrical contact between the top and bottom layers small vias or holes are cut through the middle layers. When the layers are assembled, a metal paste is forced into the small vias to create direct electrical connections or conduits. However, experimentation has shown that due to additional capacitance that is created between the top and bottom inductor coils, a vialess operational LC circuit can be created. This absence of via holes represents a significant improvement to the sensor in that it simplifies the manufacturing process and, more importantly, significantly increases the durability of the sensor making it more appropriate for use inside the human body.
[0070] Further, the invention is not limited to the implantation of a single sensor. Multiple pressure sensors may be introduced into the aneurysm space, each being positioned at different locations. In this situation, each sensor may be designed with a unique signature (obtained by changing the resonant frequency of the sensor), so that the pressure measurement derived from one sensor can be localized to its specific position within the aneurysm.
[0071] A significant design factor that relates to the performance of the sensor and the operation of the system is the Quality factor (O) associated with the sensor. The value of Q is one of the key determinates as to how far from the sensor the external read-out electronics can be located while still maintaining effective communication. Q is defined as a measure of the energy stored by the circuit divided by the energy dissipated by the circuit. Thus, the lower the loss of energy, the higher the Q.
[0072] Additional increases in Q can be achieved by removing the central capacitive plate and using capacitive coupling between the copper coils to act as the capacitor element.
[0073] In operation, energy transmitted from the external read-out electronics will be stored in the LC circuit of the sensor. This stored energy will induce a current in the LC loop which will cause the energy to be shared back and forth between the inductor and capacitor. The result is an oscillation that will vary at the resonant frequency of the LC circuit. A portion of this ocscillating energy is then coupled back to the receiving antenna of the read-out electronics. In high Q sensors, most of the stored energy is available for transmission back to the electronics, which allows the distance between the sensor and the receiving antenna to be increased. Since the transmitted energy will decay exponentially as it travels away from the sensor, the lower the energy available to be transmitted, the faster it will decay below a signal strength that can be detected by the receiving antenna and the closer the sensor needs to be situated relative to the receiving electronics. In general then, the lower the Q, the greater the energy loss and the shorter the distance between sensor and receiving antenna required for sensor detection.
[0074] The Q of the sensor will be dependent on multiple factors such as the shape, size, diameter, number of turns, spacing between turns and cross-sectional area of the inductor component. In addition, Q will be greatly affected by the materials used to construct the sensors. Specifically, materials with low loss tangents will provide the sensor with higher Q factors.
[0075] The implantable sensor ascending to the invention is preferably constructed of various glasses or ceramics including but not limited to fused silica, quartz, pyrex and sintered zirconia, that provide the required biocompatibility, hermeticity and processing capabilities. Preferably the materials result in a high Q factor. These materials are considered dielectrics, that is, they are poor conductors of electricity, but are efficient supporters of electrostatic or electroquasiatatic fields. An important property of dielectric materials is their ability to support such fields while dissipating minimal energy. The lower the dielectric loss (the proportion of energy lost), the more effective the dielectric material in maintaining high Q. For a lossy dielectric material, the loss is described by the property termed “loss tangent.” A large loss tangent reflects a high degree of dielectric loss.
[0076] With regard to operation within the human body, there is a second important issue related to Q, namely, that blood and body fluids are conductive mediums and are thus particularly lossy. The consequence of this fact is that when a sensor is immersed in a conductive fluid, energy from the sensor will dissipate, substantially lowering the Q and reducing the sensor-to-electronics distance. For example, the sensors described above were immersed in saline (0.9% salt solution), and the measured Q decreased to approximately 10. It has been found that such loss can be minimized by further separation of the sensor from the conductive liquid. This can be accomplished, for example, by encapsulating the sensor in a suitable low-loss-tangent dielectric material. However, potential encapsulation material must have the flexibility and biocompatibility characteristics of the sensor material and also be sufficiently compliant to allow transmission of fluid pressure to the pressure sensitive diaphragm. A preferred material for this application is polydimethylsiloxane (silicone).
[0077] As an example, a thin (i.e., 200 micron) coating of silicone was applied to the sensor detailed above. This coating provided sufficient insulation to maintain the Q at 50 in a conductive medium. Equally important, despite the presence of the silicone, adequate sensitivity to pressure changes was maintained and the sensor retained sufficient flexibility to be folded for endovascular delivery. One additional benefit of the silicone encapsulation material is that it can be optionally loaded with a low percentage (i.e., 10-20%) of radio-opaque material (e.g., barium sulfate) to provide visibility when examined using fluoroscopic x-ray equipment. This added barium sulfate will not affect the mechanical and electrical properties of the silicone.
[0078] As described above, it is desirable to increase the Q factor of a sensor, and the Q factor can be increased by suitable selection of sensor materials or a coating, or both. Preferably both are used, because the resulting high Q factor of a sensor prepared in this fashion is especially suitable for the applications described.
[0079] When introduced into the sac of an abdominal aorta, the pressure sensor can provide pressure related data by use of an external measuring device. As disclosed in the Allen et al. patents, several different excitation systems can be used. The readout device generates electromagnetic energy that can penetrate through the body's tissues to the sensor's implanted location. The sensor's electrical components can absorb a fraction of the electromagnetic energy that is generated by the readout device via inductive coupling. This coupling will induce a current in the sensor's circuit that will oscillate at the same frequency as the applied electromagnetic energy. Due to the nature of the sensor's electromechanical system there will exist a frequency of alternating current at which the absorption of energy from the readout device is at a minimum. This frequency is a function of the capacitance of the device. Therefore, if the sensor's capacitance changes so will the frequency at which it minimally absorbs energy from the readout device. Since the sensor's capacitance is mechanically linked to the fluid pressure at the sensor's surface, a measurement of this frequency by the readout device can give a relative measurement of the fluid pressure. If calibration of the device is performed then an absolute measurement of pressure can be made.
[0080] The circuitry used to measure and display pressure is contained within a simple to operate, portable electronic unit 400 , as shown in FIG. 28 . This unit 400 also contains the antenna needed to perform the electromagnetic coupling to the sensor. The antenna may be integrated into the housing for the electronics or it may be detachable from the unit so that it can be positioned on the surface of the body 402 in proximity to the implanted sensor and easily moved to optimize the coupling between antenna and sensor. The antenna itself may consist of a simple standard coil configuration or my incorporate ferrous elements to maximize the coupling efficiency. The electronic device would feature an LCD or LED display 404 designed to clearly display the recorded pressure in physiologically relevant units such as mm Hg. In an alternative embodiment, the display may be created by integrating a commercially available hand-held computing device such as a Palm® or micro-PC into the electronic circuitry and using this device's display unit as the visual interface between the equipment and its operator. A further advantage of this approach is that the hand-held computer could be detached from the read-out unit and linked to a standard desktop computer. The information from the device could thus be downloaded into any of several commercially available data acquisition software programs for more detailed analysis or for electronic transfer via hard media or the internet to a remote location.
[0081] Accordingly, the present invention provides for an impedance system and method of determining the resonant frequency and bandwidth of a resonant circuit within a particular sensor. The system includes a loop antenna, which is coupled to an impedance analyzer. The impedance analyzer applies a constant voltage signal to the loop antenna scanning the frequency across a predetermined spectrum. The current passing through the transmitting antenna experiences a peak at the resonant frequency of the sensor. The resonant frequency and bandwidth are thus determined from this peak in the current.
[0082] The method of determining the resonant frequency and bandwidth using an impedance approach may include the steps of transmitting an excitation signal using a transmitting antenna and electromagnetically coupling a sensor having a resonant circuit to the transmitting antenna thereby modifying the impedance of the transmitting antenna. Next, the step of measuring the change in impedance of the transmitting antenna is performed, and finally, the resonant frequency and bandwidth of the sensor circuit are determined.
[0083] In addition, the present invention provides for a transmit and receive system and method for determining the resonant frequency and bandwidth of a resonant circuit within a particular sensor. According to this method, an excitation signal of white noise or predetermined multiple frequencies is transmitted from a transmitting antenna, the sensor being electromagnetically coupled to the transmitting antenna. A current is induced in the resonant circuit of the sensor as it absorbs energy from the transmitted excitation signal, the current oscillating at the resonant frequency of the resonant circuit. A receiving antenna, also electromagnetically coupled to the transmitting antenna, receives the excitation signal minus the energy which was absorbed by the sensor. Thus, the power of the received signal experiences a dip or notch at the resonant frequency of the sensor. The resonant frequency and bandwidth are determined from this notch in the power.
[0084] The transmit and receive method of determining the resonant frequency and bandwidth of a sensor circuit includes the steps of transmitting a multiple frequency signal from transmitting antenna, and, electromagnetically coupling a resonant circuit on a sensor to the transmitting antenna thereby inducing a current in the sensor circuit. Next, the step of receiving a modified transmitted signal due to the induction of current in the sensor circuit is performed. Finally, the step of determining the resonant frequency and bandwidth from the received signal is executed.
[0085] Yet another system and method for determining the resonant frequency and bandwidth of a resonant circuit within a particular sensor includes a chirp interrogation system. This system provides for a transmitting antenna which is electromagnetically coupled to the resonant circuit of the sensor. An excitation signal of white noise or predetermined multiple frequencies, or a time-gated single frequency is applied to the transmitting antenna for a predetermined period of time, thereby inducing a current in the resonant circuit of the sensor at the resonant frequency. The system then listens for a return signal which is coupled back from the sensor. The resonant frequency and bandwidth of the resonant circuit are determined from the return signal.
[0086] The chirp interrogation method for determining the resonant frequency and bandwidth of a resonant circuit within a particular sensor includes the steps of transmitting a multi-frequency signal pulse from a transmitting antenna, electromagnetically coupling a resonant circuit on a sensor to the transmitting antenna thereby inducing a current in the sensor circuit, listening for and receiving a return signal radiated from the sensor circuit, and determining the resonant frequency and bandwidth from the return signal.
[0087] The present invention also provides an analog system and method for determining the resonant frequency of a resonant circuit within a particular sensor. The analog system comprises a transmitting antenna coupled as part of a tank circuit which in turn is coupled to an oscillator. A signal is generated which oscillates at a frequency determined by the electrical characteristics of the tank circuit. The frequency of this signal is further modified by the electromagnetic coupling of the resonant circuit of a sensor. This signal is applied to a frequency discriminator which in turn provides a signal from which the resonant frequency of the sensor circuit is determined.
[0088] The analog method for determining the resonant frequency and bandwidth of a resonant circuit within a particular sensor includes the steps of generating a transmission signal using a tank circuit which includes a transmitting antenna, modifying the frequency of the transmission signal by electromagnetically coupling the resonant circuit of a sensor to the transmitting antenna, and converting the modified transmission signal into a standard signal for further application.
[0089] The invention further includes an alternative method of measuring pressure in which a non-linear element such as a diode or polyvinylidenedifloride piezo-electric polymer is added to the LC circuit. A diode with a low turn-on voltage such as a Schottky diode can be fabricated using micro-machining techniques. The presence of this non-linear element in various configurations within the LC circuit can be used to modulate the incoming signal from the receiving device and produce different harmonics of the original signal. The read-out circuitry can be tuned to receive the particular harmonic frequency that is produced and use this signal to reconstruct the fundamental frequency of the sensor. The advantage of this approach is two-fold; the incoming signal can be transmitted continuously and since the return signal will be at different signals, the return signal can also be received continuously.
[0090] The above methods lend themselves to the creation of small and simple to manufacture hand-held electronic devices that can be used without complication.
[0091] The preceding specific embodiments are illustrative of the practice of the invention. It is to be understood, however, that other expedients known to those skilled in the art or disclosed herein, may be employed without departing from the spirit of the invention of the scope of the appended claims.
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In the disclosed method of manufacturing an implantable wireless sensor, a cavity is etched in one side of a first substrate. A conductive structureare formed on the base of the cavity. A second conductive structureare formed on a surface of a second substrate, and the two substrates are mutually imposed such that the two conductive plates and coils are disposed in opposed, spaced-apart relation. A laser is then used to cut away perimeter portions of the imposed substrates and simultaneously to heat bond the two substrates together such that the cavity in the first substrate is hermetically sealed.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. provisional application No. 60/614,320 filed Sep. 29, 2004.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention is directed toward apparatus and methods for conveying and operating analytical instrumentation within a well borehole. More specifically, the invention is directed toward measurements of borehole conditions and parameters of earth formation penetrated by the borehole using a tubular to convey the required analytical instrumentation.
2. Background of the Art
Properties of borehole environs are of great importance in hydrocarbon production. These properties include parameters related to the borehole, parameters related to properties of formations penetrated by the borehole, and parameters associated with the drilling and the subsequent production from the borehole. Borehole parameters include temperature and pressure, borehole wall imaging, caliper, orientation and the like. Formation properties include density, porosity, acoustic velocity, resistivity, formation fluid type, formation imaging, pressure and permeability. Parameters associated with drilling include weight on bit, borehole inclination, borehole direction and the like.
Properties of borehole environs are typically obtained using two broad types or classes of geophysical technology. The first class is typically referred to as wireline technology, and the second class is typically referred to as “measurement-while-drilling” (MWD) or “logging-while-drilling” (LWD).
Using wireline technology, a downhole instrument comprising one or more sensors is conveyed along the borehole by means of a cable or “wireline” after the well has been drilled. The downhole instrument typically communicates with surface instrumentation via the wireline. Borehole and formation measurements are typically obtained in real time at the surface of the earth. These measurements are typically recorded as a function of depth within the borehole thereby forming a “log” of the measurements. Basic wireline technology has been expanded to other embodiments. As an example, the downhole instrument can be conveyed by a tubular such as coiled production tubing. As another example, downhole instrument is conveyed by a “slick line” which does not serve as a data and power conduit to the surface. As yet another example, the downhole instrument is conveyed by the circulating mud within the borehole. In embodiments in which the conveyance means does not also serve as a data conduit with the surface, measurements and corresponding depths are recorded within the tool, and subsequently retrieved at the surface to generate the desired log. These are commonly referred to as “memory” tools. All of the above embodiments of wireline technology share a common limitation in that they are used after the borehole has been drilled.
Using MWD or LWD technology, measurements of interest are typically made while the borehole is being drilled, or at least made during the drilling operation when the drill string is periodically removed or “tripped” to replace worn drill bits, wipe the borehole, set intermediate strings of casing, and the like.
Both wireline and LWD/MWD technologies offer advantages and disadvantages which generally known in the art, and will mentioned only in the most general terms in this disclosure for purposed of brevity. Certain wireline measurements produce more accurate and precise measurements than their LWD/MWD counterparts. As an example, dipole shear acoustic logs are more suitable for wireline operation than for the acoustically “noisy” drilling operation. Certain LWD/MWD measurements yield more accurate and precise measurements than their wireline counterparts since they are made while the borehole is being drilled and before drilling fluid invades the penetrated formation in the immediate vicinity of the well borehole. As examples, certain types of shallow reading nuclear logs are often more suitable for LWD/MWD operation than for wireline operation. Certain wireline measurements employ articulating pads which directly contact the formation and which are deployed by arms extending from the main body of the wireline tool. Examples include certain types of borehole imaging and formation testing tools. Pad type measurements are not conceptually possible using LWD/MWD systems, since LWD/MWD measurements are typically made while the measuring instrument is being rotating by the drill string. Stated another way, the pads and extension arms would be quickly sheared off by the rotating action of the drill string.
SUMMARY OF THE INVENTION
The present invention is a borehole conveyance system that integrates wireline type downhole instrumentation into the drill string tripping operations that are typically performed in a borehole drilling operation. This increases the types of measurements that can be obtained during the drilling operation. Equipment costs and maintenance costs are often reduced. Certain wireline type tools can be used during drilling operations to yield measurements superior to their LWD/MWD counterparts, but not during any drilling operation in which the drill string is rotating. Other types of wireline tools can be used to obtain measurements not possible with LWD/MWD systems.
BRIEF DESCRIPTION OF THE DRAWINGS
So that the manner in which the above recited features, advantages and objects of the present invention are obtained and can be understood in detail, more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings.
FIG. 1 illustrates a borehole conveyance system for a wireline tool, with the conveyance system deployed using a drill string in a borehole environment;
FIG. 2 a shows the borehole conveyance system with the wireline tool contained within;
FIG. 2 b shows the borehole conveyance system with the wireline tool attached thereto and deployed in the borehole;
FIG. 3 shows a hybrid system with the wireline conveyance system combined with a LWD/MWD instrument, wherein the wireline tool is deployed in the borehole;
FIG. 4 a shows a LWD/MWD subassembly combined with a telemetry and power subsection of the borehole conveyance system to form a LWD/MWD system for measuring parameters of interest while advancing the borehole; and
FIG. 4 b shows a LWD/MWD subassembly combined with the wireline conveyance system such that the wireline tool and LWD/MWD sensors share a common power source and a common downhole telemetry unit.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates a borehole conveyance system 100 that is used to integrate wireline type downhole instrumentation into the tripping operations used periodically during a well borehole drilling operation. A wireline tool conveyance subsection 10 (wireline conveyance sub “WCS”) is operationally attached to a telemetry-power subsection 12 (“telemetry-power sub “TPS”) and suspended within a borehole 14 by means of a drill string 18 through a connector head 13 . The borehole 14 penetrates earth formation 32 . The lower end of WCS 10 is optionally connected to a wiper 17 . The upper end of the drill string 18 is terminated at a rotary drilling rig 20 , which is known in the art and illustrated conceptually. Drilling fluid or drilling “mud” is pumped down through the drill string 18 and through conduits in the TPS 12 and WCS 10 , wherein the conduits are illustrated conceptually with the broken lines 11 . Drilling mud exits the lower end of the WCS 10 and returns to the surface of the earth via the borehole 14 . The flow of the drilling mud is illustrated conceptually by the arrows 15 .
Still referring to FIG. 1 , elements in the TPS 12 communicate with an uphole telemetry unit 24 , as illustrated conceptually with the line 22 . This link can include, but is not limited to, a mud-pulse telemetry system, an acoustic telemetry system or an electromagnetic telemetry system. Downhole measurements are received by the uphole telemetry unit 24 and processed as required in a processor 26 to obtain a measure of a parameter of interest. The parameter of interest is recorded by a suitable electronic or “hard-copy” recording device 28 , and preferably displayed as a function of depth at which it was measured as a log 30 .
FIG. 2 a is a more detailed view of the WCS 10 and the TPS 12 . A wireline tool 40 is shown deployed within the mud flow conduit illustrated by the broken lines 11 . In the context of this disclosure, the term “wireline” tool includes tools operated with a wireline, tools operated with a slick line, and memory tools conveyed by drilling fluid or gravity.
Wireline logging systems have been used for decades, with the first system being operated in a borehole in the late 1920's. The tools typically vary in outside diameter from about 1.5 inches to over 4 inches. Lengths can vary from a few feet to 100 feet. Tool housings are typically fabricated to withstand pressures of over 10,000 pounds per square inch. Power is typically supplied from the surface of the earth via the wireline cable. Formation and borehole data, obtained by sensors in the downhole tool, can be telemetered to the surface for processing. Alternately, sensor data can be processed within the wireline tool, and “answers” telemetered to the surface. The patent literature abounds with wireline tool disclosures. U.S. Pat. Nos. 3,780,302, 4,424,444 and 4,002,904 disclose the basic apparatus and methods of a wireline logging system, and are entered herein by reference.
Again referring to FIG. 2 a, the upper end of the wireline tool 40 is physically and electronically connected to an upper connector 42 . The TPS 12 comprises a power supply 48 and a downhole telemetry unit 46 . The power supply 48 supplies power to the wireline tool 40 through the connector 42 , when configured as shown in FIG. 2 a. The power supply 48 also provides power to the downhole telemetry unit 46 , as illustrated by the functional arrow. The downhole telemetry unit 46 is operationally connected, through the upper connector 42 , to the wireline tool 40 via the communication link represented conceptually by the line 52 . The communication link 52 can be, but is not limited to, a hard-wire or alternately a “short-hop” electromagnetic communication link. As shown in FIG. 2 a, a wireline tool can be conveyed into a well borehole 14 (see FIG. 1 ) using a tubular conveyance means such as a drill string 18 . The WCS 10 tends to shield the wireline tool 40 from many of the harsh conditions encountered within the borehole 14 . Furthermore, the tool 40 is in communication with the surface using the downhole and uphole telemetry units 46 and 24 , respectively, over the communication link 22 which can be, but is not limited to, a mud pulse telemetry system, an acoustic telemetry system, or an electromagnetic telemetry system.
The outside diameter of the wireline tool 40 is preferably about 2.25 inches (5.72 centimeters) or less to fit within the conduit 11 of the WCS 10 and allow sufficient annular space for drilling fluid flow.
Once the desired depth is reached, the wireline tool 40 is deployed from the WCS 10 . A signal is sent preferably from the surface via the telemetry link 22 physically releasing the tool 40 from the upper connector 42 . Drilling fluid flow within the conduit 11 and represented by the arrow 15 pushes the tool 40 from the WCS 10 and into the borehole 14 , as illustrated in FIG. 2 b. If the tool 40 is a pad type tool, arms 60 are opened from the tool body deploying typically articulating pads against or near the formation 32 . The deployed tool is physically and electrically connected to a lower connector 44 , such as a wet connector. Electrical power is preferably supplied from the power supply 48 to the tool 40 by means of a wire 50 within the wall of the WCS 10 . Alternately, power can be supplied by a coiled wire (not shown) extended inside the flow conduit (illustrated by the broken lines 11 ) from the upper connector 42 to the lower connector 44 . Telemetric communication between the deployed tool 40 and the downhole telemetry unit 46 is preferably through the lower connector 44 , and is illustrated conceptually with the line 54 . Again, the communication link can include, but is not limited to, a hard wire or an electromagnetic short-hop system. Communication between the downhole telemetry unit 46 and the uphole telemetry unit 24 is again via the previously discussed link 22 . Again, it should be understood that the wireline tool 40 can be a non-pad device.
Well logging methodology comprises initially positioning the conveyance system 100 into the borehole 12 at a predetermined depth, and preferably in conjunction with some other type if interim drilling operation such as a wiper trip. This initial positioning occurs with the wireline tool 40 contained within the WCS 10 , as shown in FIG. 2 a. At the predetermined depth and preferably on command from the surface, the wireline tool is released from the upper connector 42 , forced out of the WCS 10 by the flowing drilling fluid (arrow 15 ), and retained by the lower connector 44 . This tool-deployed configuration is shown in FIG. 2 b. The system 100 is preferably conveyed upward within the borehole by the drill string 18 , and one or more parameters of interest are measured as a function of depth thereby forming the desired. log or logs 30 (see FIG. 1 ). If the wireline tool 40 is a formation testing tool, the system is stopped at a sample depth of interest, and a pressure sample or a fluid sample or both pressure and fluid samples are taken from the formation at that discrete depth. Alternately, formation pressure can be made, of formation pressure measurements and formation fluid sampled can both be acquired. The conveyance system 100 is subsequently moved and stopped at the next sample depth of interest, and the formation fluid sampling procedure is repeated.
The conveyance system 100 can be combined with an LWD/MWD system to enhance the performance of both technologies. As discussed previously, it is advantageous to use LWD/MWD technology to determine certain parameters of interest, and advantageous and sometimes necessary to use wireline technology to determine other parameters of interest. Certain types of LWD/MWD measurements are made most accurately during the drilling phase of the drilling operation. Other LWD/MWD measurements can be made with equal effectiveness during subsequent trips such as a wiper trip. As discussed previously, wireline conveyed logging can not be performed while drilling, and the conveyance system 100 can not be included in the drill string during actual drilling. Drilling LWD/MWD measurements and wireline conveyed measurements must, therefore, be made in separate runs. In order to accurately combine measurements made during two separate runs, the depths of each run must be accurately correlated over the entire logged interval.
A hybrid tool comprising the wireline conveyance system 100 and a LWD/MWD subsection or “sub” 70 is shown in FIG. 3 . As shown, the LWD/MWD sub 70 is operationally connected at the lower end to the TPS 12 and at the upper end to the connector head 13 . The LWD/MWD sub 70 comprises one or more sensors (not shown). The hybrid tool is preferably used to depth correlate previously measured LWD/MWD data with measurements obtained with the wireline conveyance system 100 .
Operation of the hybrid system shown in FIG. 3 is illustrated with an example. Assume that neutron porosity and gamma ray LWD/MWD logs have been run previously while drilling the borehole. After completion of the LWD/MWD or “first” run, the drill string is removed from the borehole and the drill bit and motor or rotary steerable is removed. The wireline conveyance system 100 , comprising a gamma ray sensor and as an example a wireline formation tester, is added to the tool string below the LWD/MWD sub 70 , as shown in FIG. 3 . The tool string is lowered into the borehole, and the wireline tool 40 (comprising the gamma ray sensor and formation tester) is deployed as illustrated in FIG. 3 . The tool string is moved up the borehole as indicated by the arrow 66 thereby forming a “second” run with the tools “sliding”.
Both the wireline tool 40 and the LWD/MWD sub 70 measure gamma radiation as a function of depth thereby forming LWD/MWD and wireline gamma ray logs. It known in the art that multiple detectors are typically used in logging tools to form count rate ratios and thereby reduce the effects of the borehole. It is also known that additional borehole corrections, such as tool standoff corrections, are typically applied to these multiple detector logging tools. As an example, standoff corrections are applied to dual detector porosity and dual detector density systems. Standoff corrections for rotating dual detector tools typically differ from standoff corrections for wireline tools. The LWD/MWD neutron porosity measurement is preferably not repeated in the second run, since LWD/MWD borehole compensation techniques, including standoff, are typically based upon a rotating, rather than a sliding tool. Furthermore, washouts and drilling fluid invasion tends to be more prevalent during the second run. Stated another way, the neutron porosity measurement would typically be less accurate if measured during the second run, for reasons mentioned above.
The second run LWD/MWD gamma ray log may not show the exact magnitude of response as the “first run” LWD/MWD log, because factors discussed above in conjunction with the neutron log. Variations in the absolute readings tend to be less severe than for the neutron log. Furthermore, the second run gamma ray log shows the same depth correlatable bed boundary features as observed during the first run.
During the second run, the tool string is stopped at desired depths to allow multiple formation tests. Formation testing results, made with the wireline tool 40 during the second run, are then depth correlated with neutron porosity, made with the LWD/MWD sub 70 during the first run made while drilling, by using the gamma ray logs made during both runs as a means for depth correlation. All data are preferably telemetered to the surface via the telemetry link 22 . Alternately, the data can be recorded and stored within the wireline tool for subsequent retrieval at the surface of the earth.
The conveyance system 100 can be combined with an LWD/MWD system to enhance the performance of both technologies using alternate configurations and methodology. FIG. 4 a shows the LWD/MWD sub 70 operationally connected to the TPS sub 12 , which is terminated at the lower end by a drill bit 72 . One or more LWD/MWD measurements are made as the drill string 18 rotates and advances the borehole downward as indicated by the arrow 67 . This will again be referred to as the “first run”.
During a second run of the drill string such as a wiper trip, the WCS 10 is added to the drill string along with a wiper 17 , as shown in FIG. 4 b. In this embodiment, the WCS 10 and LWD/MWD sub 70 share the same power supply 52 and downhole telemetry unit 46 (see FIGS. 2 a and 2 b ) contained in the TPS 12 . The tool is lowered to the desired depth, the wireline tool 40 is deployed as previously discussed, and the tool string in moved up the borehole (as indicated by the arrow 66 ) using the drill string 18 and cooperating connector head 13 . One or more wireline tool measurements along with at least one LWD/MWD correlation log are measured during this second run. The at least one LWD/MWD correlation log allows all wireline and LWD/MWD logs to be accurately correlated for depth, and for other parameters such as borehole fluids, over the full extent of the logged interval. Again, all measured data are preferably telemetered to the surface via the telemetry link 22 . Alternately, the data can be recorded and stored within the borehole tool for subsequent retrieval at the surface of the earth.
It should be noted that the step of running at least one LWD/MWD correlation log can be omitted, and only a wireline log using the tool 40 can be run if the particular logging operation does not require a LWD/MWD log, or does not require LWD/MWD log and wireline log depth correlation.
It should also be noted that the downhole element discussed previously can contain a downhole processor thereby allowing some or all sensor responses to be processed downhole, and the “answers” are telemetered to the surface via the telemetry link 22 in order to conserve bandwidth.
While the foregoing disclosure is directed toward the preferred embodiments of the invention, the scope of the invention is defined by the claims, which follow.
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A borehole conveyance system that integrates wireline type downhole instrumentation into the drill string tripping operations that are typically performed in a borehole drilling operation to increase the types of measurements that can be obtained during the drilling operation and reduce equipment costs and maintenance costs. Certain wireline type tools can be used during drilling operations to yield measurements superior to their LWD/MWD counterparts, but not during any drilling operation in which the drill string is rotating while other types of wireline tools can be used to obtain measurements not possible with LWD/MWD systems.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of and co-owned U.S. patent application Ser. No. 10/211,138, entitled “Tornado and Hurricane Roof Tie”, filed with the U.S. Patent and Trademark Office on Aug. 2, 2002 now U.S. Pat. No. 6,837,019 by the inventor herein, the specification of which is included herein by reference.
BACKGROUND OF INVENTION
1. Field of the Invention
This invention relates generally to building structures with wood roofs, and more particularly to structures exposed to extreme wind conditions, such as Tornadoes and Hurricanes, where building codes dictate that such structures be protected against structural failure to save lives of occupants. In particular, the present invention relates to a roof tie for anchoring a wood frame roof on a block construction building in order to resist uplift forces encountered during a high wind situation.
2. Background of the Prior Art
It is well known what high winds can do to a building, particularly to a wood frame construction low-rise structure. Generally, uplift forces tending to lift the roof off the structure or the entire structure off its foundation cause much of the damage sustained by the building.
Wood structures predominate in residential and light commercial construction, and when wood framing is employed, the structure must be protected from upward loads developed by high wind, which differs with geographical location and is enforced by different building codes for such areas. For example, the Bahamas and Florida, including the Florida Keys are situated in the pathway of the yearly Caribbean hurricane travel course and as such, encounter hurricanes and/or tornadoes from time to time. Houses in the Bahamas are typically constructed of cement block with a wooden top plate fastened to the top of cement block walls, for attaching a wooden roof. In the case of upward loads, the roof is generally tied to the walls using a variety of steel connectors that tie the top plate to the walls. The size and number of these steel connectors vary depending on the severity of the wind conditions in the locality of the building, and the building's geometry. Due to the house location in a susceptible high wind area, some building codes require that houses built with wooden roof support beams have a “Hurricane Tie” in place on every rafter.”
Hurricane Ties” are usually installed during the foundation and framing stages of construction. Laborers hired by the framing contractor generally install connectors and sheathing. Correct size, location, and number of fasteners (nails or bolts) are critical to sustaining the required load. Commonly, such laborers are inexperienced which results in improper or inadequate installation. In all structures, locations of connectors mandate their installation during the framing stage due to related components being placed at the same time. This process slows the foundation and framing stages of construction, which in turn increases labor costs.
From the foregoing, it is apparent that there is a critical need for a strong roof tie system that provides for uplift loads which is cost effective and easy to install.
SUMMARY OF INVENTION
The present invention provides a solution to the above and other problems by reinforcing and anchoring the roof structure to the building top plate, wherein a hold down force is applied to the ceiling rafters to counter the uplift and horizontal forces generated by high winds. The present invention can be incorporated during initial construction of a wooden roof structure.
It is an object of the present invention to provide a rooftie bracket system for a wooden roof structure of a building that reinforces the roof against damage in a high wind situation, such as a hurricane.
It is another object of the present invention to provide a roof-tie bracket system for a wooden roof construction building that provides a downward force around the periphery of the roof, thereby to better resist upward lift imparted to the roof by high winds.
It is another object of the present invention to provide a roof-tie bracket system for a wood frame roof that provides reinforcement to the roof structure, thereby providing greater resistance to damage during high wind conditions. A related object is to increase public safety in structures existing in high wind areas.
It is yet another object of the present invention to enable cost effective construction of wooden roof structures while meeting all building code requirements. A related object is to provide a roof-tie bracket system for a lowrise building that complies with the recommendation of all major building codes.
This invention relates to a novel roof-tie bracket system for bracing a wood framed roof of a building, e.g., a residential dwelling, having a structure including a foundation upon which rests a wall construction and horizontal ceiling plates. The structure is reinforced against the destructive forces of the atmosphere by high strength brackets preferably attached to every rafter where it joins the ceiling plates. The roof-tie bracket is connected to the structure by way of a plurality of fasteners, such as nails or lag bolts.
The roof-tie bracket disclosed herein offers more body, more nailing surfaces, more wrapping capability, more strength, and more durability to the purchasing public. Such roof-tie brackets may be made from a graduated increase in sheet metal gauges in a variety of straps or ties to fit many framing applications and strength requirements. Moreover, such roof-tie brackets may be prepitched to a predetermined angle of a roof, keeping in mind the different sizes of wood that may be used to pitch a roof. Such roof-tie brackets create a solid attachment between a rafter and ceiling top plate. This simple invention enables a family of roof-tie brackets that can be mass-produced and sold for a reasonable price that, in fact, can be made or put in place by any skilled or semiskilled person.
Some of the advantages of this invention include: increase in surface area of a roof-tie bracket, thereby creating more surfaces through which nails could penetrate the substructure; “prepitched” roof-tie brackets that create a snug fit over all substructures and angles, at angles consistent with industry roof pitch standards; a “decking window” that allows fastening of nails through the “deck” to the rafter beneath; “plate flaps” that further secures the roof-tie bracket to the top plate; and, in some embodiments, a “ceiling joist and cradle” that provides further for the “strapping” of ceiling joists, all in one simple Hurricane and Tornado Tie.
BRIEF DESCRIPTION OF DRAWINGS
The above and other features, aspects, and advantages of the present invention are considered in more detail, in relation to the following description of embodiments thereof shown in the accompanying drawings, in which:
FIG. 1 a shows an illustration of a roof tie in perspective according to one embodiment of the present invention;
FIG. 1 b shows an illustration of the roof tie of FIG. 1 a , with a top plate and rafter in phantom;
FIG. 2 a shows an illustration of a roof tie in perspective having a rigidity reinforcement according to one embodiment of the present invention;
FIG. 2 b shows an illustration of the roof tie of FIG. 2 a , with top plate and gable in phantom;
FIG. 3 shows an illustration of a roof tie, according to an alternative to the embodiment in FIGS. 2 a and 2 b ;
FIG. 4 a shows an illustration of a roof tie in perspective having a hold-down reinforcement according to one embodiment of the present invention;
FIG. 4 b shows an illustration of the roof tie of FIG. 4 a , with top plate and gable in phantom;
FIG. 5 shows an illustration of a roof tie, according to an alternative to the embodiment in FIGS. 4 a and 4 b ;
FIG. 6 shows an illustration of an alternate embodiment of a roof tie, with top plate and gable in phantom, and
FIG. 7 shows an illustration of a roof tie, according to an alternative to the embodiment in FIG. 6 .
DETAILED DESCRIPTION
The invention summarized above and defined by the enumerated claims may be better understood by referring to the following description, which should be read in conjunction with the accompanying drawings in which like reference numbers are used for like parts. This description of an embodiment, set out below to enable one to build and use an implementation of the invention, is not intended to limit the enumerated claims, but to serve as a particular example thereof. Those skilled in the art should appreciate that they may readily use the conception and specific embodiments disclosed as a basis for modifying or designing other methods and systems for carrying out the same purposes of the present invention. Those skilled in the art should also realize that such equivalent assemblies do not depart from the spirit and scope of the invention in its broadest form.
Referring to FIG. 1 a , a roof tie according to the present invention, indicated generally as 10 , is illustrated, comprising a tie component 13 , a cradle component 16 , and a bridge component 19 , such tie component 13 having an upper portion 22 and a lower portion 24 and such cradle component 16 having an upper portion 27 and a lower portion 29 . Such upper portion 22 of such tie component 13 comprises a riser 33 having a plurality of apertures 35 . The lower portion 24 of such tie component 13 comprises fastener extension 37 , which extends at a right angle from riser 33 and further comprises top plate flaps 40 , 41 . A plurality of apertures 35 for inserting fasteners, such as nails are disposed on such fastener extension 37 , and top plate flaps 40 , 41 . Such upper portion 27 of such cradle component 16 comprises a wall 44 having a plurality of apertures 35 and at least one fastener slot, such as 47 . The lower portion 29 of such cradle component 16 comprises fastener extension 52 , which extends at a right angle from wall 44 and further comprise top plate flaps 55 , 56 and cradle wall 59 . Cradle wall 59 is disposed on an outward edge of fastener extension 52 and extends upward, substantially perpendicular to such fastener extension 52 . In general, cradle wall 59 is preferably shorter than and substantially parallel to wall 44 . A plurality of apertures 35 for inserting fasteners, such as nails, are disposed on such fastener extension 52 , top plate flaps 55 , 56 , and cradle wall 59 . Such plurality of apertures should be disposed in a staggered fashion to prevent splitting of the top plate and rafters when inserting such fasteners.
Bridge component 19 presents a large window area 60 to permit fastening decking to a rafter. Such bridge component 19 should be wide enough to conform to the standard thickness of construction materials, such as wooden 2×4s. Bridge component 19 comprises a short riser 63 having a plurality of apertures 35 for fastening such bridge component 19 to a rafter. Bridge component 19 further comprises an overlap plate 66 disposed away from such bridge component 19 by ledge 69 and having at least one opening, such as 72 . In use, overlap plate 66 at least partly extends over wall 44 . Such fastener slots 47 are disposed such that, in use, fasteners inserted in openings 72 in overlap plate 66 can penetrate such fastener slots 47 . By having such overlap, roof tie 10 can adapt to rafters of varying heights for application in a variety of construction scenarios. Fastener slots 47 enable fasteners to be inserted in such a manner to ensure a snug fit for bridge component 19 on the top of a rafter. Overlap plate 66 extends over wall 44 such that fasteners inserted in openings 72 also enter fastener slots 47 at a variable position depending on the height of the rafter for attachment to such rafter.
An application showing use of such roof tie 10 is illustrated in FIG. 1 b presenting roof tie 10 in a position for fastening to top plate 75 and rafter 78 . Fasteners are attached to top plate 75 and rafter 78 through apertures 35 , and through openings 72 in alignment with fastener slots 47 . Using a fastener in each opening ensures a strong and secure attachment. Additional embodiments using various numbers of holes can be used based on specific engineering requirements as determined by one skilled in the art. As shown in FIG. 1 b , top plate flaps 55 , 56 , are fastened to the sides of top plate 75 , providing a wrap around most of such top plate 75 . Window area 60 is provided to enable fastening of decking material to rafter 78 .
In some embodiments, the length of the forward edge of wall 44 may be longer than the rear edge of such wall 44 , correspondingly, the forward edge of riser 33 may be longer than the rear edge of such riser 33 in order to have bridge component 19 angled to correspond to a selected pitch for a roof.
FIGS. 2 a and 2 b illustrate an alternate embodiment of a roof tie, indicated generally as 82 , according to the present invention. Roof tie 82 comprises a tie component 13 , a cradle component 16 , and bridge component 19 , such tie component 13 having an upper portion 22 and a lower portion 24 and such cradle component 16 having an upper portion 27 and a lower portion 29 . Such upper portion 22 of such tie component 13 comprises a riser 33 having a plurality of apertures 35 . The lower portion 24 of such tie component 13 comprises fastener extension 37 , which extends at a right angle from riser 33 and further comprises top plate flaps 40 , 41 . A plurality of apertures 35 for inserting fasteners, such as nails are disposed on such fastener extension 37 , and top plate flaps 40 , 41 . Such upper portion 27 of such cradle component 16 comprises a wall 44 having a plurality of apertures 35 and a plurality of fastener slots 47 . The lower portion 29 of such cradle component 16 comprises fastener extension 52 , which extends at a right angle from wall 44 and further comprise top plate flaps 55 , 56 and cradle wall 59 . Cradle wall 59 is disposed on an outward edge of fastener extension 52 and extends upward, substantially perpendicular to such fastener extension 52 . In general, cradle wall 59 is preferably shorter than and substantially parallel to wall 44 . A plurality of apertures 35 for inserting fasteners, such as nails, are disposed on such fastener extension 52 , top plate flaps 55 , 56 , and cradle wall 59 . Such plurality of apertures should be disposed in a staggered fashion to prevent splitting of the top plate and rafters when inserting such fasteners.
Bridge component 19 presents a large window area 60 to permit fastening decking to a rafter. Such bridge component 19 should be wide enough to conform to the standard thickness of construction materials, such as wooden 2×4s. Bridge component 19 comprises a short riser 63 having a plurality of apertures 35 for fastening such bridge component 19 to rafter 78 . Bridge component 19 further comprises an overlap plate 66 having openings 72 . In use, overlap plate 66 at least partly extends over wall 44 . Such fastener slots 47 are disposed such that, in use, fasteners inserted in openings 72 in overlap plate 66 can penetrate such fastener slots 47 .
For heavy-duty applications, roof tie 82 further comprises a reinforcing wing 85 . Such reinforcing wing 85 is generally triangular in shape and extends outward from a plate 88 that can be attached to riser 33 by sliding plate 88 into tabs 91 , 92 , 93 , 94 . Holes 97 in plate 88 enable attachment of such plate 88 through riser 33 into rafter 78 . The top portion of plate 88 has an extension that can overlap the short riser 63 of bridge component 19 and presents a centrally located elongated opening 100 that aligns with aperture 103 in short riser 63 to attach a fastener into rafter 78 . The lower edge of reinforcing wing 85 has a pair of base flaps 105 , 106 on each side. Such base flaps 105 , 106 have apertures 109 for attaching fasteners therethrough into top plate 75 .
Such reinforced heavy duty roof tie 82 provides vertical reinforcement to prevent balking while enabling increased rigidity to roof tie 82 , resulting in a sturdier, stronger roof tie 82 . Such increased strength can be obtained at reduced cost by enabling use of lower galvanized steel gauges for its construction. Balking is caused by misalignment of trusses due to warping of roof timbers or loosening of fastened joints, resulting in roof decking being heaved up along such misaligned roof truss.
In an alternate embodiment, short riser 63 may present a hook in the place of aperture 103 , such that elongated opening 100 can be engaged on the hook while sliding back plate 88 into tabs 91 , 92 , 93 , 94 . Attachment of fasteners to base flaps 105 , 106 would thereby provide a downward force on such hook and bridge component 19 .
FIG. 3 shows an illustration of an application according to an alternative roof tie embodiment. Roof tie 110 comprises a pair of matching tie component sections, having upper portions 112 , 113 and lower portions 114 , 115 . Such upper portions 112 , 113 comprise risers 117 , 119 , substantially parallel to each other. Bridge 121 presenting a large window area 124 overlaps the top of risers 117 , 119 . Bridge 121 should conform to the standard thickness of construction materials, such as rafter 78 . The lower portions 114 , 115 of such roof tie 110 comprise fastener extensions 127 , 129 , which extend at right angles from risers 117 , 119 , respectively, each of which fastener extensions 127 , 129 further comprise top plate flaps 131 , 132 , 133 (not shown), 134 (not shown). A plurality of apertures 137 for inserting fasteners, such as nails 138 are disposed on such risers 117 , 119 , fastener extensions 127 , 129 , and top plate flaps 131 , 132 , 133 (not shown), 134 (not shown). Such plurality of apertures should be disposed in a staggered fashion to prevent splitting of the top plates and rafter when inserting such fasteners.
For heavy-duty applications, roof tie 110 further comprises reinforcing wings 140 , 141 . Such reinforcing wings 140 , 141 are generally triangular in shape and extend outward from a plate that can be attached to risers 117 , 119 , respectively. The lower edge of each reinforcing wing 140 , 141 has a pair of base flaps 145 , 146 on each side. Such base flaps 145 , 146 have apertures 149 for attaching fasteners therethrough into top plate 75 .
Such reinforced heavy duty roof tie 110 provides vertical reinforcement to prevent balking while enabling increased rigidity to roof tie 110 , resulting in a sturdier, stronger roof tie 110 . Such increased strength can be obtained at reduced cost by enabling use of lower galvanized steel gauges for its construction. Balking is caused by misalignment of trusses due to warping of roof timbers or loosening of fastened joints, resulting in roof decking being heaved up along such misaligned roof truss.
In some embodiments, the length of the forward edges of risers 117 , 119 may be longer than the rear edges of such risers 117 , 119 in order to have bridge 121 angled to correspond to a selected pitch for a roof.
FIGS. 4 a and 4 b illustrate an alternate embodiment of a hold-down roof tie, indicated generally as 153 , according to the present invention. For heavy-duty applications, hold-down roof tie 153 further comprises turnbuckle 157 attached to bridge component 19 and fastener extension 37 . Turnbuckle 157 comprises body 160 having a first threaded portion 163 extending out of the top of such body 160 and a second threaded portion 164 extending out of the bottom of such body 160 . The distal end of such first threaded portion 163 terminates in an eye 167 having an opening for attaching to short riser 63 of bridge component 19 . Such eye 167 can be attached to short riser 63 and rafter 78 by a suitable fastener such as a nail or lag bolt. In some embodiments, short riser 63 presents a hook on which such eye 167 can be attached.
The distal end of such second threaded portion 164 terminates in an eye or some other fashion having an opening 170 . A plate 173 is attached to fastener extension 37 and to top plate 75 by suitable fasteners. A U-shaped connector 177 having a pin 180 passing through the open end of such U-shaped connector 177 projects from the top of such plate 173 . The pin 180 passes through the opening 170 on the end of such second threaded portion 164 of such turnbuckle 157 .
The alignment of the threads of such first and second threaded portions 163 , 164 is configured such that rotation of such body 160 in a first direction about its longitudinal axis causes both such first and second threaded portions 163 , 164 to be drawn into such body 160 and rotation of such body 160 in a second, opposite direction about its longitudinal axis causes both such first and second threaded portions 163 , 164 to be forced out of such body 160 . Such hold-down roof tie 153 provides additional reinforcement against uplift forces encountered in a high wind condition, resulting in a sturdier, stronger tie. Such increased strength can be obtained at reduced cost by enabling use of lower galvanized steel gauges for its construction while providing increased hold-down force.
FIG. 5 shows an illustration of an application according to an alternative hold-down roof tie embodiment. Roof tie 185 comprises a pair of matching turnbuckles 187 , 189 attached to either side of bridge 121 and fastener extensions 127 , 129 . Such fastener extensions 127 , 129 , extend at right angles from risers 117 , 119 , respectively, each of which fastener extensions 127 , 129 further comprise top plate flaps 131 , 132 , 133 (not shown), 134 (not shown). A plurality of apertures 137 for inserting fasteners, such as nails 138 are disposed on such risers 117 , 119 , fastener extensions 127 , 129 , and top plate flaps 131 , 132 , 133 (not shown), 134 (not shown). Such plurality of apertures should be disposed in a staggered fashion to prevent splitting of the top plates and rafter when inserting such fasteners.
Each turnbuckle 187 , 189 comprises a body 190 , 191 having a first threaded portion 193 , 194 extending out of the top of such body and a second threaded portion 1960 197 extending out of the bottom of such body. The distal end of such first threaded portion 193 , 194 terminates in an eye 201 , 202 having an opening for attaching to a flap 205 , 206 extending down from bridge 121 . Such eye 201 , 202 can be attached to flap 205 , 206 and rafter 78 by a suitable fastener such as a nail or lag bolt. In some embodiments, flap 205 , 206 presents a hook on which such eye 201 , 202 can be attached. In a further embodiment, flap 205 , 206 presents a loop engaged with eye 201 , 202 , as illustrated in FIG. 7 .
The distal end of such second threaded portion 196 , 197 terminates in an eye or some other fashion having an opening in which a pin 210 , 211 passes through. A plate 213 , 214 is attached to fastener extensions 127 , 129 , respectively and to top plate 75 by suitable fasteners. Pin 210 , 211 passes through the open end of U-shaped connector 217 , 218 that projects from the top of such plate 213 , 214 .
The alignment of the threads of such first and second threaded portions is configured such that rotation of such body of such turnbuckle 187 , 189 in a first direction about its longitudinal axis causes both such first and second threaded portions to be drawn into such body and rotation of such body of such turnbuckle 187 , 189 in a second, opposite direction about its longitudinal axis causes both such first and second threaded portions to be forced out of such body. Such hold-down roof tie 185 provides additional reinforcement against uplift forces encountered in a high wind condition, resulting in a sturdier, stronger tie. Such increased strength can be obtained at reduced cost by enabling use of lower galvanized steel gauges for its construction while providing increased hold-down force.
FIG. 6 illustrates an alternate embodiment of a holddown roof tie, indicated generally as 225 . Hold-down roof tie 225 further comprises loop 228 rising out of plate 173 for attaching the second threaded extension 164 of turnbuckle 157 . The opening 170 in the distal end of the second threaded extension 164 of turnbuckle 157 may be manufactured around loop 228 for added strength. In an alternate embodiment, loop 228 may be bonded to plate 173 by welding or other appropriate means.
FIG. 7 shows an alternate hold-down roof tie configuration. Roof tie 235 comprises a pair of matching turnbuckles 187 , 189 attached to either side of bridge 121 and fastener extensions 127 , 129 . Similar to the embodiment described above with regard to FIG. 6 , a loop 237 , 239 rises out of fastener extensions 127 , 129 for attaching the second threaded extension 196 , 197 of turnbuckle 187 , 189 .
The invention has been described with references to a preferred embodiment. While specific values, relationships, materials and steps have been set forth for purposes of describing concepts of the invention, it will be appreciated by persons skilled in the art that numerous variations and/or modifications may be made to the invention as shown in the specific embodiments without departing from the spirit or scope of the basic concepts and operating principles of the invention as broadly described. It should be recognized that, in the light of the above teachings, those skilled in the art can modify those specifics without departing from the invention taught herein. Having now fully set forth the preferred embodiments and certain modifications of the concept underlying the present invention, various other embodiments as well as certain variations and modifications of the embodiments herein shown and described will obviously occur to those skilled in the art upon becoming familiar with such underlying concept. It is intended to include all such modifications, alternatives and other embodiments insofar as they come within the scope of the appended claims or equivalents thereof. It should be understood, therefore, that the invention may be practiced otherwise than as specifically set forth herein. Consequently, the present embodiments are to be considered in all respects as illustrative and not restrictive.
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A building roof tie for attaching roof trusses and rafters to wood top plates in building structures, such roof tie having a sheet metal body with risers and a bridge for overlapping a rafter and flaps for wrapping on the sides of the top plate. A generally triangular shaped reinforcing wing provides strength and stability, and can also provide additional hold-down strength, allowing the roof tie to be manufactured from different weights of steel. Turnbuckles attached to the bridge provide additional hold-down strength against increased uplift forces. The roof ties are pitched to conform to a variety of framing applications. A plurality of apertures is formed in the roof tie to provide openings for fasteners for connecting the tie to the wood top plate and rafter.
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PRIORITY
The present application claims priority from to commonly owned and assigned application No. 60/716,632, entitled Stitching System and Method, filed on Sep. 13, 2005, which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to systems and methods for stitching. In particular, but not by way of limitation, the present invention relates to mechanized systems and methods for stitching.
BACKGROUND OF THE INVENTION
The stitching of patterns on fabrics using computer controlled sewing machines has become a standard practice in the industry. Fabrics that can be embroidered assume a variety of shapes and sizes. Popular shapes frequently embroidered are curved shapes that are often in the form of a cap (e.g., a baseball cap), shirt sleeves, pockets and pant legs where the fabric for embroidering includes the tubular or cylindrical-shape.
It is common to embroider tubular shaped objects (e.g., caps) with emblems, logos, letters and the like. Present embroidery equipment, however, is not particularly well-suited for providing embroidery along substantial portions of tubular or curved shaped objects. Accordingly, a system and method are needed to address the shortfalls of present technology and to provide other new and innovative features.
SUMMARY OF THE INVENTION
Exemplary embodiments of the present invention that are shown in the drawings are summarized below. These and other embodiments are more fully described in the Detailed Description section. It is to be understood, however, that there is no intention to limit the invention to the forms described in this Summary of the Invention or in the Detailed Description. One skilled in the art can recognize that there are numerous modifications, equivalents and alternative constructions that fall within the spirit and scope of the invention as expressed in the claims.
In some embodiments, the invention may be characterized as a stitching machine that includes a sewing head with a needle, an arm assembly disposed relative to the sewing head so as to allow a garment to be placed between the sewing head and the arm assembly and a non-planer needle plate coupled to the arm assembly. The non-planer needle plate in these embodiments includes an aperture that is disposed so as to allow the needle to project through the aperture after the needle has moved through the garment.
In several variations of these embodiments, a trimmer assembly is coupled to the arm assembly and the trimmer assembly includes a blade configured to trim thread while moving along an axis of the arm assembly. In many embodiments, the blade is configured to move along an axis of the arm assembly without substantial movement in a radial direction.
In another embodiment, the invention may be characterized as a trimmer assembly for a stitching machine comprising a trimmer housing adapted so as to couple with the stitching machine, a knife configured to slide within the trimmer housing along a single axis and a selector arm slideably coupled to the trimmer housing so as to be capable of sliding along a length of the trimmer housing. The selector arm in this embodiment includes one end with a hook portion that is configured to pull thread to the knife so as to trim the thread.
In yet another embodiment, the invention may be characterized as a knife for trimming thread comprising a planer portion including a slot that is configured to allow the planer portion to slide along a retainer pin and a blade portion coupled to the planer portion, wherein the blade portion is adapted so as to trim thread when the planer portion is moving along a single axis. In variations of this embodiment, the blade portion includes two tangs that are relatively disposed so as to allow thread to be trimmed when the thread is interposed between the two tangs. As previously stated, the above-described embodiments and implementations are for illustration purposes only. Numerous other embodiments, implementations, and details of the invention are easily recognized by those of skill in the art from the following descriptions and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Various objects and advantages and a more complete understanding of the present invention are apparent and more readily appreciated by reference to the following Detailed Description and to the appended claims when taken in conjunction with the accompanying Drawings wherein:
FIG. 1 is a perspective view of a stitching machine in accordance with the exemplary embodiment;
FIG. 2 a perspective front-view of the lower arm assembly depicted in FIG. 1 in a disassembled form;
FIG. 3 a perspective rear-view of the lower arm assembly and a portion of the stitching machine depicted in FIG. 1 ;
FIGS. 4A and 4B are a front view of the lower arm assembly and a side view of the lower arm assembly respectively;
FIG. 5A is a cut-away view of the lower arm assembly along line A-A of FIG. 4A ;
FIG. 5B depicts an exploded-detail view of a distal end of the lower arm assembly identified as area B in FIG. 5A ;
FIG. 5C shows an exploded and detailed view of a proximate end of the lower arm assembly identified as area C in FIG. 5A ;
FIGS. 6A , 6 B, 6 C and 6 D are respective, front, side and top views of the trimmer assembly depicted in FIG. 2 ; and
FIG. 7 is a detailed view of the trimmer assembly depicted in FIGS. 2 and 6 .
DETAILED DESCRIPTION
Referring now to the drawings, an exemplary embodiment is shown which depicts various aspects of the present invention. Shown in FIG. 1 , is a perspective view of a stitching machine 100 in accordance with the exemplary embodiment. Shown is a head portion 102 positioned above a lower arm assembly 104 . As depicted in FIG. 1 , the lower arm assembly 104 includes a non-planer needle plate 106 , which in this embodiment includes a curved (e.g., cylindrical-shaped) outer surface.
Advantageously, the curved surface of the needle plate accommodates garments with a tubular topology so as to allow a point of the garment that is being penetrated by a needle to rest against the needle plate 106 . This is in contrast with prior art stitching machines that either must deform a tubular garment to conform to a planer needle plate or leave a gap between the garment and the planer needle plate.
Referring next to FIG. 2 , shown is a perspective front-view of the lower arm assembly 200 in a disassembled form. As depicted in this embodiment, the lower arm assembly 200 includes among other components, a non-planer needle plate 202 , a trimmer assembly 204 that couples to a push-pull cable 206 via a push rod 205 for a knife of the trimmer assembly 204 and a push cable 208 that couples to a selector of the trimmer assembly 204 via a push rod 207 .
Also shown are an axial reference 210 (depicting an axial direction) and a radial reference 212 (depicting a radial direction perpendicular to the axial direction) relative to the arm assembly 200 . As discussed further herein, a knife of the trimmer assembly 204 in several embodiments is capable of trimming a thread passing through the aperture 214 of the needle plate 202 while translating along the axial direction 210 (e.g., without substantial radial translation). In this way, the amount of space occupied by the trimmer assembly 204 is substantially reduced; thus allowing the needle plate 202 to be sized and configured to curve around the trimmer assembly 204 in a non-planer manner.
Referring to FIG. 3 , shown is a perspective rear-view of the lower arm assembly 104 and a rear portion of the body 300 of the stitching machine 100 . As depicted, the lower arm assembly 104 in the exemplary embodiment protrudes from the body 300 of the stitching machine in a substantially perpendicular fashion.
Referring to FIGS. 4A and 4B , shown are a front view of the lower arm assembly 104 and a side view of the lower arm assembly 104 respectively. In FIG. 5A , shown is a cut-away view of the lower arm assembly along line A-A of FIG. 4A . FIG. 5B depicts an exploded and detailed view of a proximate end of the lower arm assembly 104 identified as area B in FIG. 5A , and FIG. 5C shows an exploded detailed view of a distal end of the lower arm assembly 104 identified as area C in FIG. 5A .
Referring next to FIGS. 6A , 6 B, 6 C and 6 D, shown are perspective, front, side and top views of the trimmer assembly 204 depicted in FIG. 2 . Details of the trimmer assembly 204 are shown in FIG. 7 , which shows a trimmer housing 700 , a spring presser 702 , a knife retainer pin 704 , a selector 706 , a knife 708 , a knife carrier 710 and a knife hold down 712 .
As depicted, the knife 708 in the exemplary embodiment includes a planer portion 714 that includes a slot 716 to accommodate the knife retainer pin 704 . In addition, the knife 708 includes a blade portion 718 that includes a first and second tangs 720 A, 720 B that are configured to trim thread when thread is interposed between the two tangs 720 A, 720 B. In particular, the knife 708 in the exemplary embodiment is capable of trimming thread while moving solely in the axial direction shown in FIG. 7 . As shown, the knife carrier 710 includes an aperture 722 to accommodate the push rod 205 that couples with the push-pull cable 206 (shown in FIG. 2 ) for the knife 708 . The push rod 205 in this embodiment enables actuation of the knife 708 along the axial direction.
Referring again to FIG. 6C , the tangs 720 A, 720 B in one embodiment are relatively disposed so as to occupy a non-planer region (i.e., one tang is positioned lower than the other tang). In some embodiments, an inside edge of one or both tangs 720 A, 720 B is intentionally roughened so as to facilitate trimming of the thread.
As shown in FIG. 7 , the selector 706 includes a hook 724 at a distal portion and a push rod coupling 726 and an aperture 727 , which accommodates the push rod 207 for the selector 706 , at a proximate portion. In addition, a slot 728 in a planer region 730 of the selector 706 is configured to accommodate the knife retainer pin 704 , and in addition, the slot 728 is shaped so that when the selector 706 is pushed by the push rod 207 in an axial direction opposite its proximate end, the selector 706 moves in a radial-outward direction so as to allow the hook end 724 of the selector 706 to move around the thread and then to move back in a radial-inward direction to capture the thread. Then the selector 706 is moved in an axial direction inward to place tension on the thread so that the knife 708 may efficiently trim the thread.
Referring again to FIG. 5B , the trimmer assembly 204 is shown positioned within the distal end of the lower arm assembly 104 . As shown the trimmer assembly 204 is in close proximity to the non-planer needle plate 106 so that there is very little distance between the blade of the knife 708 when extended and the inner portion of the aperture 214 of the needle plate 106 . In this way, a tail of trimmed thread is short (which means less follow-up trimming by hand) and the thread length to the bobbin is relatively long allowing for easy handling.
As a consequence, the present invention provides several advantages over the prior art. Those skilled in the art, however, can readily recognize that numerous variations and substitutions may be made in the invention, its use and its configuration to achieve substantially the same results as achieved by the embodiments described herein. Accordingly, there is no intention to limit the invention to the disclosed exemplary forms. Many variations, modifications and alternative constructions fall within the scope and spirit of the disclosed invention.
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A system, apparatus and method for stitching are described. One embodiment includes a sewing head including a needle; an arm assembly that is disposed relative to the sewing head so as to allow a garment to be placed between the sewing head and the arm assembly; and a non-planer needle plate coupled to the arm assembly that includes an aperture that is disposed so as to allow the needle to project through the aperture after the needle has moved through the garment.
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FIELD OF THE INVENTION
[0001] The present invention relates to semiconductor integrated circuits, and more particularly to a semiconductor capacitor, and method for fabricating the same.
BACKGROUND OF THE INVENTION
[0002] High Capacity Capacitors have been used in the semiconductor industry for years, in applications such as DRAM storage, protection from high energy environments, decoupling capacitors and many more. As integrated circuits continue to become more densely built, small and powerful decoupling capacitors are needed for optimal system performance.
[0003] A promising high-density capacitor for radio-frequency decoupling applications is reported by Klootwijt, et al., Ultrahigh Capacitance Density for Multiple ALD-Grown MIM Capacitor Stacks in 3-D Silicon”, IEEE Electron Device Letters, 29:7, July 2008 (hereafter the “Philips MIM capacitor”). Klootwijt et al discloses a method to form the 3-D capacitor 100 illustrated in FIG. 1 . According to Klootwijt et al, a macropore 110 of about 1.5 micron diameter and 30 micron depth is formed in a substrate 101 that is “(arsenic) n++ -doped silicon.” A 5-nm thermally grown SiO2 layer 121 coats the walls of the pore, then a “stack [ 125 ] of TiN/Al2O3/TiN/Al2O3/TiN is deposited by ALD” to complete the triple MIM capacitor stack. Conditions are controlled to avoid oxidation of the TiN electrode layers. “On completion, the layers are patterned for contacting the electrodes and covered with a low-temperature interlevel oxide layer. Finally, contact holes are opened, and bond pads 131 to 134 are formed.”
[0004] The process described by the above reference requires multiple lithography steps. What is needed is a simplified process to form an ultra-high density trench capacitor.
BRIEF DESCRIPTION OF THE DRAWINGS
[0005] The structure, operation, and advantages of the present invention will become further apparent upon consideration of the following description taken in conjunction with the accompanying figures. The figures are intended to be illustrative, not limiting.
[0006] FIG. 1 illustrates a MIM capacitor in accordance with prior art.
[0007] FIGS. 2 , 3 A to 5 A, and 6 illustrate the formation of a MIM stack in a cavity in accordance with embodiments of the present invention.
[0008] FIGS. 3B to 5B are cross section views corresponding to FIGS. 3A to 5A for an embodiment formed in a circular cavity.
[0009] FIGS. 7A , 7 B, 8 A, and 8 B illustrate selective etch of layers of a MIM stack in accordance with embodiments of the present invention.
[0010] FIGS. 9A , 9 B, 10 A, and 10 B illustrate forming electrodes in a MIM capacitor in accordance with embodiments of the present invention.
SUMMARY
[0011] According to an embodiment of the present invention, a layered structure can be formed within a cavity, the layered structure having a plurality of metal layers insulated from each other, where the plurality includes a set of first-type metal layers and a set of second-type metal layers. Adjacent pairs of the plurality of metal layers include a first-type metal layer and a second-type metal layer. The first-type metal layers can be selectively etched relative to the second-type metal layers by a first etch chemistry, and the second-type metal layers can be selectively etched relative to the first-type metal layers by a second etch chemistry. The structure can also include one electrode contacting just the first-type metal layers and another electrode contacting just the second-type metal layers.
[0012] Another embodiment of the present invention is a method to form a deep-trench capacitor. The method utilizes a stack of metal layers formed in a cavity, where each adjacent pair of said stack includes a first-type metal layer and a second-type metal layer. The stack also includes an insulating layer between such adjacent pairs. The method includes exposing a cross section of the stack, etching the first-type metal layers within a first area of the cross section while not appreciably etching the second-type metal layers, and etching the second-type metal layers within a second area of the cross section while not appreciably etching the first-type metal layers. The method can further include forming the stack of metal layers within the cavity. The method can further include recessing the first-type metal layers within a first area of the cross section and recessing the second-type metal layers within a second area of the cross section. The method can include backfilling such recesses with dielectric and forming a first electrode in contact with just the second-type metal layers in the first area and forming a second electrode in contact just with the first-type metal layers in the second area.
[0013] According to yet another embodiment of the present invention, the structure of claim 4 can be made according the method of claim 12 . The method to form the structure of claim 4 can further include the method of claim 18 .
DETAILED DESCRIPTION
[0014] The complicated lithography required to connect the electrodes of the Philips MIM capacitor restricts that capacitor to just a few layers (e.g., three metal layers). The present inventors have devised a method to form a MIM capacitor (“MIMCAP”) having up to fifteen plates, or any number of plates, constrained only by the thicknesses of the deposited layers and the dimension of the cavity within which the MIMCAP is formed.
[0015] Referring now to FIG. 2 , an opening such as cavity 210 is formed in a substrate 201 , according to a patterned mask. The mask may be, for example, oxide hardmask 203 on top of pad nitride 202 . The substrate may be a semiconductor wafer, which may be, for example, a silicon or gallium nitride substrate, and can be a semiconductor-on-insulator (SOI) substrate. The substrate can be heavily doped to serve as a capacitor plate, for example, silicon with arsenic (As) dopant at 1E19 to 5E21, or the capacitor plates can be formed with the metal layers only and the substrate can be undoped. The invention is not limited to particular dimensions of cavity 210 , but it can be about 1.5 micron across and 30 micron depth. The opening of cavity 210 can be the critical dimension (the minimum dimension patternable by the lithography used to form devices (not shown) in or on substrate 201 ). Cavity 210 can be a trench (formed according to a generally rectilinear pattern with a length and width), a pore (formed according to a circular pattern), an annulus, or an opening formed according to a pattern of any other shape.
[0016] Dielectric layer 221 can be formed over the sidewalls and bottom of cavity 210 . As shown in FIG. 3A , dielectric layer 221 can be a conformal layer having substantially uniform thickness on all surfaces. Layer 221 can be thermally grown, or formed by conventional deposition such as plasma-enhanced chemical vapor deposition (PECVD) or atomic layer deposition (ALD). In embodiments, layer 221 is high-K dielectric having dielectric constant greater than 2.5, and can have dielectric constant in the range of 15 to 20, or even greater than 20 . Layer 221 can be any interlayer dielectric material (ILD), which can be an high k material such as hafnium oxide (HfO2), hafnium silicate, zirconium oxide, aluminum oxide or zirconium silicate. Layer 221 can also be any other dielectric compound, and can be a combination of dielectric materials. Dielectric layer 221 can range in thickness from about 20 angstroms to about 50 angstroms, and is preferably at least 15 angstrom thick. Conformality of +/−20% is desirable, but can be more relaxed as long as no substantially weak spots exist in the dielectric film which could cause premature breakdown in operation. FIG. 3B illustrates a cross section at cut ‘ 3 B’, if cavity 210 is a pore.
[0017] FIG. 4A shows first conductive layer 231 formed over dielectric layer 221 . First conductive layer 231 is preferably a conformal layer, which can be a metal layer and can be formed by known processing such as ALD. Second dielectric layer 222 is formed over first metal layer 231 . A second conductive layer 241 can be formed over second dielectric layer 222 . Like the first conductive layer, the second conductive layer 241 can be formed of metal. Reference throughout the following description to ‘metal’ refers to any conductive material.
[0018] The sequence of dielectric, first metal, dielectric, and second metal can be repeated numerous times. For example, repeating n=four times would produce a structure with n+1=5 first metal layers interleaved with 5 second metal layers, with dielectric separating adjacent metal layers. The stack can be completed, after repeating the first four layers as desired (or not repeating even once), by depositing a final dielectric layer that fills any remaining space within cavity 210 . Such a final stack would have an equal number of first and second metal layers. Alternatively, after forming just the first four layers, or after repeating the four-layer sequence ‘n’ times, the stack can be completed by depositing another dielectric layer ( 223 in FIG. 4A if n=0), then a final first metal layer ( 232 if n=0), and finally a final dielectric layer ( 224 if n=0) that fills any remaining space within cavity 210 . The stack in such an embodiment would have 1+n second metal layers and would have 2+n first metal layers. FIG. 4B is a cross section at cut 4 B for a pore-type embodiment at an intermediate stage after depositing dielectric 223 onto second metal layer 241 .
[0019] The thickness of the metal is determined by structural integrity of the metal and the conductivity requirement as well as the number of layers desired and the dimension of the cavity. Typical thickness ranges between 50 angstroms and 500 angstroms with 100 A to 200 A being the preferred thickness. The metal layers can be deposited with typical conformal thin film deposition techniques. For cavities with high aspect ratios, ALD can be the preferred technique. Conformality of +/−50% is desirable but the metal layers do not necessarily need to be free of thin spots.
[0020] FIG. 5A illustrates just three metal layers (i.e., n=0), but the MIM capacitor according to the present invention can have many more metal layers. The simple MIM capacitor of FIG. 5A has two first-type metal layers 231 and 232 , one second metal layer 241 , and four dielectric layers 221 , 222 , 223 , and 224 . All dielectric layers of the present MIMCAP can be the same dielectric material, or some or each dielectric layer could comprise different dielectric materials. Similarly, all dielectric layers can be formed according to the same process, but the invention is not so limited. All first-type metal layers can be, but are not necessarily, the same material, so long as all of the first-type metal layers can be selectively etched relative to all the second-type metal layers. Similarly, all second-type metal layers can be, but are not necessarily, the same material, so long as all of the second-type metal layers can be selectively etched relative to all the first-type metal layers. FIG. 5B illustrates a cross section at cut ‘ 5 B’ of a pore embodiment having four metal layers, two being first-type metal layers 231 and 232 and two being second-type metal layers 241 and 242 . Five dielectric layers 221 , 222 , 223 , 224 , and 225 isolate each metal layer from the next adjacent metal layer or from the substrate 201 . The last dielectric layer 225 fills the cavity inner core.
[0021] As noted, the materials of the first-type and second-type metal layers are selected such that a first selective etch recesses just one set (ie, all the first-type or all the second-type metal layers) and a second selective etch recesses just the other set. Some selective etch rates are listed in Hussein, et al., Metal Wet Etch Process Development for Dual Metal Gate CMOS, Electrochemical and Solid-State Letters, 8 (12) G333-G336 (2005). As one example, the first-type metal layers could be formed of PVD TiN and the second-type metal layers could be formed of PVD TaSiN (Si-30%), and the first and second etches could be SC2 and HF. SC2 chemistry (DI:H2O2:HCl at a ratio of 10:1.1:1) at 60C can etch TiN at 10 A/min while only etching TaSiN at 0.01 A/min, whereas HF chemistry (H2O:HF) at a ratio of 50:1 at 60C only etches TiN at 1.32 A/min while etching TaSiN at 33.6 A/min. An alternative HF etch could be H2O:HF at a ratio of 10:1 at 25C, which only etches TiN at 2.47 A/min while etching TaSiN at 50.3 A/min. The metal materials and etch chemistries can be selected according to design requirements. In preferred embodiments, all first-type metal layers (whether or not formed of the same metal composition) be selectively etched by a single etch step (a “first etch”) that substantially does not etch the second-type metal layers, and all second-type metal layers (whether or not formed of the same metal composition) be selectively etched by a single etch step (a “second etch”) that substantially does not etch the first-type metal layers.
[0022] After depositing the complete sequence of layers, the structure can be planarized and polished as per FIG. 6 . This step can be achieved using chemical mechanical polish (CMP). Each layer of the MIM stack can have a portion extending generally parallel to the sidewalls of cavity 210 . Thus removing all overburden down to the substrate surface can expose a cross section of the stack, exposing an edge of every layer of the MIMCAP stack.
[0023] A mask layer 250 can be deposited and patterned to expose a first electrode region 251 of the planarized surface, which region can extend from the cavity sidewall to the last (innermost) dielectric layer. So long as the first electrode region extends in a first direction to expose an edge segment of each metal layer of the first type (or each metal layer of the second type), then a selective etch can recess all the first-type ( 23 x ) metal layers (or all the second-type metal layers), without significantly effecting the other set. FIG. 7A illustrates a first selective etch to recess the edge of first-type metal layers 23 x exposed within region 251 . A cross section of the structure of a pore embodiment of FIG. 7A at cut ‘ 7 B’ is shown in FIG. 7B .
[0024] After removing first mask 250 , which can be by a conventional resist strip process, a second mask 260 can be deposited and patterned to expose a second electrode region 262 of the planarized surface Like the first electrode region, the second electrode rejoin can encompass the full set of second-type metal layers and can be patterned by a single mask. So long as it extends to expose an edge segment of each layer of the heretofore not-etched metal layer set, e.g., the second electrode region can extend from the cavity sidewall to the last (innermost) dielectric layer, then a second selective etch can recess those metal layers 24 x not etched by the first selective etch. As shown in FIG. 8B , the second electrode region can be opposite the first electrode region, but this relative position is not required. The second electrode region can be located per convenience of the process integration. It can, e.g., be adjacent the first electrode region. In preferred embodiments there is no overlap of the first and second electrode regions.
[0025] FIG. 8A shows second metal layer 241 recessed by the second selective etch, and a cross section of the structure of a pore embodiment of FIG. 8A at cut ‘ 8 B’ is shown in FIG. 8B . Note that if the MIM stack had more layers, for example, with three second metal layers, then all three could be exposed by a single ‘second electrode mask’, and all three could be recessed simultaneously by a single ‘second selective etch’ step. In some embodiments, the substrate can constitute a plate of the MIMCAP. If the substrate constituted part of the ‘second-type’ plate of the ultimate capacitor structure, one option would be to recess the substrate within the second electrode region, but another option would be to pattern the second electrode (as described in conjunction with FIGS. 10A and 10B ) such that it did not extend over the substrate.
[0026] As illustrated in FIG. 9A , a dielectric material 270 can backfill the recesses formed by the two selective etch steps. Appropriate dielectric materials include oxide, nitride, or amorphous carbon. After removing excess dielectric 270 , such as by CMP, the MIMCAP electrodes can be formed. According to one embodiment, a conductive film 280 can be formed over the wafer, such film in conductive contact with the exposed metal layers of the MIMCAP and extending over the substrate surface. FIG. 9B illustrates that conductive film 280 can extend over dielectric regions 270 to avoid conductive contact with corresponding metal layers. A patterning step can form a first electrode 281 that is in contact with all second-type metal layers 24 x (and no first-type metal layers) and a second electrode 282 that is in contact with all first-type metal layers 23 x (and no second-type metal layers) as illustrated in FIG. 10A and FIG. 10B . For example, continuing with the embodiment illustrated by FIGS. 7 and 8 , the first electrode 281 can contact the MIMCAP stack only within the first exposed region 251 so that electrode 281 connects all second metal layers but is insulated from all first metal layers by the dielectric that backfilled the recesses formed by the first selective etch. And the second electrode 282 can contact the MIMCAP stack only within the second exposed region, whereby electrode 282 connects all first-type metal layers but is insulated from all second-type metal layers by the dielectric backfill in the recesses formed by the second selective etch. If the substrate constituted a plate of this MIMCAP, then electrode 281 could be formed to connect all second-type metal layers with the substrate plate, and electrode 282 could be trimmed such that it contacts all first-type metal layers and does not contact the substrate plate.
[0027] Although the invention has been shown and described with respect to a certain preferred embodiment or embodiments, certain equivalent alterations and modifications will occur to others skilled in the art upon the reading and understanding of this specification and the annexed drawings. In particular regard to the various functions performed by the above described components (assemblies, devices, circuits, etc.) the terms (including a reference to a “means”) used to describe such components are intended to correspond, unless otherwise indicated, to any component which performs the specified function of the described component (i.e., that is functionally equivalent), even though not structurally equivalent to the disclosed structure which performs the function in the herein illustrated exemplary embodiments of the invention. In addition, while a particular feature of the invention may have been disclosed with respect to only one of several embodiments, such feature may be combined with one or more features of the other embodiments as may be desired and advantageous for any given or particular application.
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An improved semiconductor capacitor and method of fabrication is disclosed. A MIM stack, comprising alternating first-type and second-type metal layers (each separated by dielectric) is formed in a deep cavity. The entire stack can be planarized, and then patterned to expose a first area, and selectively etched to recess all first metal layers within the first area. A second selective etch is performed to recess all second metal layers within a second area. The etched recesses can be backfilled with dielectric. Separate electrodes can be formed; a first electrode formed in said first area and contacting all of said second-type metal layers and none of said first-type metal layers, and a second electrode formed in said second area and contacting all of said first-type metal layers and none of said second-type metal layers.
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CROSS REFERENCE TO RELATED APPLICATIONS
This is a non-provisional application based upon U.S. provisional patent application Ser. No. 61/818,102, entitled “COUNTER KNIFE BANK DEBRIS DEFLECTOR”, filed May 1, 2013, which is incorporated herein by reference.
FIELD OF THE INVENTION
The present application relates to chopper assemblies for a combine and more specifically to a system in which debris is deflected from the counter knife bank assemblies used in such combines.
DESCRIPTION OF THE RELATED ART
Harvesting equipment such as agricultural combines frequently use integral chopper assemblies or systems to transport material away from the threshing system and also to treat the material by further cutting. It is frequently necessary to employ a residue chopper assembly that has a rotary chopper apparatus disposed within the combine housing and extending generally transverse across the path of the crop residue. A chopper grate assembly extends along the rotary chopper apparatus and has a plurality of slots through which knives attached to a counter knife bank apparatus adjustably project. The interaction between the rotary chopper and the counter knife bank apparatus cuts and reduces the size of the crop residue. In order to accommodate variable field and/or crop conditions it is necessary to provide a variation in the degree to which the knives of the counter knife bar apparatus extend through the slots in the chopper grate. The knives, when fully inserted through the slots in the chopper grate, produce a fine consistency to the chopped crop residue whereas the retraction of the knives from the slots produces a coarser consistency.
The harvesting and threshing process produces a great deal of crop residue which is accelerated through the combine and propelled rearward by the crop processing system (rotor) used in the processing of the crop material. Since the rotary chopper assembly is at the downstream end of the path of the crop residue, it is fully impacted by the debris carried around in the flow path through the combine. It has been found that the debris particularly collects adjacent the slots on the chopper grate and can span the space adjacent the leading edge of the knife elements used in the counter knife bar apparatus. The accumulation of the debris across the slots prevents free movement of the counter knife bar apparatus and requires frequent cleaning of the mechanism. Depending upon the configuration of the combine the cleaning process can be particularly complicated.
What is needed in the art therefore, is a chopper assembly in which debris is prevented from accumulating in the area between the chopper grate and the counter knife bar apparatus.
SUMMARY OF THE INVENTION
The invention seeks to provide a mechanism for preventing debris from accumulating between the chopper grate and the counter knife bar assemblies.
The invention, in one form, is a chopper assembly for harvesting equipment including a rotary chopper device and a chopper grate assembly spaced from the rotary chopper device to form a passage way for crop residue. The chopper grate assembly includes a plurality of slots extending in the direction of crop residue flow through the passageway. A knife bank assembly includes a plurality of knife elements aligned with and insertable in the slots. The knife bank assembly is displaceable toward a position where the knife elements are fully inserted through the slots into the passageway and a position where they are substantially clear of the passageway. A deflector is provided for covering the slots with the deflector being displaceable with the knife elements to uncover the slots as the knife elements are displaced through the slots and into the passageway.
The invention, in another form, is an agricultural combine with a crop processing apparatus to separate desired crop material from residue and a chopper assembly for receiving crop residue. The chopper assembly includes a rotary chopper device and a chopper grate assembly spaced from the rotary chopper device to form a passageway for crop residue. The chopper grate assembly includes a plurality of slots extending in the direction of crop residue flow through the passageway. A knife bank assembly includes a plurality of knife elements aligned with and insertable in the slots. The knife bank assembly is displaceable toward a position where the knife elements are fully inserted through the slots into the passageway and a position where they are substantially clear of the passageway. A deflector is provided for covering the slots with the deflector being displaceable with the knife elements to uncover the slots as the knife elements are displaced through the slots and into the passageway.
The invention, in yet another form, is a chopper assembly for harvesting equipment including a blower for processing crop residue and a rotary chopper device with a chopper grate assembly spaced from the rotary chopper device to form a passageway for crop residue. The chopper grate assembly includes a plurality of slots extending in the direction of crop residue flow through the passageway. A knife bank assembly includes a plurality of knife elements aligned with and insertable in the slots. The knife bank assembly is displaceable toward a position where the knife elements are fully inserted through the slots into the passageway and a position where there are substantially clear of the passageway. A deflector is positioned to direct flow of air from the blower to the vicinity of the slots and the knife elements extending through the slots.
BRIEF DESCRIPTION OF THE DRAWINGS
The above-mentioned and other features and advantages of this invention, and the manner of attaining them, will become more apparent and the invention will be better understood by reference to the following description of embodiments of the invention taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a side view of a combine incorporating a chopper assembly embodying the present invention;
FIG. 2 is a fragmentary perspective view of the chopper assembly of FIG. 1 ;
FIG. 3 is a side view of the chopper assembly of FIG. 1 in a first position;
FIG. 4 is a side view of the chopper assembly of FIG. 1 in a second position; and
FIG. 5 is a side view of a chopper assembly incorporating an alternate embodiment of the present invention.
FIG. 6 is a side view of a chopper assembly incorporating another embodiment of the present invention
Corresponding reference characters indicate corresponding parts throughout the several views. The exemplifications set out herein illustrate embodiments of the invention and such exemplifications are not to be construed as limiting the scope of the invention in any manner.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows an agricultural combine 20 which includes the usual harvesting apparatus (not all of which is shown to facilitate an understanding of the invention). An axially oriented crop processing system 22 receives harvested crop and a crop residue treatment and distribution system 24 with a crop residue spreader 26 is positioned at the aft end of combine 20 . The crop processing system includes a cylindrical threshing rotor 28 that conveys a flow of crop material in a helical flow path. As the crop material is moved through the processing apparatus 22 , the desired crop such as grain or other material is loosened and separated from crop residue such as husk and pods in a cleaning system located beneath the threshing rotor 28 . The crop processing system 22 includes a blower 34 , schematically depicted to aid in the separation of the desired crop from the crop residue. The blower 34 has a duct 35 extending aft in the combine 20 towards the cleaning system and the crop residue treatment and distribution system 24 .
Existing crop residue systems provide the ability to variably chop the crop residue but encounter the problems of crop residue plugging the adjustable apparatus. In accordance with the present invention, the crop residue treatment system 24 shown in FIGS. 2-4 minimizes, if not eliminates, plugging by crop residue material.
As specifically shown in FIG. 2 , crop residue treatment system 24 includes a rotary chopper device 50 which includes a central rotor extending transverse to the flow of crop material and which supports a plurality of knives 52 , only two of which are shown. Details of such a rotary chopper device may be found in U.S. Pat. No. 8,141,805, of common assignment with the present invention, which is hereby incorporated in its entirety. Rotary chopper device 50 has adjacent thereto a chopper grate assembly 56 which is formed from sheet material extending substantially the same length as that the axial length of the rotary chopper device 50 . The chopper grate assembly 56 is generally cylindrical in form and defines, with the rotary chopper assembly 50 , a flow path 58 for crop residue material flowing in direction A. Chopper grate 56 has a plurality of slots 60 arranged in side-by-side relation across the width of the crop residue treatment system 24 . Slots 60 extend in a direction that is generally parallel to the direction of flow A for the crop residue material.
A knife bank assembly 62 is positioned adjacent the chopper grate 56 and includes a plurality of knife elements 64 , only a portion of which are shown that are positioned to be inserted through slots 60 and into flow path 58 in between the knives 52 of rotary chopper device 50 . Individual knife elements 64 are fixed to mounting frames 66 by removable fasteners 68 . Knife mounting frames 66 are all fastened to a main cross frame 70 extending across the length of the crop residue treatment system. Cross frame 70 includes a first section 72 providing a support for knife supports 66 and an integral second section 74 bent with respect to the plane of section 72 . Section 72 has brackets 76 affixed thereto that have holes through which bolt assemblies 78 extend to provide a pivotal mounting for knife bank assembly about axis B. Knife bank assembly 62 is pivotally displaced by a crank arm 80 shown in dashed lines that has an inner end and arranged to be pivotal about axis B and an outer end receiving an actuating arm 82 also shown in dashed lines. The translation of actuating rod 82 manually or by an actuator causes crank arm 80 to pivot the knife bank assembly 62 from the positions shown in FIGS. 2 and 3 to the position shown in FIG. 4 in which the knife elements 64 fully extend into flow path 58 through slots 60 .
In existing crop residue treatment systems, debris accumulates in the generally triangular area between the leading edge of knife elements 64 and the outer face of grate assembly 56 . In accordance with the present invention, a deflector 84 shown in FIGS. 2-4 is employed to minimize, if not eliminate, accumulation of crop residue in the above-mentioned space. Deflector 84 is formed from flexible sheet material with sufficient stiffness to provide a resilient abutment on the outside of chopper grate 56 . Although one material may be stainless spring steel, it should be apparent to those skilled in the art that other materials may also be employed. Deflector 84 extends across the width of the crop residue treatment system 24 and has a first section 86 affixed to section 74 of cross frame 70 . Section 86 is secured with removable fasteners to enable replacement and fabrication although these fasteners are not shown to simplify the understanding of the present invention. Section 86 of deflector 84 continues to a second section 88 and a bend into a further section 90 and finally through an additional bend to a final section 92 that in its free state is generally contoured to fit the approximately cylindrical outer contour of chopper grate 56 . As illustrated in FIG. 2 , the trailing edge 94 of section 92 abuts the leading edge of knife elements 64 so that when the knife elements 64 are in the position shown in FIGS. 2 and 3 , the slots 60 are substantially covered. By covering the slots 60 in this position, the accumulation of crop residue debris through and around the slots is substantially minimized. It should be noted that the trailing edge 94 of section 92 may extend beyond the leading edge of knife elements 64 by providing a notch for even further coverage.
As the knife bank assembly 62 is rotated to cause the knife elements 64 to be inserted through slots 60 and into the flow area 58 , the trailing edge 94 of the deflector 84 moves with the leading edge of knife elements 64 to maintain a cover or deflector over the slots 60 to the extent that the slots 60 are not receiving a portion of the knifes 64 . Because deflector element 84 is resilient sheet material, it will bend and conform to the shape of the chopper grate 56 throughout the pivoting displacement of the knife bank assembly 62 . By placing the bend between the sections 88 and 90 in deflector 84 , the trailing edge 94 of deflector 84 is circumferentially displaced along the exterior of chopper grate 56 . This allows a smoother transition between the positions shown in FIG. 2 and the one in FIG. 4 . The deflector 84 may be formed in a plurality of sections abutting one another extending along the width of the crop residue processing system 24 or it may be formed in a single unit so long as the slots 60 are covered and uncovered as stated above.
As specifically shown in FIG. 3 , a plurality of hook elements 96 , only one of which is shown in dashed line, may be employed adjacent the trailing edge 94 of deflector 84 to drag with them any material that may have accumulated in adjacent the leading edge of knife elements 64 to further enhance the process of eliminating debris.
By providing the deflector 84 , the accumulation of any debris that impedes the pivoting movement of the knife elements through the slots and into the flow path 58 is substantially minimized. This enables freer operator movement to adjust the crop residue processing system 24 to accommodate varying crops and field conditions. Furthermore, it makes operation more efficient in that it minimizes down time for cleaning
FIG. 5 shows an alternate embodiment of the present invention in which the same basic crop processing elements are present (using the same reference characters as in FIGS. 2-4 ) but without the deflector 84 . FIG. 5 shows the knife elements 64 in position out of the flow path 58 during which debris can accumulate. In accordance with this aspect of the present invention, there is provided a deflector 98 consisting of a sheet metal deflector bringing air flow C from blower 34 and duct 35 into the region 100 between the leading edge of knife elements 64 and the outer circumference of grate assembly 56 . The accelerated flow of air into the region 100 by virtue of deflector 98 causes any debris that resides in the area to be blown away. Since the blower 34 is operated continuously, the cleaning process takes place continually.
FIG. 6 shows yet another embodiment of the invention. In this view, a grate assembly 102 has the plurality of slots as in the previous embodiments through which a plurality of knife elements 104 (only one is shown) extend. The rotary chopper assembly shown in FIGS. 2-5 is omitted to enable a clearer understanding of this aspect of the present invention. The passage for crop residue is adjacent the upper face of the grate assembly 102 .
Knife elements 104 are releasably fastened to blade supports 106 which are in turn fastened to a cross frame 108 . Frame 108 is pivotally mounted to grate assembly 102 at 110 . A crank arm 112 receives displacement inputs from a rod 114 to pivot frame 108 and blade elements 104 to variably extend through the slots in grate assembly 102 . As shown in FIG. 6 , the knife elements 104 are pivoted to be out of the crop residue passage. The blade elements 104 may be pivoted to a position where they are totally extended through the slots in grate assembly 102 and into the passageway adjacent its upper face.
In accordance with another aspect of the present invention, a deflector 116 is employed to minimize, if not eliminate the buildup of debris between the slot in the grate assembly 102 and the leading edge of the blade elements 104 . Deflector 116 includes a continuous sheet 120 having an arc contour and which is fixed to frame 108 at 118 . Sheet 120 curves around to abut the bottom face of grate assembly 102 and has slots 122 for embracing opposite faces of the blade elements 104 . Sheet 120 ends in trailing edge hook elements 124 that variably extend across the faces of blade elements 104 as they are pivoted into the passageway.
A curved guide 126 is fastened to a flange 128 integral with grate assembly 102 by fasteners 130 . The curved guide 126 directs sheet 120 in a path that facilitates following the outer contour of grate assembly 102 . Guide 126 also provides a barrier against debris entering the space between the slots in guide assembly 102 and the leading edge of blade elements 104 .
In operation, the sheet 120 covers slots in the grate assembly 102 and moves with the pivoting the cross frame 108 to keep debris away. In addition, hook elements 124 provide a cleaning away of debris as the knife elements 104 are pivoted into the slots in grate assembly 104 .
While this invention has been described with respect to at least one embodiment, the present invention can be further modified within the spirit and scope of this disclosure. This application is therefore intended to cover any variations, uses, or adaptations of the invention using its general principles. Further, this application is intended to cover such departures from the present disclosure as come within known or customary practice in the art to which this invention pertains and which fall within the limits of the appended claims.
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A chopper assembly for harvesting equipment including a rotary chopper device with a plurality of knives and a cylindrical chopper grate assembly spaced from the rotary chopper to form a passageway for crop residue. The chopper grate assembly includes a plurality of slots extending in the direction of crop residue flow. A knife bank assembly includes a plurality of knife elements aligned with and insertable in the slots with the knife bank assembly being displaceable toward and between a position where the bank knife elements are fully inserted through the slots into the passageway and a position where they are substantially clear of the passageway. A deflector is provided for covering the slots and the deflector is displaceable with the knife elements to uncover the slots as the knife elements are displaced through the slots and into the passageway.
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FIELD OF THE INVENTION
[0001] This invention relates to the distribution of musical compositions and the like, and associated advertising and identification, and particularly to the distribution of such materials over secure networks.
BACKGROUND OF THE INVENTION
[0002] U.S. Pat. No. 5,734,719 issued Mar. 31, 1998 to Tsevdos et al. discloses a digital on-demand system which allows information, such as music, to be reviewed in real time at a station by a customer and then allows selected information to be recorded on a transportable medium at the request of the customer for his purchase and carrying away. The design features are not economically feasible because of the elaborate equipment required at the reviewing station.
[0003] U.S. Pat. No. 5,790,935, issued to David W. Payton on Aug. 4, 1998, relates to a system to overcome the limitations of bandwidth and allow substantially on-demand digital information, such as a movie, to a subscriber. A profile of the user is kept and programs which will fit the user's profile are delivered over broadband transmission lines at off peak times to a local storage device maintained by the individual. This reduces the demand at peaks times, since most of the programs the user may demand are in the local storage, and only occasionally will it be necessary to access the broadband capabilities to comply with the user request.
[0004] Another form of the prior art is the MP3 system utilizing the Internet for downloading musical works. By this system, musical works are made available at a web site and can be downloaded to a computer hard drive or can be directly transferred to a compact disk (“CD”), such as a mini-disk. A good discussion of such a system appears in Fortune Magazine of Feb. 7, 2000, at page 194. This description relates to downloading music from the Internet and recording it on a small disk, which can then be inserted into a portable player. It utilizes a Voquette NatLink Adapter for transferring the audio to a mini-disk. Voquette has software which allows the user to drag different audio chips into a basket for transmission. The disadvantages of the system are that the recorded quality is poor and substantial time is required for recording.
[0005] It is evident that the use of digital networks for transporting commercial quality media carries the potential of significantly reducing expenses and inefficiencies relating to issues such as media duplication, storage, shipping, broad-based availability and meeting unexpected distribution needs.
[0006] The music distribution system is under extreme economic pressures. There is an endless variety of music compositions available and the tastes of customers can vary widely, from classical to the latest vogue. For this reason, the economic problems for a music retailer are enormous because of the cost involved in maintaining large inventories. The publisher has to undertake considerable expense to promote the music pieces. Some publishers allow the return of unsold compositions, which then raises economic problems for the publishers. Because of the inventory problems and return possibilities, it becomes extremely difficult to promote new music compositions by lesser known or unknown artists where a market is not assured. The advent of the Internet and the distribution of music compositions over the Internet to customers has been an immense competitive problem to retailers as well as to publishers.
SUMMARY OF THE INVENTION
[0007] In accordance with the invention, a plan is provided to drastically enhance media selection and distribution, dramatically reduce media inventory problems of dealers, promote sales by publishers of large varieties of music compositions and provide customers with quality renditions of both music and video media compositions. This result is achieved with a series of publisher-owned database system (“POD System”) servers that broadcast digital information over a broad bandwidth digital transport network to a large number of area media production systems (“AMPS”) or the like. Each AMPS site is provided with local data storage facilities, equipment to duplicate music compositions on a portable media, such as a CD-writer, and a printer to duplicate labeling and advertising material to be inserted, either manually or automatically, into a media carrying case with the duplicated music or video composition.
[0008] The customer is given the opportunity to listen to at least portions of music compositions so he or she can make a selection. This can be accomplished over unsecured telephone lines by the use of the Internet, or by way of a wireless handheld device. This significantly enhances the number of locations for accessing the publisher's media availability, and allows for browsing and purchasing of a broad variety of media. It also eliminates the limitations set by retail preview screens reducing loading and reliance of prior art on limited locations of private bandwidth transmission networks. In addition, with the design enhancement of a wireless browsing access feature, an Internet-compatible wireless device could now access a POD System location and order media for customer pick-up at an AMPS site. A customer could also preview/browse selections from a wireless device from any location.
[0009] After the music composition is selected and ordered, the POD System begins the transfer procedure of the files of the composition(s) selected from its data-bank computer to the AMPS site serving the customer request. The POD System identifies, in its own database, if the media being purchased is already presently cached in the database of the AMPS location serving the customer order. If the POD System file shows that the media files requested do exist in the AMPS on-site database, the POD System sends a command authorization, along with customer order certification information, to the AMPS site to authorize the duplication of the media that has been purchased. If not, then the music composition is transferred to the AMPS site for storage and duplication. The POD System also sends purchase identification information to the AMPS site and the requested point of distribution for customer pick-up. The music composition is then quickly transferred to a portable medium, such as a CD or tape, utilizing a duplicating apparatus at the dealer location. Such device, as an example, can be a CD-writer. Associated with the music transmission is the transmission of labeling, advertising and identifying material which can be passed to a printer. maintained by the dealer, and then inserted into the portable medium containing the selected music composition.
[0010] As is apparent, AMPS sites may serve media production for several retail outlets in a given area. An AMPS site may be located in a media distribution point in a particular area being served. Further, the economics to the publisher in not having to maintain an inventory is desirable. As to authors and performers of musical compositions, it enables the customer to be exposed to music compositions which would not normally be available because of the economic limits on publishers.
[0011] As indicated, in accordance with the invention, music and video compositions are provided through the use of private digital or packet-type network connections for transmission from one of several POD System locations over a switched synchronous private network or equivalent connections to an AMPS site. The media work and any associated labeling and publicity materials is automatically downloaded for the POD System to the appropriate AMPS site for duplication. The material received from the publisher is digitally stored, copied, compressed and catalogued.
[0012] The works are downloaded through the digital network connection using a switched synchronous private network to the appropriate AMPS site or satellite location. When a work is requested by a customer, the downloading system automates the file query and transfers the necessary media files to the AMPS site where the work is burned onto a portable storage device, such as a CD or equivalent. The appropriate label or album presentation is downloaded at the same time, printed and applied on the CD, at the AMPS site, either automatically or manually.
[0013] As is apparent, one of the advantages of the present invention is that the system materially reduces the expenses of traditional media distribution. The AMPS and media outlet sites can operate in a very small space, which would materially reduce the overhead for both publishers and dealers and also allow such outlets to be placed in areas not previously available to dealers. Payment is made by credit card directly to the POD System with immediate tracking and division with the AMPS site and the appropriate area outlet(s). In addition, the retail outlet location(s) can take over the credit card procedure either in its own operations or by arrangement with the charge card system on direct wholesaled inventory it has had produced through the area AMPS site. A typical payment system is shown in U.S. Pat. No. 5,724,424, issued Mar. 3, 1998 to David K. Gifford, which can be applied to either or both of the customer and the dealer.
[0014] Another of the advantages of the invention is that two types of franchises can be created for exclusive areas. One type of franchise would be for area AMPS sites. The other would be for retail outlet and distribution sites. The AMPS site franchises would provide a portion of the high-speed private digital connection. The equipment for operating the AMPS site could be purchased or leased from a certified AMPS provider.
[0015] These and other objects and the advantages of the invention will be apparent to those skilled in the art from the following detailed description of preferred embodiments, taken together with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] For the purpose of illustrating the invention, there is shown in the drawings forms which are presently preferred. It should be understood that the invention is not limited to the precise arrangements and instrumentalities shown.
[0017] [0017]FIG. 1 is a diagram of an overview of the system.
[0018] [0018]FIG. 1A is a diagram of the domestic system architecture in accordance with the invention;
[0019] [0019]FIG. 2 is a diagram showing deployment and network architecture of multiple POD and AMPS locations in the domestic system in accordance with the invention;
[0020] [0020]FIG. 3 is a diagram of an international system in accordance with the invention;
[0021] [0021]FIG. 4 is a diagram of a satellite system in accordance with the invention;
[0022] [0022]FIG. 5 is a diagram of the architecture of the media vending device in accordance with the invention;
[0023] [0023]FIG. 6 is a diagram of the media vending device showing associated networks and POD location(s);
[0024] [0024]FIG. 7 is a dimensional view of the vending apparatus that may be used in public environments such as malls and arcades;
[0025] [0025]FIG. 8 is an elevated drawing showing the discharge and insertion of CDs; and
[0026] [0026]FIG. 9 illustrates a printer and associated receptacle.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0027] Reference is made to FIGS. 1, 1A and 2 of the drawings. A typical system would perform as follows: Pre-recorded music is obtained from the publisher and stored in digital, compressed, possibly encrypted, files in a central database 22 . Each AMPS site is provided with a local caching storage device 24 for retaining any information downloaded for a period of time. Short forms of each composition are selected 26 and are available to allow the customer to preview a music or video composition from the POD System they have accessed from their browser terminal. Any POD System will allow a customer to preview a music composition and order media from a typical PC or other Internet access terminal device through a standard browser Internet connection. The sampling, since it does not require quality reproduction, can be carried over a secure SMDI connection from a POD System over the Internet. The customer makes the selection of the music composition to be purchased by making a menu selection, such as with the use of a point-and-click function on a personal monitor, or by utilizing any other compatible selection method available, such as a wireless handheld device.
[0028] The POD System storage device 22 routes the customer to a sample media file for an abbreviated preview of the album requested or of a single selection if made available in that form by the POD System. After a pre-viewed or non-previewed selection has been ordered, the POD System processes and validates the customer credit card transaction based on credit data entered via the customer's Internet terminal connection. The POD System then, within its own data files, determines if the selection being ordered is still cached in the AMPS site that will be used for the production transaction of the media. If it is not available at the AMPS site, the POD System automatically transfers the necessary encrypted files over the high-speed secured digital network to the AMPS site. The downloaded composition is retrieved at the AMPS site and then decompressed and decrypted, if applicable, 42 and recorded on a CD 44 or similar recording medium, i.e., mini-disk, at the AMPS site location. The AMPS files include instructions to a printer 46 which prints out the label and any additional advertising or label information. The paper feed to the printer can be special stock, such as aluminum-coated paper. The AMPS site is equipped to test and validate the commercial production audio or video quality that has been recorded on the CD or DVD. The portable media is placed in the quality test unit 47 . The unit then samples media from the CD 48 and displays quality levels on the AMPS site terminal 50 . The printer label can be automatically applied to the CD and other printed literature inserted into the CD case 52 , or these functions can be done manually. A similar procedure is utilized for transferring other audio information for recording on the CD. A diagram showing one form of this system appears at A in FIG. 1A. A similar system for video transmission is at B in FIG. 2.
[0029] As a collateral, a sales promotion can be added where a customer replies to a questionnaire indicating what type of music is preferred and works coming with the selected categories are downloaded to a mailbox on a daily or weekly basis utilizing the Internet. The potential customer can call into the mailbox and review the works for potential purchase. The same system can be utilized to supply streaming music to a commercial location, such as a radio station, for immediate playback or recording for later play.
[0030] Each specific AMPS site has file capacity for retaining from 10,000 to 50,000 of the most current popular selections being requested. This file storage will continually and automatically maintain a relatively current popularity status based on the current frequency of the most popular selections being requested. This data-caching feature will eliminate the necessity repeat downloads of encrypted data files to an AMPS site each time a musical or video work is needed for production after the purchase transaction is completed at the POD location. This feature reduces network traffic loading, bandwidth requirements and improves system efficiency.
[0031] The POD System can be used for tracking commercial utilization of recorded music or recorded performances for royalty and marketing information. A unique, universally-standardized code ID number can be incorporated into each recording at the point where the original customer copy is manufactured. The coding is encrypted into the digital format and is transparent to the reproduction of the musical piece and to the end user. The encrypted ID number can then be read by supporting software before being aired by a radio station. The unique universal ID of each song aired is stored in a database file at the station location at the time of performance. Performance royalties societies, such as ASCAP, can then remotely poll those performance files and determine performing royalties settlements for the artists and for demographic popularity information.
[0032] It is evident that the use of digital networks for transporting commercial-quality media carries the potential of significantly reducing expenses and inefficiencies relating to issues such as media duplication, storage, shipping, broad-based availability and meeting unexpected distribution needs. In application to international distribution, the music is prerecorded and international locations have been authorized to operate under direct business franchises.
[0033] The system can utilize satellites as shown in FIG. 4. The system can be utilized internationally, as shown in FIG. 3. For this illustration, five countries are illustrated—the US, England, Scotland, Ireland and Germany. Each of these database locations, as well as their U.S. counterpart, will be configured with separate cultural music partitions to store the music unique to each country. This type of filing structure will expedite search and find speeds when a browser is querying for one of these particular categories of music.
[0034] The main database location is operational in the U.S. The U.S. database can be enhanced to include partitioned files to store each cultural type of music used in the example. A typical small scale system, for example, would be a system for Ireland and Scotland. Each of these systems will be sized and designed similar to a large U.S. retail operation with a storage capacity of 50,000 to 70,000 songs. Each system is given CD- and MP3-reader capabilities for reading, compressing and storing local music files in the system for sale in that country. These local music files will then be packetized and bursted to the U.S. database over a switched digital network for national electronic distribution and sale. The system is equipped with CD-burner and MP3-recorder capabilities for making local copies and is equipped with all necessary system administration database functions. The system is loaded with selected music and documentation files before shipping. Each machine will have its own cultural music file partitions.
[0035] The system illustrated for England and Germany is sized and designed to operate as a small main type database location and serve as the hardware and software platform for one retail operation. It is contained within that initial store location. The storage capability of these systems can be modally expandable to house a considerably larger scale database if needed.
[0036] The hardware and software is configured to function as the central database location for the small infrastructure of that country's music distribution. High-speed E-1 digital connectivity is one type of network that could be used between sites. E-1 is the European equivalent of the North American standard T-1. It provides a slightly wider digital bandwidth capacity.
[0037] Sales and marketing tracking is an integral and required part of the integrity and operation of the international sales system. A sales tracking, marketing authorization software application is incorporated in the architecture of all main or primary database locations. Each satellite location that is functioning as a primary database location will store the “SMART” data information for the retail sites it serves. One central database location will be synchronized to poll the stored “SMART” tracking data from each designated primary database location. Each satellite site can, as an example, have a 60-day caching system for the sales files that act as an off-site back-up for the main database system.
[0038] Each musical composition, whether international or domestic, when loaded into the POD System will be automatically assigned a unique “Media, Inc.” classification and tracking number. This number resides in the original compressed file along with the musical selection. Each time the music file is requested at a POD System location, the following information is logged into the accounting summary file of the primary database: Music file number, selection name, site number requesting download and customer profile, site date and time stamp, and related purchase receipt number. This allows the “SMART” software to accurately identify and log each sales transaction associated with each selection or album, and enable the accounting capabilities that summarize royalty and settlement compensations due.
[0039] The model offers constant, available bandwidth to all sites at all times over a private synchronous network. This design permits unlimited large-scale selection availability and immediate delivery. Switched digital network resources found in the domestic environment allow such bandwidth availability to be economically feasible.
[0040] In similar ways, the switched digital application found in the international network optimizes the economic efficiencies of an international digital network. This is the most cost-effective way to transfer digital data internationally via private network architecture. However, this application imposes economic limitations that are not conducive to small data file bursts that would characterize typical transactions taking place within our domestic network model.
[0041] The limiting distinction is that this network applies a circuit set-up charge to the user each time an end-to-end “switched” connection is requested through the cloud and a time-of-day rate based on the time at the point of origination. That is, each time an originating end requests a data transfer connection, a time-of-day-sensitive surcharge is applied to the user's bill. Additional charges are then added for the length of time that connection is maintained. This makes frequent requests for relatively small file sizes economically costly and unfeasible. The only efficient way to utilize the economy of this switched digital service application is by bursting (speed downloading) larger scale files each time a request for transfer is made. For our application, file sizes would only become large scale if several transaction requests were stored at a main database site and downloaded to distant location together.
[0042] If stateside browsing and purchase requesting was allowed via the Internet, credit-card authorization capabilities, such as LIDBI, would need to be implemented at the stateside database. Payment would need to be authorized or secured before the purchase request was accepted. Transaction and authorization information would need to be transferred to the international sites at the time the music files were forwarded. If partial policy is used, the final purchase transaction would take place at the store site when the merchandise was picked-up by the customer.
[0043] The international switch digital network connection could be used to send international music file to the U.S. database for presentation and sale. File sizes would be accumulated at each primary site and downloaded to the main stateside site at optimized network times.
[0044] There is one possible way to maintain the international market delivery concepts employed by this current model while eliminating the use and expense of the switched digital network connections. This could be accomplished by downloading the accumulated files via a high-speed (broadband) connection to the Internet.
[0045] Transaction requests to the U.S. site would be made and stored during one business-day cycle. The requests would be filled during the intermediate non-business hours in time for the next international business day's deliveries. Conversely, new international music would be copied, compressed and transferred to the U.S. database via a high-speed connection over the Internet. This type of data transfer solution could become a possible usable option due to the next-day delivery model that has been presented.
[0046] It is important to realize, in using such a network, there are also inherent liabilities that could affect data transfer reliability and quality at times. Such network issues may include network blockage or downtime, packet collision due to excessive traffic and loss of asynchronous data arrival. This could result in partial corruption of digital file structure during transfer which could produce audio distortion in the reproduced music media copy. Such corruption could also result in loss of definable associated administrative tracking information or other support file information. All of these issues become trade-offs of economy versus reliability when moving away from the use of a private network for the transfer of critical information.
[0047] As an alternative, a switched network could be used for the transfer of all quality critical files, such as audio-related files, and the Internet could be used for the transfer of all other non-critical information. The related information would then need to be merged at the receiving location. These are some of the issues that may be considered to optimize the efficiency and economy of this type of deployment effort.
[0048] Additional enhancements would include CD- and MP3-reader capabilities at international retail outlets. A typical device is shown in FIG. 5 which could be maintained at any desired location. This would allow musical works from those countries to be compressed and uploaded into the local databases, then to be bursted to U.S. databases for distribution and sale.
[0049] Referring to FIGS. 5 and 6, a vending machine device is illustrated which can be placed in any location to enable a customer to obtain a completed CD bearing the musical composition selected by the customer. The CD is supplied with a case and any indemnifying or advertising matters supplied. A case 102 is provided which has a touch-screen monitor 104 . The monitor displays a series of menus listing the musical compositions available. The menus can be arranged, for example, by classification such as composer, singer or type of music such as classical, jazz, rock and the like. The customer touches the menus at his or her selection, is informed of the cost and given the opportunity to make payment. The customer inserts the cash or a credit card at 106 to pay for the purchase utilizing a system such as shown in U.S. Pat. No. 5,724,424. The completed payment causes a signal to be issued requesting the selected composition. The musical composition is then downloaded to the vending machine where it is burned onto a CD by utilizing a CD writing device 114 . Upon completion of the transfer, the tray 118 holding the CD 116 moves out of the recording mechanism and contacts a series of cams 110 , 112 which removes the CD 116 from the tray. When the CD is removed from the tray, a new CD is placed in the tray from a supply container 120 by activating cams 122 and 124 . The discharged CD is released to a receptacle 126 which allows the customer to remove the CD from the vending machine. As the musical composition is transferred, instructions are issued to the printer for printing the label and any desired advertising material. The printer 130 then prints the material 131 and discharges it to the receptacle 136 to allow the customer to assemble in a container, not shown, which is also discharged at the same time.
[0050] Although the present invention has been described in connection with musical compositions, it is equally suitable for use in video transmission or any other type of data which requires selection and associated materials. The present invention may be embodied in still other specific forms without departing from the spirit or essential attributes thereof and, accordingly, the described embodiments are to be considered in all respects as being illustrative and not restrictive, with the scope of the invention being indicated by the appended claims, rather than the foregoing detailed description. Furthermore, the appended claims indicate the scope of the invention, as well as all modifications which may fall within the range of equivalency, which are also intended to be embraced therein. Any modification of the claim language resulting in the prosecution of this patent application is not intended to limit the range of equivalency.
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This invention relates to an audio and video marketing system. A source of recorded video or audio works is provided for supplying the materials. A main data storage base maintains the audio or video works supplied from the source in storage in a digitized, compressed form. A broadband carrier is supplied for connecting the storage with a local database. The data is supplied to the local storage base as requested by the local base. Means can be supplied for transferring the data from the local storage base onto a portable storage device and for printing associated advertising and identifying data to accompany the portable storage device. Additionally, a sampling protocol is provided between the local database and the main storage data to allow determination of what data is to be transferred.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to a roulette game machine.
DESCRIPTION OF THE RELATED ART
[0002] Conventionally, medal game machines are installed as game machines in game centers and casinos. Such game machines include horse racing game machines, cards game machines, roulette game machines, and so on.
[0003] With, for example, roulette game machines, medals (coins) are thrown into a machine, numeral selection buttons provided at respective play corners are operated, and a numeral button or buttons corresponding to a prize-prospective numeral or numerals are pushed. Then a roulette disc rotates and a ball rolls in the roulette disc. And when the roulette disc rotates slowly and the ball is received and held in one of grooves in the roulette disc, it is determined whether a numeral betted by a player corresponds to that numeral, in which the ball is received. Here, when it is determined that the both numerals correspond to each other, a hit is made and medals are repaid to the player at a predetermined hit ratio.
[0004] However, a roulette game is inherently one, in which a plurality of players use a single betting board to bet on desired numerals. Therefore, when only a player concerned makes a hit, a game is not so much fevered. That is, in the case where that numeral, on which a certain player bets, corresponds to that numeral, in which a ball is received, such state can be seen by other players, and the player having won can feel a sense of superiority whereby a game is still more fevered.
[0005] With such conventional roulette game machines, however, it is hard to know how other players play. For example, even when a player wins, other players do not know how much the player having made a hit has betted on a game at this time, and conversely, even when a player loses, other players do not know how much the player has lost. That is, such conventional roulette game machines involve a problem that a roulette game lacks an inherent fun and players are not so much fevered even when a game is won.
SUMMARY OF THE INVENTION
[0006] That is, it is an object of the invention to provide a roulette game machine capable of giving an inherent fun to a roulette game.
[0007] To achieve the above object, the present invention provides a roulette game machine. The roulette game machine includes a roulette disc having a whirl, on which a multiplicity of different identification symbols are displayed circumferentially, and making a predetermined identification symbol, which is selected from the identification symbols, a hit identification symbol, and a betting board, on which identification symbols corresponding to the identification symbols are displayed, and wherein predetermined chips are given in the case where that predetermined identification symbol on the betting board, on which a player bets chips, corresponds to a hit identification symbol decided on the roulette disc.
[0008] The roulette game machine further includes a single monitor display displaying a betting board capable of having a plurality of players betting at the same time, a plurality of playing areas arranged around the monitor display, first display means provided every playing area to display an amount of chips, which can be bet by a player, designation means provided every playing area to designate a predetermined sum of chips for betting, from a total sum of chips, betting means provided every playing area to bet a designated sum of chips, selection means provided every playing area to select an optional identification symbol on the betting board, second display means provided in juxtaposition with the respective selection means to display a marking image to the effect that betting is made on an optional identification symbol as selected, and judgment means for judging whether an optional identification symbol as betted corresponds to a hit identification symbol.
[0009] Other aspects and advantages of the present invention will become apparent from the following description, taken in conjunction with the accompanying drawings, illustrating by way of example the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The invention, together with objects and advantages thereof, may best be understood by reference to the following description of the presently preferred embodiments together with the accompanying drawings in which:
[0011] FIG. 1 is a perspective view showing a roulette game machine according to an embodiment of the invention;
[0012] FIG. 2 is a plan view showing a roulette game disc;
[0013] FIG. 3 is a plan view showing a monitor display, on which a betting board and chip stock areas are displayed;
[0014] FIG. 4A is a plan view showing a chip stock area and its surrounding region in a state, in which a hand cursor is in a home position, and FIG. 4B is a plan view showing a chip stock area, its surrounding region, and the relationship between chip icons and a hand cursor immediately before the chip icons are grasped;
[0015] FIG. 5A is a plan view showing a chip stock area, its surrounding region, and the relationship between chip icons and a hand cursor in a state, in which the hand cursor grasps the chip icons, and FIG. 5B is a plan view showing a play corner in the surrounding region of a chip stock area, and the relationship between a hand cursor having been moved onto chip icons of an adjacent digit from the state in FIG. 5A , and chip icons;
[0016] FIG. 6 is a plan view showing a chip stock area, its surrounding region, and the relationship between a hand cursor grasping chip icons of a different digit from the digit in FIG. 5A and chip icons;
[0017] FIG. 7 is a plan view showing a monitor display in a state, in which a hand cursor grasping chip icons is displayed on a betting board, and respective operating systems;
[0018] FIG. 8 is a plan view showing a monitor display around a first play corner and operating members;
[0019] FIG. 9A is a schematic, plan view showing an internal construction of a track ball, and FIG. 9B is a schematic, side view showing the internal construction of the track ball;
[0020] FIG. 10A shows chip marks at a first play corner, FIG. 10B showing chip marks at a second play corner, FIG. 10C showing chip marks at a third play corner, and FIG. 10D showing chip marks at a fourth play corner;
[0021] FIG. 11 is a block diagram indicating an electrical constitution;
[0022] FIG. 12 is a flowchart indicating contents of processings in a controller; and
[0023] FIG. 13A is a schematic, side view showing a joy stick in a further embodiment, FIG. 13B being a plan view showing the relationship between microswitches and a ring in a state, in which a lever of the joy stick is in a neutral position, FIG. 13C being a plan view showing the relationship between the microswitches and the ring in a state, in which the lever of the joy stick is inclined downward, and FIG. 13D being a plan view showing the relationship between the microswitches and the ring in a state, in which the lever of the joy stick is inclined obliquely rightward and forward.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] Embodiments of the invention will be described below with reference to the drawings.
[0025] As shown in FIG. 1 , a housing 11 constituting a roulette game machine is provided on an upper surface thereof with a roulette disc 12 . Also, provided on the upper surface of housing 11 is a large-sized, rectangular monitor display 13 . Arranged at four corners lengthwise and crosswise of the monitor display 13 are a first play corner P 1 , second play corner P 2 , third play corner P 3 , and a fourth play corner P 4 . Provided at the respective play corners P 1 to P 4 on the upper surface of the housing 11 are medal slots 15 , track balls 16 , which constitute operation means and selection means, hold buttons 17 , which constitute designation means, put buttons 18 , which constitute bet means, and repayment buttons 19 for repayment of medals. Also, medal repayment ports 20 , respectively, are provided at the respective play corners P 1 to P 4 on sides of the housing 11 .
[0026] As shown in FIGS. 1 and 2 , a whirl 23 is rotatably received in a frame body 12 a of the roulette disc 12 . A multiplicity of concave-shaped ball receiving grooves 24 are formed on an upper surface of the whirl 23 . The whirl 23 is driven by a motor (not shown). A display section 25 , on which numerals N 1 including “0”, “00”, “1” to “36” are displayed in a manner to correspond to the respective ball receiving grooves 24 , is formed on the upper surface of the whirl 23 externally of the respective ball receiving grooves 24 . A ball throw-in port 29 is formed in the frame body 12 a . Connected to the ball throw-in port 29 is a ball throw-in device (not shown). As the ball throw-in device is driven, a ball B is thrown onto the whirl 23 from the ball throw-in port 29 .
[0027] A hit judgment device (not shown) is installed in a position below the roulette disc 12 within the housing 11 . The hit judgment device serves to judge which ball receiving groove 24 the ball B is received in. The hit judgment device will be described in detail in connection with an electric constitution. A ball recovery device (not shown) is mounted on a back surface of the whirl 23 . The ball recovery device serves to recover the ball B on the whirl 23 after a game is terminated. Since the ball throw-in device, the hit judgment device, and the ball recovery device are well known, a detailed explanation thereof is omitted (see JP-A-8-229190, JP-A-8-229191, JP-A-9-140857, and JP-A-9-276477, which were filed by the applicant of the present application).
[0028] As shown in FIGS. 1 and 3 , the monitor display 13 is composed of a liquid crystal monitor. A betting board 26 is displayed on the monitor display 13 . A plurality of numerals N 2 including the same numerals as the numerals N 1 displayed on the whirl 23 are arranged and displayed on the betting board 26 in a lattice manner.
[0029] Chip stock areas TH 1 , TH 2 , TH 3 , TH 4 corresponding to the respective play corners P 1 to P 4 are displayed on the monitor display 13 to be directed outward at the four corners of the betting board 26 .
[0030] As shown in FIGS. 1, 3 and 4 , displayed on the respective chip stock areas TH 1 , TH 2 , TH 3 , TH 4 are bet counters BC, win counters WC, and credit counters CC, which constitute first display means, respectively. Displayed on the bet counters BC are numerals corresponding to the number of medals betted in a single game. Displayed on the win counters WC are numerals corresponding to the number of medals paid back when a game is played and a hit is made. Displayed on the credit counters CC are numerals corresponding to the number of medals, which can be repaid from a medal repayment device described later.
[0031] Disposed on the right of the respective counters BC, WC, and CC are chip counter areas TC, which constitute first display means. Displayed below the chip counter areas TC are “the units digit”, “the tens digit”, “the hundreds digit”, and “the thousands digit”. Tip icons TI in a stacked state are displayed above display sections of the respective digits (“the units digit” to “the thousands digit”). For example, in the case where eight chip icons TI are displayed on the display section of “the tens digit” and three chip icons TI are displayed on the display section of “the hundreds digit”, it is indicated thereby that 380 repayable medals accumulate in a concerned play corner ((3×100)+(8×10)). That is, the numeral displayed on the credit counter CC corresponds to the number of chip icons TI displayed in the chip counter area TC.
[0032] As shown in FIGS. 9A and 9B , the track balls 16 comprise a support base 41 , a ball 43 rotatably received in a recess 42 of the support base 41 , a X-direction detector 45 ×, a Y-direction detector 45 Y, and so on. Shafts 47 constituting parts of the X-direction detector 45 × and the Y-direction detector 45 Y are rotatably supported by bearings 46 . Fixed to a base end of the shaft 47 is a disk 48 rotatable together with the shaft 47 . An axis of the shaft 47 of the X-direction detector 45 X extends lengthwise (a vertical direction in FIG. 9A ). Meanwhile, an axis of the shaft 47 of the Y-direction detector 45 Y extends crosswise. The shafts 47 of the both direction detectors 45 X, 45 Y, respectively, contact with the ball 43 . With such constitution, external forces are exerted to rotate the balls 43 whereby the respective shafts 47 rotate sliding on the balls 43 . That is, when the ball 43 is rotated lengthwise, the shaft 47 of the Y-direction detector 45 Y rotates, and when the ball 43 is rotated crosswise, the shaft 47 of the X-direction detector 45 ×rotates. Also, when the ball 43 is rotated slantwise (rightwardly slantwise and leftwardly slantwise), both the shafts 47 of the both direction detector 45 X, 45 Y rotate.
[0033] The disks 48 of the both direction detector 45 X, 45 Y are formed with a plurality of slits 51 at regular intervals. As shown in FIG. 9B , a floodlight 49 and an optical receiver 50 are arranged in positions, between which each disk 48 is interposed. The respective optical receivers 50 can receive light from the floodlights 49 through the slits 51 . That is, when the shaft 47 rotates, the optical receiver 50 intermittently receives light from the floodlight 49 . A signal of the optical receiver 50 is output to a controller C described later. The controller C judges a quantity of rotation of the respective shafts 47 , that is, direction and quantity of rotation of the ball 43 on the basis of signals from the two optical receivers 50 . That is, the track ball 16 in the embodiment detects direction and quantity of rotation of the ball 43 by means of a rotary encoder system.
[0034] As shown in FIG. 3 , displayed on the monitor display 13 are hand cursors HC corresponding to the respective play corners P 1 to P 4 . The hand cursors HC assume a configuration of a human hand. The respective hand cursors HC are different in display color by the respective play corners P 1 to P 4 (in the embodiment, for example, the hand cursor HC at the first play corner P 1 is red-colored, the hand cursor HC at the second play corner P 2 is green-colored, the hand cursor HC at the third play corner P 3 is blue-colored, and the hand cursor HC at the fourth play corner P 4 is white-colored). In actual games, respective players identify their hand cursors HC by the help of color.
[0035] The balls 43 of the track balls 16 are operated to cause the respective hand cursors HC to be freely moved on the monitor display 13 . That is, when the ball 43 is rotated rightward, the hand cursor HC is also moved rightward, and when the ball 43 is rotated forward, the hand cursor HC is also moved forward.
[0036] Subsequently, the electric constitution of the roulette game machine will be described.
[0037] As shown in FIG. 11 , the track balls 16 , hold buttons 17 , put buttons 18 , repayment buttons 19 , medal repayment devices 30 , and detection devices 33 , which detect the number of medals thrown in, at the respective play corners P 1 to P 4 are connected to the controller C, which constitutes a part of the first display means, a part of the second display means, a part of the designation means, a part of the bet means, and the judgment means.
[0038] Also, connected to the controller C are the monitor display 13 and a hit judgment device 31 . The controller C causes the monitor display 13 to display the betting board 26 , the chip stock areas TH 1 , TH 2 , TH 3 , TH 4 , and the hand cursors HC.
[0039] The hit judgment device 31 detects a position of the ball B received in the ball receiving groove 24 of the whirl 23 , that is, a numeral N 1 to output the same to the controller C. The controller C judges a hit number (the numeral N 1 of that ball B receiving groove, in which the ball is received) on the basis of a signal from the hit judgment device 31 .
[0040] The controller C judges direction and quantity of rotation of the ball 43 on the basis of an input signal from the receivers 50 of the track ball 16 . And the controller C moves an image of the displayed hand cursor HC on the basis of judged direction and quantity of rotation of the judged ball 43 .
[0041] As shown in, for example, FIG. 4B , the controller C causes an image of the hand cursor HC to be displayed in a state, in which the hand cursor HC grasps chip icons TI having been displayed just therebelow, when the controller receives an ON signal from the hold button 17 in a state, in which an image of the hand cursor HC is displayed in the chip counter area TC (a state, in which a player pushes the hold button 17 ).
[0042] That is, the controller C calculates direction and quantity of rotation of the ball 43 to judge that an image of the hand cursor HC is present in a predetermined area within the chip counter area TC, and further makes a selected object of those chip icons TI of a predetermined digit, which are disposed in a position below the image of the hand cursor HC in the predetermined area. When an ON signal from the hold button 17 is input, the controller C displays an image composed of those chip icons TI, which have a predetermined digit selected according to a position of the hand cursor HC. The controller C displays an image composed of an image of chips of the number corresponding to times (times, at which a player pushes the hold button 17 ), at which an ON signal from the hold button 17 is input, and an image of the hand cursor HC, in a state, in which the chips are grasped (see FIGS. 5 and 6 ). At this time, the controller C displays a total sum of chips in a position, in which an image of the grasped chips is displayed. The controller C displays an image, in which the hand cursor HC grasps chip icons TI, and correspondingly modifies images of chip icons TI of the respective digits into images of subtracted chip icons TI to display the same.
[0043] The controller C moves an image of the hand cursor HC in a state of grasping chips according to rotation of the ball 43 of the track ball 16 . And when an image of the hand cursor HC moves onto the betting board 26 (see FIG. 7 ), in which state an ON signal from the put button 18 is input (a player pushes the put button 18 ), the controller C erases the grasped chip icons TI from the hand cursor HC and marks an image of a chip mark TM, which serve as a mark to correspond to the image of the hand cursor HC, on the betting board 26 (see FIG. 8 ). At this time, the controller C displays a sum of chips in a position of the marked chip image.
[0044] With the embodiment, the controller C displays images of chip marks TM for the respective play corners P 1 to P 4 in different configurations. FIGS. 10A to 10 D are views showing patterns of chip marks TM for the respective play corners P 1 to P 4 , FIG. 10A showing a chip mark TM for the first play corner P 1 , FIG. 10B showing a chip mark TM for the second play corner P 2 , FIG. 10C showing a chip mark TM for the third play corner P 3 , and FIG. 10D showing a chip mark TM for the fourth play corner P 4 .
[0045] The controller C serving as judgment means judges whether a hit numeral N 1 output as a result of a game from the hit judgment device 31 corresponds to a numeral N 2 , marked by a player, on the betting board 26 .
[0046] The controller C displays predetermined numerical values in the bet counters BC, win counters WC, and the credit counters CC on the chip stock areas TH 1 , TH 2 , TH 3 , TH 4 in accordance with a numeric data input as a game proceeds.
[0047] Subsequently, a main processing operation of the controller C will be described with reference to a flowchart shown in FIG. 12 .
[0048] First, the controller C starts inputting of bets in STEP 101 . In the next STEP 102 , the ball B is thrown onto the whirl 23 . In STEP 103 , it is determined whether a predetermined period of time has elapsed, and when it is determined that a predetermined period of time has elapsed, inputting of bets is closed in STEP 104 and a hit numeral is determined in STEP 105 on the basis of an output signal from the hit judgment device 31 . Also, when a player bets, it is determined whether the hit numeral corresponds to a numeral thus betted. Then, in STEP 106 , in the case where a numeral N 2 betted onto the betting board 26 corresponds to the hit numeral N 1 , chips conformed to a bet rate are given, and in the case of non-correspondency, chips are recovered. That is, display on the respective counters BC, WC, and CC in the respective chip stock areas TH 1 to TH 4 is modified according to a sum of chips. Then the controller C ends the processing once and returns again to STEP 101 .
[0049] Subsequently, an explanation will be given to an operation when the roulette game machine is played.
[0050] First, a player throws medals into a medal slot 15 . Then a numeral conformed to the number of thrown medals is displayed in the credit counter CC. Here, it is assumed that the number of medals thrown at this time is 1235. Accordingly, “1235” is displayed in the credit counter CC as shown in FIG. 4A . In addition, the hand cursor HC stands by to be displayed in an upper portion of the chip stock area TH 1 (the same is for the chip stock areas TH 2 to TH 4 ), as a home position, in the figure prior to the start of a game.
[0051] Subsequently, the ball 43 of the track ball 16 is rotated downward to move the hand cursor HC downward, that is, toward the chip icons TI. Then the hand cursor HC is moved above desired chip icons TI and the put button 18 is pushed. At this time, it is assumed that the hand cursor HC is moved above the chip icons TI of “the tens digit” in FIG. 4B . When the hold button 17 is pushed in this state, display of the hand cursor HC is changed to a state to grasp the chip icons TI (see FIG. 5A ). At this time, the number of chip icons TI grasped by the hand cursor HC is changed corresponding to those times, at which the hold button 17 is pushed. Here, it is assumed that the hold button 17 is pushed twice.
[0052] Accordingly, the hand cursor HC changes to a state to grasp two chip icons TI of “the tens digit” as shown in FIG. 5A . A numeral equal to the number of grasped medals is displayed on the chip icons TI grasped by the hand cursor HC. Here, since two chip icons TI of “the tens digit” are grasped, “20” is displayed on the chip icons TI grasped by the hand cursor HC. Also, at the same time when the hand cursor HC grasps chip icons TI, the chip icons TI having been displayed in a state of being stacked in the tip counter area TC and the credit counter CC are subjected to subtraction to be displayed.
[0053] Further, in the case where it is desirable to bet many medals, for example, in the case where it is desirable to bet additional 100 medals, the ball 43 is rotated leftward and the hand cursor HC is moved leftward, that is, onto chip icons TI of “the hundreds digit” as shown in FIG. 5B . Then the hold button 17 is pushed once to cause the hand cursor HC to grasp chip icons TI of “the hundreds digit”. At this time, “120” is displayed on the chip icons TI grasped by the hand cursor HC, and the chip icons TI of “the hundreds digit” having been displayed in a state of being stacked in the tip counter area TC and the credit counter CC are subjected to subtraction to be displayed, as shown in FIG. 6 .
[0054] Subsequently, the ball 43 is rotated forward to move the hand cursor HC onto the betting board 26 from the chip stock area TH 1 as shown in FIG. 7 . Then the chip icons TI grasped by the hand cursor HC are moved onto a numeral N 2 , which is believed to possibly make a hit. Here, the chip icons are moved onto four numerals, that is, “5”, “6”, “8”, and “9”. When prospective numerals have been decided, the put button 18 is pushed whereby a chip mark TM of a predetermined pattern is marked centrally of “5”, “6”, “8”, and “9” as shown in FIG. 8 . Here, displayed on the marked chip mark TM is the same numeral (120) as the numeral displayed on the chip icons TI. Also, simultaneously with marking of the chip mark TM, the chip icons TI are erased from the hand cursor HC, and the same numeral as the numeral displayed on the chip mark TM is displayed on the bet counter BC.
[0055] At this time, in the case where a numeral is still displayed on the credit counter CC, that is, in the case where the remainder of medals is present, the above-mentioned operation is repeated whereby betting (marking) can be made in a plurality of places in the same chip stock area TH 1 (TH 2 to TH 4 ). In this case, a numeral displayed on the bet counter BC makes a total of numerals displayed on the chip marks TM. Thereby, a player can judge, at a glance, how many medals are betted in a game at this time even when the player makes betting in a plurality of places. Here, in the case where different play corners (here, the second play corner P 2 and the fourth play corner P 4 ) make a bet on the same numeral, a pattern of the chip mark TM is divided into two sections to be displayed as indicated by an arrow A in FIG. 8 . That is, an upper half of the chip mark TM is displayed to represent a pattern for the second play corner P 2 and a lower half of the chip mark TM is displayed to represent a pattern for the fourth play corner P 4 . Also, in the case where three play corners make a bet on the same numeral, a pattern of the chip mark TM is divided into three sections to be displayed, and in the case where four play corners make a bet on the same numeral, a pattern of the chip mark TM is divided into four equal sections to be displayed. Of course, patterns corresponding to the respective play corners P 1 to P 4 are displayed on the divided surface sections also in this case.
[0056] In addition, when chip marks TM are displayed on the betting board 26 and then positions, in which the chip marks are displayed, are to be modified, the hand cursor HC is moved to that chip mark TM, which is desired to be modified, and the put button 18 is pushed, whereby the chip mark TM is erased from the betting board 26 . Then the erased chip mark TM is returned to a state, in which it is grasped by the hand cursor HC.
[0057] Subsequently, when a predetermined period of time has elapsed, the ball B is thrown onto the whirl 23 . And when a judgment for a hit is made, display on the respective counters BC, WC, and CC in the chip stock areas TH 1 to TH 4 of the respective play corners P 1 to P 4 is modified, and the chip marks TM marked on the betting board 26 are erased. Thereafter, the hand cursor HC is moved to a position of a new numeral N 2 , and the put button 18 is pushed in the same manner as that described above, whereby positions, in which the chip marks TM are displayed, can be modified.
[0058] As described above in detail, the embodiment constitutes a roulette game machine in the above-mentioned manner to thereby be able to produce the following effects.
[0059] According to the embodiment, the betting board 26 is displayed on a single monitor display 13 and the respective track balls 16 provided for the respective play corners P 1 to P 4 are operated to move the hand cursors HC on the betting board 26 , thereby enabling making a bet on a prospective numeral or numerals.
[0060] That is, according to the embodiment, the plurality of play corners P 1 to P 4 own and use a single monitor display 13 in common. As a result, players at the respective play corners P 1 to P 4 can show to other players and a surrounding gallery what numeral N 2 or numerals N 2 are betted by them and can also see where other players make a bet. Thereby, players are uplifted by a sense of competition with other players to be able to play a game more pleasantly than playing on a roulette game machine of the prior art.
[0061] The hand cursors HC of the respective play corners P 1 to P 4 are made different in color from one another to be displayed on the monitor display 13 . Thereby, respective players and a surrounding gallery can discriminate what numeral N 2 or numerals N 2 are betted by other players, so that tactics among players is improved prior to the start of a game to be able to play a roulette game more pleasantly.
[0062] After a numeral N 2 or numerals N 2 are decided, a chip mark or chip marks TM are marked on the numeral N 2 or numerals N 2 . Thereby, even when the hand cursors HC are moved to other positions after the decision of the numeral or numerals, players and a surrounding gallery can discriminate, at a glance, where betting is made, so that it is possible to play a roulette game more pleasantly and more amusingly.
[0063] Patterns of chip marks TM displayed on the monitor display 13 are changed for the respective play corners P 1 to P 4 to afford discrimination from outside. Thereby, which player bets and what numeral N 2 or numerals N 2 are betted can be quickly confirmed by respective players and a surrounding gallery, so that it is possible to play a roulette game more pleasantly and more amusingly.
[0064] In addition, the invention may be embodied in the following manner.
[0065] While the roulette disc 12 in the embodiment is of a type, in which the ball B is actually thrown in, it may be of a type, in which instead of throwing an actual ball B in, a roulette disc is displayed as an image on the monitor display. In this case, it does not matter if display is such that the whirl 23 itself does not rotate.
[0066] While the play corners P 1 to P 4 are provided at four corners in the embodiment, the number of play corners may be two or more. Of course, also in this case, the track ball 16 and the respective buttons 17 , 18 , 19 are provided at respective play corners.
[0067] While the embodiment is materialized as a roulette game machine making use of exclusive medals for a game, it may be materialized as a roulette game machine of a type, in which coins are used for a game and a premium such as cake, toy, or the like is repaid.
[0068] While the track ball 16 having a rotary encoder is used in the embodiment to materialize cursor moving means, it suffices that cursor moving means assume other configurations. For example, a joy stick 51 shown in FIG. 13 may be used to constitute cursor moving means.
[0069] A support 52 constituting the joy stick 51 is supported on a housing 11 . A lever 53 is supported on the support 52 to be inclinable lengthwise and crosswise. Mounted on an upper end of the lever 53 is a grip 54 projecting from the housing 11 . A ring 55 is supported on a lower end of the lever 53 . Also, microswitches SW 1 , SW 2 , SW 3 , SW 4 are mounted lengthwise and crosswise on the support 52 in a manner to surround the grip 54 .
[0070] As shown in FIG. 13B , when the lever 53 is in a neutral position, the ring 55 does not contact with any one of the microswitches SW 1 to SW 4 and any ON signal is not output from the microswitches SW 1 to SW 4 . In this state, a controller (not shown) does not move the hand cursor HC. For example, when the lever 53 is inclined rearward, the ring 55 contacts with the microswitch SW 1 as shown in FIG. 13C to have the microswitch SW 1 outputting an ON signal to the controller. When an ON signal is input into the controller C from only the microswitch SW 1 , the controller moves the hand cursor HC rearward. Also, when the lever 53 is inclined obliquely rightward and forward, the ring 55 contacts with the microswitches SW 2 , SW 3 as shown in FIG. 13D and ON signals are output to the controller from the microswitches SW 2 , SW 3 . When ON signals are input into the controller C from the microswitches SW 2 , SW 3 , the controller moves the hand cursor HC obliquely rightward and forward.
[0071] In this manner, even when the joy stick 51 provided with the lever 53 and the microswitches SW 1 to SW 4 is used, the same effect as that in the embodiment can be produced. In addition, other joy sticks provided with a flood switch and a light receiving switch may be used.
[0072] While the hand cursors HC in the embodiment are made different in color from one another for the respective play corners P 1 to P 4 to afford discrimination from outside, all the hand cursors HC may be embodied in configuration to be displayed in the same manner.
[0073] While the hand cursors HC in the embodiment are made different in color from one another for the respective play corners P 1 to P 4 to afford discrimination from outside, they may be embodied to be identical to one another in color and different in shape from one another for the respective play corners P 1 to P 4 . For example, numbers (numerals) of the play corners may be displayed on the respective hand cursors HC to afford discrimination of the respective hand cursors from outside.
[0074] While the chip marks TM in the embodiment are displayed to be changed in pattern for the respective play corners P 1 to P 4 to afford discrimination from outside, the chip marks TM in all the play corners P 1 to P 4 may be identical in pattern to one another but different in color to afford discrimination of the chip marks TM in the respective play corners P 1 to P 4 . Also, the chip marks TM may be embodied to be changed in shape.
[0075] While the numerals N 1 , N 2 are displayed as discriminating characters on the roulette disc 12 and the betting board 26 in the embodiment, mascot characters, alphabets, or the like may be embodied instead of the numerals N 1 , N 2 to be displayed.
[0076] The present examples and embodiments are to be considered as illustrative and not restrictive, and the invention is not to be limited to the details given herein, but may be modified within the scope and equivalence of the appended claims.
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A roulette game machine includes a single monitor display displaying a betting board capable of having a plurality of players betting at the same time, a plurality of playing areas arranged around the monitor display, first display means provided every playing area to display an amount of chips, designation means provided every playing area to designate a predetermined sum of chips for betting, betting means provided every playing area to bet a designated sum of chips, selection means provided every playing area to select an optional identification symbol on the betting board, second display means provided in juxtaposition with the respective selection means to display a marking image to the effect that betting is made on an optional identification symbol as selected, and judgment means for judging whether an optional identification symbol as betted corresponds to a hit identification symbol.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention generally relates to a solar cell package and more particularly to a solar cell package including an improved double-sided solar cell mounted within a tubular transparent enclosure and having associated therewith a surface for redirecting incident rays to impinge on at least one side surface of the solar cell, whereby both sides of the solar cell is illuminated.
2. Description of the Prior Art
The prior art, of course, is replete with photovoltaic devices adapted to induce a current flow through an electrical circuit in response to incident solar radiation. While such devices are frequently employed in a celestial space environment the costs thereof attending usage in a terrestrial environment severely limits their utility. Substantial attention now is being given to the reduction of costs attending the use of photovoltaic devices, hereinafter referred to as solar cells, in a terrestrial environment so that the advantages thereof may be more fully appreciated.
Unlike most semiconductor devices, conventional solar cells have a significant value resulting solely from the material used in their fabrication, as opposed to the value added thereto as a consequence of fabrication. Consequently, cost reduction, and therefore increased usage of solar cells can be realized simply by reducing the quantity of silicon employed therein, once the processing steps for growing silicon cells are automated.
Currently, there are indications that single crystal silicon wafers cannot be fabricated and handled for minimum costs at thicknesses indicated suitable for adequate performance levels, such as four mills or less. Currently, the most practical thickness is in the range of for six-to-eight mills, or the thickness of two thin-type solar cells arranged in back-to-back contact. Therefore, in order to realize maximum cost effectiveness, fabrication and handling of solar cells having a thickness twice the thickness for adequate performance levels is desirable. However, from a cost effectiveness standpoint it is still necessary to make effective use of the total quantity of material included in the solar cells in order to realize cost savings.
Moreover, solar cells and similar devices usually are protected from the deleterious effects of terrestrial environments through use of glass sheets provided in an hermetically sealing relation therewith. The resulting device, while capable of withstanding the effects of wind, snow, rain, hail, blowing sand and the like, generally is considered to be impractical for many uses because of its cost in terms of time and material devoted to the fabrication thereof.
It generally is recognized that from a cost effectiveness standpoint it is cheaper to utilize a transparent or glass enclosure of a tubular configuration for encasing solar cells, since less material is used per unit area and glass tubes can be drawn as cheaply as being fabricated in any other structural form. However, one significant problem associated with the use of tubular enclosures or solar cells is that difficulty often is encountered in the rejection of excess heat from the solar cells.
In view of the foregoing, it should readily be apparent that there currently exists a need for a simplified solar cell package which is economic to fabricate and practical to employ in a terrestrial space environment.
It is therefore the general purpose of the instant invention to provide in a solar cell array for terrestrial use an economic and improved solar cell through which an increase in the usage of solar cells is realized in terrestrial environments.
OBJECTS AND SUMMARY OF THE INVENTION
It is therefore the general purpose of the instant invention to provide an economic and improved solar cell package for use in a terrestrial environment.
It is another object to provide an improved doublesided solar cell package which is both economic to fabricate and operates with increased efficiency.
It is another object to provide for use in a solar cell package a double-sided silicon solar cell having a thickness substantially equal to twice the thickness normally accepted to be adequate for achieving solar cell performance at acceptable levels.
It is another object to provide an improved solar cell package having a protective enclosure which is economic to fabricate, simple to employ, and possesses a capability for rejecting excess heat.
It is another object to provide for use in a terrestrial environment an improved solar cell package including a doublesided solar cell mounted in a tubular enclosure formed of a transparent material having associated therewith a reflector for directing incident solar energy to impinge against both faces of the cell.
Another object is to provide an improved solar cell package which is particularly useful in a terrestrial environment although not necessarily restricted in use thereto, since the improved solar cell package which embodies the principles of the instant invention may be equally useful when installed aboard spacecraft and the like.
These and other objects and advantages are achieved through the use of a solar cell package including a transparent enclosure of a tubular configuration having disposed therein a double-sided solar cell mounted on a pedestal formed of conductive material and associated with reflectors configured to direct incident solar energy to impinge on at least one of the faces of the solar cell, whereby both surfaces are simultaneously illuminated, as will hereinafter become more readily apparent by reference to the following description and claims in light of the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top plan view of a solar cell array which embodies the principles of the instant invention.
FIG. 2 is a modification of the array shown in FIG. 1.
FIG. 3 is a cross sectional view of a pair of adjacent solar cell packages, taken generally along line 3--3 of FIG. 1, but on an enlarged scale.
FIG. 4 is a cross sectional view of a pair of solar cell packages taken generally along line 4--4 of FIG. 2, but on an enlarged scale.
FIG. 5 is a bottom plan view of a single solar cell included within one of the solar cell packages shown in FIGS. 3 and 4, but, for the sake of clarity, removed from its pedestal.
FIG. 6 is a top plan view of one of the solar cells shown in FIGS. 3 and 4.
FIG. 7 is a cross sectional view taken generally along line 7--7 of FIG. 6 illustrating the solar cells cross section.
FIG. 8 is a fragmented view illustrating one manner in which the solar cell packages are connected.
FIG. 9 is a view of one end of one of the solar cell packages, illustrating the electrical connections provided for connecting the solar cell package within an electrical circuit, and openings provided therein for accommodating forced-air cooling of the package.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, wherein like reference characters designate like or corresponding parts throughout the several views, there is depicted in FIG. 1, a solar cell array, generally designated 10, which comprises the principles of the instant invention. As shown in FIG. 1 the solar cell array 10 includes a plurality of solar cell packages, each being generally designated 12, arranged in side-by-side parallelism and supported at each of their opposite ends by manifolds designated 14 and 16. It will, of course, be appreciated that the solar cell packages 12 include housings, of alternate configurations designated 18 and 19, of a suitable length, while the manifolds 14 and 16 preferably support the housings for rotation in a manner which accommodates a tracking of the path of the sun across the sky, as will hereinafter become more readily apparent.
Referring now to FIG. 3, it can be seen that each solar cell package 12 includes a substantially transparent housing 18 comprising an elongated tubular body having a non-circular cross sectional configuration. As a matter of interest, the housing 18 is so dimensioned in cross section as to be provided with a major diameter substantially greater than its normally minor diameter for thus imparting thereto an elliptical configuration. Within the housing 18 there is mounted a solar cell assembly, generally designated 20, the purpose of which is to convert incident solar radiation to electrical energy. The solar radiation, of course, is afforded passage through the housing 18, due to its transparency.
The solar cell assembly 20 includes a pedestal 22 having a body 24 terminating in a pair of laterally extended, longitudinal plates 26. Each of the plates, in turn, terminates in a deflected footing 28 configured to engage the internal surface of the housing for supporting the body 24. Each footing 28 preferably is of a cross sectional configuration substantially conforming to the cross sectional configuration of the surface area of contact, not designated, provided within the housing 18. As a practical matter, the pedestal 22 is fabricated from a conductive material, such as copper foil, and is bonded to the internal surface of the housing 18 employing a layer 30 of compliant adhesive. While the particular adhesive employed is deemed to be a matter of convenience only, a silicone adhesive serves quite satisfactorily for this purpose. While the adhesive employed is varied as desired, the adhesive employed must be capable of conducting heat, whereby excessive heat is afforded a discharge path from the pedestal 22 to the housing 18, in order to maximize heat rejection through the housing wall. Thus the wall of the housing becomes a component of a heat transfer path.
Mounted on the apex of the pedestal 22 is a double-sided solar cell 32, the purpose of which is to convert solar radiation to electrical energy at each of its opposite faces simultaneously. As best illustrated in FIGS. 3 and 4, rays A of radiation pass through the transparent wall of the housing 18 and strike the upper surface, designated 34, of the solar cell 32, while the rays B of radiation are reflected to strike the lower surface 36 of the solar cell 32.
As illustrated in FIGS. 1 and 3, the surfaces of the plates 26 are polished so that the rays B are reflected toward the surface 36 of the solar cell. The surface of the plates 26 are, where so desired, coated in a manner which establishes therefor a highly reflective surface for purposes of redirecting the rays B to impinge on the lower surface 36 of the solar cell 32.
As best shown in FIGS. 2 and 4, the housing, where desired, may be of a circular cross sectional configuration, which is employed in instances where non-circular glass tubing tends to increase cost and low-cost requirements which are of utmost concern.
As shown, transparent housing 19 is of a substantially circular cross sectional configuration, while the double-sided solar cell 32 is of a width substantially equal to the internal diameter of the housing. The configuration of the pedestal 22 also is of a modified configuration, in that the longitudinal plates 26 are foreshortened in width, with the footing 28 being projected from the body 24 and bonded to the internal surface of the housing.
Since the longitudinal plates 26 are, in effect, deleted in the embodiment shown in FIG. 4, it is desirable to provide for the solar cell package illustrated in FIG. 4 an external reflector 38 having a surface 40 so configured as to reflect rays B of solar energy to impinge against the lower surfaces 36 of the solar cells 32 while rays A strike the upper surfaces 34 in the same manner in which the rays A strike the surfaces 34 of the solar cells 32 illustrated in FIG. 3. Consequently, the solar cell packages 12 illustrated in FIGS. 1 and 2 function in substantially the same way with the exception that solar cell packages 12 having housings 18, FIG. 3, are provided with internal reflective surfaces 26 while the solar cell packages 12 having housings 19 of circular cross sectional configurations, FIG. 4, are provided with external reflecting surfaces 40.
Referring now to FIGS. 5, 6 and 7, wherein the doublesided solar cell 32 is illustrated with more particularity, but not to scale for the sake of clarity, it can be seen that the solar cells 32 include a P silicon wafer 42, into the opposite faces of which is diffused an N silicon layer 44. As a practical matter, the P silicon wafer 42 is of a thickness of approximately six-to-eight mills. This thickness is substantially twice the thickness required for achieving adequate performance levels for a single-sided solar cell. In order to make contact with the high resistivity wafer at the center of the cell, without employing an excessively complex grid pattern, calculations indicate that if low resistivity of approximately 0.2 ohms per centimeter material is used, contact spacing of one centimeter is adequate. Contact spacing of the diffused layer or N slicon layer 44 is 0.25 centimeters or less. The pattern illustrated in FIGS. 5 through 7 is deemed adequate for providing a contact arrangement which permits collection of photon generated electrons from each of the opposite sides of the double-sided solar cell 32.
In order to provide the contacts, after the layer 44 is diffused into all exposed surfaces of the wafer 42, etching is employed for purposes of removing the N silicon layer 44 along a central zone 46 of the lower surface 36 of the solar cell 32 while edge zones 48 of the wafer are exposed along the opposite edges of the upper surface 34 of the cell 32. The zones 46 and 48 are then metallized to provide three contact stripes designated 50 and 52. The contact stripe 50 is then bonded to the body 24 of the pedestal 22 whereby an electrical contact is established between the pedestal 22 and the contact stripe 50.
By connecting the three contact stripes the electrical resistance due to the resistivity of the wafer is rendered acceptable. Such connection is effected by bonding a lead 54 to each of the contact stripes 52 and to the pedestal 22 in the manner generally indicated in FIG. 7. In practice, a contact grid 56 of known design, FIGS. 5 and 6, is bonded to the layer 44 excepting, of course, in those areas at which the junction formed between the N silicon layer 44 and the P silicon wafer has been etched through for purposes of accommodating current collection. The solar cells 32 are, where desired, connected in series by leads connected in a suitable manner between each N silicon layer 44 and an adjacent P silicon wafer 42. In such instances, the leads employed are formed of a heat conductive material and are bonded to the housing for establishing heat transfer paths additional to the paths, aforementioned, established by the pedestal 22.
As best illustrated in FIG. 8, each solar cell package 12 includes a head 60 and a tail 62. Within the head 60 there is provided a plug 64 formed of a suitable insulating material, such as a ceramic or the like, which serves as a closure for a housing 18, or 19 as the case may be, as well as a support for coupling the package with the manifold 14. Mounted in each of the plugs 64 is a button contact 66 and an annular contact 68. The contact 68 is embedded in the plug 64 in concentric relation with the button contact 66. A pair of leads 70 serve to connect the contacts 66 and 68 to the pedestal 22 and to grid 56, respectively. Thus the double-sided solar cell 32 is provided with simple contacts through which connection within a power support circuit, not designated, is afforded.
As illustrated, the manifold 14 is provided with a plurality of spring finger contacts 72, the purpose of which is to connect each ring contact 68 in circuit series with an adjacent button contact 66 for purposes of connecting the solar cell packages 12 of the array 10 in series. The spring fingers, of course, also accommodate angular displacement of the housings for the solar cell packages, whereby tracking of the sun across the sky is facilitated. Such rotation may be achieved manually or, preferably, through a use of a drive unit, not shown.
Located at the tail end 62 of each of the housings 18 and 19, as the case may be, there is a plug 74 the primary purpose of which is to serve as a closure for the housing, as well as to serve as a coupling member for uniting the solar cell package 12 with the manifold 16.
In some instances dissipation of heat must be enhanced even though the pedestals 22 are connected to circuit leads attached to the housing which serve to conduct heat to said housing of the solar cell package. To achieve this, the manifold 14 is provided with a fitting 76 adapted to be connected with a source of coolant under pressure, not shown, while a network of interconnected manifold passageways 78 are provided for conducting a stream of fluid coolant, such as air, throughout the manifold. In such instances, an O ring 79 is mounted in circumscribing relation with each of the plugs 64 and 74 for purposes of establishing a substantial hermetic seal between the plugs and the manifold whereby a plenum chamber, not designated, is provided at each of the appropriate ends of the packages, as illustrated in FIG. 8. A series of bores 80 extend through the plugs 64 and 74 for accommodating passage of coolant through the plugs. In order to facilitate passage of a coolant through the solar cell packages 12, the manifold 16 also is provided with a plurality of interconnected passageways 82 which conduct coolant discharged from the packages 12 for subsequent disposal. Thus it is possible to maintain the double-sided solar cells 32 at acceptable levels of temperature.
OPERATION
It is believed that in view of the foregoing description of the invention its operation should be apparent. However, with a view to assuring a complete understanding thereof its operation will be reviewed briefly at this point.
With the solar cell array 10 fabricated in the manner hereinbefore described, it is prepared for use simply by positioning the array in a suitable location and orienting the individual solar cell package to receive incident radiation. Of course, where desired, the packages may be connected with a tracking system, not shown, which includes a drive mechanism for imparting rotary motion to the solar cell packages 12, for purposes of tracking the sun across the sky.
With the individual solar cell packages mounted in a coupled relation in a supported relationship with the manifolds 14 and 16, rays A of incident radiation pass through the transparent wall of the housings to impinge upon the upper surfaces 34 of the double-sided solar cells 32, while rays B are reflected to impinge against the lower surfaces of the solar cells. Where the housing 18, which is of a substantially eliptical cross sectional configuration, is employed the surfaces of the longitudinal plates 26 function as reflectors for redirecting the rays B toward the surfaces 36 of the cells 32. However, where the housing 19, which is of a substantially circular cross sectional configuration, is employed, the reflecting surfaces 40 of the reflector 38 serve to redirect the rays B causing these rays to pass through the transparent housing and impinge on the lower surface 36 of the solar cell 32.
As a consequence of the radiaton incident upon the cells 32 a photovoltaic current is established and caused to flow through a voltage pick-off circuit including the contacts 66 and 68 and the spring finger 72. This current is then conducted from the array 10 employing a suitable electrical circuit, not shown.
In order to achieve a desired cooling of the cells 32 air, or other suitable coolant, is introduced into the manifold 14, under pressure, through the fitting 76 and caused to flow through the bores 80 and, consequently, the individual solar cell packages 12. Thus excessive heat is removed by convection from the solar cell packages 12.
In view of the foregoing, it should readily be apparent that the solar cell packages which embody the principles of the instant invention provide a practical solution to various problems encountered when employing photovoltaic cells in a terrestrial environment.
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In a solar cell array of terrestrial use, an improved double-sided solar cell package consisting of a photovoltaic cell having a metallized P-contact strip and an N-contact grid provided on opposite faces of the cell, a transparent tubular body forming an enclosure for the cell, a pedestal supporting the cell from within the enclosure comprising an electrical conductor connected with the P-contact strip provided for each face of the cell, and a reflector having an elongated reflective surface disposed in substantially opposed relation with one face of the cell for redirecting light to impinge thereon whereby the cell is subjected to incident radiation at each of its opposite faces.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority as a continuation-in-part of U.S. patent application Ser. No. 12/916,206 filed Oct. 29, 2010 and entitled “SYSTEM AND METHOD TO DETECT CHILD PRESENCE.” The content of the above-identified patent document(s) is hereby incorporated by reference.
TECHNICAL FIELD
[0002] Generally, the present disclosure relates to detecting the presence of a child in enclosed areas such as the wash drum of a washing machine or the interior of a refrigerator.
BACKGROUND
[0003] Many homes, offices, and buildings contain machines, such as refrigerators and washing machines, which have confined areas with doors that are secured or even sealed by automatic latching (mechanical, magnetic, etc.). Children, particularly small children, are known to explore and climb into such confined areas, which may result in serious injury or death if the child becomes trapped inside for an extended period of time or if the machine is activated while the child in within the machine.
[0004] Accordingly, there is a need in the art to detect the presence of a child within a confined area of a machine and to prevent activation of the machine while a child is inside.
SUMMARY
[0005] The presence of a child within an enclosed space in a machine, such as a washing machine, dishwasher or refrigerator, is detected using one or more MEMS sensors positioned to detect movement within the enclosed space through various measured characteristics. In preference, combinations of different types of MEMS sensors are utilized to detect the movement. For instance, movement may be attributed to the presence of a child inside the enclosed space rather than other factors with increased reliability if the determination is made based upon whether shifts in the center of gravity for a load supported inside the machine coincide with noise emanating from the interior of the enclosed space.
[0006] Before undertaking the DETAILED DESCRIPTION below, it may be advantageous to set forth definitions of certain words and phrases used throughout this patent document: the terms “include” and “comprise,” as well as derivatives thereof, mean inclusion without limitation; the term “or,” is inclusive, meaning and/or; the phrases “associated with” and “associated therewith,” as well as derivatives thereof, may mean to include, be included within, interconnect with, contain, be contained within, connect to or with, couple to or with, be communicable with, cooperate with, interleave, juxtapose, be proximate to, be bound to or with, have, have a property of, or the like; and the term “controller” means any device, system or part thereof that controls at least one operation, such a device may be implemented in hardware, firmware or software, or some combination of at least two of the same. It should be noted that the functionality associated with any particular controller may be centralized or distributed, whether locally or remotely. Definitions for certain words and phrases are provided throughout this patent document, those of ordinary skill in the art should understand that in many, if not most instances, such definitions apply to prior, as well as future uses of such defined words and phrases.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] For a more complete understanding of the present disclosure and the advantages thereof, reference is now made to the following brief description, taken in connection with the accompanying drawings and detailed description, wherein like reference numerals represent like parts:
[0008] FIG. 1 is a block diagram of one system implementing child detection within an enclosed space of a machine according to one embodiment of the present disclosure;
[0009] FIG. 2 is a high level flowchart of a safety process for detecting presence of a child within an enclosed space of a machine according to one embodiment of the present disclosure;
[0010] FIG. 3 is a high level flowchart of an alternate safety process based upon detecting presence of a child within an enclosed space of a machine according to another embodiment of the present disclosure;
[0011] FIG. 4 is a high level flowchart of an alternate safety process based upon detecting presence of a child within an enclosed space of a machine according to yet another embodiment of the present disclosure;
[0012] FIG. 5 is a block diagram of a second system implementing child detection within an enclosed space of a machine according to an embodiment of the present disclosure; and
[0013] FIG. 6 is a block diagram of a third system implementing child detection within an enclosed space of a machine according to an embodiment of the present disclosure.
DETAILED DESCRIPTION
[0014] FIGS. 1 through 6 , discussed below, and the various embodiments used to describe the principles disclosed in this patent document, are by way of illustration only and should not be construed in any way to limit the scope of the disclosure.
[0015] Detection of a child in a confined area using a child detection system (CDS) may detect the presence of a child through motion translated into an electrical signal by at least one motor or one or more sensors. By detecting the electrical signal, a user may be alerted to the presence of a child in a machine.
[0016] FIG. 1 is a block diagram of one system of implementing a child detection system (CDS) detecting the presence of a child in an enclosed spaced within a machine according to one embodiment of the present disclosure. System 100 includes an activation console 102 that electrically communicates via control signals with an engine or electric motor 104 , which in turn is coupled to a device associated with or within an enclosed space 106 within the machine. During operation of the system 100 , the activation console 102 is normally used to selectively activate the electric motor 104 to drive some mechanical device within the machine. Thus, the electric motor 104 may be coupled to the enclosed space 106 by a belt passing through or around a portion of the enclosed space 106 , by projection of a portion of the drive shaft of the electric motor 104 into the enclosed space, or by some other mechanical drive linkage. In one illustrative embodiment, machine 100 is a washing machine with a wash cylinder forming the enclosed space 106 , where the wash cylinder or drum is rotated by the electric motor 104 . In another illustrative embodiment, machine 100 is a dishwasher with a rotating sprayer within the enclosed space 106 that is rotated by the electric motor 104 . It is desirable to avoid activating the electric motor 104 when a child (or, equivalently, a small animal) is located within the enclosed space 106 of the machine 100 . Detection of the child within the enclosed space 106 of a machine 100 prior to activation of the electric motor 104 may prevent significant harm from occurring to the child.
[0017] In the exemplary embodiment of a washing machine, movement of the child within the enclosed space 106 formed by the wash cylinder is mechanically transferred to and causes motion within the electric motor 104 . Since electric motors also function as electric generators, mechanical movement of the wash cylinder in response to the child shifting therein is thus transformed into at least one electrical signal that may be detected at the activation console 102 . Similarly, in the exemplary embodiment of a dishwasher, movement by the child within the enclosed space 106 may cause movement of the rotating sprayer, which movement is transferred to and causes motion within the electric motor 104 . By detecting the presence of the child based on motion within the enclosed space 106 , a user of the machine 100 may be alerted to the presence of the child, for example, by sounding an acoustic alarm device (not shown) within the activation console 102 and/or flashing or otherwise activating one or more lights (also not shown) forming part of the activation console or otherwise visible from the exterior of the system 100 .
[0018] In the example shown in FIG. 1 , activation console 102 is intended to refer to any device that may be used to engage electric motor 104 into an operational state, to impart kinetic (mechanical) energy to a device associated with or within the enclosed space 106 . Activation console 102 may comprise one or more input devices and one or more screens that display the operational status, information, or other items related to the machine 100 .
[0019] Electric motor 104 in the example of FIG. 1 is intended to refer to any device capable of generating kinetic energy and transferring that energy to the machine associated with or within the enclosed space 106 , and that is conversely capable of detecting the transfer of kinetic energy to that machine from within enclosed space 106 . Examples of the electric motor 104 include, but are not limited to, an electromagnetic motor configured to transform an electric current into rotational kinetic energy. In one embodiment, during a period in which electric motor 104 is not in an active state as determined by the control signals from activation console 102 , kinetic energy or movement within the enclosed space 106 is mechanically transferred into the electric motor 104 , as by movement of a belt or other drive linkage between the electric motor 104 to the machine associated with or within enclosed space 106 (e.g., rotation or other shifting of the wash cylinder) or by direct rotation of the drive shaft of the electric motor 104 (e.g., by movement of the rotating sprayer).
[0020] The machine associated with or within the enclosed space 106 may be any device, apparatus, or unit that accepts mechanical drive force from the electric motor 104 . Examples of such mechanical drive force input include kinetic energy in the form of motion from an apparatus such as the wash cylinder and a connecting belt in a washing machine or a rotating sprayer in a dishwasher.
[0021] Those skilled in the art will recognize that the complete structure of a machine including an enclosed space posing a danger to children is not depicted in the drawings, and that the full details of operation of such a machine are not described. Instead, for simplicity and clarity, only so much of such a machine as is either unique to the present disclosure or necessary for an understanding of the present disclosure is depicted and described.
[0022] FIG. 2 is a high level flowchart of a safety process based upon detecting presence of a child within an enclosed space of a machine according to one embodiment of the present disclosure. The process 200 is preferably implemented within the machine controller 108 or similar control system of the machine 100 including an enclosed space 106 , such as within the controller 108 mounted within the activation console 102 for system 100 and coupled to electric motor 104 , generating control signals for starting and stopping operation of electric motor 104 . In the exemplary embodiment illustrated FIG. 2 , user activation of a user control to initiate operation of the machine is detected (step 202 ) and a check is made to determine whether motion has been detected inside the machine (step 204 ) since the machine was last operational. For example, the monitoring system electrically coupled to the electric motor 104 may set a flag if, at any time between the machine ending a last operational cycle and user activation of the control to start another operational cycle of the machine, movement within the enclose space 106 of the machine is detected based on current received from the electric motor 104 . Current or another electrical signal output from the electric motor 104 may reflect that motion occurred in the enclosed space.
[0023] If monitoring for motion within the enclosed space of the machine (step 206 ) was detected at any time during the monitoring period (which may be all or any part of the time since the machine was last operational), the electric motor 104 is inhibited from being activated. If the motor 104 is inhibited from being activated or the system 100 is otherwise inhibited from being activated or engaged (step 208 ), operator intervention may be required (step 210 ) to “unlock” the machine 100 and resume operational status. The operator may be required to perform a predefined routine to restart the machine 100 (step 212 ), such as checking the interior of the enclosed space 206 as determined by opening and closing a door on the machine (detected using a door sensor, not shown) or manually canceling the activation of the machine 100 and re-initiating operation, to override the safety block resulting from detection of motion within the machine. If no motion was detected in the enclosed space 106 of the machine 100 during the monitoring period, the machine 100 is allowed to be activated or engaged (step 214 ) and a corresponding update is displayed on the activation console 102 (step 214 ).
[0024] FIG. 3 is a high level flowchart of an alternate safety process based upon detecting presence of a child within an enclosed space of a machine according to another embodiment of the present disclosure. Where process 200 is implemented within a machine controller 108 for the system 100 , process 300 may be performed by a controller 110 or control system within or associated with the electric motor 104 (that is, a control system responding to switching signals to connect and disconnect various circuits within the electric motor 104 ). Thus, process 300 may be used separately from or in addition to process 200 within a particular system 100 .
[0025] In process 300 , monitoring of the motor for current caused (for example) by electromotive force produced by mechanical rotation of the motor's drive shaft is initiated (step 302 ). Such monitoring may be initiated, for instance, upon completion of a prior operating cycle for the machine 100 —that is, the machine controller (not shown) may signal the motor control system to initiate monitoring upon completion of the prior operational cycle for the machine.
[0026] As long as no current within the electric motor 104 is detected, indicating movement of the motor by an external force, the monitoring process continues. If current is detected within the motor 104 (step 304 ), that subsequent motor operation is restricted (step 306 ). For example, operation of the motor may be prevented or inhibited until a clearing signal is received by the motor controller 110 (for example, from the machine controller 108 ).
[0027] FIG. 4 is a high level flowchart of an alternate safety process based upon detecting presence of a child within an enclosed space of a machine according to yet another embodiment of the present disclosure. The process 400 is substantially similar to the process 300 illustrated in FIG. 3 , with the addition of allowing manual override of a motor lock after the restriction of motor operation. Manual override may be provided, for example, by a user accessible switch (not shown) within the activation console that is directly connected to the motor 104 . If a manual override is provided, upon restriction of the motor operation (step 306 ) the process begins polling for activation of the manual override (step 402 ). A particular set of actions may be required for the manual override, such as activation of a preset combination of user input buttons or keys at the activation console 102 , including activation concurrently or in a predetermined sequence. Alternatively, or in addition thereto, a door to the enclosed space 106 may need to be opened and closed prior to the motor being re-enabled.
[0028] FIG. 5 is a block diagram of a second system implementing child detection within an enclosed space of a machine according to an embodiment of the present disclosure. The system 500 is substantially similar to the system 100 of FIG. 1 , but with the further inclusion of one or more sensor(s) 502 connected to the activation console 102 and monitoring a portion of the enclosed space 106 (or a device associated with or within that space). Sensor(s) 502 may be either passive or active (or a combination of active and passive sensors), and may be any device capable of generating an electrical current or other signal based upon the detection of force or energy (including without limitation vibration, temperature, and air pressure). For example, the sensor 502 could be a passive pressure sensor located inside a refrigerator, washing machine, dishwasher, etc., and may be either a single large-area sensor or an array of coordinately operated sensors at various locations on interior surfaces of the enclosed space 106 . In either case, the pressure sensor(s) are used to detect changes in pressure at various locations that would be caused by movement of a child inside the enclosure, and to pass an electrical signal to the activation console 102 . Alternatively, the sensor(s) 502 may include in any combination of temperature sensor(s), accelerometer(s), one or more gyroscopes, infrared light emitter(s) and/or detector(s), or acoustic sensor(s) (i.e., microphone), or any of the sensors discussed herein. The sensor(s) 502 are configured and controlled to detect movement within the enclosed space 106 and/or the presence of an object with temperature in the range of human temperatures within the enclosed space 106 . Those skilled in the art will understand that the particular sensors utilized will depend on the nature of the machine 100 , since (for example) temperature sensors may be appropriate for refrigerators but not dishwashers. The activation console 102 may receive the signal and inhibit activation, or allow activation, as appropriate.
[0029] FIG. 6 is a block diagram of a third system implementing child detection within an enclosed space of a machine according to an embodiment of the present disclosure. System 600 is similar to systems 100 and 500 , but includes sensor(s) 602 . As shown, sensor(s) 602 may be mounted on or within the activation console 102 and/or the electric motor 110 . Preferably, however, at least some sensor(s) 602 are mounted within or in association with the enclosed space 106 (e.g., on walls for the enclosure).
[0030] Sensor(s) 602 are preferably one or more micro electro-mechanical system (MEMS) switches, configured to sense one or more of pressure (either due to direct physical forces or of air pressure), vibration or shock (acceleration), acoustic events, and temperature. MEMS sensors 602 are configured to monitor conditions inside the enclosed space of the machine 600 and to each generate an electrical signal to the machine controller 108 within the activation console 102 . The machine controller 108 employs MEMS sensors 602 to detect machine conditions that indicate the presence of a child within the enclosed space 106 .
[0031] The particular type and arrangement of MEMS sensors 602 within machine 600 , and the programming of machine controller 108 based upon signals from the MEMS sensors 602 , will necessarily depend upon the nature and function of the machine 600 . For example, pressure-sensitive MEMS sensors 602 positioned within vertical supports for the cabinet of a refrigerator would allow the machine controller 602 to monitor for movement within the interior of the enclosure by changes in the distribution of pressures (resulting from movement of a child's weight within the enclosed space), with the machine controller 108 determining whether shifts in pressure indicate presence of a child within the enclosed space by the regularity/variability of the pressure changes or the direction of movement indicated by such changes. A two-dimensional array of temperature-sensitive MEMS sensors 602 could monitor the interior of the refrigerator for movement of relatively “warm” spots while the refrigerator door is closed, with the machine controller 108 determining whether shifts in the location of warm spots indicate presence of a child within the interior of the refrigerator based upon the speed of movement and other factors. One or more vibration-sensitive MEMS sensors 602 could monitor for vibrations consistent with impact due to movement of a child within the refrigerator enclosure, with the machine controller 108 allowing for levels of background vibration while a compressor for the refrigeration system is running. Acoustic-sensitive MEMS sensors 602 may monitor for noise, with the machine controller 108 identifying the source of the noise and ascertaining regularity or irregularity to determine whether the noise indicates the presence of a child inside the refrigerator.
[0032] In each of the above cases, changes detected by MEMS sensor 602 may be qualified and/or disregarded, or filtered, based on whether the door to the enclosed space 106 is open or closed at the time the changes are detected. Thus, for example, a change in the center of gravity for the load supported by a refrigerator's internal frame need not be considered indicative of the presence of a child inside the refrigerator while the door is open (which might be due to items being placed inside), unless such changes continue after the door is closed. Further, the reliability of a determination may be considered increased when combinations of more than one indicator is detected, such as when detected changes in the center of gravity for the load supported inside a refrigerator while the door is closed coincide with detection of noise emanating from the interior of the refrigerator.
[0033] It should be noted that steps 204 and 206 in FIG. 2 may be performed by reading signals from the MEMS sensors 602 , and determining whether motion within the machine is detected based on such signals. In such a case, motion inside the enclosed space may be determined directly from movement of warm spots or the emanation of noise from the interior, or indirectly from pressure (center of gravity) shifts or vibrations.
[0034] It should also be noted that a variety of actions may be initiated by or within the machine in addition to or in lieu of steps 208 , 210 and 212 in FIG. 2 . For example, merely inhibiting operation of a motor may be insufficient to protect a child trapped within the enclosed space of the machine. As noted above, audible and visual warning indicators may be activated until disabled by the user. In addition, a latching mechanism for securing closure of the door to the enclosed space may be electronically opened. In the case of a refrigerator, an electromagnet repelling the magnetic seal of the door may be activated to cause the door to open.
[0035] It should be understood that although an exemplary implementation of one or more embodiments of the present disclosure are illustrated in the drawings and described above, the principles of the present disclosure may be readily implemented or adapted using any number of currently known techniques. The present disclosure should in no way be limited to the exemplary implementations, drawings, and techniques illustrated and described herein, including the exemplary design and implementation illustrated and described herein, but may be modified within the scope of the appended claims along with their full scope of equivalents.
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The presence of a child within an enclosed space in an appliance, such as a washing machine, dishwasher or refrigerator, is detected using one or more MEMS sensors positioned to detect movement within the enclosed space through various measured characteristics. In preference, combinations of different types of MEMS sensors are utilized to detect the movement. Movement may be attributed to the presence of a child inside the enclosed space, rather than resulting from other influences, with increased reliability if the determination is made based upon such combinations of different characteristics. Safety processes may be initiated upon detecting the presence of the child.
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FIELD OF THE INVENTION
[0001] The present invention is related in general to semiconductor integrated circuits, and particularly to electrically erasable and programmable read-only memory (EEPROM) devices. The present invention involves the novel concepts of programming the EEPROM device with body hot-electron injection, and using the body voltage to control the drain current. The devices are specifically adapted for integration through their small footprint and low programming power consumption.
BACKGROUND OF THE INVENTION
[0002] Non-volatile memories are a large part of the microelectronics infrastructure. There is a great need for devices in which information never, or only very rarely, has to be refreshed, and are fast, small, and consume little power. Such devices, and arrays made with these devices, have been known in the art for some time. For instance, one can find information on non-volatile memories in: “Nonvolatile Semiconductor Memories, Technology, Design and Applications” Edited by Chenming Hu, IEEE Press, New York, 1991.
[0003] Electrically erasable and programmable read-only memory (EEPROM) devices are the most widely spread, and useful of all the non-volatile memories. Practically all EEPROM-s are of the floating gate type, where the presence, or absence, of a charge on a floating gate alters the threshold of the device. Thus, the information is stored in the form of charge on a floating gate. An electrically programmable device of this type has to be able to change the amount of charge on the floating gate by purely electrical means. An overview of such conventional EEPROM-s can be found in: “Endurance brightens the future of Flash, fast memory as a viable mass-storage alternative,” Kurt Robinson, Electronic Component News, “Technology Horizons”, November 1988.
[0004] EEPROM devices usually use channel hot-electron injection for programming in order to achieve a fast programming speed of less than 10 μsec. In such conventional devices, during programming operation a large drain-to-source voltage is applied and a large gate-to-source voltage is also applied. Electrons flowing from source to drain gain energy from the large drain voltage and become hot electrons. The large gate voltage attracts the hot electrons, which are confined mostly near the drain region, towards the gate electrode, thus causing a gate current to flow. This gate current charges up the floating gate, causing an increase in the threshold voltage of the floating gate portion of the EEPROM device.
[0005] Although the gate voltage and the drain voltage during programming are both large during channel hot electron programming, the voltage difference (Vgate−Vdrain) is usually almost zero, or slightly negative. That is, the electric field in the gate insulator does not favor the injection of hot electrons from near the drain region into the gate insulator. Consequently, only a small fraction of the hot electrons near the drain actually contribute to the gate current, making channel hot electron programming a very inefficient process. For a typical EEPROM device, the maximum ratio of gate current to channel current is in the range of 10 −11 to 10 −8 , depending on the details of the device design and the voltages applied. With such a low programming current efficiency, typical EEPROM device requires a channel current of about 1 mA per bit during programming in order to achieve a programming speed of less than 110 μsec. The corresponding power dissipation during programming is about 5 mW per bit, assuming a drain to source voltage of 5 volt.
[0006] With such large power dissipation during programming, conventional EEPROM devices using channel hot-electrons for programming are not suitable for low power operations, particularly to battery-powered applications, where frequent reprogramming is required. As mobile and battery-operated systems are becoming more and more prevalent, there is an urgent need for EEPROM devices that dissipate relatively little power, even during programming.
SUMMARY OF THE INVENTION
[0007] In view of the above described difficulties with the current state of the art EEPROM-s, the present invention aims for several objectives to remedy the situation.
[0008] The object of this invention is a fast, low programming power, and suitable for very large scale integration (VLSI) EEPROM device.
[0009] It is another object of the present invention to teach important steps in the manufacturing methods of such EEPROM devices.
[0010] It is a further object of this invention to teach the integration of the novel EEPROM devices into memory arrays.
[0011] It is also an object of the invention to teach the integration of such EEPROM memory arrays into systems.
[0012] A common-gate (plate) EEPROM device having a substrate hot-electron injector is put forward in this invention. Also, in the new device the body voltage, instead of the gate voltage, is used to turn on and off the device channel. The common-gate configuration is conducive to the implementation of the device in SOI, or more generally, in a thin film technology.
[0013] During programming, the device body is reverse biased, and the common control gate is positively biased, with respect to the source and drain. A charge injector attached to the body causes electron injection into the device body, or substrate. As these substrate electrons drift vertically towards the gate electrode, they gain energy from the electric field caused by the reverse bias between the device body and the source and drain. The electrons with sufficient energy to surmount the silicon-SiO 2 energy barrier are injected into the floating gate, thus changing the threshold voltage of the EEPROM device. Since substrate hot-electrons directly impinge on the gate insulator, injection efficiency can easily be orders of magnitude higher than that during channel hot-electron injection. The injection efficiency is about 1×10 −4 , and it takes about 1 μsec to inject enough hot electrons into the floating gate to cause a threshold voltage shift of about 1.4 V. This injection efficiency is about 4 to 7 orders of magnitude higher than the channel hot electron injection in conventional EEPROM devices. For the nominal write conditions, the injection efficiency is about 8×10 −5 , and the write time is 1.2 μsec with a power consumption of 20 μW per bit during programming.
[0014] During erase operation, electrons in the floating gate are removed by tunneling. Depending on the device design, electrons in the floating gate can be removed by tunneling to the control gate or plate, or by tunneling back to the device body or source and drain. For example, the plate electrode can be negatively biased relative to the device body, source and drain, causing electrons to tunnel from the floating gate into the device body and source and drain. A voltage difference of 10V between the source/drain and plate during the erase operation is adequate for such a purpose.
[0015] During standby, the device body is reverse biased relative to the source and drain, causing the device to have a high threshold voltage. To read the device memory state, the device body is held at the same voltage as the source, causing the device to have a low threshold voltage.
[0016] In the fabrication of the disclosed EEPROM device an important step is a layer transfer. In such a step the device is transferred from a first wafer to a second wafer, ending in an up-side-down orientation relative to as it was on the first wafer. This step allows standard processing on both wafers, with the result that the up-side-down device provides easy access for contacting its body region, and several, or a great many, devices can share a common gate, or plate. These aspects lead to a small cell size in memory arrays.
[0017] In a memory array of the disclosed devices, the drain is connected to the bitline, the device body is connected to the wordline, while the control gate is a plate electrode.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] These and other features of the present invention will become apparent from the accompanying detailed description and drawings.
[0019] [0019]FIG. 1. shows in a cross sectional view one embodiment of the invention, a stack gate configuration EEPROM device.
[0020] [0020]FIG. 2. shows the EEPROM device threshold voltage as a function of the device body voltage.
[0021] [0021]FIGS. 3. to 14 . outline the process in cross sectional views for fabricating two adjacent stack gate EEPROM devices in a memory array configuration.
[0022] [0022]FIG. 3. shows the starting material as a silicon-on-insulator (SOI) wafer.
[0023] [0023]FIG. 4. shows the formation and patterning of the gate insulator and the floating gate.
[0024] [0024]FIG. 5. shows the formation of the heavily doped n-type source and drain regions.
[0025] [0025]FIG. 6. shows the formation of planarized isolation oxide.
[0026] [0026]FIG. 7. shows the formation of an insulator layer and a polysilicon layer on top of the floating gate.
[0027] [0027]FIG. 7A. illustrates the transferring the device structure layer from a first substrate, or wafer, to a second substrate.
[0028] [0028]FIG. 8. show illustrates the structure after bonding to another wafer.
[0029] [0029]FIG. 9. shows the structure in cross section in the width direction at this stage of the precessing.
[0030] [0030]FIG. 10. shows the structure after patterning an oxide layer to expose the device body regions.
[0031] [0031]FIG. 11. shows the formation of a polysilicon layer.
[0032] [0032]FIG. 12. shows the structure after reactive ion etching of the polysilicon layer.
[0033] [0033]FIG. 13. shows the structure after the deposition of a layer of oxide, planarization of the oxide layer, and doping the polysilicon sidewalls by ion implantation.
[0034] [0034]FIG. 14. shows the structure after etching the oxide to form contacts to the source and drain regions.
[0035] [0035]FIG. 15. shows in a cross sectional view one embodiment of the invention, a split gate configuration EEPROM device.
[0036] [0036]FIGS. 16. to 29 . outline the process in cross sectional views for fabricating two adjacent split gate EEPROM devices in a memory array configuration.
[0037] [0037]FIG. 16. shows the starting material comprising an SOI wafer.
[0038] [0038]FIG. 17. shows the structure after gate polysilicon and gate insulator have been formed and patterned.
[0039] [0039]FIG. 18. shows the structure after a shallow heavily doped n-type layer has been formed.
[0040] [0040]FIG. 19. shows the structure after oxide is deposited and planarized to form isolation regions.
[0041] [0041]FIG. 20. shows the structure after an insulator layer is formed on the polysilicon regions that form the floating gates.
[0042] [0042]FIG. 21. shows the structure after a layer of polysilicon has been deposited.
[0043] [0043]FIG. 22. shows the structure after bonding to a second SOI wafer.
[0044] [0044]FIG. 23. shows the structure after isolation oxide regions have been formed.
[0045] [0045]FIG. 24. shows the cross section view along the device width direction of the floating gate region at this stage of the processing.
[0046] [0046]FIG. 25. shows the cross section view along the device width direction of the regular gate region at this stage of the processing.
[0047] [0047]FIG. 26. shows the structure after patterning of an oxide layer and formation of a polysilicon layer.
[0048] [0048]FIG. 27. shows the structure after reactive ion etching of the polysilicon layer.
[0049] [0049]FIG. 28. shows the structure after the deposition of a layer of oxide, planarization the oxide layer, and doping the polysilicon regions by ion implantation.
[0050] [0050]FIG. 29. shows the structure after etching the oxide to form contacts to the source and drain regions.
[0051] [0051]FIG. 30. Schematically shows an electronic system containing an EEPROM array of the present invention as its component.
DETAILED DESCRIPTION OF THE INVENTION
[0052] An EEPROM device having a substrate hot-electron injector for high-speed and low-power programming is disclosed. This device is adapted for large scale integration. It fits with standard silicon technology processing, it is tightly packable on chips with each device having appropriate isolation. For a given linewidth capability, the size of the devices is state of the art. The control lines operating this device are similar in number and complexity to the current practice in EEPROM arrays. EEPROM arrays built with these devices can be incorporated in electronic systems practically by a simple “plug in”. At the same time, such arrays inherit the low-power, high-speed advantage of the disclosed devices.
[0053] In the embodiments to be described the EEPROM body is p-type, and the programming charge is consisting essentially of electrons. However, this should not be read as a limitation on the invention. It is understood that an embodiment where the body is n-type, and consequently other regions of the device are also changed in type, and the programming charge consists essentially of holes, is within the scope of the invention. Most embodiments where the body is p-type, can also be implemented in configurations where the body is n-type.
[0054] The invented EEPROM device rests on the top of an insulating layer. The insulating layer in one embodiment is SiO 2 , which in turn is on top of a silicon substrate. This embodiment is typical of an SOI technology. The disclosed devices are also compatible with a general thin film technology framework. In thin film technologies layers of various materials are deposited, which at times may not be of the same high quality as those of SOI technology. However, thin film technology can offer other advantages, such as cost of manufacturing.
[0055] The fabrication of the invented EEPROM device is benefitting from a layer transfer step. In such a step the device is transferred from a first substrate to a second substrate, ending in an up-side-down orientation relative to its orientation on the first substrate. This step allows standard processing steps on both substrates, with the result that the up-side-down device provides easy access for contacting its body region, while many devices can share a single gate, or plate. These aspects lead to a small cell size in a memory array.
[0056] The disclosed device differs from those in the art in that programming is done by charge injection through the body, and the device is turned on or off not by the gate, but through the body effect, by an appropriate bias on the source-body junction.
[0057] Charge injection into the body is accomplished by various injection means. In differing embodiments differing means may be used. Injecting minority carriers through a semiconductor p-n junction is one preferred embodiment. In another embodiment injection of electrons into the body can be achieved from a metal-semiconductor junction, a so called Schottky barrier junction. Yet another embodiment can use injection of carriers via tunneling across an appropriately biased thin insulating barrier.
[0058] [0058]FIG. 1 shows in a cross sectional view one embodiment of the invention, a stack gate configuration EEPROM device. In a stack gate structure the floating gate overlaps the device channel region completely.
[0059] The device rests on a plate 104 , which is the control gate of the device. In the memory array the plate is contacted and controlled by the plate-line 114 . In many embodiments the plate is shared by two, or by a plurality of memory cell devices. The plate is isolated from the floating gate 105 by insulator 122 . Insulator 122 in a preferred embodiment is SiO 2 . The floating gate is isolated by another insulator 121 , typically SiO 2 , from the source 103 , body 101 , and drain 102 . Insulators 61 and 81 isolate one device from another device at the gate level and at the body level, respectively. The p-type body is contacted by an n + -type electron injector 106. This arrangement is an embodiment of injection means, namely in the form of a p-n semiconductor junction. In an EEPROM memory array, besides the plate-line 114 , further control lines are also contacting the device. The bitline 112 contacts the drain 102 . The wordline 111 contacts the body 101 , since in this device the drain current is being controlled by a voltage between the source and the body. A source-line 113 contacts the source 103 , and an injection line 116 contacts the electron injector 106 .
[0060] During programming, the device body 101 is reverse biased with respect to the source 103 and drain 102 , the control gate 104 is positively biased with respectively to the source 103 and drain 102 , and the injector 106 is forward biased with respected to the device body 101 . Electrons are injected from the injector 106 into the device body 101 or substrate. As these substrate electrons drift vertically towards the gate electrode 104 , they gain energy from the electric field caused by the reverse bias between the device body 101 and the source 103 and drain 102 . The electrons with sufficient energy to surmount the silicon-SiO 2 energy barrier 121 are injected into the floating gate 105 , thus changing the threshold voltage of the EEPROM device.
[0061] During erase operation, electrons in the floating gate 105 are removed by tunneling. Depending on the device design, electrons in the floating gate can be removed by tunneling to the control gate or plate 104 , or by tunneling back to the device body 101 or source 103 and drain 102 . For example, the plate electrode 104 can be negatively biased relative to the device body 101 , source 103 and drain 102 , causing electrons to tunnel from the floating gate 105 into the device body 101 and source 103 and drain 102 .
[0062] During standby, the device body 101 is reverse biased relative to the source 103 and drain 102 , causing the device to have a high threshold voltage. To read the device memory state, the device body 101 is held at the same voltage as the source 103 , causing the device to have a low threshold voltage.
[0063] In one embodiment the p-type silicon body 101 has a uniform doping concentration of 1×10 17 cm −3 , with an oxide thickness of 7 nm for insulator 121 , and an oxide thickness of 20 nm for insulator 122 . The operating voltages for this embodiment are given in Table 1. As a naming convention, the ‘1’ is referred to as a true state.
TABLE 1 bitline wordline injector-line source-line plate-line read 1 V 0 V 0 V 0 V 2 V write ‘0’ 0 V −4 V −4 V 0 V 4.5 V write ‘1’ 0 V −3.2 V −4 V 0 V 4.5 V erase 4 V 4 V 4 V 4 V −6 V standby 0 V −3 V 0 V 0 V 2 V
[0064] In FIG. 2 the EEPROM device threshold voltage as a function of the device body voltage is shown for the same as embodiment that gives Table 1. FIG. 2 shows the threshold voltage in the erased state 22 (no injection charge) and in the programmed state 21 (charge injection=1.5×10 12 cm −2 ). It clearly indicates that under a common-gate voltage of 2V, the device is turned off in the standby mode by a reverse body-bias of 3V, and the device programmed state can be satisfactorily read with zero body-bias in the read mode.
[0065] [0065]FIGS. 3. to 14 . outline the process in cross sectional views for fabricating two adjacent stack gate EEPROM devices in a memory array configuration.
[0066] [0066]FIG. 3 shows the starting material comprising a silicon-on-insulator (SOI) wafer. It has a first substrate, typically a Si wafer 31 , and an insulating layer 32 on top of the substrate, typically SiO 2 . On top of the insulator there is a high quality Si layer 33 . This Si layer, 33 , is where devices are being fabricated.
[0067] [0067]FIG. 4. shows the formation and patterning of the gate insulator 121 and the floating gate 105 . The floating gate is formed from a layer of polysilicon.
[0068] [0068]FIG. 5. shows the formation of the heavily doped n-type source 103 and drain 102 regions, using the patterned floating gate as a ion implantation mask. The source 103 and drain 102 are defining the body 101 region.
[0069] [0069]FIG. 6. shows the formation of planarized isolation oxide 61 .
[0070] [0070]FIG. 7. shows the formation of an insulator layer 122 and a polysilicon layer 104 on top of the floating gate 105 . This polysilicon layer forms the plate (control gate of the devices) 104 electrode of the memory array.
[0071] [0071]FIG. 7A. shows an illustration of transferring the device structure layer from a first substrate 31 , or wafer, to a second substrate 83 . Device layer 999 is a multitude of layers at this point of the process, including all the processing shown in FIGS. 3 to 7 . This device layer is, by methods known in art, bonded or transferred onto a second insulting layer, typically SiO 2 82 . Once the first substrate 31 and insulator 32 are removed, the devices in layer 999 are resting on a new, second, substrate in an up-side-down position in comparison to their position on the first substrate.
[0072] There are several ways known in the art that a layer transfer can be carried out, such as the so called SmartCut (a registered trademark of SOITEC Corporation) technique, or the so called ELTRAN (Epitaxial Layer TRANsfer, a registered trademark of Canon K.K.) process, as described in U.S. Pat. No. 5,371,037 to T. Yonehara, titled: “Semiconductor Member and Process for Preparing Semiconductor Member”, and further techniques as well. For the embodiments of the present invention any known layer transferring technique or process can be used.
[0073] [0073]FIG. 8. shows the structure after bonding to another, (second) wafer 83 , and after the substrate 31 and oxide 32 of the original SOI wafer has been removed after bonding, and after isolation oxide 81 has been formed to isolate the two memory devices from their neighbors. Thus, the silicon that forms the device regions now lie on top of the plate electrode 104 and the floating gate regions 105 . The devices are in an up-side-down position in comparison as they were on the first substrate 31 .
[0074] [0074]FIG. 9. shows the structure in cross section in the width direction at this stage of the processing. It shows that the device body 101 and floating gate 105 of the individual devices are isolated by 61 and 81 , but in this embodiment there is a common plate electrode 104 for the memory array. This plate electrode in various embodiments can belong to individual cells, be shared by two cells, or can be shared by a large plurality of cells, for instance by a whole subarray, or even a whole array.
[0075] [0075]FIG. 10. shows the structure after forming and patterning an oxide layer 1011 to expose the device body regions 101 .
[0076] [0076]FIG. 11. shows the formation of a polysilicon layer 1111 . This polysilicon layer will be used to form the heavily n-type doped injector electrode and to form a heavily doped p-type contact to the device body.
[0077] [0077]FIG. 12. shows the structure after reactive ion etching of the polysilicon layer 1111 without using a masking step, showing the polysilicon sidewalls 1112 . Alternatively, the polysilicon layer can be patterned using a masking step, but the resulting polysilicon regions will be larger than the sidewalls, leading to a larger device area.
[0078] [0078]FIG. 13. shows the structure after the deposition of a layer of oxide 1312 , planarization of the oxide layer, and doping the polysilicon sidewalls by ion implantation. The p + polysilicon regions are the body contacts 1311 , and the n + polysilicon regions are the electron injectors 106 , the means for injecting a programming current in this embodiment.
[0079] [0079]FIG. 14. shows the structure after etching the oxide 1312 to form contacts to the source 103 and drain 102 regions. It shows that the pair of devices share a common source 103 to minimize device area in an array.
[0080] The stack gate device configuration can have an over-erasure exposure. Over-erasure occurs when the erase process results in a net negative amount of charge in the floating gate 105 , causing the floating gate to be positively charged and the threshold voltage of the device to be smaller than intended. A split gate device structure embodiment has no exposure to over erasure. In the split gate device structure the device channel is divided into two parts in series, one part is covered by the floating gate 105 , and the other by the control gate 104 . Thus, even if over-erasure occurs, the device threshold voltage is determined by the control gate part of the device. In all other aspects the stack gate and split gate configuration devices work identically.
[0081] [0081]FIG. 15. shows in a cross sectional view one embodiment of the invention, a split gate configuration EEPROM device. The device rests on a plate 104 , which is the control gate of the device, and in this embodiment it also extends 124 over part of the body 101 . The shallow n + -type region 125 connects the device channel of the floating gate region 105 with the device channel of the gate region 124 . Regions 104 and 124 , of course, are electrically connected. In the memory array the plate is contacted and controlled by the plate-line 114 . In many embodiments the plate is shared by two, or by a plurality of memory cell devices. The plate is isolated from the floating gate 105 by insulator 122 . Insulator 122 in a preferred embodiment is SiO 2 . The floating gate is isolated by another insulator 121 , typically SiO 2 , from the source 103 , body 101 , and drain 102 . Insulators 61 and 81 isolate one device from another device in the gate level and in the body level, respectively. The p-type body is contacted by an n + -type electron injector 106 . This arrangement is an embodiment of the injection means, namely as a p-n semiconductor junction. In an EEPROM memory array besides the plate-line 114 , further control lines are contacting the device. The bitline 112 contacts the drain 102 . The wordline 111 contacts the body 101 , since in this device the drain current is being controlled by a voltage between the source and the body. A source-line 113 contacts the source 103 , and an injection line 116 contacts the electron injector 106 .
[0082] [0082]FIGS. 16. to 29 . outline the process in cross sectional views for fabricating two adjacent split gate EEPROM devices in a memory array configuration.
[0083] [0083]FIG. 16. shows the starting material comprising an SOI wafer: the first substrate typically a Si wafer 31 , the insulating layer 32 on top of the wafer, typically SiO 2 , and the high quality Si layer on top the insulator 33 . This Si layer 33 is the one where devices are being fabricated.
[0084] [0084]FIG. 17. shows the structure after gate polysilicon and gate insulator 121 have been patterned. Two polysilicon regions will be used in one device, with one polysilicon region forming the floating gate 105 and another polysilicon region forming the gate electrode 124 of the split gate device.
[0085] [0085]FIG. 18. shows the structure after a shallow heavily doped n + -type source 103 and drain 102 regions, using the patterned floating gate as a ion implantation mask. The shallow n + -type region 125 connects the device channel of the floating gate region 105 with the device channel of the gate region 124 .
[0086] [0086]FIG. 19. shows the structure after oxide is formed and planarized to form isolation regions 61 .
[0087] [0087]FIG. 20. shows the structure after an insulator layer 122 is formed on the polysilicon regions that form the floating gates 105 . No insulator is formed on the polysilicon regions that form the regular gate electrodes 124 .
[0088] [0088]FIG. 21. shows the structure after a layer of polysilicon has been deposited 104 . This polysilicon layer is in electrical connection to the gate polysilicon regions 124 , but is insulated from the floating gate regions 105 by insulator 122 . Thus, this polysilicon 104 becomes the control gate of the two split gate devices. In the memory array arrangement, this polysilicon layer functions as a plate electrode, connected to plate-line 114 .
[0089] The next step is the layer transfer, which occurs for the split gate embodiment in the same manner as for the stack gate embodiment. This step is as illustrated on FIG. 7A, and described in the discussion of FIG. 7A.
[0090] [0090]FIG. 22. shows the structure after bonding to another, (second) wafer 83 , and after the substrate 31 and oxide 32 of the original SOI wafer has been removed after bonding. Thus, the silicon that forms the device regions now lies on top of the plate electrode 104 , the floating gate regions 105 and gate regions 124 . The devices are in an up-side-down position in comparison as they were on the first substrate 31 .
[0091] [0091]FIG. 23. shows the structure after isolation oxide regions 81 have been formed to isolate the pair of devices from their neighbors in the memory array.
[0092] [0092]FIG. 24. shows the cross section view along the device width direction of the floating gate region 105 at this stage of the processing. It shows that the device body 101 and floating gate 105 of the individual devices are isolated by 61 and 81 , but in this embodiment there is a common plate electrode 104 for the memory array. This plate electrode in various embodiments can belong to individual cells, be shared by two cells, or can be shared by a large plurality of cells, for instance by a whole subarray, or even a whole array.
[0093] [0093]FIG. 25. shows the cross section view along the device width direction of the regular gate region 124 at this stage of the processing. It shows that the device body 101 is isolated by 61 and 81 , but in this embodiment there is a common plate electrode 104 , shorted to the gate 124 , for the memory array. This plate electrode in various embodiments can belong to individual cells, be shared by two cells, or can be shared by a large plurality of cells, for instance by a whole subarray, or even a whole array.
[0094] [0094]FIG. 26. shows the forming and patterning an oxide layer 1011 , and formation of a polysilicon layer 1111 . This polysilicon layer will be used to form the heavily n + -type doped injector electrode and to form the heavily doped p + -type contact to the device body.
[0095] [0095]FIG. 27. shows the structure after reactive ion etching of the polysilicon layer 1111 without using a masking step, showing the polysilicon sidewalls 1112 . Alternatively, the polysilicon layer can be patterned using a masking step, but the resulting polysilicon regions will be larger than the sidewalls, leading to a larger device area.
[0096] [0096]FIG. 28. shows the structure after the deposition of a layer of oxide 1312 , planarization of the oxide layer, and doping the polysilicon sidewalls by ion implantation. The p + polysilicon regions are the body contacts 1311 , and the n + polysilicon regions are the electron injectors 106 , the means for injecting a programming current in this embodiment.
[0097] [0097]FIG. 29. shows the structure after etching the oxide 1312 to form contacts to the source 103 and drain 102 regions. It shows that the pair of devices share a common source 103 to minimize device area in an array.
[0098] [0098]FIG. 30. Schematically shows an electronic system 1000 containing an EEPROM array 100 of the present invention as its component. The electronic system 1000 can be digital, such as a computing device, or computer, or it can have analog components as well, such as a communication device. Furthermore, any battery operated system, such as a cellphone, portable computer, or sophisticated toy is a system that can take advantage of the present invention. Any electronic system using EEPROM-s can benefit from the herein disclosed device. The availability of such a low powered fast EEPROM will likely spur new applications, as well.
[0099] Many modifications and variations of the present invention are possible in light of the above teachings, and could be apparent for those skilled in the art. The scope of the invention is defined by the appended claims.
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A low programming power, high speed EEPROM device is disclosed which is adapted for large scale integration. The device comprises a body, a source, a drain, and it has means for injecting a programming current into the body. The hot carriers from the body enter the floating gate with much higher efficiency than channel current carriers are capable of doing. The drain current of this device is controlled by the body bias. The device is built on an insulator, with a bottom common plate, and a top side body. These features make the device ideal for SOI and thin film technologies.
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FIELD OF THE INVENTION
The present invention relates to a tensioner for endless driving elements, such as chains and belts, and particularly a tensioner having a tensioning piston provided with locking means, and a locking piston which is implemented such that it is adapted to be engaged with and disengaged from the locking means so as to arrest or release the movement of the tensioning piston.
BACKGROUND OF THE INVENTION
Such a tensioner is known e.g. from EP 0 657 662 A 2. This chain tensioner comprises a tensioning piston having a plurality of locking grooves on the outer circumference thereof, the locking grooves being engaged by a spring-loaded locking piston. The front face of the locking piston is beveled and can be acted upon by an oil pressure so as to disengage the locking position. The locking means guarantees that a locking effect is produced when the engine oil hydraulic system is switched off and that the locking piston can no longer retract. This has the effect that a certain pretension is maintained, even if the engine is at rest, in spite of possible oil leakage from the pressure chamber. Hence, a predetermined tension, which is independent of the engine oil hydraulic system, will exist when the engine is started. As soon as sufficient pressure has built up, the locking means will be disengaged and the tensioning piston will operate in the usual way.
A similar tensioner is known e.g. from DE 195 48 923 A1. In addition, conventional locking devices are provided on chain tensioners and the like, but these locking devices only serve to carry out a readjustment and to limit the retraction path of the tensioning piston to a pre-determined value. Such structural designs are used for wear compensation. Locking de-vices connected to the engine oil hydraulic system are disadvantageous insofar as they are subjected to the fluctuations of the hydraulic pressure and to a possible pressure build-up in the area of the tensioning piston. In the case of conventional locking devices, the locking piston is forced back by the teeth on the tensioning piston against the force of a spring, and this will entail wear.
It is therefore the object of the present invention to improve the structural design of a tensioner of the type used with chaims and belts.
In accordance with the present invention, this object is achieved by the features that the locking piston comprises an operating section causing said locking piston to move to the arresting position and to the release position, and a locking area used for engagement with the locking means of the tensioning piston and arranged separately from the operating section. Due to the fact that the operating point of the locking piston and the point of engagement are separated from one another, it is no longer necessary that the locking area is acted upon by operating forces so as to disengage the locking piston. In the case of hydraulically operated tensioners this means e.g. that the locking area of the locking piston need no longer be exposed directly to the engine oil hydraulic pressure. Actuation in one direction (arresting position) as well as in the other direction (release position) takes place at some other point. A great variety of operating mechanisms for achieving a piston movement can be employed. This separation of the locking function and of the operating function also permits the locking piston to be controlled in a purposeful manner in dependence upon the operating parameters. Conventional locking devices of the readjustment type as well as locking devices which are readjustable by an engine oil hydraulic system are always provided with operating means acting directly on the locking area.
According to an advantageous embodiment, the operating section of the locking piston can be provided with a piston area which is adapted to have applied thereto an operating pressure of a hydraulic fluid, the operating direction of the piston area being directed towards the release position of the locking piston. This measure has the effect that the locking piston will be displaced to the release position in response to application of a hydraulic pressure. Such a structural design could be used in internal combustion engines and connected to the engine oil hydraulic system.
In accordance with a preferred embodiment, a spring means can be provided, which acts on the operating area of the locking piston and which is effective in the direction of the arresting position of the locking piston. This measure has the effect that the locking piston is primarily forced into the arresting position by the spring force of the spring means. This means that an operating force in the opposite direction must always be larger so as to cause unlocking.
According to an advantageous embodiment, the locking area of the locking piston can be designed such that a hydraulic force balance is caused. Such a structural design allows the locking area of the locking piston to be subjected to a pressure medium, without the pressure medium causing any essential force component on the locking area for operating the locking piston. A person skilled in the art knows that, in order to achieve this, he must cause forces to act in opposite directions so that these forces will compensate each other (as far as the actuation is concerned). Hence, such a tensioner could definitely be arranged in the pressure chamber of the tensioning piston; pressure fluctuations of the pressure in the pressure chamber will not have any influence on the operation of the locking piston, neither into the arresting position nor into the release position. In hitherto used devices comprising controlled locking devices, such pressure fluctuations have always prevented the locking piston from moving immediately to its arresting position, when e.g. the engine hydraulic system had been switched off. The locking effect only occurred when the pressure had been reduced to a certain extent by leakage at the locking area of the locking piston. Such a delay is prevented by the structural design chosen.
In accordance with an advantageous embodiment, the locking area can be provided in the form of a locking opening in a locking plunger which extends away from the operating section, at least a portion of the locking means of the tensioning piston extending through the locking opening. The locking opening guarantees that a pressure medium in its interior will produce force components over the whole area of the opening and that the forces will compensate each other in such a way that the actuation of the locking piston will not be supported. This is a simple structural measure by means of which the locking area can be designated such that is not subjected to the influence of pressure forces.
In addition, the locking opening may be provided with a locking projection, which is arranged on the inner surface of the locking opening on one side thereof and which is used for engagement with the locking means of the tensioning piston. Such a locking projection on the inner side does not have any influence on the force conditions in the operating direction of the locking piston and guarantees nevertheless a reliable engagement with the locking means of the tensioning piston.
According to one variant, the locking means of the tensioning piston may comprise a lock-ing rod provided with teeth and extending through the locking opening of the locking piston. The operating paths of the tensioning piston and of the locking piston will therefore cross and individual components of the two pistons will interengage. A very compact and very robust structural design is provided in this way.
The locking rod can have a circular basic cross-section, the locking opening in the locking plunger being then implemented as an elongated hole which is adapted to this basic cross-section. This length (seen in the direction of the longitudinal axis of the locking piston) of the elongated hole can then correspond to at least to the operating stroke of the locking piston between the release position and the arresting position. This means that the locking rod and the locking piston part providing the locking opening can also mutually guide themselves, since the amount of play must be chosen precisely such that the locking rod can be dis-placed freely in the elongated hole in the release position. In the case of such a variant, the locking rod can also be implemented as an extension of the actual tensioning piston having a smaller diameter. However, also other cross-sections are possible instead of the circular cross-section.
When, in accordance with one variant, the inner surface of the locking opening is provided on one side thereof with an undercut portion which merges with the locking projection, the locking opening provides also in the arresting position a contact shoulder for close contact with the locking rod. When the locking piston is implemented as a plastic component or as a cast member, this undercut portion will also reduce the accumulation of material.
In accordance with one embodiment, the tensioning piston is guided in a housing, a pressure chamber is formed between the housing and the tensioning piston, the locking means extend from the inner to the outer side of the pressure chamber, and the teeth are located outside of the pressure chamber in the fully retracted position of the tensioning piston. This is to be regarded as an additional measure for displacing the locking area of the locking piston away from the pressure area of a fluid-operated tensioning piston. Depending on the structural design of the housing, the locking area will then only be subjected to a leakage flow of the fluid. Oscillating conditions occurring in the pressure medium during operation of the tensioning means will therefore not affect the locking piston.
According to a preferred embodiment, the locking piston can be guided in a housing such that it is separated from a pressure chamber of the tensioning piston. The two pistons can also be arranged in a common housing; in this case, only the locking means and the locking area cross each other and are adapted to be brought into engagement with one another.
According to a further embodiment of the tensioner for an internal combustion engine hav-ing an engine oil circuit, the piston area of the locking piston can be acted upon by the hy-draulic pressure of the engine oil circuit. By selecting an advantageous supply means, it can here be guaranteed that hydraulic oscillations of the type occurring in the area of the pres-sure chamber of the tensioning piston are decoupled as far as possible from the operation of the locking piston. In the simplest case, this delimitation is effected via a non-return valve.
BRIEF DESCRIPTION OF THE DRAWINGS
In the following, an embodiment of the present invention will be explained in detail making reference to a drawing, in which:
FIG. 1 shows a hydraulic chain tensioner according to the present invention in a fully sec-tional view,
FIG. 2 shows the chain tensioner of FIG. 1 in a sectional view along line II—II and
FIG. 3 shows the chain tensioner of FIG. 1 in a sectional view along line II—II.
DETAILED DESCRIPTION OF THE INVENTION
The chain tensioner 1 shown in FIG. 1 to 3 is provided with a locking function, in particular when the hydraulic circuit is switched off.
The chain tensioner 1 essentially comprises a cast housing 2 which consists e.g. of an aluminium die casting, a tensioning piston 3 which is axially guided in the housing 2 , and a locking piston 4 which is guided in the housing 2 at right angles to the tensioning piston 3 . The tensioning piston 3 is guided in a cylindrical bore 5 in the housing 2 and comprises a cylindrical guide sleeve 6 and a piston head 7 press-fitted into the guide sleeve 6 and consisting e.g. of a suitable plastic material. The guide sleeve 6 is preferably produced from steel. A portion of the piston head 7 rests on the end face of the guide sleeve 6 so that it is guaranteed that an endless driving element, e.g. a chain, or the tensioning area of a tensioning rail will come into contact only with the piston head 7 . In the interior of the guide sleeve 6 , the piston head 7 merges with a cylindrical locking rod 8 having, at the free end thereof, locking teeth 9 acting as locking means. The locking teeth are implemented as a circumferentially extending annular groove having a triangular cross-section, so that a sawtooth profile is formed in cross-section. The direction of the sawtooth profile is chosen such that an extension, but not a retraction, of the tensioning piston 3 can be blocked. Between the piston head 7 and the locking rod 8 a hollow-cylindrical annular space 10 is provided in the middle area of the locking rod 8 , said annular space having arranged therein a helical compression spring (not shown). The compression spring rests on the back 11 of the piston head 7 and on the base 12 of the bore 5 .
The chain tensioner 1 is shown at a position of transport. At this position, the tensioning piston 3 is fully retracted and arrested by a securing pin 12 . The compression spring, not shown, in the annular space 10 is compressed in its maximum tensioning condition. When the chain tensioner 1 has been installed with the aid of the fastening sleeves 13 and 14 on the housing 2 , the securing pin 12 is removed, whereby the transport position will be re-leased. The tensioning piston 3 is then in tensioning contact with e.g. the contact area of a tensioning rail, which, in turn, is pressed against a chain.
From the sectional view of FIG. 3 it can be seen that the annular space 10 and the free space of the bore 5 extending below the tensioning piston 3 can communicate via a hydrau-lic channel 37 in the housing 2 with the engine oil hydraulic system of an internal combustion engine to which the chain tensioner 1 is secured. This means that engine oil can flow into this pressure chamber via a non-return valve 36 . The hydraulic fluid flows into the hy-draulic channel 37 via the non-return valve 36 which is press-fitted into a lateral bore 38 of the housing. This hydraulic channel extends parallel to the locking teeth 9 and parallel to the bore 29 in the bottom. Also a locking plunger 16 extends in this hydraulic channel 37 so that both the locking plunger 16 and the locking teeth 9 on the locking rod 8 are subjected to the hydraulic pressure. Due to the displaced section along line II—II, the non-return valve 36 is shown in FIG. 2 in a view which is only a fragmentary sectional view. In the operating state, the tensioning function is primarily applied by this hydraulic pressure whose force exceeds the tensioning force of the spring. The hydraulic fluid in the pressure chamber is therefore subjected to the vibrations of the tensioning piston 3 and relief only takes place via leakage flows. When the engine oil hydraulic pressure increases, the tensioning force of the tensioning piston 3 will increase as well.
The locking piston 4 , which is displaceable in the housing 2 at right angles to the tensioning piston 3 , comprises a cylindrical operating section 15 and a locking plunger 16 arranged on said operating section 15 . Only the locking plunger 16 crosses the locking rod 8 of the tensioning piston 3 . The operating section 15 is provided with an annular piston area 17 . In addition, said operating section 15 is guided in a cylindrical bore 18 such that it is axially displaceable therein. Between the piston area 17 and the base area 19 of the operating section a pressure chamber 20 is defined, which communicates via a supply passage 21 with the engine oil hydraulic system. It follows that, when pressure is built up in the pressure chamber 20 , this will have the effect that the locking piston 4 is displaced upwards (cf. FIG. 1 ) to a release position. In the unloaded condition, the locking piston 4 is pressed down-wards into an arresting position (cf. FIG. 1 ) via a compression spring 22 which is arranged in a cylindrical bore 23 of the operating section 15 and which rests on a support disk 24 se-cured by a retainer ring 25 , said cylindrical bore 23 being open at the rear. The spring force is dimensioned such that, in the operating state, it will be bridged by the pressure in the pressure chamber 20 .
The locking plunger 16 is rectangular in cross-section and extends in a guide opening 26 through the housing 2 and projects beyond the housing on one side thereof. In addition, the locking plunger 16 is provided with hollow spaces 27 , which permit the locking plunger 16 to be also implemented as an injection-molded part consisting of plastic materials (so as to avoid accumulations of material).
The bore 5 for the tensioning piston 3 and the guide bore 26 for the locking plunger 16 communicate only via a small connection opening 28 , which is just large enough to permit passage of the portion of the locking rod 8 provided with the locking teeth 9 , and the hydraulic channel 37 . The free end of the locking teeth 9 is received in and displaceably guided in the bore 29 in the bottom of the housing 2 .
The locking teeth 9 of the locking rod 8 extend through a locking opening 30 provided in the locking plunger 16 . This locking opening 30 extends at right angles to the operating direc-tion of the locking piston 4 . The inner circumference of the locking opening is fully defined by the locking plunger 16 so that said locking opening can only be engaged from the left or from the right (cf. FIG. 1 ). In addition, when seen in a cross-sectional view, the locking open-ing 30 is implemented as an elongated hole, which is adapted to the cross-sectional shape of the locking teeth 9 of the locking rod 8 . The length of said elongate hole is chosen such that it exceeds the length of the operating path of the locking piston 4 . The locking opening is provided on one side thereof with an undercut portion 31 whose cross-section is, how-ever, designed such that, at the arresting position, the locking teeth 9 of the locking rod 8 will come into contact with a shoulder 32 of the locking opening so that the undercut portion 31 will remain free. On one side of the locking opening 30 , a locking projection 33 projects partly into said undercut portion 31 and partly into said locking opening 30 . The end face of said locking projection 33 has an arcuate form so that it will precisely fit in between the lock-ing teeth 9 . The locking projection 33 is designed such that it is adapted to be brought into engagement with a respective annular groove between the teeth of the locking teeth 9 . Also said annular groove is triangular in cross-section, the part of said groove merging with the undercut portion 31 being, however, rounded.
At the side of the bore 18 , a vent channel 34 is arranged through which also a leakage flow can escape from the pressure chamber 20 .
In the following, the mode of operation and the function of the chain tensioner 1 will be ex-plained in detail.
The locking teeth 9 of the locking rod 8 extend through a locking opening 30 provided in the locking plunger 16 . This locking opening 30 extends at right angles to the operating direction of the locking piston 4 . The inner circumference of the locking opening 30 is fully defined by the locking plunger 16 so that the locking opening can only be engaged from the left or from the right (cf. FIG. 1 ). In addition, when seen in a cross-sectional view, the locking opening 30 is implemented as an elongated hole, which is adapted to the cross-sectional shape of the locking teeth 9 of the locking rod 8 . The length of the elongate hole is chosen such that it exceeds the length of the operating path of the locking piston 4 . The locking opening is provided on one side thereof with an undercut portion 31 whose cross-section is, however, designed such that, at the arresting position, the locking teeth 9 of the locking rod 8 will come into contact with a shoulder 32 of the locking opening so that the undercut portion 31 will remain free. On one side of the locking opening 30 , a locking projection 33 projects partly into the undercut portion 31 and partly into the locking opening 30 . The end face of the locking projection 33 has an arcuate form so that it will precisely fit in between the locking teeth 9 . The locking projection 33 is designed such that it is adapted to be brought into engagement with a respective annular groove between the teeth of the locking teeth 9 . Also the annular groove is triangular in cross-section, the part of said groove merging with the undercut portion 31 being, however, rounded.
Assuming now that the internal combustion engine is switched off, the tensioning piston 3 and the locking piston 4 will not have applied thereto any hydraulic pressure. In this condition, the tensioning piston 3 is prevented from retracting by the locking piston 4 , which is forced into the arresting position by the compression spring 22 . This means that, when the engine is being started, a retraction of the tensioning piston 3 will be prevented in spite of strong forces occurring at the piston head 7 , before a suitable hydraulic pressure can build up in the hydraulic circuit. It follows that, in spite of the insufficient hydraulic pressure, a predetermined tension will always be given when the engine is started. As soon as a sufficient hydraulic pressure has built up after the start of the engine, the locking piston 4 will be displaced to the release position due to the pressure that builds up in the pressure chamber 20 . Also the hydraulic pressure in the pressure chamber of the tensioning piston 3 is increased such that the tensioning force will be applied mainly through this hydraulic pressure. This hydraulic pressure is load-dependent and increases in the case of higher speeds, whereby the tension will be increased. In this condition, the tensioning piston 3 can operate in the normal way, as in the case of conventional hydraulic chain tensioners. The locking teeth 9 can move freely within the locking opening 30 because the locking projection 33 is retracted. Also hydraulic fluid penetrates into the locking opening 30 through the connection channel 37 and the connection opening 28 . Due to the fact that the locking opening 30 is implemented as a circumferentially closed elongated hole, the hydraulic pressure will, however, not influence the operation of the locking piston 4 . On the contrary, force components will be generated both towards the release position and towards the arresting position so that the hydraulic pressure will not influence the operating behavior of the locking piston 4 within the locking opening 30 . Nor do the undercut portion 31 and the locking projection 33 produce any effect in the operating direction, since what matters is the area projected perpendicularly to the operating direction. It follows that the operation of the locking piston 4 is only influenced by the compression spring 22 and the hydraulic pressure in the pressure chamber 20 . The pressure chamber 20 is, however, decoupled from the pressure chamber of the tensioning piston 3 and its pressure fluctuations caused by vibrations on the endless driving element, e.g. the chain. A reliable extension and retraction behavior of the locking piston 4 is achieved in this way.
According to a further embodiment, the locking piston could also be operated electrically or pneumatically.
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A tensioner for endless driving elements, such as chains and belts, comprising a tensioning piston provided with locking means, and a locking piston which is adapted to be engaged with and disengaged from the locking means so as to arrest or release the movement of tensioning piston, the locking piston comprising an operating section causing locking piston to move to the arresting position and to the release position, and a locking area used for engagement with the locking means of the tensioning piston and arranged separately from the operating section.
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FIELD OF THE INVENTION
The present invention relates to methods for dental implantology generally, and particularly for subantral augmentation.
BACKGROUND OF THE INVENTION
Treatment of edentulous patients with osseointegrated fixtures made of titanium is a well known procedure in the art. The procedure includes installing a fixture in the alveolar bone of an at least partially edentulous jaw. Usually about 4 months are required for proper healing after fixture installation in the mandible, while about six months are required after installation in the maxilla.
After healing, an abutment is installed on the upper portion of the fixture. After about two weeks, an artificial tooth may be screwed on to the abutment and the procedure is completed.
A review of osseointegrated implantology may be found in "A Fifteen Year Study of Osseointegrated Implants in the Treatment of the Edentulous Jaw", R. Adell et al., Int. J. Oral Surg., 1981, 10:387-416.
Installation of implants requires sufficient alveolar bone height, generally about 10 mm, for the implant fixture to be properly osseointegrated. Various factors may cause a lack of available alveolar bone height, e.g., a thin edentulous maxillary alveolar ridge, especially in the area of the free end, a flat palate or atrophic maxillary alveolus. In order to create increased bone height, the subantral augmentation technique, popularly known as the sinus lift technique, was developed, the first such procedure being introduced by Dr. Hilt Tatum of the United States in 1975.
A summary of the prior art method of subantral augmentation is described hereinbelow. The prior art requires cutting a "trapdoor" in the lateral maxillary wall and causing greenstick fracture thereof.
SUMMARY OF THE INVENTION
The present invention seeks to provide improved methods for subantral augmentation. Unlike the prior art, which is an open procedure, the present invention is a closed procedure. The present invention does not cut a "trapdoor" in the lateral maxillary wall and does not require a greenstick fracture thereof.
There is thus provided in accordance with a preferred embodiment of the present invention, a method for subantral augmentation without osteotomy including the steps of lifting the schneiderian membrane from the antral floor, and placing graft material between the schneiderian membrane and the antral floor.
In accordance with a preferred embodiment of the present invention, the method includes the step of drilling a hole in the lateral maxillary wall, wherein the schneiderian membrane is lifted by a tool introduced through the hole. The graft material may be introduced through this hole.
Additionally in accordance with a preferred embodiment of the present invention, the method further includes the step of providing optical apparatus in the maxillary sinus region.
Further in accordance with a preferred embodiment of the present invention, the method includes the step of placing a resorbable membrane on at least one of the antral floor and the schneiderian membrane before the step of placing graft material between the schneiderian membrane and the antral floor.
The graft material is intended to create a temporary stable structure which supports the resorbable membrane on top of which rests the schneiderian membrane.
Alternatively, in accordance with a preferred embodiment of the present invention, the schneiderian membrane is lifted by grasping the membrane with a tool introduced through the maxillary sinus, and wherein the graft material is introduced via the maxillary sinus through an incision in the schneiderian membrane, the incision being subsequently packed by a portion of the graft material.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be understood and appreciated from the following detailed description, taken in conjunction with the drawings in which:
FIG. 1 is a simplified, front view illustration of a human face, showing the position of the maxillary sinus;
FIG. 2 is a simplified, sectional illustration of the maxillary sinus, lateral maxillary wall, antral floor, schneiderian membrane and reflected mucoperiosteal flap;
FIG. 3 is a simplified pictorial illustration of an arcuate osteotomy performed during a prior art subantral augmentation;
FIG. 4 is a simplified sectional illustration of fracturing the antral floor medially during the prior art subantral augmentation;
FIG. 5 is a simplified sectional illustration of the subantral space filled with graft material and the mucoperiosteal flap sutured, according to the prior art subantral augmentation;
FIG. 6 is a simplified pictorial illustration of two holes drilled in the lateral maxillary wall during subantral augmentation performed in accordance with a preferred embodiment of the present invention;
FIG. 7 is a simplified sectional illustration of lifting the schneiderian membrane and inserting a resorbable membrane, in accordance with a preferred embodiment of the present invention;
FIG. 8 is a simplified sectional illustration of filling the subantral space with graft material, in accordance with a preferred embodiment of the present invention;
FIG. 9 is a simplified sectional illustration of the subantral space filled with graft material and the mucoperiosteal flap sutured, in accordance with a preferred embodiment of the present invention;
FIG. 10 is a simplified sectional illustration of lifting the schneiderian membrane and inserting a resorbable membrane, in accordance with another preferred embodiment of the present invention; and
FIG. 11 is a simplified sectional illustration of filling the subantral space with graft material, in accordance with another preferred embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Anatomy of the maxillary sinus region will now be briefly described with reference to FIGS. 1 and 2. FIG. 1 is a simplified, front view illustration of a human face 5, showing the position of the maxillary sinus 10. FIG. 2 is a simplified, sectional illustration of the maxillary sinus 10, clearly showing the lateral maxillary wall 12, the antral floor 14, schneiderian membrane 16 and reflected mucoperiosteal flap 18. The remaining portion of the mucoperiosteal flap is shown at reference numeral 20. The antral floor 14 is simply the medial side of the maxillary wall. The schneiderian membrane 16 covers the inner surface of the maxillary sinus 10, and is also known as the sinus membrane.
The prior art method of subantral augmentation is now described with reference to FIGS. 3-5. As seen in FIG. 3, an osteotomy 22 of the lateral maxillary wall 12 is made, taking care not to damage the schneiderian membrane (not seen in FIG. 3). The osteotomy 22 may be arcuate as shown in FIG. 3, or may be rectangular. A plurality of holes 24 are drilled in the lateral maxillary wall 12, superior to the osteotomy 22. The osteotomy 22 and holes 24 together form the outline of a "trapdoor" 26.
In FIG. 4, trapdoor 26 is greenstick-fractured medially along the location of holes 24. The schneiderian membrane 16 is lifted away from the antral floor 14, creating a subantral space 28.
In FIG. 5, the subantral space 28 is filled with graft material 30 and the two portions 18 and 20 of the mucoperiosteal flap are sutured at reference numeral 32. After osseointegration of the graft material 30 and sufficient healing, the subantral space 28 is sufficiently augmented for placement of implants (not shown). Sometimes the implants may be placed concomitantly with the graft material 30.
Reference is now made to FIGS. 6-9 which illustrate subantral augmentation performed in accordance with a preferred embodiment of the present invention.
In accordance with a preferred embodiment of the present invention, as shown in FIG. 6, two holes 40 and 42 may be drilled in the lateral maxillary wall 12. Preferably, care is exercised not to perforate the schneiderian membrane (not shown in FIG. 6). However, it is not essential to maintain the schneiderian membrane free of perforations, as will be appreciated hereinbelow with reference to FIGS. 7 and 8. Moreover, in accordance with another preferred embodiment of the present invention, the maxillary wall does not have to be damaged at all, as will be described hereinbelow with reference to FIGS. 10 and 11.
Reference is now made to FIG. 7. A tool, such as a freer elevator 50 may be inserted through hole 42 and used to lift the schneiderian membrane 16 from the antral floor 14, thereby creating a subantral space 51. Alternatively, the schneiderian membrane 16 may be separated from and lifted away from the antral floor 14 by other suitable means.
Illumination and/or optical observation apparatus, such as endoscopic apparatus 52, may be inserted through hole 40, as shown in FIG. 7. A resorbable membrane 54 may be inserted through hole 42 by means of an insertion tool 56. Resorbable membrane 54 may be made, for example, of collagen or of Paroguide brand membrane, manufactured by Coletica of France. Resorbable membrane 54 is shown in FIG. 7 in rolled or bunched form for easy insertion through hole 42. After insertion, the membrane 54 is preferably spread below the schneiderian membrane 16. Another resorbable membrane (not shown) may also be spread along the antral floor 14, if needed.
Small holes (not shown) may be drilled in the area of the inferior maxillary wall 12 to aid in osseointegration of graft material 60.
In FIG. 8, the subantral space 51 is filled with graft material 60, preferably introduced, such as by injection through a hollow cannula 62 inserted through hole 42. Alternatively, graft material 60 may be introduced directly through hole 42. Graft material 60 may be, for example, small rolls or particles of collagen or fibrin, perhaps coated with hydroxyapatite, and autogenous particles, such as from the maxillary tuberosity, mixed with blood. The graft material 60 supports the schneiderian membrane 16 during and after filling of the subantral space 51. Any tears or perforations in the schneiderian membrane 16 may be packed by graft material 60.
In FIG. 9, the subantral space 51 has been completely filled with graft material 60. Preferably an additional resorbable membrane 53 may be placed against the lateral surface of the lateral maxillary wall 12, thereby helping to seal holes 40 and 42. The two portions 18 and 20 of the mucoperiosteal flap may then be sutured at reference point 66.
Thus, the present invention provides a closed technique for subantral augmentation, in contrast with the prior art which requires opening a trapdoor in the lateral maxillary wall.
It is appreciated that instead of drilling two holes 40 and 42, one single enlarged hole 42 may be drilled which is sufficient for also passing therethrough endoscopic apparatus 52.
As mentioned hereinabove, in accordance with another preferred embodiment of the present invention, the maxillary wall 12 does not have to be damaged at all, as is now described with reference to FIGS. 10 and 11.
Instead of drilling holes in the lateral maxillary wall, a tool, such as a flexible, and preferably articulated, membrane elevator 70, may be inserted into the maxillary sinus 10, such as through one of the nostrils (not shown in FIG. 10), and be used to grip and lift the schneiderian membrane 16 from the antral floor 14, thereby creating a subantral space 72, as seen in FIG. 10. A resorbable membrane 74 may be introduced by another tool 75 into the maxillary sinus 10, such as through the same nostril, and spread along the antral floor 14. An incision may have to be made in the schneiderian membrane 16 to allow placement of the resorbable membrane 74. Endoscopic apparatus 76 may be inserted through the nostril (not shown).
Reference is now made to FIG. 11. In a similar fashion as described hereinabove with reference to FIG. 8, subantral space 72 may be filled with graft material 80, preferably introduced through a hollow tube 82 inserted through one of the nostrils (not shown). Any tears or perforations in the schneiderian membrane 16 may be packed by graft material 80. The subantral space 72 may be completely filled with graft material 80 which becomes osseointegrated with the maxillary wall 12.
It is appreciated that various features of the invention which are, for clarity, described in the contexts of separate embodiments may also be provided in combination in a single embodiment. Conversely, various features of the invention which are, for brevity, described in the context of a single embodiment may also be provided separately or in any suitable subcombination.
It will be appreciated by persons skilled in the art that the present invention is not limited to what has been particularly shown and described hereinabove. Rather, the scope of the present invention is defined only by the claims that follow:
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A method for subantral augmentation including the steps of lifting the schneiderian membrane from the antral floor, and placing graft material between the schneiderian membrane and the antral floor, without fracturing the lateral maxillary wall.
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BACKGROUND OF THE INVENTION
This invention relates to a method of employing an extruded, open-cell alkenyl aromatic polymer foam in roofing systems.
Roofing systems typically comprise multiple layers of various materials configured to protect and optionally to insulate a roof deck or upper surface of a structure or building. The roofing system protects the deck and the interior of the structure from the weather, including wind, rain, and other precipitation.
The critical component of a roofing system is the membrane. The membrane is a sheet or mat of a solid, elastomeric substance which protects the deck from the aforementioned weather elements. Conventional membranes include those of EPDM (ethylene-propylene-diene elastomer), modified bitumen, and plasticized polyvinylchloride. The membrane may be dark, medium, or light in color, but is usually dark.
When installing a new roofing system, the membrane is placed or laid on top of the roof deck. A protective layer may be typically inserted between the membrane and the deck. The protective layer may take the form of an insulative plastic foam or, more commonly, a non-foam material such as a wood or wood composite panel. Commercially-employed plastic foams include polystyrene bead foam, closed-cell extruded polystyrene foam, and closed-cell polyisocyanurate and polyurethane foams.
Optionally, a paving layer may be placed or laid on top of the membrane. The paving layer typically comprises materials such as gravel or stone ballast, shingles, brick, or concrete. The paving layer functions to physically protect the membrane from foot traffic and direct exposure to sunlight and the weather.
When replacement or recovery roofing systems are installed in existing structures or buildings, they are often installed over existing roofing systems. In a typical recovery system, a protective layer is applied or laid on top of the existing roofing system, usually an old membrane or an old paving layer; a new membrane is applied or laid on top of the protective layer; and, optionally, a new paving layer is applied on top of the new membrane. The protective layer protects the new membrane from the rough and uneven surfaces often encountered on the upper surfaces of existing roofing systems, provides mechanical support underneath the new membrane, and, in the case of plastic foams, provides additional insulation.
A problem commonly encountered with roofing systems is rupture of the membrane due to distortion or deterioration of the protective layer underneath the membrane. The distortion and deterioration problems arise from the exposure of the protective layer to extreme heat from direct sunlight or moisture buildup due to weather exposure. The membrane, which is typically dark and elastomeric, absorbs significant heat from the sunlight, and further does not allow for timely escape of moisture trapped underneath it. When the insulating and/or protective layer becomes distorted or deteriorated, the membrane and the protective layer may separate to form void pockets, which leave the membrane with diminished mechanical support on its undersurface. The diminished support renders the membrane more subject to rupture.
The source of distortion and deterioration problems of the material in the protective layer varies according to the nature of the material. Some materials are susceptible to heat, some are susceptible to moisture, and some have inherently low mechanical strength.
Extruded, closed-cell polystyrene foams offer excellent mechanical strength and water resistance, but can become distorted at high service temperatures (greater than 165° F.) due to their relatively low heat distortion temperature. Such high service temperatures are typically encountered under a dark membrane in direct sunlight.
Expanded polystyrene bead foams typically better maintain their shape in a high temperature environment than extruded, closed-cell polystyrene foams because they typically have better bowing characteristics. Their bowing characteristics are better because the coalesced expanded bead structure allows for greater mechanical relaxation compared to the solid, cellular form of extruded, closed-cell foams. However, the coalesced expanded bead structure also results in lower mechanical strength and lower resistance to water transmission.
Closed-cell polyisocyanate foams have high heat distortion temperatures (250° F.-275° F.) (121° C.-135° C.), but have poor moisture resistance. Moisture weakens the cellular structure of such foams, and renders them subject to physical deterioration over time. Moisture also diminishes the insulation value of the foam. They are also relatively friable, which affects their handling characteristics.
Closed-cell polyurethane foams, like closed-cell polyisocyanate foams, have high heat distortion temperatures and poor moisture resistance. They are also relatively friable, which affects their handling characteristics.
Wood panels and wood composite panels have high heat distortion temperatures, but have poor moisture resistance. Moisture weakens the wood, and renders it subject to physical deterioration over time. Further, the panels provide little insulation compared to foams.
It would be desirable to have a foam which could be deployed underneath a membrane in a roofing system. It would further be desirable if such foam had a heat distortion temperature of 190° F. (88° C.) or more. It would further be desirable if such foam had excellent moisture resistance and mechanical strength similar to that of extruded, closed-cell polystyrene foams.
SUMMARY OF THE INVENTION
According to the present invention there is a roofing system for a structure. The process comprises a roof deck; a protective layer of a plurality of panels of an extruded alkenyl aromatic polymer foam situated above and adjacent the deck; and a substantially waterproof membrane situated above and adjacent to the foam. The foam comprises an alkenyl aromatic polymer material having greater than 50 percent by weight alkenyl aromatic monomeric units, and has from 30 to 80 percent open cell content.
Further according to the present invention there is a recovery roofing system for a structure. The roofing system comprises a pre-existing roofing system; a protective layer of a plurality of panels of an extruded alkenyl aromatic polymer foam situated above and adjacent the pre-existing roofing system; a substantially waterproof second membrane situated above and adjacent to the foam. The pre-existing roofing system comprises a roof deck and a first membrane situated above and adjacent the roof deck.
Further according to the present invention there is a process for constructing a roofing system for a structure. The process comprises providing a roof deck; applying above and adjacent to the upper surface of the roof deck a protective layer of a plurality of panels of an extruded alkenyl aromatic polymer foam; and applying a substantially waterproof membrane above and adjacent to the upper surface of the foam.
Further according to the present invention there is a process for constructing a recovery roofing system for a structure. The process comprises providing a pre-existing roofing system; applying above and adjacent to the upper surface of the pre-existing roofing system a protective layer of a plurality of panels of an extruded alkenyl aromatic polymer foam; and applying above (on top of) and adjacent to the upper surface of the foam a second membrane which is substantially waterproof. The pre-existing roofing system comprises a roof deck and a first membrane situated above and adjacent the roof deck.
In the above systems and processes, the protective layer is situated adjacent to and preferably contiguous to the membrane. Being contiguous is preferred because maximum physical protection is afforded the membrane.
When any component (roofing decks, membranes, protective layers, paving layers) of a roofing system or replacement roofing system is described as being adjacent to another component, they are situated in parallel and proximity to one another, but may or may not be in direct physical contact. When a component is described as being contiguous to another component, they are in direct physical contact.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the present invention will be better understood upon reviewing the drawings together with the remainder of the specification.
FIG. 1 is a cross-sectional view of a roofing system of the present invention.
FIG. 2 is a cross-sectional view of a recovery roofing system of the present invention.
FIG. 3 is a cut away view of the roofing system illustrated in FIG. 1.
FIG. 4 is a cut away view of the recovery roofing system illustrated in FIG. 2.
DETAILED DESCRIPTION OF THE INVENTION
The present invention affords new roofing systems and recovery roofing systems with enhanced longevity and performance. Longevity and performance are enhanced by improving the physical support and integrity of the roofing membrane. The improved physical support and integrity make the formation of membrane rupture less likely, resulting in a reduced incidence of water leakage through the roofing system.
The physical support and integrity of the membrane is enhanced by employing a protective layer of an extruded, open-cell alkenyl aromatic polymer foam underneath the membrane. The foam offers excellent heat and moisture resistance and mechanical strength.
The foam further enhances the heat insulation of the roofing system.
FIGS. 1 and 3 illustrate a new roofing system 20 of the present invention.
Roofing system 20 comprises in sequence a roof deck 10, a protective (foam) layer 12, a membrane 14, and a paving layer 16 stacked one on top of the other. Protective layer 12 comprises the extruded, open-cell alkenyl aromatic foam described herein. If insulation additional to that provided by protective layer 12 is desired, an insulating foam plastic material such as an extruded, closed-cell alkenyl aromatic polymer foam may be provided between protective layer 12 and roofing deck 10. It is understood that paving layers in the embodiments herein are optional.
FIGS. 2 and 4 illustrate an embodiment of a recovery roofing system 34 of the present invention. In employing a recovery roofing system, the cost of removing the pre-existing system is avoided by placing a new roofing system directly on top of the pre-existing roofing system. The pre-existing roofing system comprises a roof deck 22, a first membrane 24, and a first paving layer 26. The new roofing system comprises protective layer 28, second membrane 30, and second paving layer 32. If insulation additional to that provided by protective layer 28 is desired, another layer of an insulating foam plastic material such as an extruded, closed-cell alkenyl aromatic polymer foam may be provided between the first paving layer 26 and protective layer 28.
The extruded, alkenyl aromatic polymer foam provides enhanced performance in roofing systems over other materials employed in protective layers for roofing membranes in the prior art.
The extruded, open-cell foam offers moisture resistance and mechanical strength similar to that of a corresponding extruded, closed-cell alkenyl aromatic polymer foam, but also affords a higher heat distortion temperature. The open-cell foam has a heat distortion temperature up to 210° F. (99° C.), while the closed-cell foam has one of up to 175° F. (79° C.). Though not bound by any particular theory, the higher heat distortion temperature is believed due to the open-cell structure, which allows cell gas pressure to be relieved more readily than a closed-cell structure.
The extruded, open-cell foam affords a better heat distortion temperature than a corresponding expanded bead polystyrene foam, and has better mechanical strength and exhibits much lower water transmission. The extruded, open-cell foam has a unitary, cellular structure rather than a coalesced bead structure like the bead foam.
The extruded, open-cell foam exhibits much better moisture resistance than a closed-cell polyisocyanate foam or polyurethane foam, and, thus, is much less subject to physical deterioration. The open-cell foam affords a lower range of heat distortion temperatures than the polyisocyanate or polyurethane foam, but the afforded range is entirely sufficient for temperatures commonly encountered in roofing applications. Further, with respect to the polyurethane foam, the open-cell foam is more rigid, which makes it more effective in providing mechanical support. Further, the open-cell foam has friability characteristics (less friability) superior to those of polyisocyanurate and polyurethane foams.
The extruded, open-cell foam exhibits much better moisture resistance than a wood or wood composite panel. The open-cell foam affords heat distortion temperatures less than that of the wood or wood composite panel, but affords a range which is entirely sufficient for temperatures commonly encountered in roofing applications. Further, the open-cell foam provides much better insulation per unit thickness than the wood or wood composite panel.
The open-cell foam has a heat distortion temperature of from 175° F. to 210° F. (79° C. to 99° C.) and more preferably from 190° F. to 205° F. (88° C. to 96° C.) according to ASTM D-2126-87. The high heat distortion temperature of the foam enables it to be employed in high service temperature environments (175° F. to 210° F.) (79° C. to 99° C.) such as underneath dark roofing membranes in direct sunlight. The present foam has an excellent heat distortion temperature due to its open-cell structure.
The open-cell foam has an open cell content of 30 percent or more, preferably of 30 to 80 percent, and most preferably 40 to 60 percent according to ASTM D-2856-87.
The open-cell foam has a density of 1.5 pcf to 6.0 pcf (24 kg/m 3 to 96 kg/m 3 ) and preferably a density of 2.0 pcf to 3.5 pcf (32 kg/m 3 to 48 kg/m 3 ) according to ASTM D-1622-88.
The open-cell foam has an average cell size of from 0.08 millimeters (mm) to 1.2 mm and preferably from 0.10 mm to 0.9 mm according to ASTM D-3576-77.
The open-cell foam is particularly suited to be formed into a plank, desirably one having a minor dimension in cross-section (thickness) of greater than 0.25 inches (6.4 millimeters) or more and preferably 0.375 inches (9.5 millimeters) or more. Further, preferably, the foam has a cross-sectional area of 30 square centimeters (cm) or more.
The open-cell foam is substantially non-crosslinked. Substantially non-crosslinked means the foam is substantially free of crosslinking, but is inclusive of the slight degree of crosslinking which may occur naturally without the use of crosslinking agents or radiation. A substantially non-crosslinked foam has less than 5 percent gel per ASTM D-2765-84, method A.
The open-cell foam comprises an alkenyl aromatic polymer material. Suitable alkenyl aromatic polymer materials include alkenyl aromatic homopolymers and copolymers of alkenyl aromatic compounds and copolymerizable ethylenically unsaturated comonomers. The alkenyl aromatic polymer material may further include minor proportions of non-alkenyl aromatic polymers. The alkenyl aromatic polymer material may be comprised solely of one or more alkenyl aromatic homopolymers, one or more alkenyl aromatic copolymers, a blend of one or more of each of alkenyl aromatic homopolymers and copolymers, or blends of any of the foregoing with a non-alkenyl aromatic polymer. Regardless of composition, the alkenyl aromatic polymer material comprises greater than 50 and preferably greater than 70 weight percent alkenyl aromatic monomeric units. Most preferably, the alkenyl aromatic polymer material is comprised entirely of alkenyl aromatic monomeric units.
Suitable alkenyl aromatic polymers include those derived from alkenyl aromatic compounds such as styrene, alphamethylstyrene, ethylstyrene, vinyl benzene, vinyl toluene, chlorostyrene, and bromostyrene. A preferred alkenyl aromatic polymer is polystyrene. Minor amounts of monoethylenically unsaturated compounds such as C 2-6 alkyl acids and esters, ionomeric derivatives, and C 4-6 dienes may be copolymerized with alkenyl aromatic compounds. Examples of copolymerizable compounds include acrylic acid, methacrylic acid, ethacrylic acid, maleic acid, itaconic acid, acrylonitrile, maleic anhydride, methyl acrylate, ethyl acrylate, isobutyl acrylate, n-butyl acrylate, methyl methacrylate, and vinyl acetate. The foams are preferably substantially free of rubbery or rubber-like substances such as those with C 4-6 diene monomeric content. Preferred foams comprise substantially (that is, greater than 95 percent) and most preferably entirely of polystyrene.
The open-cell foam is generally prepared by heating an alkenyl aromatic polymer material to form a plasticized or melt polymer material, incorporating therein a blowing agent to form a foamable gel, and extruding the gel through a die to form the foam product. Prior to mixing with the blowing agent, the polymer material is heated to a temperature at or above its glass transition temperature or melting point. The blowing agent may be incorporated or mixed into the melt polymer material by any means known in the art such as with an extruder, mixer, or blender. The blowing agent is mixed with the melt polymer material at an elevated pressure sufficient to prevent substantial expansion of the melt polymer material and to generally disperse the blowing agent homogeneously therein. A nucleating is blended in the polymer melt or dry blended with the polymer material prior to plasticizing or melting. The foamable gel is typically cooled to a lower temperature to optimize or attain desired physical characteristics of the foam. The gel may be cooled in the extruder or other mixing device or in separate coolers. The gel is then extruded or conveyed through a die of desired shape to a zone of reduced or lower pressure to form the foam. The zone of lower pressure is at a pressure lower than that in which the foamable gel is maintained prior to extrusion through the die. The lower pressure may be superatmospheric or subatmospheric (evacuated or vacuum), but is preferably at an atmospheric level.
More specifically, the foam may be prepared by: a) heating an alkenyl aromatic polymer material comprising more than 50 percent by weight alkenyl aromatic monomeric units to form a melt polymer material; b) incorporating into the melt polymer material an amount of a nucleating agent sufficient to result in a foam having from 30 percent to 80 percent open cell content; c) incorporating into the melt polymer material at an elevated pressure a blowing agent to form a foamable gel; d) cooling the foamable gel to a suitable foaming temperature; and e) extruding the foamable gel through a die into a region of lower pressure to form the foam. The foaming temperature ranges from 118° C. to 145° C. wherein the foaming temperature is from 3° C. to 15° C. higher than the highest foaming temperature for a corresponding closed-cell foam. The foaming temperature must be 133° C. or more. The foaming temperature further must be 33° C. or more higher than the glass transition temperature (according to ASTM D-3418) of the alkenyl aromatic polymer material.
Any blowing agent useful in making extruded alkenyl aromatic polymer foams maybe employed. Useful blowing agents include 1-chloro-1,1-difluoroethane (HCFC-142b), chlorodifluoromethane (HCFC-22), 1,1-difluoroethane (HFC-152a), 1,1,1-trifluoroethane (HFC-143a), 1,1,1,2-tetrafluoroethane (HFC-134a), water ethanol, carbon dioxide, ethyl chloride, and mixtures of the foregoing. A preferred blowing agent comprises a mixture of carbon dioxide and ethyl chloride.
The amount of nucleating agent employed will vary according to desired cell size, foaming temperature, and composition of the nucleating agent. Open-cell content increases with increasing nucleating agent content. Useful nucleating agents include calcium carbonate, calcium stearate, talc, clay, titanium dioxide, silica, barium stearate, diatomaceous earth, and mixtures of citric acid and sodium bicarbonate. Preferred nucleating agents are talc and calcium stearate. The amount of nucleating agent employed may range from 0.01 to 5 parts by weight per hundred parts by weight of a polymer resin. The preferred range is from 0.4 to 3.0 parts by weight.
Extensive teachings to the preparation of the open-cell foam are seen in co-pending application U.S. Ser. No. 08/264,669, filed Jun. 23, 1994.
The open-cell foam optionally further comprises carbon black. Carbon black enhances the thermal resistance or insulation of the foam. The carbon black may comprise between 1.0 and 25 weight percent and preferably between 4.0 and 10.0 weight percent based upon the weight of the alkenyl aromatic polymer material in the foam. The carbon black may be of any type known in the art such as furnace black, thermal black, acetylene black, and channel black. A preferred carbon black is thermal black. A preferred thermal black has an average particle size of 150 nanometers or more.
Small amounts of an ethylene polymer such as linear low density polyethylene or high density polyethylene may be incorporated into the foamable gel to enhance open-cell content upon extrusion and foaming.
Various additives may be incorporated in the foam such as inorganic fillers, pigments, anti oxidants, acid scavengers, ultraviolet absorbers, flame retardants, processing aids, and extrusion aids.
EXAMPLES
The following are examples of the present invention, and are not to be construed as limiting. Unless otherwise indicated, all percentages, parts, or proportions are by weight.
Open-cell alkenyl aromatic polymer foam structures of the present invention are made according to the process of the present invention.
Example 1
An open-cell extruded polystyrene foam was tested for dimensional stability at 205° F. for 3 hours according to test method ASTM D2126-87. The heat distortion characteristics of the foam were excellent. The length difference was 0.2 percent of initial, the width difference was -0.1 percent of initial, and the thickness difference was 0.2 percent of initial.
The foam had 50 to 70 percent open cell content, 2.19 pcf (35 kg/m 3 ), and a 0.30 millimeter cell size.
Example 2
An open-cell extruded polystyrene foam was tested for bowing when one side was exposed. A Thermotron FM-46 oven with minimum inner dimensions of 42 inches (107 cm) by 38 inches (97 cm) and a capability of maintaining a constant temperature 205° F.±5° F. was used. The foam was attached to a wooden platform with four metal corner fasteners in the oven. The platform was left in place for the desired period of time. The foam was exposed to a temperature of 200° F. for 30 minutes while the other side supported by a wooden platform remained at ambient conditions.
The bowing characteristics of the foam were excellent considering the extreme temperature conditions to which the foam was exposed. The maximum bow was an average of 17 millimeters. Bowing was determined by measuring the distance from the bottom of the foam to the platform. If the foams were placed on a roof under a membrane, bowing would be less because of the restraining influence of the membrane. Under normal hot-roof conditions under a membrane, such as exposure temperatures of 190° F. or less, preferred foams would have a maximum bow of not more than 6 millimeters.
The sample had 50 to 70 percent open cell content, 2.19 pcf (35 kg/m 3 ), and a 0.30 millimeter cell size.
While embodiments of the foam and the process of the present invention have been shown with regard to specific details, it will be appreciated that depending upon the manufacturing process and the manufacturer's desires, the present invention may be modified by various changes while still being fairly within the scope of the novel teachings and principles herein set forth.
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A roofing system (20) for a structure such as a building. The system (20) includes a roof deck (10), a plurality of panels (12) of an extruded alkenyl aromatic polymer foam above and adjacent the deck (10); and a substantially waterproof membrane (14), above and adjacent to the foam. The foam has an open cell content of 30 percent or more. The foam provides excellent mechanical support for the membrane (14), and is water resistant. The foam further has a high heat distortion temperature, and is substantially free of distortion at high service temperatures encountered in roofing systems. Further disclosed is a recovery roofing system employing the above foam. Further disclosed are processes for constructing a new roofing system and a recovery roofing system.
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BACKGROUND OF THE INVENTION
The present invention relates to a device for the localized fastening of elements having an edge, especially of plates to a supporting structure.
In a particular use, it relates to a device for the localized fastening of plates made of building materials to a supporting structure, for the purpose of covering or forming at least partially frontages of buildings or internal walls, where the plates can be made of various building materials, for example asbestos cement, wood or glass, which are single or multi-layer.
At the present time, for the fastening of covering plates, continuous sections are often used, and these are engaged in grooves made in the end faces of the plates and are fastened to a supporting structure. In other cases, fastening members screwed to a supporting structure are used. When the plates are made of glass, they are usually adhesively bonded to a supporting structure, and auxiliary retaining and safety elements screwed to the supporting structure are added.
Furthermore, the Patent FR-A-2,531,755 shows a hook which is cut out from a metal sheet and which is fastened flat to the end face of a plate and then catches on a lug secured to the supporting structure, and the U.S. Pat. No. 2,816,436 shows a U-shaped wire engaged transversely on the edge of a plate in order to grip this, its end being fastened to a supporting structure by means of a nail.
These known arrangements are relatively complicated to put into effect and present problems especially at the time of assembly of the plates and also when one of several plates forming a surface is to be changed, for example because it is damaged.
SUMMARY OF THE INVENTION
The object of the present invention is, in particular, to overcome the disadvantages of the state of the art and provides a localized fastening device which is especially simple to produce and put into effect during both the assembly and the removal of the plates.
The device according to the invention for the localized fastening of a component having an edge, such as a plate, to a supporting structure comprises a first element fastened to the structure or integrated in this (also called the supporting member) and having a catching lug, and a second element fastened to the edge of the plate and interacting with the said catching lug, in order to fasten the plate to the supporting structure in a localized manner.
According to the invention, the said second element comprises a first part bearing against the front face of the said plate, a second part engaged behind the rear face of the said plate and a third part connecting the said first and second parts and extending across the end face of the plate, this second element being at least partially deformable elastically, in such a way that its third part is deformable substantially parallel to the end face of the plate, so as to generate, in one direction of deformation of this part, an elastic effect of gripping the edge of the plate between the said first and second parts of the second element and, in its other direction of deformation, a spreading apart of the said first and second parts of the second element, so as to release the edge of the plate. The second element will also be called the gripping element in this specification.
The invention can have many alternative embodiments, some of which are described below.
The third part of the gripping element can comprise at least one branch inclined at least partially relative to the transverse direction of the end face of the plate and elastically deformable at least parallel to the end face of the plate.
The third part of the gripping element can comprise two branches at least inclined oppositely relative to the transverse direction of the end face of the plate and parallel to the end face of the plate.
The third part of the gripping element can comprise two branches which are at least partially arcuate in opposite directions and elastically deformable parallel to the end face of the plate. These branches can be made arcuate, in such a way that their ends are close together and their central parts distant from one another.
The gripping element can be composed of a wire made of an elastically deformable material and comprising two branches forming its third part and oppositely inclined parallel to the end face of the plate, the close-together ends of these branches being joined by means of a turned loop forming one of its first or second parts, and their other ends having turned extensions forming the other of these parts.
The gripping element can be formed by a wire made of an elastically deformable material and comprising a branch arcuate parallel to the end face of the plate and forming the said third part and, at the ends of these branches, turned extensions forming the said first and second parts.
The gripping element can be composed of a wire made of an elastically deformable material and comprising two branches forming its third part, these branches being arcuate parallel to the plane of the plate, in such a way that their ends are close together and their central parts distant from one another, two corresponding ends of these branches being joined by means of a turned loop forming one of its first and second parts, and their other ends having turned extensions forming the other of these parts.
The extensions can bear one on the other, one having a groove, in which the other is engaged, and/or these extensions may be inserted in a connecting piece, especially a crimped ring.
In a special alternative manner of assembly, the second part of the said second element extends behind the catching lug of the supporting member which has a bearing zone for the rear face of the plate, the edge of the plate and this catching lug being retained or gripped between the first and second parts of the gripping element.
The bearing surfaces of the catching lug of the supporting member and of the second part of the gripping element can be made inclined correspondingly in the direction engaging this second part behind this lug.
The supporting member can comprise a part which extends outwards and against which the end face of the plate comes to bear.
The supporting member can be composed of a section which extends parallel to the edge of the plate and which comprises a longitudinal bearing zone for the plate and, set back, a longitudinal rib forming the catching lug.
This section of the supporting member may be of U-shaped cross-section, the ends of its branches forming longitudinal bearing zones for two plates placed on either side and being equipped laterally with two mutually confronting ribs which form opposite catching lugs for second retaining elements for these plates.
This section of the supporting member may include a longitudinal rib which extends outwards and bears against the end face of the plate, its rib forming the said catching lug at the rear of this bearing rib.
The rear face of the plate can bear on the bearing zone of the supporting member by means of a longitudinal sealing strip.
The deformation of the gripping element in the direction spreading apart its first and second parts can be such that this element can be extracted by being shifted perpendicularly relative to the end face of the plate.
In another special alternative manner of assembly, the second part of the gripping element bears against the rear face of the plate and, at the rear of the latter, has at least one catching lug bent towards the edge of the plate and engaging behind the catching lug of the supporting member.
The second part and catching lug of the gripping element can be such that, by pivoting, they grip the catching lug of the supporting member between them or release this, at the same time as the edge of the plate is gripped between the first and second parts of the gripping element or is released.
The gripping element can be composed of a wire made of an elastic material shaped in the manner of a hairpin which is such that its head extends against the front face of the plate and its branches extend across the end face of the plate, being inclined relative to the transverse direction of the said end face and forming a V, and extending against the rear face of this plate, the ends of its branches being bent towards the edge of the plate, so as to form catching lugs.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be understood better from a study of plate-fastening devices described by way of non-limiting examples and illustrated in the drawing in which:
FIG. 1 shows an outside elevation view of a wall portion formed from an assembly of plates fastened by means of a first fastening device according to the present invention;
FIG. 2 shows a vertical section according to II--II of the assembly illustrated in FIG. 1;
FIG. 3 shows a horizontal section according to III--III of the assembly shown in FIG. 1;
FIG. 4 shows, in a horizontal section corresponding to that of FIG. 3, an assembly equipped with another fastening device according to the present invention;
FIG. 5 shows an outside elevation view of the assembly of FIG. 4;
FIG. 6 shows an alternative embodiment of the fastening device illustrated in FIGS. 4 and 5;
FIG. 7 shows another alternative embodiment of the fastening device illustrated in FIGS. 4 and 5;
FIG. 8 shows a perspective rear view of plates assembled by means of another localized fastening device according to the present invention;
and FIG. 9 shows in perspective an alternative embodiment of one of the elements of the fastening devices shown in FIG. 4.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIGS. 1 to 3, there will now be described a first fastening device designated as a whole by the reference 1 and intended, on the one hand, for retaining the horizontal lower edge 2 of a rectangular plate 3 extending vertically and, on the other hand, for retaining the horizontal upper edge 4 of a rectangular plate 5 extending vertically below and at a distance from the plate 3.
As best shown in FIG. 2, the fastening device 1 comprises a first element called a supporting member 6 comprised of a horizontal section designated and of U-shaped cross-section and comprising a vertical web 7 and two horizontal wings 8 and 9 extending at a distance from one another. The web 7 is at the opposite and at the rear of the space separating the plates 3 and 5, and the wings 8 and 9 extending towards the edges 2 and 4 of these plates.
The ends 10 and 11 of the wings 8 and 9 of the section 6 are equipped with catching lugs 12 and 13 which extend facing one another. These lugs 12 and 13 form the catching lug of the supporting member 6. In cross-section, these ribs 12 and 13 have in succession, from the ends 10 and 11 of the wings 8 and 9, parts 14 and 15 extending vertically, parts 16 and 17 inclined towards the vertical web 7 of the supporting member 6 and end parts 18 and 19 inclined in the opposite direction to the vertical web 7 of the section 6. The combination of vertical part 14, inclined part 16, and end part 18 form catching lug 12. Likewise catching lug 13 is formed from individual parts 15, 17, and 19.
Longitudinal sealing strips 20 and 21 are secured to the front faces of the ends 10 and 11 of the wings 8 and 9 of the supporting member 6 and to the parts 14 and 15 of the catching lugs 12 and 13. In the example, these front faces have a longitudinal groove and these sealing strips 20 and 21 include a longitudinal rib, the said longitudinal groove and the said longitudinal rib being engaged one in the other.
Furthermore, that part 14 of the catching lug 12 associated with the upper wing 8 of the supporting member 6 is extended, in front of the parts 16 and 18 of this catching lug 12, by a longitudinal extension 22 of L-shaped cross-section which first extends downwards and which has a horizontal branch 23 extending outwards beyond the longitudinal sealing strip 20. The longitudinal extension 22 and the horizontal branch 23 form an edge of the supporting member 6 which is parallel to the end face 2a of plate 3.
As can be seen clearly from FIG. 2, the rear face of the edge 2 of the plate 3 bears against the longitudinal sealing strip 20, and its lower end face 2a bears on the horizontal branch 23 of the longitudinal extension 22 of the supporting member 6, and the inner face of the edge 4 of the plate 5 bears on the longitudinal sealing strip 21, its upper end face 4a being horizontally level with the end 19 of the catching lug 13 of the lower wing 9 of the supporting member 6.
The fastening device 1 also possesses, on the one hand, a gripping element shown generally at 24 and, on the other hand, another gripping element shown generally at 25. These elements respectively retain the plates 3 and 5 on the horizontal supporting member 6, and the gripping elements 24 and 25 are of identical structure.
In particular, the gripping element 24 is formed by a wire made of an elastically deformable material, for example steel, which comprises a first part 28 bearing against the front face of the plate 3, a second part 30 engaged behind the catching lug 12 of the supporting member 6 and a third part 26 and 27 confronting the end face 2a of the plate 3, these parts being constructed in the following way.
The gripping element 24 comprises two straight branches 26 and 27 (making up the third part of the gripping element 24) which extend across the lower end face of the plate 3 and which bear on the lower face of the horizontal branch 23 of the longitudinal extension 22 of the supporting member 6. These branches 26 and 27 are inclined relative to the transverse direction of the end face 2a of the plate 3, so as to form a V divergent towards the vertical web 7 of the supporting member 6.
The close-together ends of the branches 26 and 27 of the gripping element 24 are joined by means of a loop 28 which forms the first part of the gripping element 24, and is turned upwards and which comes to bear against the outer face of the lower edge 2 of the plate 3. The other ends of the gripping element 24 have extensions 29 and 30 which form the second part of the gripping element, which are turned up at the rear of the parts 16 and 18 of the catching lug 12 of the supporting member 6 and which bear on the part 16 of this lug, in such a way that they tend to engage behind the latter in the direction of part 14. It will therefore be seen that the parts 16 and 18 form a catching lug 12 for the gripping element 24.
The gripping element 24 is formed so as to generate a spring effect which tends, parallel to the end face 2a of the plate 3, to open the angle of its branches 26 and 27 forming its third part and reduce the passageway defined, on the one hand, by its first part composed of the loop 28 and, on the other hand, by its second part composed of extensions 29 and 30 bearing respectively on the front face of the plate 3 and on the catching lug composed of the wings 16 and 18 of the section 6. As a result of this, therefore, the edge 2 of the plate 3 is gripped between, on the one hand, the loop 28 of the gripping element 24 bearing on its front face and, on the other hand, the sealing strip 20 bearing on its rear face.
In order to remove the gripping element 24, for example, the jaw of a pair of pliers is introduced between the plates 3 and 5 towards the vertical web 7 of the supporting member 6, and the furthest ends of the branches 26 and 27 are gripped on either side, in order to reclose the V formed by these branches 26 and 27 and, by pivoting, bring the extensions 29 and 30 closer together parallel to the end face 2a of the plate 3, and the branches 26 and 27 pivoting relative to the loop 28 and the extensions 29 and 30 moving away from the catching lug 12 of the supporting member 6. When the branches 26 and 27 are brought into substantially parallel positions, as represented by broken lines in FIG. 3, so as to extend substantially in the transverse direction of the end face 2a of the plate, the gripping element 24 is made to slide in the direction moving it away from the end face 2a of the plate 3, thus freeing the extensions 29 and 30 from the catching lug 12 of the supporting member 6. The gripping element 24 is then removed by extracting it from the supporting member 6 and by causing it to pass between the edges of the plates 3 and 5.
The procedure for assembling the gripping element 24 is carried out in reverse order. A gripping element 24 is taken and is gripped so as to close the V formed by its branches 26 and 27 by bringing their extensions 29 and 30 closer together. The gripping element 24 is slid into the supporting member 6 so as to bring its extensions 29 and 30 to the rear of the catching lug 12 of the supporting member 6 and its loop 28 to bear against the outer face of the edge 2 of the plate 3, and then it is released. The spring effect of the gripping element 24 brings it into the position for clamping the plate 3, as shown in FIGS. 1 to 3 and described above. It is possible advantageously to change the position of the gripping element 24 along the edge 2 of the plate 3 by gripping it, as before, so as to open gripping element 24 and make it slide along.
The gripping element 25, of a structure identical to that of the gripping element 24, functions and can be assembled and removed in the same way as the latter. Its two branches inclined relative to the transverse direction of the edge 4 of the plate 5 bear on the end face 4a of this plate and on the end part 19 of the catching lug 13. Its turned loop bears on the front face of the edge 4 of the plate 5, and the turned extensions of its branches are engaged behind the parts 17 and 19 of the catching lug 13 of the supporting member 6.
Referring to FIG. 1, it will be seen that the horizontal section of the supporting member 6 forms a horizontal branch of a cross-shaped supporting structure which comprises another horizontal section 31 in the extension of the supporting member 6 and two vertical sections 32 and 33, these four sections being connected by means of a bevel cut and, if appropriate, being fastened to a basic supporting structure. The horizontal section 31 is of the same cross-section as the horizontal section of the supporting member 6, whilst the sections 32 and 33 have the cross-section of the horizontal section of the supporting member 6 without the longitudinal bearing extension 22.
As a result of the horizontal section 31, the lower edge of a plate 34 and the upper edge of a plate 35, which are adjacent to the plates 3 and 5, can be fastened by means of fastening elements similar to the preceding gripping elements 24 and 25 and assembled in the same way. As a result of the vertical sections 32 and 33, the vertical edges of the plate 3 and 5 and the vertical edges of the plates 34 and 35 can be fastened by means of fastening elements similar to the elements 24 and 25 and functioning in the same way.
As a result of the structure illustrated particularly in FIG. 1, the edges of vertical plates forming a vertical wall can be retained at any suitably selected points on a supporting structure formed from various intersecting sections arranged horizontally and vertically. The wall thus obtained is also leakproof because of the peripheral sealing strips, such as 20 and 21, which are associated with the various sections and against which the edges of the plates bear.
Referring now to FIGS. 4 and 5, there will now be described another fastening device designated as a whole by the reference 36 and comprising a supporting member, shown generally at 37 and identical to the supporting member 6 of the preceding example, and a gripping element designated as a whole by the reference 38 and used in the same way as the gripping element 24 described in the preceding example.
This gripping element 38, likewise composed of a wire made of an elastically deformable material, preferably steel, differs from the gripping element 24 in that its branches 39 and 40, (which make up the third part of the gripping element 38) extending across the end face 41 of a vertical plate 42 which it is to retain, are arcuate, in such a way that their ends are adjacent and their central parts are distant from one another. These branches 39 and 40 extend into the plane parallel to the end face 41 of the plate 42.
As in the preceding example, the outer ends of the branches 39 and 40 of the gripping element 38 are joined by means of a loop 43 which forms the first part of the gripping element 38 and which bears against the outer face of the plate 42, and the inner ends of these branches 39 and 40 likewise have parallel extensions 44 and 45 turned at the rear of a longitudinal catching lug 46 of the supporting member 36, as in the preceding example, these extensions this time being adjacent. The extensions 44 and 45 form the second part of the gripping element 38.
Referring to FIG. 6, it will be seen that the extension 44 of the branch 39 has a longitudinal groove 47, into which the curve of the extension 45 of the branch 40 is slightly engaged. Referring to FIG. 7, this shows an alternative embodiment, in which the branches 48 and 49 which form the second part of a gripping element 50, otherwise identical to the gripping element 38, are surrounded by a crimped ring 51.
The gripping element 38 is designed to retain the plate 42 on the supporting member 36 by gripping, in the same way as the gripping element 24 of the preceding example. This time, however, the spring effect of the gripping element 38 tends to bring its extensions 44 and 45 located at the rear of the catching lug 46 of the supporting member 36 closer to its loop 43 located at the front of the plate 42, the central parts of the branches 39 and 40 tending to move away from one another.
If action is taken, for example by means of pliers, on the moved-apart central parts of the branches 39 and 40 of the gripping element 38 in the direction bringing them closer together, parallel to the end face 41 of the plate 42, its extensions 44 and 45 move away from its loop 43. The gripping element 38 is then in the position represented by broken lines in FIG. 4. In this position, the gripping element 38 can be separated from the supporting member 36 in the same way as the gripping element 24 of the preceding example. To assemble it, branches 39 and 40 are gripped again, and the gripping element 38 is brought into position in such a way that its extensions 44 and 45 extend at the rear of the catching lug 46 of the supporting member 36 and its loop 43 at the front of the plate 42, and it is then released. The gripping element 38 assumes its above-described clamping position under the effect of its elasticity.
By means of one of the two arrangements described with reference to FIGS. 6 and 7, the extensions 44 and 45 of the gripping element 38 and the extensions 48 and 49 of the equivalent gripping element 50 are maintained in contact during the operations of assembly and removal and therefore cannot engage one above the other.
The examples described above are not limiting. In particular, the sections could have notches in their catching ribs, so it is possible to assemble and remove the second wire-shaped fastening elements by sliding parallel to the sections, after their extensions and loops have been spread apart. The sections could be replaced by short elements fastened to a supporting structure. The sealing strips could be omitted. The second elements serving for gripping could be of a different structure, whilst at the same time functioning in an equivalent way, and in particular the second elements of FIGS. 4 and 5 could comprise only a single arcuate branch equipped with turned extensions at its ends.
Referring now to FIG. 8, there will be described another fastening device designated as a whole by the reference 137 and designed for retaining the lower part of a vertical plate 138 and the upper part of a vertical plate 139 placed underneath, in relation to a vertical supporting structure (not shown).
The fastening device 137 comprises a first fastening element designated as a whole by the reference 140 and comprising a flat part 141 bearing on and fastened to the front face of the supporting structure by means of screws (not shown) extending through two holes 142 provided laterally relative to the horizontal end faces 143 and 144 of the plates 138 and 139 and opposite the space separating them. The flat part 141 is extended upwards and downwards by two vertical catching lugs 145 and 146 which are offset outwards relative to the front face of the supporting structure, the end edge of these catching lugs 145 and 146 being horizontal.
The fastening device 137 also possesses a wire fastening element designated as a whole by the reference 147 (a gripping element) and, in this example, composed of a wire made of an elastic material. This wire 147 is formed in the manner of a hairpin, the branches of which are bent perpendicularly relative to their plane, so as to define a groove which comprises a first part bearing against the front face of the plate 138, a second part bearing against its rear face and a third part bearing against its end face and in which the lower part of the plate 138 is gripped.
The wire 147 comprises a head 148 (forming the first part of the gripping wire 147) bearing against the outer face 149 of the plate 138, two branch parts 150 (forming the third part of the gripping wire 147) bearing against -he lower horizontal end face 143 of the plate 138 and inclined in the plane of the end face 143 relative to the transverse direction of this end face 143, at the same time opening, and, in the extension of these branch parts 150, two branch parts 151 which extend vertically and upwards and which bear against the rear face 152 of the plate 138. The upper ends of these branch parts 151 are extended by parts bent towards the edge 143 of the plate 138, forming catching lugs 153 (forming the second part of the gripping wire 147) which are engaged behind the upper catching lug 145 of the fastening element 140 so as to carry the plate 138.
As a result of the elasticity of the wire 147, the branch parts 150 tend to open by pivoting parallel to the end face 143 of the plate 138 and thus move the branch parts 151 away from one another. This effect ensures that the lower edge of the plate is gripped between the head 148 and the branch parts 151 of the wire 147. Furthermore, the branch parts 151 bearing against the rear face 152 of the plate 138 and catching lugs 153 extending them are arranged relative to one another in such a way as to grip the upper catching lug 145 of the first fastening element 140 by pivoting parallel to the lower end face 143 of the plate 138.
The fastening device 137 also possesses a second wire fastening element designated as a whole by the reference 154, which is identical to the wire fastening element 147 described above and which is mounted on the upper edge of the plate 139, opposite to the wire fastening 147, in such a way that its catching lugs 155 are engaged behind the lower catching lug 146 of the first fastening element 140.
It can be seen that FIG. 8 partially illustrates another fastening device, designated as a whole by the reference 156, which is identical to the preceding fastening device 137, but which is oriented at 90 degrees relative to the latter, so as to retain the adjacent vertical edges 157 and 158 of the plate 139 and of another vertical plate 159.
An assembly of plates comprising particularly the plates 138, 139 and 159 can especially be mounted on a supporting structure in the following way by means of devices identical to the fastening devices 137 and 156.
First of all, a set of first fastening elements 140 is fastened to the supporting structure, these being distributed according to the dimensions of the plates, in such a way that each plate can, for example, be retained at two locations on each of their sides.
Two wire fastening elements 147 are mounted on each of the edges of the plates. The plates are offered to the supporting structure in succession at the locations where they are to be mounted, and the second fastening elements are positioned and attached in the following way.
For example by means of pliers which are engaged on the side of the end face of the plate 138 being fastened, perpendicularly relative to the front face of the latter, the branch parts 150 of the wire 147 are grasped so as to bring them closer together by causing them to pivot towards one another parallel to the end face 143 of the plate 138. The edge of the plate 138 being released in this way, by means of the pliers the wire 147 is made to slide along the end face 143 of this plate, in order to engage the catching lug 145 of the element 140 fastened to the supporting structure between the rear branch parts 150 and the catching lugs 153 of the wire 147, and then the pliers are opened and withdrawn. The branch parts 150 open and the branch parts 151 pivot, at the same time spreading apart in such a way that the edge of the plate 138 is gripped between these branch part 151 and the head 148, at the same time as the branch parts 151 and the catching lugs 153 pivot in order to grip the catching lug 145 between them.
The above-mentioned operations are repeated for each of the plates to be fastened.
The various plates are thus retained on the supporting structure. They can also be removed separately by proceeding in reverse order, the pliers engaging into the spaces separating the plates.
Referring to FIG. 9, it can be seen that this shows another embodiment of a wire fastening element, designated as a whole by the reference 160, which is mounted on the edge of a plate 161 and the structure of which differs from that of the wire fastening element 147 only in that its branch parts 162 bearing against the end face 163 of the plate 161 form a loop which makes it possible to fit the wire fastening element 160 onto edges of plates 161 having very different thicknesses.
Of course, that part of the fastening devices described with reference to FIGS. 8 and 9 which grips the edge of the plate could have the structure of the fastening devices described with reference to FIGS. 4 to 7.
The fastening devices which have just been described can be put to many uses, especially for constructing the cladding of building frontages or for constructing all walls or coverings, both internal and external, vertical, inclined or horizontal, by means of plates which can be made of very different materials.
The present invention is not limited to the examples described above. Many alternative embodiments are possible, without departing from the scope defined by the accompanying claims.
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Device for punctually fixing a part presenting an edge such as a plate (138) on a support structure, comprising a first element (40) fixed to the structure or integrated to the latter and presenting a hooking lug (145) as well as a second element (147) fixed to the edge of the plate and cooperating with a hooking lug in order to punctually fix the plate to the support structure. The second element (147) comprises a first portion (148) bearing against the front face of the plate, a second portion (151) engaged behind the rear face of the plate and a third portion (150) connecting said first and second portions and extending through the edge (153) of the plate. The second element (145) is at least partly elastically deformable so that its third portion (147) is deformable substantially in parallel to the edge of the plate so as to produce in one deformation direction of the portion an elastic pinching effect on the edge of the plate between the first and second portions of the second element and, in its other deformation direction a spacing between the first and second portions of the second element thereby releasing the edge of the plate.
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CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation of application Ser. No. 09/108,532 filed Jul. 1, 1998, pending and is related to commonly owned Ser. No. 09/004,389, filed Jan. 8, 1998.
TECHNICAL FIELD
The present invention relates to a method of reinforcing a plastic pallet, and more particularly to a method of reinforcing a plastic pallet by applying a plurality of sheet strips along relatively weak structural portions of the pallet to form a plurality of substantially rectangular hollow vertical cross-sections along the length of the relatively weak structural portions for improved stiffness.
BACKGROUND ART
Replacing wood pallets with plastic pallets has been a goal for many years. The advantages of the plastic pallets are many as compared to wood, including greater durability, lighter weight, more consistent dimensions, improved cleanliness, water resistance, higher residual value for recycling, and no nails which may damage products being supported thereon.
One major hurdle to overcome with plastic is the cost. Plastic pallets are more expensive than wood by three to five times. This cost can be offset by the number of trips or shipments that can be achieved with plastic versus wood pallets. Another major hurdle is the stiffness of plastic pallets. Racking loaded pallets in warehouses for up to 30 days is common, and the combination of low tensile strength and creep limit the use of plastic.
There are three conventional methods of overcoming these weaknesses. The first is to add reinforcement such as steel or a composite to the pallet. This generally adds significant cost and weight and complicates recycling of the pallet. The second is to make the pallet taller. This limits the height of product to be stacked on the pallet. The third is to use reinforced or engineered resins. Again, this adds significant cost and weight. All three obviously limit the acceptance of plastic pallets.
U.S. Pat. No. 3,580,190 provides a partial solution to the stiffness problem by attaching top and bottom sheets 22 , 24 to the structural network 23 , as shown in FIG. 1 thereof. However, this solution does not resolve the bending stiffness problem because large lateral and longitudinal unsupported areas still exist, such as in areas 26 , 37 , 38 , 49 and 50 . In other words, this design merely further stiffens the support column areas 67 , 68 , 69 , 97 , 98 , 99 , 28 , 30 , 32 , which already provide substantial stiffness merely as a result of their height. The weakness of this design is apparent in column 6, lines 60-71, where Fowler recommends the use of a material having a flexural modulus (or Young's modulus) greater than about 200,000 psi. Such a high modulus material is apparently required because the structure described does not provide significant resistance to deflection along the length and width of the pallet. High modulus materials add substantial cost to the pallet.
Further complicating the problem, modern pallets typically require large openings for receipt of pallet jacks. For example, the pallet shown in FIGS. 1-3 includes a top deck portion 16 supported on a plurality of support columns 18 , which are attached to support rails 20 , which form the bottom deck 19 . Such structure cooperates to form two large openings 11 , 13 on each side of the pallet 10 , as well as four bottom openings 15 formed in the lower deck 19 . In this configuration, the rails 20 of the lower deck 19 are typically structurally weak, resulting in poor deflection stiffness. Such problems have proven very difficult to overcome because of the very thin nature of the lower deck 19 . Similarly, the thin design of the top deck 16 results in the same deflection problem between columns 18 .
Because pallets are exposed to significant abuse, any solution to the stiffness problem must not adversely effect the impact strength of the pallet.
Accordingly, a need exists for improving the stiffness of modern plastic pallets configured to receive a pallet jack, without reducing impact strength of the pallet.
SUMMARY OF THE INVENTION
The present invention provides a method of reinforcing a modern plastic pallet by affixing sheet strips along relatively weak structural portions of the pallet to form a plurality of substantially rectangular hollow vertical cross-sections along the length of the relatively weak structural portions for improved stiffness without loss of impact strength.
More specifically, the present invention provides a method of reinforcing a plastic pallet having a thin top deck portion, a plurality of support columns extending from the top deck portion and a plurality of support rails connected to the support columns to form a thin bottom deck portion, wherein the support rails each include a sheet portion with a plurality of vertical ribs extending therefrom. The method includes the step of welding a plurality of plastic sheets to the vertical ribs between the support columns to form a plurality of substantially rectangular hollow vertical cross-sections along the length of the support rails for improved stiffness. It is contemplated that the substantially rectangular hollow vertical cross-sectional areas may be filled with a secondary material, such as structural foam for improved structural integrity.
Accordingly, an object of the present invention is to provide a method of structurally reinforcing a modern plastic pallet configured to receive a pallet jack, in a manner which improves stiffness without loss of impact strength.
The above object and other objects, features and advantages of the present invention are readily apparent from the following detailed description of the best mode for carrying out the invention when taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a perspective view of a modern plastic pallet in accordance with the present invention;
FIG. 2 shows a bottom exploded perspective view of the pallet of FIG. 1;
FIG. 3 shows a top exploded perspective view of the pallet of FIG. 1;
FIG. 4 shows a cut-away perspective sectional view of a pallet in accordance with an alternative embodiment of the invention;
FIG. 5 shows a top exploded perspective view of a pallet in accordance with a second alternative embodiment of the invention; and
FIG. 6 shows a bottom exploded perspective view of the pallet of FIG. 5 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In a racking scenario, the modern plastic pallet 10 (which is configured to receive a pallet jack from any side), shown in FIG. 1, is supported from below on two opposing edges 12 , 14 , and loaded on the top deck portion 16 . The pallet must support this load with a minimum of deflection. The top deck portion 16 is supported by a plurality of support columns 18 extending from the top deck portion 16 and attached to the support rails 20 , which form the bottom deck 19 . The support rails 20 are generally relatively weak structural portions of the pallet because they are thin in vertical cross-section and are supported only at opposing ends by the columns 18 . Accordingly, the support rails 20 tend to deflect when the pallet is loaded.
Using simple beam formulas it is known that the deflection increases as the load or the span distance increases and decreases as the material modulus (E) or section moment of inertia (I) increases. Since the load and the span are defined for a given application, the variables used to minimize deflection are the material and the section design.
A good rule of thumb with plastics is that as the E value increases for a given material, the impact strength decreases. There are engineered materials that can solve these problems but they are too expensive for wide spread use. The most common method is to use a commodity resin such as polyethylene or polypropylene and add a filler to stiffen the resin. Fillers add weight and reduce impact strength for a given material as well as impact the recyclability in some cases. They also add cost, which can be the biggest problem to overcome. So, the ideal pallet would use a commodity resin because of cost, weight, and impact strength. Accordingly, optimizing the design of the pallet is the preferred method to achieve improved pallet performance.
As mentioned above, deflection decreases as the section moment of inertia (I) increases. For a pallet, the easiest method to increase stiffness is to increase height. However, in practice there is a maximum allowable height for pallets, and existing pallets are generally designed at this maximum value. Accordingly, the only alternative is to maximize the moment of inertia for each pallet component, namely the top deck 16 and bottom deck support rails 20 .
For a given section geometry, the highest I value is for a solid section. For instance, the stiffest top deck design is one that is a solid plastic. Obviously, this is impractical because of weight and cost. Most designs attempt to overcome this by using ribbed sections instead of solid sections to minimize the loss of I and reduce the weight to an acceptable level. Another method is to use foaming agents along with the ribs to minimize the weight of the ribs and improve the I value. Both methods have a limit to their effectiveness. Namely, ribs are not the ideal geometry to maximize the I value, and while foaming improves this slightly, it also reduces the impact strength of the material.
It is known that for a given section the material closest to the neutral axis has the least effect on the I value, and the material farthest away has the greatest effect. In other words, a hollow or I-beam section is stiffer than a rectangular section of equal height and area. Therefore, the object of the design is to create hollow or boxed sections everywhere possible. Conventional injection molding techniques make this almost impossible to create, but by using a simple secondary operation, we are able to make a boxed top deck 16 and bottom deck 19 .
A pallet in accordance with the present invention includes the top deck portion 16 , which is injection molded conventionally and consists of a flat upper surface 22 with a series of ribs 24 protruding from the upper surface 22 as shown in FIG. 2 . The top deck portion 16 includes a plurality of pockets 26 for receiving the support columns 18 . A plurality of plastic sheet strips 28 are sonically welded to the ribs 24 to form a plurality of substantially rectangular hollow boxed sections between the pockets 26 within the top deck 16 (as described later with reference to FIG. 4 ). Alternatively, other attachment methods such as vibratory welding, hot plate welding, adhesive etc. may be used for attachment of the plastic sheet strips 28 .
The bottom deck 19 is constructed similarly but has the support columns 18 integrally molded therewith. Ribs 30 protrude downwardly from the sheet portions 32 of the support rails 20 , and a plurality of plastic sheet strips 34 are welded to the ends of the ribs 30 to form a plurality of boxed cross-sections along the length of the rails 20 between the columns 18 . The top and bottom decks 16 , 19 may be joined permanently by welding, or can be snapped together as commonly known in the art.
The method described above is preferably used to stiffen conventional ribbed pallet designs. The small sheets of plastic 34 are welded into critical deflection areas of the existing pallets for stiffening. Also, new pallets could be designed to accept the sheets for applications that require racking, and would eliminate the sheets for lighter, lower cost applications. For example, the ribs 30 may be recessed in order to receive the sheets 34 in a position flush with the bottom surface of the support rails 20 .
The method described above is particularly applicable for use in pallets such as that shown in FIG. 1 which has a very thin top deck 16 and bottom deck 19 to allow four-way entry of pallet jacks. The method described may be used to maximize the moment of inertia of each deck member.
Referring to FIG. 4, an alternative embodiment of the invention is shown. Similar to the embodiment shown in FIG. 1, the bottom deck rails 40 include a sheet portion 42 with a plurality of vertical ribs 44 extending therefrom. The plastic sheet strips 46 are welded to the ribs 44 to form the plurality of substantially rectangular hollow vertical cross-sections 48 along the length of the support rails 40 . Of course, numerous ribs 44 could be added to create numerous rectangular cross-sections for further improved structural integrity.
The pallet shown in FIG. 4 differs from the earlier embodiment described with reference to the FIGS. 1-3 in that a large sheet 50 is welded to the ribs 52 across the breadth of the upper deck 54 for improved structural integrity of the upper deck 54 .
It is contemplated that good results could be achieved even by only welding the peripheral ribs to the plastic sheet strips. It is further contemplated that the plastic sheet strips need not be welded, but could be affixed in any manner, such as adhesive, etc. It is also contemplated that the sheet strips need not be plastic.
Referring to FIGS. 5 and 6, a second alternative embodiment of the invention is shown. In this embodiment, the pallet 110 includes a thin top deck 116 connected to a thin bottom deck 119 by nine support columns 118 . The bottom deck 119 is comprised of a plurality of support rails 120 which extend between the columns 118 . Each support rail 120 includes a sheet portion 122 . Because each support rail 120 forms a relatively weak structural portion of the pallet 110 , an extruded plastic rectangular tube 127 is welded against each respective sheet portion 122 to add stiffness to each support rail by forming substantially rectangular vertical cross-sections along the length of each support rail 120 . Similarly, the top deck 116 includes open channels 128 adjacent the top sheet 130 , and an extruded plastic rectangular tube 131 is welded within each channel 128 against the top sheet 130 between the columns 118 to form substantially rectangular vertical cross-sections along the length of each channel 128 between the columns 118 for improved stiffness. In this configuration, the rectangular tubes 127 , 131 may be inexpensively extruded, and add substantial structural integrity to the pallet 110 without limiting the pallet's ability to receive pallet jacks from any side thereof.
While the best mode for carrying out the invention has 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 method is provided for reinforcing a plastic pallet having a plurality of relatively weak structural portions each including a sheet portion with a plurality of vertical ribs extending therefrom. The method contemplates affixing a plurality of sheet strips to the vertical ribs in the plurality of relatively weak structural portions, respectively, to form a plurality of substantially rectangular hollow vertical cross-sections along the length of the relatively weak structural portions for improved stiffness.
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CROSS REFERENCE TO RELATED APPLICATIONS AND PATENT
This application is a divisional of commonly assigned, copending United States application Ser. No. 07/363,784, filed: June 9, 1989, entitled "METHOD AND APPARATUS FOR REDUCING THE STICKINESS OF THE FIBERS OF COTTON FLOCKS CONTAMINATED WITH HONEY DEW".
This application is related to copending United States application Ser. No. 07/132,790, filed Dec. 10, 1987, entitled "TREATMENT OF COTTON", and now granted as U.S. Pat. No. 4,888,856 on Dec. 26, 1989, which application is a divisional application to United States Application Ser. No. 06/833,987, filed Feb. 26, 1986, entitled "TREATMENT OF COTTON", now U.S. Pat. No. 4,796,334, granted Jan. 10, 1989, which is related also to copending United States application Ser. No. 07/207,252, filed June 15, 1988, entitled "TREATMENT OF COTTON", and which application is a continuation application to the aforementioned parent application, namely United States application Ser. No. 06/833,987. This application is also related to the commonly assigned United States applications Ser. No. 07/359,495, filed May 31, 1989, and entitled "METHOD OF AND APPARATUS FOR TREATING COTTON CONTAMINATED WITH HONEYDEW", and Ser. No. 07/359,494, filed May 31, 1989, and entitled "METHOD OF AND APPARATUS FOR REDUCING THE STICKINESS OF COTTON FLOCKS".
BACKGROUND OF THE INVENTION
The present invention broadly relates to an apparatus for treating cotton flocks at an early stage of cotton processing and, more specifically, pertains to a new and improved apparatus for reducing the stickiness of the fibers of honeydew-contaminated cotton flocks.
Generally speaking, the present invention also relates to a new and improved method of the type hereinbefore described and which method entails heating the honeydew-contaminated cotton flocks.
It is known that cotton flocks of certain provenances or origins are contaminated or coated to varying degrees with sugar-containing secretions from insects. These secretions containing sugar are generally known as honeydew. A large number of proposals have been made as to how honeydew can be made to caramelize by heating cotton flock samples for the purpose of determining the degree of honeydew contamination from the resulting change in the color of the cotton flocks. This is namely very important because, in the event of considerable contamination, the cotton flocks become sticky or tacky and tend to stick or adhere to various parts of the yarn production plant or to form laps or coils at rolls or rollers or other rotatable members, this being very undesirable since it results in frequent interruption of the yarn manufacturing process and in an inferior yarn.
A method of the aforementioned type is already disclosed in European Patent Application No. 86.102352.1, published Oct. 8, 1986 under European Patent Publication No. 196,449. The object of this known method is to convert any contaminating honeydew into a non-sticky or non-tacky and brittle state or condition by supplying heat for a short period of time and preferably without causing any discoloration or change in the color of the cotton flocks, so that the brittle sugar deposits can be crushed and removed in the course of subsequent processing.
A number of devices or apparatuses for performing this prior art method have been proposed in the abovementioned European Patent Application No. 86.102352.1, published under European Patent Publication No. 196,449. One device or apparatus is intended to heat the fiber flocks before the actual opening of the raw cotton bales, i.e. directly at the start of the yarn manufacturing process. On the other hand, other devices or apparatuses are intended for treating fiber slivers between the card and drafting arrangement or during drafting.
In spinning mills, in which the cotton spun is heavily contaminated with honeydew, efforts are made to keep the ambient air moisture or humidity very low, and experience has shown that this results in reduction of the frequency of interruptions in the yarn manufacturing process. However, the very low air humidity is undesirable as such, since the cotton fibers suffer mechanical damage during yarn manufacture such that the yarn quality is not at an optimum although the best types of cotton in terms of quality originate from provenances where the honeydew contamination is quite considerable. Also, very dry air causes problems with regard to electrostatic charges which result, for example, in undesirable accumulations of fly fibers. Furthermore, in the case of a very low air humidity, the operating staff or personnel finds the climatic conditions inside the spinning mill unpleasant.
As a result of such difficulties many yarn manufacturers first wash the cotton flocks in order to remove the honeydew deposits. However, washing is not only expensive, but also results in reduction or deterioration of yarn quality.
Since only some types of cotton or deliveries of cotton are contaminated with honeydew, the installation of special continuous treatment plants, for instance in accordance with the disclosure of the aforesaid European Patent Application No. 86.102352.1, published under European Patent Publication No. 196,449, is in many cases undesirable, particularly since there is frequently no space at all for any subsequent installation.
SUMMARY OF THE INVENTION
Therefore, with the foregoing in mind, it is a primary object of the present invention to provide a new and improved apparatus for reducing the stickiness or tackiness of the fibers of cotton flocks contaminated with honeydew, and which apparatus does not exhibit the aforementioned drawbacks and shortcomings of the prior art.
Another and more specific object of the present invention aims at providing a new and improved apparatus reducing the stickiness or tackiness of the fibers of cotton flocks contaminated with honeydew, and which apparatus does not require extensive preparatory operations and permits using the simplest possible means requiring a minimum of space, so that by means of the inventive apparatus cotton bales or at least large parts thereof are pretreated, at least hours or preferably days or even weeks prior to the actual yarn manufacturing process, such that interruptions of the yarn manufacturing process due to honeydew contamination are largely avoided without the cotton fibers being exposed to mechanical damage and without the subsequent yarn processing having to take place in the presence of very low air humidity.
Now to implement these and still further objects of the invention, which will become more readily apparent as the description proceeds, the method of the present invention of reducing the stickiness or tackiness of the fibers of cotton flocks contaminated with honeydew is manifested, among other things, by the steps of heating the cotton flocks while still in bale form in a high-frequency field, i.e. electrical or electromagnetic field and bringing the honeydew to an elevated temperature, thus substantially evaporating the water contained in the honeydew contamination. The step of heating the cotton flocks entails a temperature increase of the cotton flocks to reach a temperature in the region of the temperature of ebullition or boiling point of water. The term "high-frequency" as used in this disclosure is intended to also encompass microwave frequencies.
Although it is generally known that cotton fibers very rapidly absorb ambient humidity, it has surprisingly been found that after the pretreatment of the cotton bales according to the new and improved method of the present invention, the stickiness or tackiness of the honeydew contamination is essentially reduced. Furthermore, it has surprisingly been found that the contaminations thus treated only slowly re-absorb moisture from the air or from the fibers to which they adhere, so that it is readily possible to pretreat the bales even more than a week prior to their use for yarn manufacture without the risk of increased stickiness or tackiness during actual yarn manufacture. This behavior is attributed to a change of the condition or state of the honeydew contamination as a result of the heat treatment. This change of properties occurs particularly when the cotton flocks undergo appropriate heating.
Preferably, the high-frequency field is produced by field generating elements arranged at opposite sides of the bale or bale portion. This ensures that a good depth of penetration of the energy is achieved so that the treatment of entire bales is rendered possible.
The high-frequency field may be a high-frequency electrical field which is generated between the plates of a capacitor, such plates constituting field generating elements. A problem can arise here inasmuch as the capacitance of the capacitor varies during evaporation of water, so that the resonant or oscillatory circuit formed by the electrical components associated with the capacitor and intended to oscillate at a very accurately set frequency, the permissible frequencies being regulated by law, tends to drift away from resonance. In other high-frequency installations this phenomenon is counteracted by varying the spacing of the capacitor plates.
This is basically possible with respect to the inventive method. However, there is a preferred arrangement in which an additional capacitor is connected in parallel to the capacitor formed by the aforesaid capacitor plates between which the cotton bale is located, adjustment being effected by a change or alteration of the adjustable additional capacitor. According to the invention, there is thus rendered possible a very rapid and accurate adjustment or adaptation of the resonant frequency of the load circuit.
In a preferred variant of the inventive method, the high-frequency field is the electromagnetic field of a microwave generator or of a plurality of microwave generators jointly heating the cotton bale. Although this may be somewhat surprising at first, since it would be initially assumed for technical reasons and considerations that the penetration depth of microwaves or microwave energy into a densely compressed cotton bale would be relatively limited. However, it has been found that this penetration depth rapidly increases with increasing temperature within the cotton bale, so that very uniform heating of the entire cotton bale is possible. This uniform heating particularly occurs when the field generating elements are disposed laterally of the cotton bale and means are provided in order to repeatedly reflect the microwave radiation to and fro through the cotton bale. This arrangement also beneficially influences the escape of water vapor occurring during heating, such water vapor ascending and being extractable from the top of the associated oven or furnace.
A characteristic of heating by means of microwaves, i.e. microwave energy, also resides in the fact that these microwaves appear to selectively act on the honeydew contaminations so that the latter reach a temperature somewhat higher than the temperature of the cotton itself. This ensures that the moisture is very rapidly expelled from the honeydew contamination and that the required change of state or condition or structure of the honeydew contamination occurs without the cotton flocks themselves having to be heated to a temperature at which a fire hazard would occur. The selective action on the honeydew contaminations also enables the treatment times to be shortened and the required amount of energy to be reduced. This, in turn, is for the benefit of the method in terms of economy of operation and constructional expenditure.
A particular feature of the method according to the invention is characterized in that the gases or air used to cool the microwave generator or each microwave generator, subsequent to flowing through the or each microwave generator, are injected into the microwave oven containing the cotton bale or bales and flow through the microwave oven to achieve an additional drying of each of the cotton bales and/or carry away escaping water vapor or steam. In this manner, the flow of gas or air used for cooling is utilized for a two-fold purpose in that the heat carried away from the microwave generators is not lost, in that it is beneficially used to extract moisture.
It has been found according to the inventive method that the treatment time can be readily selected in the range of 5 minutes to 90 minutes, depending on the moisture of the cotton bales, it being advantageous to use power in the range of 0.02 to 0.08 kilowatts per kilogram bale weight. Thus with average power and average moisture it is possible to treat a cotton bale in less than 30 minutes, so that a single microwave oven would be able to handle or cope with the entire daily production of a medium-sized cotton spinning mill. With such a treatment time there is also sufficient time available to ensure that produced water vapor or steam escapes from the cotton bale. The treatment is preferably continued until the residual moisture in the cotton is on average in the range of 4% to 1% water.
A further particularly preferred feature of the inventive method is characterized in that the microwave generator power during the pretreatment is reduced by an open loop control system or a closed loop control system in accordance with a predetermined or measured course of moisture reduction. This method results in very protective treatment of the cotton and in substantial energy saving, particularly because the cotton can steam out during reduced energy supply times, thus also reducing the risk of local overheating of the cotton.
As alluded to above, the invention is not only concerned with the aforementioned method aspects, but also relates to a new and improved construction of apparatus for carrying out the inventive method.
To achieve the aforementioned measures, the inventive apparatus, in its more specific aspects, is manifested, among other things, by the features that the apparatus comprises an oven or furnace for accommodating cotton bales, field generating elements or means arranged at opposite sides of the cotton bales for heating the latter inside the oven, and means for generating an airflow through the oven.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood and objects other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein throughout the various figures of the drawings, there have been generally used the same reference characters to denote the same or analogous components and wherein:
FIG. 1 is a schematic cross-section through a first exemplary embodiment of the apparatus constructed according to the invention and in which a cotton bale is heated by means of microwaves or microwave energy; and
FIG. 2 is a schematic cross-section through a second exemplary embodiment of the apparatus constructed according to the invention and in which cotton bales can be heated by means of high-frequency energy.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Describing now the drawings, it is to be understood that to simplify the showing thereof, only enough of the structure of the apparatus for realizing the inventive method of reducing the stickiness or tackiness of the fibers of honeydew-contaminated cotton flocks in bale form has been illustrated therein as is needed to enable one skilled in the art to readily understand the underlying principles and concepts of this invention. Turning attention now specifically to FIG. 1 of the drawings, the exemplary embodiment of apparatus illustrated therein by way of example and not limitation will be seen to comprise a microwave oven or furnace 11 shown in a sectional view taken through a substantially vertical plane. This microwave oven 11 is specially designed to treat cotton bales 12 in accordance with the inventive method and one or more cotton bales 12 can be treated therein. The microwave oven 11 itself comprises a base or bottom 13, a left side wall 14 and a right side wall 15, a top or upper side 16 which is formed as a chimney, tapered upwards and merges into a connecting pipe or stud 17. The microwave oven 11 also possesses a back or rear wall 18 which for the sake of clarity is shown only in broken lines in FIG. 1, and a door hinged on one of the side walls 14 and 15 to enable the cotton bale or bales 12 to be introduced into the microwave oven 11. The hinged door is not particularly shown in the drawing. If desired the back or rear wall 18 can also be constructed as a door so that the cotton bales 12 can be introduced through the front and taken out at the rear.
In a top plan view or a horizontal sectional view the microwave oven 11 is of a substantially square or rectangular configuration and its dimensions are adapted to those of a conventional cotton bale 12, but can be selected to be somewhat smaller if, and this is basically possible, only a fraction of a cotton bale 12, for instance half a cotton bale 12, is to be treated in one operation. Within the microwave oven 11 the cotton bale 12 stands with its layers 12' extending substantially horizontal on a platform 19 which is constructed as a grid through which there can pass microwaves, so that the bottom or lower side 21 of the cotton bale 12 is somewhat higher than the base or bottom 13 of the microwave oven 11. The platform 19 stands on individual legs 22 or the like between which there are suitable openings not particularly shown in the drawings. The interior or inner space of the microwave oven 11 should be larger than the space occupied by the cotton bale 12 and/or have a guide to prevent the cotton bale 12 from jamming in the microwave oven 11 if the cotton bale 12 expands and becomes larger due to the heat treatment.
The middle or center part of the base or bottom 13 is constructed as a course-mesh screen or perforate plate 23 which is non-pervious to microwaves or microwave energy so that air 24 coming from below can flow through this screen or perforate plate 23 and through the aforesaid openings provided between the individual legs 22. The top of the platform 19 is also constructed as a screen or perforate plate to enable the air 24 to have access to the cotton bale 12 and also to enable water vapor or steam escaping from the cotton bale 12 to pass through the platform 19.
Individual microwave generators 25 are arranged laterally of the microwave oven 11 although the drawing only shows four such microwave generators 25, namely two on the left side and two on the right side. The microwave generators 25 are arranged one above the other in two substantially horizontal planes. Although not shown in the drawing, further microwave generators 25 can be arranged in planes behind or in front of the plane of the drawing of FIG. 1, for example, to provide a total of twelve such microwave generators 25. A radiation outlet 26 of each microwave generator 25 projects through an associated waveguide into one of the side walls 14 and 15 of the microwave oven 11 and is directed towards the interior thereof. In this manner, radiation lobes or beams 27 of substantially funnel-divergent shape are formed, during operation, by the associated microwave generators 25, the arrangement being such as to give the maximum possible energy density in the cotton bale 12.
A plurality of wave agitators or wavers 28 are mounted at the side walls 14 and 15 of the microwave oven 11, each wave agitator 28 consisting basically of a circular metallic rotor mounted on a rotational axle or spindle 29 and driven to perform slow rotary movements, for example, ten revolutions per minute. The purpose of these wave agitators 28 is initially to reflect the radiation passing through the cotton bale 12 back and forth, so that each radiation lobe or beam 27 repeatedly passes through the cotton bale 12 before being completely absorbed. Reflection of microwaves, which reflection occurs at each metal or metallic surface, results in the energy density in the cotton bale 12 being rendered uniform to some extent. The operation of the wave agitators or wavers 28 serves to provide further uniformity of the energy density within the cotton bale 12.
The individual microwave generators 25 have to be cooled during operation, for which purpose air is pumped through these microwave generators 25 by any suitable pumping means 58. In the present example this air, after cooling the microwave generators 25, is injected or blown into collecting headers or pipes 30 which lead to an air chamber 45 located beneath the coarse-mesh screen or perforate plate 23 of the microwave oven 11. In this manner the heated-up air passes into the microwave oven 11 and ensures further heating of the cotton bale 12 and the removal of water vapor escaping as a result of the heat treatment of the cotton bale 12, such water vapor initially ascending to the connecting pipe or stud 17 and then being suction-extracted by a blower or fan, generally indicated by reference numeral 50.
The microwave generators 25 each preferably have a maximum power output of about 1.2 kilowatts, and this means that with a total of twelve microwave generators 25 it is possible that a cotton bale 12 weighing approximately 220 kilograms and having an original 6% water content can be dried in about 14 minutes to have a residual moisture of 4% water. If even dryer cotton is required, for instance cotton with a residual moisture of 1%, the treatment time is extended to about 35 minutes.
It is actually not the residual moisture in the cotton itself that is important. What is important is that the moisture of the honeydew deposits or contaminants, which moisture may initially be much higher than the average moisture in the cotton bale 12, is itself reduced, this being particularly favorably achievable by means of microwaves, since microwave energy is preferentially absorbed by the water contained in honeydew. It can therefore be stated that drying of cotton to a residual moisture of 2% to 4% is sufficient to expel the excess water from the honeydew and, as assumed, bring about a change of state or condition or structure thereof, so that the tendency of these deposits to re-absorb water is substantially reduced.
Fire monitoring devices, i.e. signalling fire detectors, as schematically conveniently indicated in FIG. 1 by reference numeral 52, are installed at individual locations in the microwave oven 11 itself to detect any fire and immediately stop the supply of energy to the microwave generators 25. If required the signals of these signalling fire detectors 52 can be used to inject a quenching gas into the microwave oven 11 in order to immediately extinguish any developing fire. A particular advantage of microwave heating is that the energy supply can be immediately stopped and that the microwave oven 11 is immediately cool after the microwave generators 25 have been switched off, so that the risk of any fire outbreak by additional absorbed heat is extremely small.
A further possibility of pretreating entire cotton bales 12 or fractions thereof in accordance with the invention is schematically illustrated in FIG. 2. An oven 31 of this embodiment is of similar configuration to the microwave oven 11 in FIG. 1 but, instead of using microwave generators 25, two substantially rectangular capacitor plates 32 and 33 are provided within this oven 31, the plate 32 being arranged substantially in parallel with the left side wall 14 of the oven 31 and the plate 33 substantially in parallel with the right side wall 15 of the oven 31.
A high-grade dielectric is used between the two substantially rectangular capacitor plates 32 and 33 and the associated side walls 14 and 15 of the oven 31. In this embodiment the cotton bale 12 likewise rests on a platform 35 of grid-like construction and an air current or flow 43 is generated from below in the upward direction to remove water vapor occurring during treatment. This air current or flow 43 can be produced by means of a blower or fan, generally indicated by reference numeral 54 in FIG. 2, connected to a connecting pipe or stud 34 via a line or conduit. A high-frequency electrical alternating field forms between the two capacitor plates 32 and 33, with the result that the cotton bale 12, which represents a high-loss dielectric, is heated. In this manner, the maximum heat absorption is in the zone of high water content, for example, in the honeydew.
The high-frequency electrical alternating field is generated by a high-frequency generator 36 which feeds electrical energy to a working or operating circuit comprising an inductance 37 and the capacitor formed by the capacitor plates 32 and 33 between which there is located the cotton bale 12 serving as a dielectric. The frequency of the power supply and therefore of the high-frequency electrical alternating field must be maintained within close limits in view of regulations set by law in a number of countries, such regulations concerning limitation of stray radiation from industrial high-frequency installations. The working or operating frequency usually selected will be the industrial frequency of 27.12 MHz±0.6% or, in rare cases 13.56 MHz±0.05%.
Since the energy transmission from the high-frequency generator 36 to the working or operating circuit can be at a maximum only if the resistance of the working or operating circuit is adapted to that of the high-frequency generator 36, and since the resistance of the working or operating circuit varies according to the nature and moisture content of the actually provided cotton bales 12, it is necessary to match or adapt, during the heating process, the working or operating circuit to the high-frequency generator 36.
This is achieved, according to the invention, in that an additional capacitor 38 is connected in parallel with the load circuit and is adjusted by a controller or control unit 39 via a motor 40 and a transmission 41 or equivalent structure in order to keep constant at all times the resonant or oscillatory frequency of the load circuit.
The actual value fed to the controller or control unit 39 is the anode current of the high-frequency generator 36 or a value equivalent or corresponding thereto, and the controller or control unit 39 compares this actual value or equivalent value with a predetermined desired or reference value. In the event of any deviation, a signal is applied to the motor 40 which adjusts the additional capacitor 38 via the transmission 41 until the desired or reference value of the anode current is restored.
In operation, the cotton bale 12 is heated by the high-frequency electrical field between the two substantially rectangular capacitor plates 32 and 33 such that the moisture is expelled from the honeydew and the latter is brought to the desired or required state or condition.
Also in this exemplary embodiment of the inventive apparatus the inner space of the oven 31 should be greater than the cotton bale 12 or have a suitable guide. Here again it is advantageous to guide the waste heat of the high-frequency generator 36 through the oven 31 in the form of a heated air current or flow. Suitable fire monitoring devices or fire detectors 52 are here likewise shown in FIG. 2.
If the cotton bale 12 to be pretreated is held together by metal strapping or bands, such metal strapping or bands should be removed and replaced by suitable plastic strapping or bands prior to introducing the cotton bale 12 into the oven 31.
While there are shown and described present preferred embodiments of the invention it is to be distinctly understood that the invention is not limited thereto, but maybe otherwise variously embodied and practiced within the scope of the following claims. ACCORDINGLY,
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The invention relates to an apparatus for reducing the stickiness or tackiness of the fibers of honeydew-contaminated cotton flocks by heating the same. For this purpose, the cotton flocks while still in bale form are heated in a high-frequency electrical or electromagnetic field until the honeydew is brought to an elevated temperature and the water contained in the honeydew contamination is substantially evaporated, the temperature preferably being such that the cotton flocks reach a temperature in the region of the temperature of ebullition of boiling point of water.
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BACKGROUND OF THE INVENTION
This invention relates in general to multi-stage servovalves and in particular to a two-stage, shear-type, fail-fixed servovalve with motion amplification in its second stage and a method for actuating the second stage.
Servovalves are used broadly to interface between an electrical control system and mechanical metering or actuating devices, for example, as engine control equipment in an aircraft flight control system for controlling the fuel flow to a gas turbine in response to an electrical control signal. In the latter case, a control signal typically controls the operation of the servovalve such that the velocity of a servopiston changes with the control signal. The servopiston itself may be mechanically coupled to a fuel metering valve or the like, whose status determines the fuel flow to the engine. In such an arrangement, it is desirable to use a fail-fixed servovalve, i.e., a valve which causes the servopiston to lock in place immediately under certain conditions. In one case, the piston must be locked when a loss of the electrical control signal occurs in order to safeguard against unwanted change in fuel flow to the engine. In another instance, the piston must be locked when the electrical control signal exceeds a predetermined value in either direction in order to prevent unwanted fuel flow change if and when a malfunction occurs in the electrical control system.
In a two-stage electrohydraulic servovalve, a fluid under pressure is used to move a mechanical element, e.g. a spool or a piston. In the second stage, the pressurized fluid is vented to a servopiston chamber in accordance with the position of the mechanical element. One type of currently used two-stage servovalve, e.g. as shown in U.S. Pat. No. 4,227,443, further includes a torque motor in the first stage which moves a jet nozzle in response to an electrical control signal. The nozzle directs the flow of fluid toward a pair of input orifices, each receiving fluid for a separate fluid path. The two fluid paths terminate at opposite ends of a common bore in a housing. A spool is movably disposed in the bore such that the spool's position is controlled by the relative flow of fluid through the two fluid paths. A feedback spring has one end attached to the spool and the other end affixed to the nozzle. The spring repositions the jet pipe when the spool attains a position corresponding to the reference value of the control signal. The spool has a plurality of relieved areas interspaced with a plurality of lands. The housing contains passages which communicate between the bore and a high pressure fluid reservoir and a low pressure fluid sump respectively, and between the bore and opposite ends of a servopiston chamber. A servopiston, movably disposed within a servopiston chamber, is actuated by pressurized fluid vented through the aforesaid passages as the spool moves within the bore of the housing opening and closing the passages.
It is commonplace to actuate the first stage of the servovalve with either a DC control signal or a pulse width modulated control signal, provided the latter's frequency is high enough so that the torque motor, in the first stage, does not respond to each individual waveform applied to its inputs. Thus, a DC control signal of one-half of the maximum rated current applied to the first stage actuates that stage in a similar fashion as a pulse width modulated control signal which has an average value of one-half of the rated current if the frequency of the latter signal is high enough. The displacement and actual position of the spool, in the above-noted patent, is normally directly proportional to the time average torque motor current from a null or reference current. A detailed description of this spool-type servovalve appears in U.S. Pat. No. 4,227,443, which is assigned to the assignee herein and is incorporated herein by reference.
The spool-type servovalve, as described above, requires a spool which is closely fitted to the bore of the housing to prevent significant leakage around the spool when the spool blocks the passages between the high and low pressure reservoirs and the servopiston chamber. Even with a close fit, the rate at which fluid seeps between the spool and the bore is not constant. Therefore when the spool closes the passages leading to the servopiston chamber, the leakage around the spool causes the servopiston to move slightly or creep at a rate which is difficult to predict or to maintain constant. When the spool and bore wear with use, the creep is even more difficult to determine. The requirement for a close fit makes the spool-type servovalve costly to manufacture since the spool must be machined to fit the bore precisely. Spool-type servovalves are also vulnerable to contaminant material, such as grit in the fluid supply, which is capable of jamming the spool in the bore.
Electrohydraulic two-stage servovalves currently in use in aircraft flight control systems commonly operate in a closed system at hydraulic supply pressures on the order of 3,000 psi. In a closed system, the hydraulic fluid, usually oil, is recirculated and fine-filtered. Since the fluid is exposed to very few elements external to the system, few external contaminants are introduced into the system and the amount of grit, or similar contaminate material in the fluid which may affect the operation of the servovalve, can be kept to a minimum.
In an engine control system, the engine fuel itself is preferably used as the hydraulic fluid. Such a system is by necessity an open system and hence fine-filtering requires large or multiple filters or frequent filter element replacement. An engine control system of this type should therefore be tolerant of comparatively large amounts of contaminant. Further, such a control system normally operates at a lower pressure, i.e., in the range from 200 to 1,000 psi. Hence, the servovalves of such a control system have smaller second stage force levels or contaminant shearing force levels than those of a high pressure system, unless the spools are made larger.
OBJECTS OF THE INVENTION
It is an object of the present invention to provide an improved servovalve.
It is another object of the present invention to provide a shear-type, fail-fixed servovalve which is relatively tolerant of contaminant material.
It is a further object of this invention to provide a shear-type, fail-fixed servovalve which has a high second stage force and which responds quickly to a change of the control signal.
It is still another object of this invention to provide a shear-type, fail-fixed servovalve which has relatively less leakage in its fail-fixed position than prior art spool-type, fail-fixed servovalves.
It is still a further object of this invention to provide a shear-type, fail-fixed servovalve which is capable of being precisely adjusted at various positions and which has enhanced reliability over comparable prior art servovalves.
It is another object of this invention to eliminate the feedback spring used in conventional shear-type servovalves by causing the piston in the second stage of the servovalve to respond to the movement of the jet pipe in either direction from the null position.
It is an additional object of this invention to provide a shear-type, fail-fixed servovalve which is simpler and less costly to manufacture than conventional spool-type servovalves.
These and other objects of the invention, together with the features and advantages thereof will become apparent from the following detailed specification when considered with the accompanying drawings.
SUMMARY OF THE INVENTION
The shear-type servovalve in accordance with the principles of this invention includes a piston having a piston head linearly and movably positioned in one chamber and a piston rod connected thereto. The piston rod extends into at least one other chamber and is linearly movable therein along its axis which is substantially parallel to a planar surface defining in part the last recited chamber. Two passages extend through the piston and communicate with said one chamber on opposite sides of the piston head. Each passage includes an input orifice at one end of the piston rod. An angularly movable jet of fluid is directed at the input orifices. The jet has a null angular position disposed at a predetermined offset angle with respect to said axis at which fluid is supplied, in predetermined relative amounts, to the input orifices. Means responsive to a selectively variable control signal for changing the angular position of the jet is effective to produce a magnified linear piston displacement by varying the relative amounts of fluid supplied to the input orifices. At least one shoe is supported on the piston rod. Means may be included for yieldingly urging the shoe against the plate surface. Ports in the plate surface are adapted to be opened and closed by the shoe in accordance with the linear position of the piston.
A method of actuating the piston in the second stage of the two-stage servovalve includes the step of providing an angularly movable jet of fluid. The jet has a null angular position at a predetermined offset angle with respect to the axis of the linearly movable piston. The method further includes the step of changing the angular position of the jet in response to a control signal which produces a magnified linear piston motion in the second stage.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a cross-sectional view of a servovalve in a first operational mode;
FIG. 2 is a cross-sectional view of the servovalve in another operational mode;
FIG. 3 is a cross-sectional view of the servovalve in still another operational mode;
FIG. 4 is a cross-sectional view of the servovalve in a further operational mode;
FIG. 5 is a cross-sectional view of the servovalve in still a further operational mode; and
FIG. 6 is a cross-sectional view of another embodiment of a servovalve in accordance with the principles of the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, FIG. 1 illustrates a preferred embodiment of the invention. The servovalve shown includes a housing 12, having a first chamber 14, a second chamber 16, a third chamber 18 and a fourth chamber 19 with chambers 14 and 16 intermediate chambers 18 and 19. Chambers 14 and 16 are defined in part by a substantially planar surface 20 of a plate or plate portion 21, which is part of housing 12, and by chamber walls 22, 24 and 25 normal to the surface 20. A piston 26 includes piston head 28, which is linearly moveable along its axis 64 within chamber 18. A piston rod 30 is affixed to piston head 28. Piston rod 30 extends through chambers 14 and 16, substantially parallel to surface 20 and slidably engages chamber walls 24, 22 and 25 in a fluid-sealing relationship. The seal may be provided by O-rings positioned in grooves 34, 36 and 38 located in chamber walls 24, 22 and 25 respectively.
A first internal fluid passage or receiver tube 40 extends through piston rod 30 between one end 42 and the other end 32 of the piston rod. A second internal fluid passage or receiver tube 44 similarly extends through piston rod 30 between opposite ends thereof. Each fluid passage 40 and 44 has corresponding input and output orifices. A first output orifice 46, communicates between first fluid passage 40 and chamber 18, to one side of piston head 28. A second output orifice 48 communicates between second fluid passage 44 and chamber 18 on the opposite side of piston head 28. First and second input orifices 50 and 52, corresponding to fluid passages 40 and 44 respectively, are positioned proximate each other at piston rod end 42 and are disposed in a chamber 19. A shroud 54, which includes circumferentialy spaced, radial passages 56, extends from piston rod end 42 into chamber 19.
A jet pipe 58 is adapted to receive a flow of pressurized fluid from a fluid supply passageway 130 which communicates with a high-pressure fluid supply reservoir, the latter being omitted in FIG. 1. The jet pipe is supported at a pivot point 60 such that it can be angularly moved to direct a jet of fluid through its nozzle 66 at the first and second input orifices 50, 52 and thereby vary the relative amounts of fluid supplied to the latter. In the first stage, a conventional torque motor 62, or the like, is provided for angularly positioning jet pipe 58 and is adapted to respond to a selectively variable control signal applied at terminals 61 and 63. Thus, jet pipe 58 is adapted to be turned through an angle proportional to a current applied to terminals 61, 63. The control signal may be DC or pulse width modulated as described in the background of the invention.
FIG. 1 illustrates jet pipe 58 in its position wherein it is disposed at a predetermined angle with respect to the axis 64 of piston head 28 and piston rod 30. In this null position, nozzle 66 is adapted to provide fluid in predetermined relative amounts to input orifices 50 and 52. In the aforementioned position, the relative amounts of fluid passing through passages 40 and 44 produce balanced forces on opposite sides of piston head 28, such that piston 26 remains stationary in the position shown in FIG. 1. Shroud 54, into which nozzle 66 extends, is adapted to limit the movement of the nozzle and hence the angular movement of the jet pipe. Shroud 54 further functions to contain the fluid sprayed from nozzle 66 and to direct the major portion of the fluid flow to the two input orifices. When the jet pipe assumes a first or a second extreme angular position in response to a maximum rated control signal or a minimum rated control signal respectively, shroud 54 limits the jet pipe motion so that the jet is directed substantially toward one input orifice and prevents the jet of fluid from fanning out significantly before the fluid reaches input orifices 50, 52. Radial passages 56 in shroud 54 allow fluid that does not enter input orifices 50, 52 to enter chamber 19. The shroud therefore increases the recovered pressure especially when the jet pipe nozzle is at the maximum distance from input orifices 50, 52.
In the second stage, first and second shoes 70 and 68 are carried by piston rod 30 by a pair of supports 78 and 72 respectively. Shoes 68 and 70 are disposed in chambers 16 and 14 respectively. Supports 72 and 78 are affixed to piston rod 30 and maintain the axial position of the shoes relative to the piston head and the piston rod. Set screws or other means, not shown herein, for adjusting the axial position of shoes 68 and 70 may be incorporated within supports 72 and 78 respectively.
Shoes 68, 70 include first surfaces 69, 71, respectively and second surfaces 73, 75, opposite said first shoe surfaces. A pair of leaf springs 74 is interposed between piston rod 30 and shoe surface 73 and yieldingly urges the shoe surface 69 into contact with plate surface 20. Support 72 includes a vent 76 adapted to communicate with chamber 16. Alternatively, such communication may occur by way of a bore through piston rod 30. Another pair of leaf springs 80 is interposed between piston rod 30 and shoe surface 75 and yieldingly urges shoe surfaces 71 into contact with plate surface 20. A vent 82 communicates with chamber 14. Vent 82 may be replaced by a bore through piston rod 30, as explained above. Shoe 70 has an internal bore 84 therein and a smaller bore 86 therethrough. The smaller bore 86 is adapted to provide communication from shoe surface 75 of shoe 70 to bore 84. A preselected area of surface 75 is isolated from the fluid in chamber 14 by an O-ring 88 set in a pair of grooves disposed in surface 75 and piston rod 30. The purpose of this arrangement will become clear from the discussion below.
Plate surface 20 has six ports in the illustrated embodiment of the invention. Chamber 14 has first, second and third ports, 114, 98 and 124 respectively, communicating therewith. Similarly, chamber 16 has first, second and third ports, 110, 94 and 90, respectively communicating therewith. Port 90 is open to chamber 16 and connects the latter to a high-pressure fluid supply PS through fourth passageway 92. Ports 94 and 98 both communicate with second passageway 96. Ports 110 and 114 both communicate with first passageway 112. Passageway 112 is adapted to communicate with a servopiston chamber 118 through means including a pair of ports 127, 129 in housing 12 and in said servopiston chamber respectively, and specifically with a first portion 116 of chamber 118 positioned to one side of servopiston head 122. Passageway 96 is adapted to communicate with other portion 120 or the second portion of servopiston chamber 118 through means including a pair of ports 131, 135 in housing 12 and in said servopiston chamber respectively, the second portion being on the opposite side of servopiston head 122. The pressures on opposite sides of head 122 are designated P C1 , P C2 respectively. Servopiston head 122 is movably disposed within chamber 118 and responds to varying flows of fluid to the chamber and/or changing pressures P C1 and P C2 . Its piston rod may actuate a fuel metering device or other apparatus, not shown in FIG. 1.
Port 124 communicates with a low pressure fluid sump P R through a third passageway 126. A return fluid path 128 communicates with chamber 19 and passageway 126. A fluid supply passageway 130 communicates with chamber 16 to supply the jet pipe 58 with high pressure fluid.
As an example of the operation of the servovalve described herein, the null position of jet pipe 58 shown in FIG. 1 corresponds to an electrical control signal equal to 50% of the maximum rated control signal. In the null position, input orifices 50 and 52 receive predetermined relative amounts of the fluid emitted by nozzle 66 and each creates a force on piston head 28. When the forces acting on opposite sides of piston head 28 are in balance, the piston remains stationary. In this piston position, which corresponds to the null position of jet pipe 58, predetermined ports 94, 110, 98 and 114 are closed by shoes 68 and 70 so that substantially all fluid flow to or from servopiston chamber 118 is blocked. As described hereinabove, the position of shoes 68, 70 may be precisely adjusted over the ports by appropriate adjusting means in supports 72 and 78. Therefore, the position of the shoes may be changed to reduce leakage around the shoes between each of chambers 14 and 16 and passages 96, 112 when the piston is in the aforementioned piston position. If the means for adjusting is incorporated, the manufacture and assembly of the shoes, supports and piston rod is simplified and these parts do not have to meet the close tolerances required in prior art servovalves. These factors are reflected in lower production costs.
Chamber 16 is filled with fluid at a pressure which approaches that of high-pressure supply P S . In operation, chamber 14 is also filled with a fluid under pressure and, as will be described hereinafter, the pressure in that chamber is substantially equal either to P C1 or P C2 , depending on the position of piston head 28, piston 26 and thus of shoes 68 and 70. By virtue of vents 76 and 82, pressurized fluid is applied to surfaces 73 and 75 of shoes 68 and 70 respectively. This pressure urges shoes 68 and 70 against plate surface 20 and thus enhances the seal with surface 20. The pressure loading of shoes 68 and 70 is counterbalanced by the pressures P C 1 and P C 2 in passageways 112 and 96 respectively, which act on surfaces 69 and 71 of those shoes.
Passageway 126 communicates with low pressure reservoir P R . Therefore, the presure loading of shoe 70 is normally greater than that of shoe 68 because the pressure in passageway 126 does not provide enough counteracting force to the pressure in chamber 14 which is applied to surface 75 of shoe 70 through vent 82. To limit the force urging shoe 70 toward plate surface 20, the area of surface 75 which is exposed to the pressure in chamber 14 is limited by O-ring 88. Thus, the area inside the O-ring is not subject to the pressure applied to the area of surface 75 external thereto. In order to create a low pressure inside O-ring 88, a small bore 86 communicates with the low pressure region of bore 84 and passageway 126. Leaf springs 74, 80 provide additional forces urging shoe surfaces 69, 71, respectively, into contact with plate surface 20 to insure a minimum pressure for sealing the ports at all times.
It will be clear from the foregoing discussion that shoes 68 and 70 are yieldingly urged against surface 20 with which the shoes make sliding contact. Although the pressure loading of the shoes is sufficient to seal the ports in the piston position shown in FIG. 1, it nevertheless allows the shoes to push aside or ride over grit or other contaminant material that may be introduced into the servovalve by the fluid. This tolerance to contaminants helps prevent the servovalve from jamming, thus making it suitable for use with fuel, which is filtered to normal levels, as the hydraulic fluid in an engine control system.
The angular displacement of jet pipe 58 from its null position is normally proportional to the percentage change of maximum rated control signal that is applied to torque motor 62 through terminals 61, 63. Thus, a 25% change in the maximum rated control signal moves the jet pipe through 25% of its total angular sweep. In accordance with the present invention, the null position of jet pipe 58 is at a predetermined offset angle α with respect to axis 64. This offset angle provides motion amplification for the second stage of the servovalve. For example, in one embodiment of the invention where the jet pipe is at an offset angle α of five degrees (5°) from axis 64 and the tip of nozzle 66 is located one inch (1") from pivot point 60, piston head 28 and piston 26, and thus shoes 68 and 70, will be linearly displaced along axis 64 by ±0.125 inches in response to an angular movement of ±0.7 degrees of jet pipe 58. In such an arrangement, the motion amplification is approximately 10 to 1, i.e., piston head 28 moves 0.125 inches when the nozzle 66 moves 0.012 inches along its circumferential arc.
In a conventional arrangement, when the torque motor 62 is impressed with a control signal equal to 25% of the maximum rated control signal, the jet pipe will change its angular position by 25%. Since the null position in the embodiment under discussion corresponds to 50% of maximum rated control signal, 25% of maximum represents a decrease in signal amplitude and causes jet pipe 58 to be angularly displaced in a first direction relative to the null position, e.g. upward, i.e. in a clockwise direction about point 60. This change in angular position will cause relatively more fluid to enter input orifice 50 and passage 40 than is supplied to orifice 52 and passage 44. As the balance on opposite sides of piston head 28 is disturbed, piston 26 is caused to move to the left because of the increased pressure on the rod-side of the piston head and the decreased pressure on the opposite side. Shoes 68 and 70 will likewise slide to the left so as to open predetermined ports 110 and 114. This position is shown in FIG. 2. With port 110 open, there is now communication between chamber 16 and passageway 112, so that pressure P C1 will approach supply pressure P S . As consequence, the pressure in portion 116 of servopiston chamber 118 likewise approaches P S .
Simultaneously, shoe 70 opens port 114 and hence the pressure in chamber 14 will approach supply pressure P S . Shoe 70 also opens port 98 and thus communication is provided between portion 120 of servopiston chamber 118, passage 96, port 98, bore 84, port 124 and passageway 126 to low pressure fluid sump P R . In this position of piston 26, pressure P C2 becomes substantially equal to PR The result of the above-described operation is to raise the pressure in portion 116 of servopiston chamber 118 and simultaneously lower the pressure in portion 120. Hence, servopiston 117 is caused to move to the right.
When the control signal applied to torque motor 62 drops to 0% of the maximum rated control signal, jet pipe 58 will angularly move still further upward, until nozzle 66 is in close proximity to shroud 54. As previously explained, shroud 54 limits the total angular movement of the jet pipe and thereby insures that even in the extreme clockwise positon of the jet pipe, a substantial amount of the fluid emitted by nozzle 66 will be received by orifice 50. Piston 26 is now caused to move to the left against stop 132, as shown in FIG. 3. At this point, port 110 is completely uncovered by shoe 68. Accordingly, pressure P S is vented through passageway 112 and pressure P C1 will approximate pressure P S . Shoe 68 continues to block port 94 and shoe 70 is now blocking predetermined port 124. Hence, passageway 96 is now isolated from chamber 14 and passageway 126 and no hydraulic fluid is allowed to escape therefrom. Pressure P C2 will increase to a value approximately equal to P S to balance the forces acting on opposite sides of servopiston head 122. However, relatively little fluid flows from portion 120 of servopiston chamber 118 and consequently servopiston 117 is locked in place. Stated differently, when pressure P C2 is isolated, it increases in value to balance the forces on head 122 developed by P C1 but the servopiston remains stationary because the fluid is relatively incompressible and fluid flow is blocked from portion 120. There is some leakage in the valve under shoes 68, 70. This leakage causes servopiston 117 to creep, i.e., to move very slowly. In the present invention, such creep occurs at a relatively slow rate compared with prior art servovalves because of the configuration of the shoes and the cooperation between the shoes, the plate surface and the ports.
In the one specific embodiment of the invention, the locking of servopiston 122, i.e., the point at which shoe 70 has closed port 124, occurs at approximately 12.5% of the maximum rated control signal. For all signals less than this 12.5% current, the servopiston is locked in place and thus provides the aforementioned fail-fixed action.
When the control signal returns to 50% maximum rated control signal from 0%, jet pipe 58 swings downward, i.e. in a counterclockwise direction. Piston 26 responds to this change in angular position by moving to the right due to the varied relative amounts of fluid supplied to opposite sides of the piston head. Hence, the piston in the present invention responds to the movement of the jet pipe without the necessity of return springs. Likewise, shoes 68 and 70 will again pass through the position shown in FIG. 2. Hence, hydraulic fluid is vented to chamber portion 116 and vented away from chamber portion 120. Portions 116 and 120 of servopiston chamber 118 again are affected by this flow and pressure change and, as a result, servopiston 117 moves to the right. When the control signal reaches 50% of maximum rated value, jet pipe 58 again assumes its null position and piston 26 assumes the position illustrated in FIG. 1. Since shoes 68 and 70 again block ports 94, 110, 98 and 114, pressures P C1 and P C 2 are approximately equal to each other and since the flow is blocked by the shoes, the servopiston remains stationary.
A detailed description of the actuation of the servopiston with respect to the opening and closing of the ports is provided in U.S. Pat. No. 4,227,443 which is incorporated herein by reference.
When a control signal equal to 75% of the maximum rated value is impressed on torque motor 62, jet pipe 58 angularly moves in a counterclockwise direction from the null position shown in FIG. 1. More fluid is now directed at input orifice 52, which results in an imbalance of forces acting on piston head 28. Accordingly, piston head 28 and piston 26 are now caused to move to the right. As shoes 68 and 70 move to the right, shoe 68 opens predetermined port 94 and admits fluid at the high pressure P S to passageway 96. Hence, pressure P C2 now approaches P S . Simultaneously, shoe 70 opens port 114. Thus pressure P C1 in portion 116 of servopiston chamber 118 is vented to low pressure sump P R . The position of piston 26 and shoes 68, 70 for this situation is illustrated in FIG. 4. Servopiston 117 is now caused to move to the left due to the flow of hydraulic fluid in passages 96 and 112 and the pressure differential between P C2 and P C1 . When the control signal is equal to 100% of the maximum rated value, jet pipe 58 reaches its extreme counterclockwise displacement from the null position and nozzle 66 is now in close proximity to shroud 54. The action causes piston 26 to move further to the right until piston head 28 butts stop 133 or some other suitable stop, as shown in FIG. 5. In this position, port 94 is uncovered by shoe 68 and, as a consequence, pressure P C2 substantially equals P S . Simultaneously, shoe 68 blocks port 110 and shoe 70 now blocks predetermined port 124 which communicates with low pressure sump P R . Thus passageway 112, which communicates with portion 116 of servopiston chamber 118, is sealed off. Therefore, servopiston 117 is locked in place because the hydraulic fluid flow is blocked. This is the other fail-fixed position and it corresponds to a control signal which exceed a predetermined value. For the example under consideration, the predetermined value is 87.5% of maximum rated control signal.
FIG. 6 illustrates another embodiment of the present invention in which corresponding reference numerals have been carried forward. Chambers 18 and 16 are intermediate chamber 14 and an additional fourth chamber 119. A piston 26 includes piston head 28 and piston rod 30 includes left-hand and right-hand extensions 141 and 151 respectively, as well as passages 140 and 144 which terminate in output orifices 146 and 148 respectively, on opposite sides of piston head 28. Piston head 28 is moveably disposed in chamber 18 along axis 164 of the piston head and the piston rod. The left-hand extension 141 of the piston rod extends into a fourth chamber 119 and slideably engages chamber wall 145. An O-ring set in a groove 147 in chamber wall 145 provides a fluid-tight seal. End 142 of piston rod extension 141 is located in chamber 119 and includes a pair of input orifices 150 and 152 corresponding to passages 140 and 144, respectively. A shroud 154, which includes circumferentialy spaced, radial passages 156, extends from end 142 of piston rod extension 141. A vent 149 is adapted to communicate between the low pressure fluid sump P R and chamber 119.
The right-hand extension 151 of piston rod 30 extends through chamber 16 and into chamber 14 and it slideably engages chamber walls 24 and 22. O-rings set in grooves 134 and 136 respectively provide a fluid seal with walls 24 and 22. Piston rod extension 151 includes a section 153 which is substantially parallel to plate surface 20 and which supports shoes 68 and 70, in chambers 16 and 14 respectively. The operation of the servovalve shown in FIG. 6 is similar to that of FIG. 1, except that the jet pipe 58 moves in a counterclockwise in response to a control signal which is equal to 25% of the maximum rated control signal. Conversely, jet pipe 58 moves clockwise in response to a control signal which is equal to 75% of the maximum rated control signal. However, piston head 28, and therefore piston rod 30 and extensions 141 and 151, move to the left when a control signal equal to 25% of the maximum rated control signal is applied to torque motor 62.
Although extension 151 is shown to be coaxial with piston axis 164, it will be understood that the invention is not so limited. For example, if the structure of housing 12 so dictates, extension 151 may take the shape of a dog leg, provided only that shoes 68 and 70 move in a direction parallel to plate surface 20.
A similar structural variation is possible for piston rod extension 141, provided only that jet pipe 58 has a null position disposed at a predetermined offset angle with respect to the axis 164 of the piston rod.
The servovalve in accordance with the present invention is capable of handling various supply pressures P S . This is true even though the frictional forces which resist the movement of shoes 68, 70 increase with increasingly higher supply pressures P S . To compensate for the added frictional drag on shoes 68 and 70, the force applied to piston 26 may be increased by enlarging the area of piston head 28. Since the size of piston head 28 in the second stage of the servovalve is relatively independent of the size of all other elements, i.e. of the piston rod, shoes, etc., the force required to move shoes 68, 70 can be developed without significant design modifications.
The servovalve, in accordance with the present invention, could be constructed with chambers 14 and 16 combined as one chamber. In this embodiment, internal passages through shoes 68 and 70 and rod 30 would allow communication between passages 96 and 112 and the high and low pressure reservoirs. Another variation of this latter embodiment would utilize a single shoe yieldably supported by rod 30.
Various dimensional combinations are possible in the servovalve which constitutes the subject matter of the present invention. In one embodiment of the invention, nozzle 66 is preferably spaced a maximum of five inside diameter nozzle lengths from input orifices 50, 52 when the piston head 28 abuts shoulder 132. Ports 94, 110, 98 and 114 are rectangular in shape, having a length of approximately 0.100 inches of stroke relative to piston 26, by 0.190 inches wide for an 8 gallon per minute servovalve. Port 124, which leads to the sump by way of passageway 126, consists of a long slot, approximately 0.025 inches of piston stroke by 0.760 inches wide. Piston head 28 has an area of approximately 1.25 square inches. These dimensions provide fail-fixed action for approximately 12.5% of the stroke of the piston 26 at each end of travel, as described hereinabove. Specifically, in such an embodiment the valve is fail-fixed or locked for control signals below 12.5% of the maximum rate value and for control signals exceeding 87.5% maximum rated value.
The invention herein is not limited to the particular embodiment disclosed. For example, the shear-type fail-fixed servovalve may be modified by including a spring which moves piston 26 in a specified direction upon the loss of the supply pressure P S . Further, piston head 28 need not be fixedly or directly connected to piston rod 30. For example, the connection may be by means of gear and flexible receiver tubes may be substituted for passages 40 and 44. Other mechanical connections will now become apparent to those skilled in the art. The predetermined offset angle α may be changed where a different motion amplification factor is desired. Further, an adjustment mechanism may be incorporated for variably adjusting the offset angle. Additionally, the means for yieldingly urging shoes 68, 70 may be modified by excluding leaf springs 74, 80 from one or both shoes, by omitting O-ring 88, or by any combination thereof.
The dimensions of shoes 68, 70 and ports 94, 110, 98, 114 and 124 may be varied to provide for different responses by servopiston 117. The location of ports 90, 92, 98, 110, 114 and 124 in surface 20 may be varied in order to provide different responses by servopiston 117. One shoe may have a plurality of passages extending therethrough which are adapted to communicate with one or more predetermined ports. Surfaces 69, 71 of the shoes may conform to a curved plate surface 20 and be modified to closely fit the curvature of the latter surface. The conforming curved surfaces may provide for better sealing of chambers 14 and 16 from passages 96, 112 and 126. Torque motor 62 may be replaced by any means which varies the angular position of jet pipe 58 in response to a control signal.
Thus, from the foregoing discussion it will be clear that the present invention is not limited to the apparatus and method specifically disclosed herein, but that numerous variations, modifications, partial and complete substitutions, equivalents and changes will now occur to those skilled in the art, all of which fall within the scope of the disclosed invention. Accordingly, it is intended that the invention disclosed herein be limited only by the spirit and scope of the appended claims.
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A shear-type, fail-fixed servovalve is disclosed which includes a piston whose piston head is movably disposed in one chamber of a multi-chamber housing. A piston rod is attached to the piston head and extends into the other chambers. Two passages extend through the piston rod and communicate with the chamber on opposite sides of the piston head. A pair of input orifices are located proximate each other at one end of the piston rod, each corresponding to one passage. An angularly movable jet pipe emits fluid directed at the input orifices. The jet pipe has a null angular position disposed at a predetermined offset angle with respect to the axis of the piston rod, and directs fluid towards the pair of orifices. Means responsive to a selectively variable control signal for changing the angular position of the jet pipe is provided which is effective to produce a magnified linear piston displacement by varying the relative amounts of fluid supplied to the input orifices. Shoes supported by the piston rod slide over ports in a plate surface in another chamber and the ports are opened and closed in accordance with the linear position of the piston. The opening and closing of these ports, in turn, determines the linear displacement of a separate servopiston. A method of operating a two-stage servovalve is disclosed which includes the step of changing the angular position of the jet pipe and producing magnified linear position displacement thereby.
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TECHNICAL FIELD
The present invention relates to the field of static random access memory (SRAM) arrays, and to a SRAM memory architecture providing for bit line partitioning.
BACKGROUND OF THE INVENTION
FIG. 1 shows a SRAM memory array architecture of the prior art. This architecture utilizes a six transistor memory cell 200 as shown in FIG. 2 . The six transistor SRAM bit cell 200 shown in FIG. 2 utilizes a first supply voltage, VDD 217 , and a ground connection 218 . The cell also includes a word line WLC. Bit lines BTC and BBC provide a connection to read and write data to the cell. The bit cell also includes a storage cell which includes four transistors, 206 , 208 , 210 , 212 , configured to store data. As is known in the art, transistors 206 and 208 act as load transistors and transistors 210 and 212 act as cross coupled storage transistors. As shown in the bit cell 200 , the load transistors 206 and 208 are PMOS transistors, and storage transistors 210 and 212 are NMOS transistors. NMOS Transistors 214 and 216 arc word line, or row select, pass transistors.
In a static mode, when the cells in the memory array are not in write or read mode, bit lines BTC and BBC, shown in FIG. 2, are precharged to a VDD level, and the word line shown in FIG. 2 as WLC is at logic zero. In this static state, a programmed cell can maintain the information equivalent to logic 0 or logic 1, since n-channel devices 214 and 216 are off, which isolates the storage cell that includes devices 206 , 208 , 210 and 212 .
In a write mode, the WLC line (e.g. WL 0 , WL 1 . . . WLN) which is coupled to a row of cells (e.g. N 00 , N 01 . . . N 0 M), as shown in FIG. 1, which contains the cell being written to, is driven to logic 1 or VDD to turn on (open) the pass transistors, thereby providing access to the storage cell. To write to the cell to be programmed to store a binary 1 , the bit line BTC for the cell being written to is driven to logic 1, and the bit line BBC is driven to logic 0. This results in the cell being programmed to logic 1, where the voltage at node 202 will be set at logic 1 and the voltage at node 204 will be set at logic 0 as is known in the art. To program the cell to logic 0 the bit line BTC is driven to logic 0 and the bit line BBC is driven to logic 1, such that 202 will be set at logic 0 and 204 will be set at logic 1 as is known in the art.
In the static mode, in between read and write operations, the bit lines BTC and BBC are held at a precharge voltage VDD using the PMOS transistors 102 of the precharge circuit 106 shown in FIG. 1 . In the static mode the word line (WL 0 , WL 1 , . . . WLN) pass transistors 214 and 216 shown in FIG. 2 are held closed as the WLC voltage is at logic zero.
To read the data from the cell the WLC voltage is changed to logic 1. The signal of voltage logic 1 on WLC is applied to the gates of the word line pass transistors 214 and 216 , which opens the word line pass transistors 214 and 216 , so that current can flow through the transistors. In addition to the WLC voltage being set to logic 1, the precharge circuit 106 is closed so that the bit lines BTC and BBC are allowed to float. With the word line pass gate transistors open, one of the bit lines BTC and BBC will discharge depending on which node 202 or 204 is at zero. For example, if the cell is programmed at logic 0 then the BTC bit line will discharge through the NMOS transistor 214 and the cross coupled storage transistor 210 , and BBC would remain floating at the VDD level. If the cell was programmed at logic 1 then BBC would discharge through 216 and 212 , and BTC would remain at VDD. The switch (SW 0 , SW 1 . . . SWM) connected to the cell which is being read will be closed (conductive) and the sense circuitry 104 will read the difference in voltage in the bit lines BTC and BBC to determine whether the data is 1 (one) or 0 (zero).
In the prior art Static Random Access (SRAM) memory architecture 100 as shown in FIG. 1, there are three stages of operation. At stage 1 memory read/write operations require that all bit lines (BT 0 , BB 0 , BT 1 , BB 1 , . . . BTM, BBM) be precharged to logic 1 by the precharge circuitry 106 , the precharge circuitry provides PMOS transistors 102 , which in the static mode are opened by a PRCHG voltage signal 108 being at logic 0, which is applied to the gates of the PMOS transistors 102 . Also all word lines (WL 0 , WL 1 . . . WLN) are set to logic 0 before read read/write operation for any cell occurs.
At stage 2 of the memory read/write mode all are of the PMOS transistors 102 are closed (PRCHG voltage 108 is set to logic 1), so that the voltage on the bit lines is allowed to float, instead of being held at VDD. One of the word lines (e.g. WL 0 ) is driven to logic 1 All the 6T (6-transistor)core memory cells (e.g. bit cells N 00 , N 01 . . . N 0 M) coupled to this word line begin to discharge the bit lines (e.g. BT 0 , BB, BT 1 , BB 1 . . . BTM, BBM). The discharge of the bit lines at this stage causes a large active AC power dissipation.
Stage 3 of the memory bit cell read/write operation is selecting one of the switches (SW 0 , SW 1 . . . SWM) in the MUX block 103 by setting Y 0 , Y 1 . . . or YM to logic 1. As shown in FIG. 1, Y 0 is selecting column 1 . To write data to a bit cell at this stage requires using a write circuit 104 to program the selected individual bit cell, by applying a voltage differential to bit lines BT 0 and BB 0 . (The write circuitry and sense circuitry is known to one of skill in the art, and shown as block 104 in FIG. 1.) To read data from the bit cell requires amplifying the differential signal between the bit lines BTC and BBC using a sense amplifier and then routing this to an output circuit.
Regardless of which mode is used, whether read or write, a bit line for each column of SRAM memory bit cells of the complete array will be discharged during every read/write operation, and before a new read/write cycle can begin, and the array has to precharged again. This is because the same PRCHG signal is applied to the gates of all of the PMOS transistors 102 of the precharge circuit 106 , and all of the bit cells coupled to word line with logic 1 have word line pass transistors (e.g., 214 and 216 ) which are opened as a result of the word line generating a logic 1 signal. Stated another way, all the bit lines have to precharged again because all have been discharged during the read/write operation.
One problem with this prior approach is that, for each read/write cycle, enough power to precharge and discharge all of the bit line pairs in the array is consumed, while all that is really needed is to program or read information for one bit line pair (e.g. BTC and BBC) during each read or write cycle.
As disclosed in the patent application filed on Apr. 9, 2002, entitled LOW POWER STATIC RAM ARCHITECTURE (U.S. application Ser. No. 10/119,191) which has common inventors to the present application, and is assigned to the National Semiconductor Corporation, the assignee of the present application, one approach to reduce the power consumed during each read write cycle is to implement an 8 bit memory cell where a column select signal can be used in conjunction with the a word select signal to limit the power discharge during each cycle to a particular column. The U.S. application Ser. No. 10/119,191 referred to above is hereby incorporated by reference in its entirety. As further discussed in the pending patent application Ser. No. 10/215,678 filed on Aug. 10, 2002, entitled LOW AC POWER STATIC RAM ARCHITECTURE, and in the pending patent application Ser. No. 10/215,676 filed on Aug. 10, 2002, entitled BIT LINE SHARING AND WORLD LINE LOAD REDUCTION FOR LOW AC POWER SRAM ARCHITECTURE the SRAM architecture can be further modified to decrease power consumption by providing for word line and bit line sharing and by providing for sector selection where sections of the columns of memory cells can be selected for reading and writing. Both the LOW AC POWER STATIC RAM ARCHITECTURE application and the BIT LINE SHARING AND WORLD LINE LOAD REDUCTION FOR LOW AC POWER SRAM ARCHITECTURE application referred to above are hereby incorporated by reference in their entirety.
The invention herein provides further designs which further decrease the power consumption of the SRAM.
SUMMARY
The present invention is directed to a static RAM system which allows for significant reduction in power consumption over prior systems by providing for partitioning columns of bit cells. One embodiment includes a plurality of columns of bit cells, wherein the columns of bit cells are partitioned into a plurality of sectors of bit cells. This embodiment provides a number of sector select circuits, where local bit lines couple sectors of bit cells with sector select circuits. The embodiment also provides a number of global bit lines which are coupled to the sector select circuits. The sector select circuits include a switch which couples the local bit line with the global bit line so that a selected bit cell in the sector of bit cells can be read from, or written to.
Another embodiment provides a sector select circuit for use in a SRAM system having a plurality of local bit lines and a plurality of global bit lines. The sector select circuit includes a mux circuit for coupling a local bit line of the SRAM with a global bit line of the SRAM system, and a first input for receiving a column select signal form the SRAM system. The sector select circuit also includes a second input for receiving a sector select signal from the SRAM system, and a local column select signal generation circuit which generates a local column select signal in response to receiving a sector select signal and column select signal. The mux circuit is coupled to the local column select signal circuit, and in response to a local column select signal, the mux couples the local bit with the with the global bit line.
Another embodiment provides a SRAM system having an array of bit cells including columns and rows of bit cells, wherein the columns of bit cells are partitioned into sectors of bit cells, and form an array of columns and rows of sectors of bits cells. Bit cells of the sectors of bit cells are coupled to a local bit line. An array of sector selection circuits including columns and rows of sector selection circuits are coupled to the sectors of bit cells, wherein a sector selection circuit is coupled to the local bit line coupled to bit cells of the sector of bit cells. The system also provides for column select lines which are coupled to a column of sector selection circuits, and sector selection lines, which are coupled rows of sector selection circuits. The system also provides global bit lines coupled to the column of sector selection circuits. The sector selection circuits include a first circuit and a switch, wherein the first circuit detects when a sector selection signal is present on the sector selection line and when a column selection signal is present on the column selection line and when both signals are present closes the switch whereby a local bit line to be coupled with a global bit line.
The features and advantages of the present invention will be more fully appreciated upon consideration of the following detailed description of the invention and the accompanying drawings, which set forth an illustrative embodiment in which the principles of the invention are utilized.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view of an SRAM system of the prior art.
FIG. 2 is a view of an SRAM bit cell of the prior art.
FIG. 3 is a view of the SRAM memory system of the present invention.
FIGS. 4 a-d are illustrations describing SRAM bit cells used in an embodiment of the present invention.
FIGS. 5 a-c are views of embodiments of sector select circuits of the present invention.
FIG. 6 is a view of an embodiment of an SRAM memory system of the present invention.
FIGS. 7 a-c are views of embodiments of sector select circuits of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 3 shows an embodiment of the present invention. The SRAM architecture shown in FIG. 3 includes word lines (WL 0 , WL 1 . . . WLN- 1 , and WLN) and an array, including columns and rows, of bit cells 410 . As shown in FIG. 3, and as discussed in more detail below, the 6T bit cells 410 share local bit lines and share word line pass gate transistors 304 .
FIGS. 4 a - 4 d show the relationship between an 8 transistor bit memory cell 400 (as described in the above referenced U.S. application Ser. No. 10/119,191) and the 6T bit cell 410 with bit line sharing and word line sharing as shown in FIG. 3 . Specifically, FIG. 4 a shows a four transistor configuration 401 used for storing a bit of information. To perform a write or read operation to, or from, the four transistor configuration 401 the column select transistors 402 must be opened by providing a column select signal on line YSC, and the word line pass gate transistors 404 must also be opened by providing a signal on the word line WLC. Once the word line pass gate transistors 404 and column select transistors 402 are opened the four transistor configuration 401 can be read from, or written to, by either sensing or applying a voltage across the bit lines BTC and BBC. FIG. 4 b shows a configuration where adjacent 8 transistor bit memory cells 400 share bit lines. Specifically area 412 shows the word line pass gate transistors 404 as both being coupled to the bit line BB 01 which is shared by the eight transistor bit cells 414 and 416 .
FIG. 4 c shows a cell where the column select pass gate transistors 402 are coupled to a shared word line pass gate transistor 418 , which is in turn coupled to the shared bit line BB 01 . This configuration allows the overall number of word line pass gate transistors to be reduced by 50%. FIG. 4 d represents the configuration of the four transistors 401 and the column select transistors 402 , as shown in FIG. 4 c , by showing a box corresponding to the “6T bit cell” 410 . FIG. 4 d also shows the shared bit lines are BT 00 , BB 01 and BT 12 and the shared word line gate pass transistors 418 .
Turning now back to FIG. 3, the SRAM architecture 300 , shows an embodiment of the present invention with shared word line pass gate transistors 304 , and with shared local bit lines (e.g. 0 LBB 01 , KLBB 01 . . . KLBTMM) between adjacent 6T bit cells 410 , combined with bit line partitioning to further reduce power consumption and total capacitive load associated with each read/write operation. The overall power saving ratio depends on the sector size relative to the total memory size.
In the SRAM architecture 300 , the column select signals YS are sectorized, or partitioned, into local column select signals LYSA. This partitioning of the column select line YS allows for further load reduction, where the load reduction depends on the ratio of the sector size over the total memory size.
As shown in FIG. 3 the bit lines are partitioned into sections of local bit lines which correspond to the partitioning of the column select lines. Specifically, each bit line is partitioned into K sectors. Thus, instead of having bit lines BB 00 and BT 01 for column 0 , as shown in FIG. 1, there are local bit lines 0 LBT 00 and 0 LBB 01 for section 1 , 1 LBT 00 and 1 LBT 01 for section 2 and so forth, where the local bit lines are partitioned as 01 BT 00 , 0 LBB 01 , 1 LBT 00 , 1 LBB 01 , KLBBMM, KLBTMM for K sectors and M columns. During each read/write operation, only one sector is activated, and the local column select signal is present on only one LYSA line, where the LYSA line with the local column select signal is coupled to the 6T bit cells in the sector which contains the 6t bit cell which is being written to, or read from.
Each sector of the memory array of bit cells includes a sector selection circuit 302 . As discussed in more detail below, the operation and principles of different sector selection circuits, in the SRAM architecture is essentially identical, but some modifications are necessary to account for the sector selection circuits position in the overall array of 6T bit cells 410 .
As shown in FIGS. 5 a - 5 c , the sector selection circuit includes a column mux circuit 502 , and a precharge circuit 504 . The sector selection circuit also includes an AND gate 508 , which operates as a circuit for receiving a sector select signal (SS) and for receiving a column select signal YS. The sector select signal is received at input port 510 , and the column select signal is received at input port 512 . The precharge circuit 504 of the sector select circuit 302 serves to precharge local bit lines LBB and LBT to the voltage VDD. The mux 502 serves to couple the selected local bit lines LBT and LBB with the corresponding global bit lines GBT and GBB.
Because the local bit lines LBT and LBB are shared between adjacent 6T bit cells 410 , the precharge circuit 504 is shared between adjacent sectors of adjacent columns of bit cells 410 . One exception to this is noted in connection with the bit line 0 LBT 00 of column 0 at the left hand side of the SRAM architecture shown in FIG. 3 . For the sector select circuit in the far left hand column, the “sector corner” circuit, one additional precharge 504 and mux 502 circuit is provided (detail for the “sector corner” circuit is shown in FIG. 5 a ). The shared global bit lines are GBT 00 and GBB 01 for column 0 , GBB 01 and GBT 12 for column 1 and so forth. The bit lines BT and BB alternate every other column as shown in FIG. 3 . Hence the “sector A” selection circuitry, shown in FIG. 5 b , and the “sector B” selection circuitry, shown in FIG. 5 c alternate, every other column like the bit lines.
The local bit lines LBT and LBB can be accessed for reading or writing to a selected 6T bit cell 410 through the global bit lines GBT and GBB, where the selected mux switches 502 are opened to connect a specific global bit line with a selected pair of local bit lines, and the word lines (e.g. WL 0 , WL 1 . . . ) and the local column select signals, LYSA, are utilized to select a specific 6T bit cell for reading or writing. In one embodiment the transmission gates 502 are implemented using NMOS transistors. The switches 502 are controlled by the local column select signals LYSA.
Further details of the SRAM architecture can be illustrated by example. Consider for instance, the situation where 6T bit cell N01 is being read from. In this situation a column select signal voltage is generated on column select line Y 1 . This voltage on line Y 1 is received by the NOR gate 306 , of the global bit line precharge circuit 308 . The NOR gate 306 then outputs a voltage which causes the PMOS transistor 308 , which is coupled to the global bit line GBB 01 , to close, and thus GBB 01 is allowed to float. Further, the NOR gate 310 receives the voltage on Y 1 and in response outputs a voltage which closes the PMOS transistor 312 which allows the global bit line GBT 12 to float. The column select signal Y 1 is also transmitted through the buffer 318 as signal YS to the sector select circuits in column 1 . (As shown these are “sector A” circuits.) The sector select circuit in column 1 corresponds to the sector select circuit 506 shown in FIG. 5 b . The column signal YS is received by the AND gate 508 . A sector select signal is also generated sector select line SS 0 . The sector select signal SS 0 is also received by the AND gate 508 . In response to receiving the signals on sector select line and the column select line the AND gate 508 outputs a local column select signal LYSA, on the local column select line LYSA. This local column select signal closes (makes conductive) a switch of the mux 502 thereby coupling the local bit line LBT with the global bit line GBT. Additionally, the voltage output by the AND gate, LYSA, is applied to the gate of the one of the PMOS transistors of the precharge circuit 504 which causes one of the transistors to close and thus the local bit line LBT of sector 1 of column 1 is allowed to float. Note that the “sector A” circuit 520 is the only sector select circuit of the SRAM architecture 300 which receives a sector select signal and a column select signal, and hence it is the only sector select circuit which outputs a local column select signal LYSA.
The signal LYSA output by the AND gate 508 is also output to the 6T bit cells 410 of the first sector of column 1 on a local column select line LYSA. This LYSA signal is received by the column select pass gate transistors 402 (see FIG. 4 c ) of the 6T bit cells 410 , and in response the column select pass gate transistor open. A signal is also generated on the word line WL 0 and in response to this signal the word line pass gate transistors 304 (as shown in FIG. 3) coupled to the WL 0 word line open.
In addition to outputting a signal LYSA in response to the sector select signal SS 0 and the column select YS signal, the sector select circuit also outputs a line select signal LYSB. The LYSB signal is input to the line select signal input port LYSB for sector select circuit shown as “Sector Corner” 302 in FIG. 3 . This sector select circuit is shown in detail in FIG. 5 a . The line select signal LYSB causes a PMOS transistor of the precharge circuit 504 of the sector selection circuit which receives it to close which allows the local bit line LBB 01 to float. The signal LYSB also closes a switch in the mux 502 of the Sector Corner 302 circuit, which couples the local bit line LBB 01 with the global bit line GBB 01 .
Reference is now made to the SRAM mux circuit 314 , where in response to the signal on Y 1 switches S 1 and S 2 of the mux 314 are closed, and thereby couples the global bit lines GBB 01 and GBT 12 with the sense amplifier write circuit 316 . The sense amplifier write circuit operates to sense a voltage differential between the global bit lines GBB 01 and GBT 12 thereby reading data stored in the bit cell 410 shown as N 01 . To write data to the N 01 the sense amplifier write circuit applies a voltage differential between the bit cells GBB 01 and GBT 12 .
In the manner described above data can be written to read from any of the bit cells (N 00 -NNM). By way of a hi-level summary example to read information at bit cell N 00 , the YS 0 and SS 0 are turned on. The corresponding precharge circuits are turned off and the switches are closed to couple the local bit lines with the global bit lines. The differential signal at 0 LBB 01 and 0 LBT 00 will be passed to the global bit line GBB 01 and GBT 00 respectively.
The load reduction ratio depends on the number of sectors in memory. For example, in a 256×256 memory with 16 sectors, each sector will contain 16 bit cells vertically. The load for the local bit line will be the 16 bit cells in the sector. Transistors in the sector will be the total load for the global bit line. If the load of the sector mux is similar to the load for a bit cell, then the load for the global bit line equals the load of the 16 bit cells. Therefore, the load can be reduced from 256 to 32. In addition sector select circuitry which generates the sector select signal may also create an additional load. In one embodiment the load of the sector select circuit is equivalent to 16 bit cells, so the total load reduction is from 256 to 48.
It should be noted that the invention has been described above in connection with a synchronous SRAM where the precharge circuit is turned on and off in connection.,with reading and writing information to the bit cell. The invention herein can also be applied to an asynchronous SRAM where the precharge circuits are not clocked on and off, and are instead always held in an on state. FIG. 6 shows an asynchronous SRAM system 600 . In this asynchronous system 600 , the gates of the PMOS transistors 602 of the precharge circuits 608 sector select circuits 604 , 606 and 608 are connected to ground. Further, the gates of the PMOS transistors 610 of the global bit line precharge circuit 612 are connected to ground. This means the local bit lines ( 0 LBT 00 -KLBTMM) and the global bit lines (GBT 00 -GBTMM) are in a state of constant precharge. In prior asynchronous SRAM (similar to the system shown in FIG. 1, but with the PMOS transistors 102 held in an open condition) large power consumption occurred because the there is a short circuit path between Vdd and ground through the PMOS precharge transistors 602 and through the bit cells for both the selected columns and the non-selected columns. As discussed in more detail in patent application Ser. No. 10/119,191 this large power consumption has limited the actual use of asynchronous SRAM systems. By employing the asynchronous system shown in FIG. 6, there is a significant reduction in power consumption. This reduction in AC power dissipation for asynchronous memories is realized by partitioning columns of bit cells into sectors as described above. Reduced power consumption within the memory is achieved due to the proportional reduction of the short circuit current between Vdd and Gnd as only the one selected sector of bit cells consumes power, while the rest of the unselected sectors will be inactive and remain in the precharged state. This technique also reduces the peak AC current by the same argument.
For example, to read information at bit cell N 00 , the YS 0 and SS 0 are turned on, and the switches of the mux of corresponding sector selection circuit are closed to couple the local bit lines with the global bit lines. The corresponding word line WL 0 is also turned on, and the differential signal at 0 LBB 01 and 0 LBT 00 will be passed to the global bit line GBB 01 and GBT 00 respectively. Thus, the present a SRAM asynchronous system as shown in FIG. 6 reduces the amount of power consumed during read and write operations, as only the local bit lines discharged are 0 LBB 01 and 0 LBT 00 . Additionally aspects of asynchronous SRAM systems are discussed in patent application Ser. No. 10/119,191.
Although specific embodiments and methods of the present invention are shown and described herein, this invention is not to be limited by these methods and embodiments. Rather, the scope of the invention is to be defined by the following claims and their equivalents.
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A SRAM system which provides for reduced power consumption. The SRAM system utilizes an array of bit cells. Columns of bit cells in the array are partitioned into sections. Each section of bit cells shares a local bit line. A sector select circuit provides for precharging the local bit lines. The sector select circuit also includes a mux for connecting a local bit line to a global bit line. The sector select circuit includes a device for detecting when a sector select signal and a column select signal are present. When both of these signals are present the sector select circuit couples the local bit line with the global bit line, and disengages the precharging of the local bit line.
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RELATED APPLICATIONS
This application is a national stage filing under 35 U.S.C. §371 of International Application No. PCT/KR2012/003181, filed Apr. 25, 2012, which claims the benefit of Korean Patent Application No. 10-2011-0039206 filed on Apr. 26, 2011, each of which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
An embodiment of the present invention relates to a feed apparatus, a current collector, and a power transfer apparatus of the magnetic induction type, considering lateral deviation. More particularly, the present invention relates to a feed apparatus, a current collector, and a power transfer apparatus of magnetic induction type, considering lateral deviation so that even if a moving body such as an electric vehicle is deviated from a feed line laid in the road by a certain distance to the left or the right, it can be effectively supplied with power necessary for operation.
DESCRIPTION OF RELATED ART
The matters described in this section are intended to simply provide background information for an embodiment of the present invention and do not constitute conventional technology.
Drawing 1 a shows an electric vehicle traveling on the road while being supplied with power from a feed line laid in the road and Drawing 1 b simplifies only the feed core, the feed line and the current collector necessary for supplying power excluding the electric vehicle and the road from Drawing 1 a.
As shown in Drawing 1 a and Drawing 1 b , when power of high frequency is supplied to the feed line ( 114 ) on the feed core ( 112 ), the electric vehicle ( 100 ) which is traveling on the road is supplied with power necessary for traveling according to the principle of electromagnetic induction acting between the feed apparatus ( 110 ) including the feed core ( 112 ) and the feed line ( 114 ) and the current collector ( 130 ).
Drawing 1 c shows a cross section cut along the line of A-A′ in Drawing 1 b and viewed in an X direction.
For Drawing 1 c , a detailed illustration of drawing numbers for describing the look of a magnetic field is omitted and for drawing numbers indicated in the description of Drawing 1 c , refer to Drawing 1 b.
As shown in Drawing 1 c , magnetic flux is generated from the feed line ( 114 ) in an arrow direction of semicircle and causes induced electromotive force to be generated in the current collection line ( 134 ).
Drawing 2 illustrates the look of the magnetic field generated according to the positioning relationship between the feed core ( 112 ), the feed line ( 114 ) and the current collector ( 130 ) from Drawing 1 c.
Drawing 2 (A) illustrates the arrangement of the feed core ( 112 ), the feed line ( 114 ), and the current collector ( 130 ) and the magnetic field generated when the electric vehicle ( 100 ) travels on the road so that the current collector ( 130 ) of the electric vehicle ( 100 ) would be positioned on the top of the center of the feed core ( 112 ) and the feed line ( 114 ) laid in the road to receive maximum power (that is, when the current collector ( 130 ) is positioned home) and Drawing 2 (B) illustrates the arrangement of the feed core ( 112 ), the feed line ( 114 ), and the current collector ( 130 ) and the magnetic field generated when the current collector ( 130 ) is positioned deviated from the center of the feed core ( 112 ) and the feed line ( 114 ) to the left or right by a certain distance (that is, when the current collector ( 130 ) is misaligned).
As shown in Drawing 2 (A), if the current collector ( 110 ) is positioned on the top of the center of the feed apparatus ( 110 ) while the electric vehicle ( 100 ) is traveling, the output of induced electromotive force can be generated at the current collection line ( 134 ) coiled at the current collection core ( 132 ) in a normal size. The arrow illustrated in a semicircle in Drawing 2 (A) gives a conceptual indication of the direction of a magnetic field contributing to the induced electromotive force of the current collector ( 130 ).
Meanwhile, Drawing 2 (B) has a problem that when the electric vehicle ( 100 ) travels so that the current collector ( 110 ) would be misaligned more than a certain distance, not only such magnetic flux as not contributing to induced electromotive force is increased but also such magnetic flux as being in the opposite direction to the direction contributing to induced electromotive force becomes high and power transfer from the feed apparatus ( 110 ) to the current collector ( 130 ) is not carried out smoothly.
DESCRIPTION OF THE INVENTION
Technical Task
In order to solve this problem, the first purpose of an embodiment of the present invention is to effectively supply power for operation to a moving body such as an electric vehicle while it is traveling on the road even if it is deviated from a feed line laid in the road by a certain distance to the left or the right.
The second purpose of an embodiment of the present invention is to greatly reduce the usage of a feed core and not to greatly lower the efficiency of power transfer by having a cutting part in the feed core.
Means to Solve the Task
In order to accomplish the abovementioned purposes, the first embodiment of the present invention provides a feed apparatus which include a feed main unit having a predetermined width and length, a U-shaped feed core forming a feed projection unit projected in the same direction and being perpendicular to both said width direction and said length direction at the left and the right end of said width direction, with respect to a cross section of said feed main unit in said width direction; and a pair of feed lines coiled respectively at the left and the right end of said feed main unit.
Said feed lines may be coiled adjacent to said feed projection unit.
Said feed lines may be coiled directly at said feed projection unit.
Said feed core may have multiple cutting parts in parallel to said width direction.
Said feed core may have regular intervals between each of said multiple cutting parts.
In order to accomplish the abovementioned purposes, the second embodiment of the present invention provides a feed apparatus which includes a feed main unit having a predetermined width and length, an E-shaped feed core forming a feed projection unit projected in the same direction and being perpendicular to both said width direction and said length direction at the left and the right end of said width direction, with respect to a cross section of said feed main unit perpendicular to said length direction and a central projection unit in the same direction as said feed projection unit in the center of said width direction; and a pair of feed lines coiled respectively at the left and the right end of said feed main unit.
Said feed lines may be coiled adjacent to or directly at said feed projection unit.
Said feed core has multiple cutting parts in parallel to said width direction and can be divided into multiple core pieces.
For said feed core, the thickness of said cutting part in said length direction may be larger than that of said core piece.
In order to accomplish the abovementioned purposes, the third embodiment of the present invention provides a feed apparatus which includes a feed main unit having a predetermined width and length, a U-shaped feed core forming a feed projection unit projected in the same direction and being perpendicular to both width direction and said length direction at the left and the right end of said width direction, with respect to a cross section of said feed main unit perpendicular to said length direction; and feed lines coiled in the length direction of said feed core at the center in the width direction of said feed main unit.
Said feed core may have multiple cutting parts in parallel to said width direction and be divided into multiple core pieces.
For said feed core, the thickness of said cutting part in said length direction may be similar to that of said core piece.
For said feed core, the intervals between cutting parts may be regular.
In order to accomplish the abovementioned purposes, the fourth embodiment of the present invention provides a current collector which includes a current collection main unit having a predetermined width and length, a ∩-shaped current collection core forming a current collection projection unit projected in the same direction and being perpendicular to both said width direction and said length direction at the left and the right end of said width direction, with respect to a cross section of said current collection main unit perpendicular to said length direction; and a current collector including current collection lines coiled at said current collection core.
Said current collection lines may be coiled respectively at the current collection projection unit projected at said left end and said right end.
Said current collection core may have extending parts extended in said width direction respectively at the ends of the current collection projection unit projected at said left end and said right end.
Said current collector may be installed in the lower part of a vehicle.
In order to accomplish the abovementioned purposes, the fifth embodiment of the present invention provides a power transfer apparatus which includes a feed apparatus as provided in one claim among claim 1 through claim 13 and a current collector as provided in one claim among claim 14 through claim 17 , provided that said feed projection unit and said current collection projection unit are projected in the opposite direction to each other.
Effect of the Invention
According to an embodiment of the present invention, it has an effect of effectively supplying power necessary for operation to a moving body such as an electric vehicle charging while traveling on the road, even if it is deviated from a feed line laid in the road to the left or the right by a certain distance.
It also has an effect of greatly reducing the usage of a feed core while not greatly lowering the efficiency of power transfer by having cutting parts in the feed core.
BRIEF DESCRIPTION OF THE SEVERAL VIEW OF THE DRAWING
Drawing 1 a shows an electric vehicle traveling on the road while being supplied with power from a feed line laid in the road
Drawing 1 b simplifies only the feed core, the feed line and the current collector necessary for supplying power excluding the electric vehicle and the road from Drawing 1 a.
Drawing 1 c shows a cross section cut along the line of A-A′ in Drawing 1 b and viewed in an X direction.
Drawing 2 a - 2 b illustrates the magnetic field generated according to the positioning relationship between the feed core ( 112 ), the feed line ( 114 ) and the current collector ( 130 ) from Drawing 1 c.
Drawing 3 a shows a power transfer apparatus according to the first embodiment of the present invention.
Drawing 3 b shows a U-shaped assembled feed core without cutting part and an E-shaped assembled feed core without cutting part.
Drawing 4 shows a cross section cut along the line of A-A′ in Drawing 3 a and viewed in an X direction.
Drawing 5 a - 5 b illustrates the magnetic field generated in the power transfer apparatus shown in Drawing 3 a and Drawing 4 .
Drawing 6 illustrates a power transfer apparatus according to the second embodiment of the present invention.
Drawing 7 illustrates a cross section cut along the line of A-A′ in Drawing 6 and viewed in an X direction.
Drawing 8 a - 8 b illustrate the magnetic field generated in the power transfer apparatus of Drawing 6 and Drawing 7 .
THE BEST FORM FOR AN EMBODIMENT OF THE INVENTION
From now on, a desired embodiment of the present invention will be explained in detail on reference to the attached drawings. Note that the same components in the drawings are indicated by the same reference numbers and symbols as much as possible, although they are shown in different drawings. If a detailed explanation of related function or configuration is considered to unnecessarily obscure the gist of the present invention, such a detailed explanation will be omitted.
In addition, such terms as ‘the first’, ‘the second’, ‘A’, ‘B’, ‘(a)’, and ‘(b)’ may be used in explaining the components of the present invention. These terms are simply intended to distinguish the corresponding component from others but do not limit the nature, sequence or order of the corresponding component. When it is described that one component is “connected”, “combined”, or “accessed” to another component, it should be understood that the former can be directly connected or accessed to the latter but the third component may be “connected”, “combined”, or “accessed” between each of the components.
Drawing 3 a illustrates a power transfer apparatus according to the first embodiment of the present invention and Drawing 4 illustrate a cross section cut along the line of A-A′ in Drawing 3 a and viewed in an X direction. Meanwhile, Drawing 3 b illustrates a U-shaped assembled feed core without cutting part and an E-shaped assembled feed core without cutting part.
From now on, a power transfer apparatus according to the first embodiment of the present invention is explained on reference to Drawing 3 a , Drawing 3 b and Drawing 4 .
As illustrated in Drawing 3 a and Drawing 4 , a power transfer apparatus according to the first embodiment of the present invention includes a feed apparatus ( 300 ) and a current collector ( 400 ).
The feed apparatus ( 300 ) according to the first embodiment of the present invention may consist of a feed core ( 310 ), a feed line ( 320 ), and an input power source ( 330 ) and the current collector ( 400 ) according to the first embodiment of the present invention may consist of a current collection core ( 410 ), a current collection line ( 420 ), a current collection circuit ( 430 ), and a battery ( 440 ).
The feed core ( 310 ) includes a feed main unit ( 312 ) having a predetermined width and length and a feed projection unit ( 314 , 315 ) in which the cross section of the feed main unit ( 312 ) cut perpendicular to the length direction of the feed core ( 310 ) is projected to the left end and the right end in the width direction of the feed core ( 310 ). The feed projection unit ( 314 , 315 ) is perpendicular to both the width direction and the length direction of the feed core ( 310 ), forming the feed core ( 310 ) in a U-shape. The feed core ( 310 ) has the feed projection unit ( 314 , 315 ) so that a magnetic field can be easily transferred to the current collector ( 400 ).
Depending upon the applicable embodiment, the feed core ( 310 ) may include a central projection unit ( 316 ) projected in the same direction as the feed projection unit ( 314 , 315 ) in an intermediate portion in the width direction of the feed main unit ( 312 ). This makes the feed core ( 310 ) shaped in such a form as an E-shape lying on its side and transfers more magnetic field to the current collector ( 400 ) than a U-shaped feed core.
A pair of feed lines ( 320 ) is coiled respectively at the left end and the right end of the feed main unit ( 312 ).
The left feed line ( 320 a ) is coiled at the left end of the feed main unit ( 312 ) in the length direction of the feed core ( 310 ) adjacent to the left feed projection unit ( 314 ) and the right feed line ( 320 b ) is coiled at the right end of the feed main unit ( 312 ) in the length direction of the feed core ( 310 ) adjacent to the right feed projection unit ( 315 ). In some cases, a pair of feed lines ( 320 a , 320 b ) may be coiled respectively at the left and the right feed projection unit ( 314 , 315 ).
The feed core ( 310 ) may be configured in an assembled type, as shown in Drawing 3 b , or have a cutting part ( 340 ), as shown in Drawing 3 a.
The feed core ( 310 ) may have multiple cutting parts ( 340 ) parallel to the width direction of the feed core ( 310 ). Thus, the feed core ( 310 ) may be divided into multiple core pieces in an E-shape (or U-shape).
In this case, as shown in Drawing 3 a , the intervals between adjacent cutting parts ( 340 ) may be regular and the thickness of the cutting part ( 340 ) may be larger than, similar with, or smaller than that of the core piece in an E-shape (or U-shape).
As shown in Drawing 3 a , by forming the cutting part ( 340 ) in the feed core ( 310 ), when the feed core with the capacity half of that of an assembled feed core as shown in Drawing 3 b , the output is reduced by about 10% of that being induced to the current collector ( 400 ), compared to the case of Drawing 3 a . However, the capacity of the ferrite core used in the feed core ( 310 ) can be reduced half and the reduction of the output induced to the current collector ( 400 ) is not large, indicating high economic feasibility.
Meanwhile, the current collection core ( 410 ) includes a current collection main unit ( 412 ) having a predetermined width and length and a current collection projection unit ( 414 , 415 ) projected in the same direction and being perpendicular to both the width direction and the length direction of the current collection core at the left and the right end of the width direction of the current collection core ( 410 ), so that a cross section of the current collection main unit ( 412 ) in the width direction would be in a ∩-shape. In this case, the current collection projection unit ( 414 , 415 ) is projected in the opposite direction to the feed projection unit ( 314 , 315 ).
In addition, the end of the current collection projection unit ( 414 , 415 ) may have an extension ( 416 , 417 ) extended in the width direction of the current collection core ( 410 ). By having the extension ( 416 , 417 ) at the end of the current collection projection unit ( 414 , 415 ), the current collection projection unit ( 414 , 415 ) have an effect of increasing an effective cross-sectional area on a magnetic path and reducing magnetic resistance.
Meanwhile, the extension may be formed turning out from the current collection projection unit ( 414 , 415 ) with the center of the feed main unit ( 412 ), as indicated by reference numbers of 416 and 417 , or have an additional projection towards the center of the current collection main unit ( 412 ) in the width direction of the current collection core ( 410 ) (that is, in the opposite direction to those indicated by reference numbers of 416 and 417 based on the current collection projection unit ( 414 , 415 )).
A pair of the current collection lines ( 420 ) may be coiled respectively at the left current collection projection unit ( 414 ) and the right current collection projection unit ( 415 ) of the current collection core ( 410 ), and in some cases, it may be coiled at the feed main unit ( 412 ).
When an input power source ( 330 ) is applied to the feed lines ( 320 ) of Drawing 3 a , a magnetic field is generated from the feed lines ( 320 ), bringing about an induced electromotive force is generated from the current collection lines ( 420 ). The current collection lines ( 420 a , 420 b ) coiled respectively at the left and the right current collection projection units ( 414 , 415 ) of the current collection core ( 410 ) are connected respectively to the current collection circuit ( 430 ) in parallel to generate the voltage of desired level and charge the battery ( 440 ). Or, two current collection lines ( 420 a , 420 b ) are connected to the current collection circuit ( 430 ) in series to charge the battery ( 440 ). Note that the current collection circuit ( 430 ) may include a rectifier and a regulator.
Drawing 5 illustrates the magnetic field generated in the power transfer apparatus shown in Drawing 3 a and Drawing 4 . Indication of reference number is omitted to illustrate the magnetic field in Drawing 5 and the reference numbers of Drawing 4 are referred in the description of Drawing 5 .
Drawing 5 (A) illustrates the magnetic field generated when the current collector ( 400 ) is positioned home so that the maximum power would be transferred to the current collector ( 400 ) and Drawing 5 (B) illustrates the magnetic field generated when the current collector ( 400 ) is misaligned.
When the current collector ( 400 ) is positioned home as shown in Drawing 5 (A), the output of induced electromotive force can be generated at the current collection lines ( 420 ) coiled at the current collection core ( 410 ) in a normal magnitude. The arrow illustrated in a semicircle in Drawing 5 (A) gives a conceptual indication of the direction of a magnetic field contributing to the induced electromotive force of the current collector ( 400 ).
When the current collector ( 400 ) is misaligned as shown in Drawing 5 (B), the magnetic flux not contributing to induced electromotive force becomes high but the magnetic flux in the opposite direction to that of contributing to induced electromotive force is not high.
Meanwhile, in a power transfer apparatus looking like that of Drawing 2 , if the sum of the voltage generated from the current collection line is 1651V as a result of simulation of the output collected in the current collection line ( 134 ) in such conditions that the feed core ( 110 ) is 72 cm in width and the current collector ( 130 ) is 110 cm in width and positioned home as shown in Drawing 2 (A), the sum of the voltage generated from the current collection line ( 134 ) is 148V with the current collector ( 130 ) misaligned by 30 cm, as shown in Drawing 2 (B), indicating that the voltage generated is reduced much. Because when the voltage induced to the current collector ( 130 ) decreases, the induced current also decreases, it can be known that the output induced to the current collector ( 130 ) sharply decreases.
However, in a power transfer apparatus looking like that of Drawing 5 , if the sum of the voltage generated from the current collection line ( 420 ) is 1726V as a result of simulation of the voltage collected in the current collector ( 400 ) in such conditions that the feed core ( 310 ) is 72 cm wide and the current collector ( 400 ) is 110 cm wide and positioned home as shown in Drawing 5 (A), the sum of the voltage generated from the current collection line ( 420 ) is 1559V with the current collector ( 400 ) misaligned by 30 cm with the same condition as shown in Drawing 2 (B), indicating the voltage generated is not reduced much and it is more effective than that of Drawing 2 (B).
Drawing 6 illustrates a power transfer apparatus according to the second embodiment of the present invention, and Drawing 7 illustrates a cross section cut along the line of A-A′ in Drawing 6 and viewed in an X direction.
As shown in Drawing 6 and Drawing 7 , the second embodiment of the present invention includes a feed apparatus ( 600 ) and a current collector ( 700 ).
The appearance of a feed core ( 610 ) shown in Drawing 6 and Drawing 7 is similar to that of the feed core ( 300 ) shown in Drawing 3 a and Drawing 4 , so a detailed explanation for the feed core ( 610 ) is omitted.
A feed line ( 620 ) is coiled at the central part in the width direction of a feed main unit ( 612 ) in the length direction of the feed core ( 610 ).
When an input power source ( 630 ) is applied to the feed line ( 620 ) of Drawing 6 , a magnetic field is generated from a feed line ( 720 ). Current collection lines ( 720 a , 720 b ) coiled respectively at the left and the right current collection projection units ( 714 , 715 ) of a current collection core ( 710 ) are connected respectively to a current collection circuit ( 730 ) in parallel to generate the voltage of desired level and charge a battery ( 740 ). Because the form and function of the feed apparatus ( 600 ) are similar to those of the current collector ( 400 ), more detailed explanation is omitted.
Drawing 8 illustrates the magnetic field generated in the power transfer apparatus shown in Drawing 6 and Drawing 7 . Indication of reference number is omitted to illustrate the magnetic field in Drawing 8 and the reference number of Drawing 7 are referred in the description of Drawing 8 .
Drawing 8 (A) illustrates the magnetic field generated when the central part in the width direction of the current collector ( 700 ) is positioned on the top of the central part in the width direction of the feed apparatus ( 600 ) (that is, when the current collector ( 700 ) is positioned home) so that the maximum power would be transferred to the current collector ( 700 ) and Drawing 8 (B) illustrates the magnetic field generated when the current collector ( 700 ) is misaligned.
When the current collector ( 700 ) is positioned home as shown in Drawing 8 (A), the output of induced electromotive force can be generated at the current collection lines ( 720 ) coiled at the current collection core ( 710 ) in a normal magnitude. The arrow illustrated in a semicircle in Drawing 8 (A) gives a conceptual indication of the direction of a magnetic field contributing to the induced electromotive force of the current collector ( 700 ).
Meanwhile, when the current collector ( 700 ) is misaligned by a certain distance as shown in Drawing 8 (B), the magnetic flux not contributing to induced electromotive force becomes high but the magnetic flux in the opposite direction to that of contributing to induced electromotive force is smaller than when the current collector ( 700 ) is positioned home and the reduction in voltage of the current collector ( 130 ) is less than when the current collector ( 130 ) is misaligned by a certain distance in Drawing 2 .
For example, in a power transfer apparatus looking like that of Drawing 8 , if the voltage generated from the current collector ( 700 ) is 2782 V in such conditions that the feed core ( 610 ) is 72 cm wide and the current collector ( 700 ) is 110 cm wide with the same conditions as Drawing 5 and the current collector ( 700 ) is positioned home as shown in Drawing 8 (A), the voltage generated from the current collector ( 700 ) which is misaligned by 30 cm as shown in Drawing 8 (B) is 1870V, indicating the voltage generated is not reduced much and it is more effective than that of Drawing 2 (B).
Table 1 shows the comparison of the output of induced electromotive force between the current collector ( 700 ) positioned home and misaligned by 30 cm in Drawings 2 , 5 , and 8 .
TABLE 1
Output voltage
Output voltage
Maintenance ratio of
at home
at misalignment
misalignment to home
position
by 30 cm
position
Drawing 2
1651 V
148 V
9.0%
Drawing 5
2063 V
1559 V
75.9%
Drawing 8
2782 V
1870 V
67.2%
As indicated in Table 1, in Drawing 2 , the maintenance ratio of a 30 cm-misalignment to home position is only 9.0% and indicates that it is hard to effectively generate induced electromotive force to the current collector. In Drawings 5 and 8 , however, the ratio is 75.9% and 67.2%, respectively, indicating that even though the current collector is misaligned by a certain distance, a considerable amount of induced electromotive force can be generated in the current collector.
The present invention is not necessarily limited to the abovementioned embodiments, although all of the components of the embodiments of the present invention are combined or operated in an assembly. That is, one or more of such components may be combined selectively to operate within the range of the purpose of the present invention.
In addition, because the terms of “include”, “consist of”, or “have” stated above mean that unless otherwise specified, the applicable components can be included, they should be construed as including other components, not as excluding them. All the terminology including technical or scientific terms, unless otherwise defined, have the same meanings as being generally understood by those who have common knowledge in the related art of the present invention. Terms in general use, like those defined in a dictionary, should be construed as coinciding with the meaning of the context of related art and unless obviously defined in the present invention, should not construed as having excessively formal meanings.
The abovementioned discussion is merely an adumbrative explanation of the technical philosophy of the present invention and anyone who has common knowledge of the related art of the present invention may alter or change in various ways within the range not deviated from the intrinsic nature of the present invention. Therefore, the embodiments of the present invention are not to limit but to explain the technical philosophy of the present invention, and the range of the technical philosophy of the present invention is not limited by the embodiments. The protection range of the present invention should be construed under the scope of claims below, and the entire technical philosophy within the same range should be construed as being included in the scope of rights of the present invention.
AVAILABILITY IN THE RELATED INDUSTRY
As abovementioned, the present invention is a useful invention in that even if a moving body such as an electric vehicle which is charged while traveling on the road is deviated from a feed line laid in the road by a certain distance to the left or the right, it can be effectively supplied with power necessary for operation.
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An embodiment of the present invention relates to a feed apparatus, a current collector, and a power transfer apparatus of the magnetic induction type, considering lateral deviation. An embodiment of the present invention relates to a power transfer apparatus comprising a feed apparatus and a current collector wherein the feed apparatus includes: a feed main unit having a predetermined width and length; a feed core forming a feed projection unit projected in the same direction and being perpendicular to both the width direction and the length direction at the left end and the right end of the width direction, with respect to a cutting side of the feed main unit in the width direction; and a pair of feed lines coiled respectively at the left end and the right end of the feed main unit in a length direction of the feed core adjacent to the feed projection unit, and the current collector includes: a current collection main unit having a predetermined width and length; a current collection core having a current collection projection unit projected in the same direction and being perpendicular to both the width direction and the length direction at a left end and a right end of a width direction, with respect to a cutting side of the current collection main unit in the width direction, and equipped with an extension unit extended toward each width direction in the current collection projection unit; and a current collection line coiled respectively at the left side and the right side of the current collection projection unit of the current collection core.
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RELATED APPLICATIONS
[0001] This application is continuation of U.S. application Ser. No. 11/865,616, filed 1 Oct. 2007; which is a continuation of U.S. application Ser. No. 11/298,912, filed 9 Dec. 2005, now U.S. Pat. No. 7,283,389. These applications are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to electrically programmable and erasable non-volatile memory, and more particularly to charge storage memory with a bias arrangement that reads the contents of the charge storage structure of the memory cell with great sensitivity.
[0004] 2. Description of Related Art
[0005] Electrically programmable and erasable non-volatile memory technologies based on charge storage structures known as EEPROM and flash memory are used in a variety of modern applications. A number of memory cell structures are used for EEPROM and flash memory. As the dimensions of integrated circuits shrink, greater interest is arising for memory cell structures based on charge trapping dielectric layers, because of the scalability and simplicity of the manufacturing processes. Various memory cell structures based on charge trapping dielectric layers include structures known by the industry names PHINES, NROM, and SONOS, for example. These memory cell structures store data by trapping charge in a charge trapping dielectric layer, such as silicon nitride. As more net negative charge is trapped, the threshold voltage of the memory cell increases. The threshold voltage of the memory cell is reduced by removing negative charge from, or adding positive charge to, the charge trapping layer.
[0006] Conventional memory cell structures rely on a transistor structure with source, drain, and gate. However, common transistor structures have drain and source diffusions that are laterally separated from each other by a self-aligned gate. This lateral separation is a factor that resists further miniaturization of nonvolatile memory.
[0007] Thus, a need exists for a nonvolatile memory cell that is open to further miniaturization and whose contents can be read with great sensitivity.
SUMMARY OF THE INVENTION
[0008] A gated diode nonvolatile memory device, an array of gated diode nonvolatile memory devices, methods of operating a gated diode nonvolatile memory device and an array of gated diode nonvolatile memory devices, and methods of manufacturing a gated diode nonvolatile memory device and an array of gated diode nonvolatile memory devices, are disclosed.
[0009] The gated diode nonvolatile memory device has a charge storage structure, dielectric structures(s), and a diode structure. Examples of a charge storage structure materials include floating gate material, charge trapping material, and nanocrystal material. Depending on the threshold voltage scheme of the charge storage structure, the charge storage state of the charge storage structure stores one bit or multiple bits.
[0010] The dielectric structures(s) are at least partly between the charge storage structure and the diode structure, and at least partly between the charge storage structure and a source of gate voltage, such as a word line. The diode structure has a first node and a second node separated by a junction. Example junctions of the diode are a homojunction, a heterojunction, and a graded heterojunction. Example diode structure with the first node and second node, include a pn diode and a Schottky diode.
[0011] The first node and the second node are at least partly adjacent to the one or more storage dielectric structures. The diode structure has a cross-section in which the second node has opposite sides isolated from neighboring devices by isolation dielectric. Despite this isolation dielectric on opposite side of the second node, the second node may be connected to neighboring devices. For example, if the neighboring devices are also gated diode nonvolatile memory devices, a lower portion of the second node beyond the isolation dielectric may be connected to neighboring devices via a second node of each of the neighboring devices. In this way, the same bit line combines the current flowing through diode structures otherwise separated by isolation dielectric. In another embodiment, the second node is connected to a bit line distinct from bit lines connected to second nodes of the neighboring devices. In this case, the second node does not have a lower portion beyond the isolation dielectric that is connected to neighboring devices.
[0012] Additional logic circuitry applies a bias arrangement to determine a charge storage state of the charge storage structure and to measure a read current flowing through the diode structure in reverse bias to determine the charge storage state of the charge storage structure. The read current includes a band-to-band read current component.
[0013] The bias arrangement applied by the logic circuitry causes multiple voltage differences in the gated diode nonvolatile memory device, such as a voltage difference between a source of gate voltage (typically a word line) and the second node of the diode structure, and another voltage difference between the first node and the second node of the diode structure. These voltage differences resulting from the bias arrangement cause sufficient band-to-band tunneling current for measuring the read current to determine the charge storage state of the charge storage structure. At the same time, these voltage differences fail to change the charge storage state of the charge storage structure. In one example, the voltage difference between the gate and the second node is at least about 10 V, and the voltage difference between the first node and the second node is at least about 2V.
[0014] In addition to the bias arrangement for reading the contents of the gated diode nonvolatile memory device, other bias arrangements are applied to change the contents of the gated diode nonvolatile memory device. For example, other bias arrangements adjust the charge storage state of the charge storage structure by increasing a net positive charge in the charge storage structure, and by increasing a net negative charge in the charge storage structure. Example charge movement mechanisms to increase a net positive charge in the charge storage structure are band-to-band hot hole tunneling and Fowler-Nordheim tunneling. The electron movement can be between the charge storage structure and the diode structure, between the charge storage structure and the gate, or both.
[0015] Example charge movement mechanisms to increase a net negative charge in the charge storage structure are band-to-band hot electron tunneling and Fowler-Nordheim tunneling. The electron movement can be between the charge storage structure and the diode structure, between the charge storage structure and the source of gate voltage, or both.
[0016] An embodiment of a nonvolatile memory device integrated circuit includes an array of the gated diode nonvolatile memory devices. In some embodiments, to increase the storage density, multiple arrays that are vertically displaced from each other are combined. Depending on the addressing scheme used, the sources of gate voltage (typically word lines), the first nodes of the diode structures, and the second nodes of the diode structures, are interconnected between different vertically displaced arrays, or isolated between different vertically displaced arrays. Generally, a greater degree of interconnection simplifies the addressing and the fabrication, at the cost of increased power consumption from charging and discharging extra circuitry.
[0017] In one interconnection scheme, the word lines of different arrays are interconnected, but the first nodes and second nodes of different arrays are isolated from each other. In another interconnection scheme, the word lines of different arrays are isolated from each other, but the first nodes and second nodes of different arrays are interconnected. In yet another interconnection scheme, the word lines of different arrays, and the first nodes and second nodes of different arrays are isolated from each other.
[0018] Some embodiments of an array of gated diode nonvolatile memory cells include diode columns, gate rows, and nonvolatile storage structures. Each diode column has a first node column and a second node column separated by a junction. Opposite sides of the second node column are isolated from neighboring diode columns by isolation dielectric. The gate rows overlap the diode columns at intersections. These intersections are the locations of the nonvolatile storage structures. Typically, these nonvolatile storage structures are part of nonvolatile storage structure columns.
[0019] Each nonvolatile storage structure has a charge storage structure and one or more storage dielectric structures. The dielectric structures are at least partly between the charge storage structure and the particular diode column at the intersection, at least partly between the charge storage structure and the particular gate row at the intersection, and at least partly adjacent to the first node column and the second node column of the particular diode column at the intersection.
[0020] Despite this isolation of the second node column on opposite sides of the second node column, the second node column may be connected to neighboring diode columns. For example, a lower portion of the second node column beyond isolation dielectric may be connected to neighboring diode columns via the second node column of the neighboring diode columns. In this way, the same bit line combines the current flowing through diode structures otherwise isolated from each other. In another embodiment, the second node column is connected to a bit line distinct from bit lines connected to second nodes columns of the neighboring diode columns. In this case, the second node column does not have a lower portion beyond isolation dielectric that is connected to neighboring diode columns.
[0021] In some embodiments, the substrate region is a well in a semiconductor substrate. In other embodiments, the substrate region is simply the semiconductor substrate.
[0022] In other embodiments, the nonvolatile memory cell has a floating gate design or a nanocrystal design. In another embodiment, the nonvolatile memory cell has a charge trapping material design.
[0023] Applicant incorporates herein by reference U.S. patent application Ser. No. 11/024,339 filed on 28 Dec. 2004, now U.S. Pat. No. 7,130,215, U.S. patent application Ser. No. 11/023,747 now U.S. Pat. No. 7,072,219 filed on 28 Dec. 2004, U.S. patent application Ser. No. 11/024,075 filed 28 Dec. 2004 now U.S. Pat. No. 7,072,220, U.S. patent application Ser. No. 10/973,176 filed 26 Oct. 2004, U.S. Provisional Patent Application Ser. No. 60/608,528 filed 9 Sep. 2004, U.S. Provisional Patent Application Ser. No. 60/608,455 filed 9 Sep. 2004, U.S. patent application Ser. No. 10/973,593, filed 26 Oct. 2004, U.S. patent application Ser. No. 11/191,365 filed 28 Jul. 2005, U.S. patent application Ser. No. 11/191,366 filed 28 Jul. 2005, U.S. patent application Ser. No. 11/191,329 filed 28 Jul. 2005, U.S. patent application Ser. No. 11/191,367 filed 28 Jul. 2005, U.S. patent application Ser. No. 11/298,288 filed on 9 Dec. 2005 (Attorney Docket No. MXIC 1640-1) and U.S. patent application Ser. No. 11/299,310 filed on 9 Dec. 2005 (Attorney Docket No. MXIC 1642-1).
[0024] Other aspects and advantages of the technology presented herein can be understood with reference to the figures, the detailed description and the claims, which follow.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] FIG. 1 is a simplified diagram of a gated diode nonvolatile memory cell.
[0026] FIGS. 2A , 2 B, and 2 C are simplified diagrams of a gated diode nonvolatile memory cell, showing various charge storage structures having different materials.
[0027] FIGS. 3A , 3 B, 3 C, and 3 D are simplified diagrams of a gated diode nonvolatile memory cell, showing various examples of a diode structure, such as the pn diode and the Schottky diode.
[0028] FIGS. 4A and 4B are simplified diagrams of a gated diode nonvolatile memory cell, showing examples of a pn diode with a homojunction.
[0029] FIG. 5 is a simplified diagram of a gated diode nonvolatile memory cell, showing an example of a pn diode with a heterojunction.
[0030] FIGS. 6A and 6B are simplified diagrams of a gated diode nonvolatile memory cell operation performing electron tunnel injection.
[0031] FIGS. 7A and 7B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band hot electron injection.
[0032] FIGS. 8A and 8B are simplified diagrams of a gated diode nonvolatile memory cell operation performing hole tunnel injection.
[0033] FIGS. 9A and 9B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band hot hole injection.
[0034] FIGS. 10A and 10B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band sensing with different amounts of net positive or net negative charge characterizing the charge storage structure.
[0035] FIGS. 11A and 11B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band sensing with different amounts of net positive or net negative charge characterizing the charge storage structure, but with a different diode node arrangement than in FIGS. 10A and 10B .
[0036] FIGS. 12A and 12B are simplified diagrams of neighboring gated diode nonvolatile memory cells, with and without interconnected second nodes.
[0037] FIGS. 13A and 13B are simplified diagrams of an array of gated diode nonvolatile memory cells with interconnected second node columns, performing band-to-band sensing.
[0038] FIGS. 14A and 14B are simplified diagrams of an array of gated diode nonvolatile memory cells without interconnected second node columns, performing band-to-band sensing.
[0039] FIGS. 15A and 15B are simplified diagrams of an array of gated diode nonvolatile memory cells with interconnected second node columns, performing band-to-band sensing, where the doping arrangement of the diode structures is different from FIGS. 13A , 13 B, 14 A, and 14 B.
[0040] FIGS. 16A and 16B are simplified diagrams of an array of gated diode nonvolatile memory cells without interconnected second node columns, performing band-to-band sensing, where the doping arrangement of the diode structures is different from FIGS. 13A , 13 B, 14 A, and 14 B.
[0041] FIGS. 17A and 17B are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which electron tunnel injection is performed on selected cells.
[0042] FIGS. 18A , 18 B, and 18 C are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which band-to-band hot hole injection is performed on selected cells.
[0043] FIGS. 19A , 19 B, and 19 C are exploded view diagrams of multiple arrays of gated diode nonvolatile memory cells, with different interconnections of the word lines, first node columns, and second node columns, between different arrays.
[0044] FIG. 20 is a simplified diagram of an integrated circuit with an array of gated diode nonvolatile memory cells and control circuitry.
[0045] FIGS. 21A-21H illustrate a sample process flow for multiple arrays of gated diode nonvolatile memory cells.
[0046] FIGS. 22A and 22B are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which band-to-band sensing is performed on selected cells.
DETAILED DESCRIPTION
[0047] FIG. 1 is a simplified diagram of a gated diode nonvolatile memory cell. Nodes 102 and 104 form a diode separated by a junction. A combined charge storage and dielectric structure 106 substantially surrounds the first diode node 102 . The combined charge storage and dielectric structure 106 is also partly adjacent to the second diode node 104 . In this cross-sectional view, dielectric 110 on either side of the second diode node 104 isolates the second diode node 104 from neighboring devices, such as other gated diode nonvolatile memory cells. The gate structure 108 applies a gate voltage.
[0048] FIGS. 2A , 2 B, and 2 C are simplified diagrams of a gated diode nonvolatile memory cell, showing various charge storage structures having different materials. In FIG. 2A , a charge trapping material structure 202 locally stores charge, schematically shown here as positive charge on the portion of the charge trapping material near the diode junction. Oxide structures are between the charge trapping material structure 202 and the gate structure, and between the charge trapping material structure 202 and the diode structure. Representative dielectrics between the charge trapping material structure 202 and the gate structure include silicon dioxide and silicon oxynitride having a thickness of about 5 to 10 nanometers, or other similar high dielectric constant materials including for example Al 2 O 3 . Representative between the charge trapping material structure 202 and the diode structure include silicon dioxide and silicon oxynitride having a thickness of about 2 to 10 nanometers, or other similar high dielectric constant materials.
[0049] Representative charge trapping structures include silicon nitride having a thickness of about 3 to 9 nanometers, or other similar high dielectric constant materials, including metal oxides such as Al 2 O 3 , HfO 2 , and others.
[0050] In some embodiments, the gate structure comprises a material having a work function greater than the intrinsic work function of n-type silicon, or greater than about 4.1 eV, and preferably greater than about 4.25 eV, including for example greater than about 5 eV. Representative gate materials include p-type poly, TiN, Pt, and other high work function metals and materials. Other materials having a relatively high work function suitable for embodiments of the technology include metals including but not limited to Ru, Ir, Ni, and Co, metal alloys including but not limited to Ru—Ti and Ni-T, metal nitrides, and metal oxides including but not limited to RuO 2 . High work function gate materials result in higher injection barriers for electron tunneling than that of the typical n-type polysilicon gate. The injection barrier for n-type polysilicon gates with silicon dioxide as the outer dielectric is around 3.15 eV. Thus, embodiments of the present technology use materials for the gate and for the outer dielectric having an injection barrier higher than about 3.15 eV, such as higher than about 3.4 eV, and preferably higher than about 4 eV. For p-type polysilicon gates with silicon dioxide outer dielectrics, the injection barrier is about 4.25 eV, and the resulting threshold of a converged cell is reduced about 2 volts relative to a cell having an n-type polysilicon gate with a silicon dioxide outer dielectric.
[0051] FIG. 2B shows a gated diode nonvolatile memory cell resembling the gated diode nonvolatile memory cell of FIG. 2A , but with a floating gate 204 , often made of polysilicon. FIG. 2C shows a gated diode nonvolatile memory cell resembling the nonvolatile memory cell of FIG. 2A , but with a nanoparticle charge storage structure 206 .
[0052] Each charge storage structure can store one bit or multiple bits. For example, if each charge storage structure stores two bits, then there are four discrete levels of charge stored by the gated diode nonvolatile memory cell.
[0053] In some embodiments, programming refers to making more positive the net charge stored in the charge trapping structure, such as by the addition of holes to or the removal of electrons from the charge storage structure; and erasing refers to making more negative the net charge stored in the charge storage structure, such as by the removal of holes from or the addition of electrons to the charge trapping structure. However, in other embodiments programming refers to making the net charge stored in the charge storage structure more negative, and erasing refers to making the net charge stored in the charge storage structure more positive. Various charge movement mechanisms are used, such as band-to-band tunneling induced hot carrier injection, E-field induced tunneling, and direct tunneling from the substrate.
[0054] FIGS. 3A , 3 B, 3 C, and 3 D are simplified diagrams of a gated diode nonvolatile memory cell, showing various examples of a diode structure, such as the pn diode and the Schottky diode. In FIGS. 3A and 3B , the diode structure is a pn diode. In FIG. 3A , the first node 302 substantially surrounded by the combined charge storage and dielectric structure is doped n-type, and the second node 304 is doped p-type. The gated diode nonvolatile memory cell of FIG. 3B interchanges the node materials of FIG. 3A , such that the first node 312 substantially surrounded by the combined charge storage and dielectric structure is doped p-type, and the second node 314 is doped n-type. In FIGS. 3C and 3D , the diode structure is a Schottky diode. In FIG. 3C , the first node 322 substantially surrounded by the combined charge storage and dielectric structure is a metal material, and the second node 324 is a semiconductor material. The gated diode nonvolatile memory cell of FIG. 3D interchanges the node materials of FIG. 3C , such that the first node 332 substantially surrounded by the combined charge storage and dielectric structure is a semiconductor material, and the second node 334 is a metal material.
[0055] FIGS. 4A and 4B are simplified diagrams of a gated diode nonvolatile memory cell, showing examples of a pn diode with a homojunction. In FIG. 4A , both the first node 402 and the second 404 of the diode structure are silicon. In FIG. 4B , both the first node 412 and the second 414 of the diode structure are germanium. Because of the smaller bandgap of germanium compared to silicon, the gated diode nonvolatile memory cell tends to generate a greater band-to-band current with the configuration of FIG. 4B than with the configuration of FIG. 4A . Regardless of the material used in the homojunction diode structure, the diode structure can be single crystal or polycrystalline. A polycrystalline design results in higher memory cell density, due to the ability to deposit multiple layers of memory cells in the vertical direction.
[0056] FIG. 5 is a simplified diagram of a gated diode nonvolatile memory cell, showing an example of a pn diode with a heterojunction. The first node 502 substantially surrounded by the combined charge storage and dielectric structure is germanium. The second node 504 is silicon. The first node 502 and the second node 504 are joined by a graded transition layer junction 506 .
[0057] FIGS. 6A and 6B are simplified diagrams of a gated diode nonvolatile memory cell operation performing electron tunnel injection. In FIG. 6A , the electron tunnel injection mechanism moves electrons from the gate structure 608 biased at −10 V to the charge storage structure 606 . The first diode node is biased at 10 V or is floating, and the second diode node 604 is biased at 10 V. In FIG. 6B , the electron tunnel injection mechanism moves electrons from the first diode node 602 biased at −10 V or is floating, to the charge storage structure 606 . The gate structure 608 is biased at 10 V, and the second diode node 604 is biased at −10 V.
[0058] FIGS. 7A and 7B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band hot electron injection. In FIG. 7A , the band-to-band hot electron injection moves electrons from the diode structure to the charge storage structure 606 . The n-type first diode node 602 biased at 0 V, the gate structure 608 is biased at 10 V, and holes of the resulting electron-hole pairs flow into the p+-type second node 604 biased at −5 V. In FIG. 7B , the band-to-band hot electron injection moves electrons from the diode structure to the charge storage structure 606 . The n-type second diode node 604 biased at 0 V, the gate structure 608 is biased at 10 V, and holes of the resulting electron-hole pairs flow into the p+-type first node 602 is biased at −5 V.
[0059] FIGS. 8A and 8B are simplified diagrams of a gated diode nonvolatile memory cell operation performing hole tunnel injection. In FIG. 8A , the hole tunnel injection mechanism moves holes from the gate structure 608 biased at 10 V to the charge storage structure 606 . The first diode node is biased at −10 V or is floating, and the second diode node 604 is biased at −10 V. In FIG. 8B , the hole tunnel injection mechanism moves holes from the first diode node 602 biased at 10 V or is floating, to the charge storage structure 606 . The gate structure 608 is biased at −10 V, and the second diode node 604 is biased at 10 V.
[0060] FIGS. 9A and 9B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band hot hole injection. In FIG. 9A , the band-to-band hot hole injection moves holes from the diode structure to the charge storage structure 606 . The p-type first diode node 602 is biased at 0 V, the gate structure 608 is biased at −10 V, and electrons of the resulting electron-hole pairs flow into the n+-type second node 604 is biased at 5 V. In FIG. 9B , the band-to-band hot hole injection moves holes from the diode structure to the charge storage structure 606 . The p-type second diode node 604 is biased at 0 V, the gate structure 608 is biased at −10 V, and electrons of the resulting electron-hole pairs flow into the n+-type first node 602 biased at 5 V.
[0061] Band-to-band currents flowing through the diode structure determine the charge storage state of the charge storage structure with great precision, due to combined vertical and lateral electrical fields. Larger vertical and lateral electrical fields give rise to larger band-to-band currents. A bias arrangement is applied to the various terminals, such that the energy bands bend sufficiently to cause band-to-band current in the diode structure, while keeping the potential difference between the diode nodes sufficiently low enough such that programming or erasing does not occur.
[0062] In example bias arrangements, the diode structure is reverse biased. Additionally, the voltage of the gate structure causes the energy bands to bend sufficiently such that band-to-band tunneling occurs through the diode structure. A high doping concentration in the one of the diode structure nodes, with the resulting high charge density of the space charge region, and the accompanying short length of the space charge region over which the voltage changes, contributes to the sharp energy band bending. Electrons in the valence band on one side of the diode structure junction tunnel through the forbidden gap to the conduction band on the other side of the diode structure junction and drift down the potential hill, deeper into the n-type diode structure node. Similarly, holes drift up the potential hill, away from either n-type diode structure node, and toward the p-type diode structure node.
[0063] The voltage of the gate structure controls the voltage of the portion of the diode structure by the dielectric structure which is between the diode structure and the charge storage structure. As the voltage of the gate structure becomes more negative, the voltage of the portion of the diode structure by this dielectric structure becomes more negative, resulting in deeper band bending in the diode structure. More band-to-band current flows, as a result of at least some combination of 1) an increasing overlap between occupied electron energy levels on one side of the bending energy bands, and unoccupied electron energy levels on the other side of bending energy bands, and 2) a narrower barrier width between the occupied electron energy levels and the unoccupied electron energy levels (Sze, Physics of Semiconductor Devices, 1981).
[0064] The net negative or net positive charge stored on the charge storage structure further affects the degree of band bending. In accordance with Gauss's Law, when a negative voltage is applied to the gate structure relative to the diode structure, a stronger electric field is experienced by portions of the diode structure which are near portions of the charge storage structure having relatively higher net negative charge. Similarly, when a positive voltage is applied to the gate structure relative to the diode structure, a stronger electric field is experienced by portions of the diode structure which are near portions of the charge storage structure having relatively higher net positive charge.
[0065] The different bias arrangements for reading, and bias arrangements for programming and erasing, show a careful balance. For reading, the potential difference between the diode structure terminals should not cause a substantial number of charge carriers to transit a dielectric to the charge storage structure and affect the charge storage state. In contrast, for programming and erasing, the potential difference between the diode structure terminals can be sufficient to cause a substantial number of carriers to transit a dielectric and affect the charge storage state by band-to-band hot carrier injection.
[0066] FIGS. 10A and 10B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band sensing with different amounts of net positive or net negative charge characterizing the charge storage structure. In FIGS. 10A and 10B , band-to-band sensing mechanism creates electron-hole pairs in the diode structure. Resulting electrons flow into the n+-type first diode node 602 biased at 2 V, and resulting holes flow into the p-type second diode node 604 biased at 0 V. The gate structure 608 is biased at −10 V. In FIG. 10A , the charge storage structure 606 stores relatively more negative net charge by the diode structure junction between the n+-type first diode node 602 and the p-type second diode node 604 . In FIG. 10B , the charge storage structure 606 stores relatively more positive net charge by the diode structure junction between the n+-type first diode node 602 and the p-type second diode node 604 . Greater band bending in the diode structure occurs in FIG. 10A than in FIG. 10B , and greater band-to-band sensing current flows in FIG. 10A than in FIG. 10B .
[0067] FIGS. 11A and 11B are simplified diagrams of a gated diode nonvolatile memory cell operation performing band-to-band sensing with different amounts of net positive or net negative charge characterizing the charge storage structure, but with a different diode node arrangement from FIGS. 10A and 10B . In particular, the first node 602 of the diode structure substantially surrounded by the combined charge storage and dielectric structure is p+-type, and the second node of the diode structure 604 is n-type. The band-to-band sensing mechanism creates electron-hole pairs in the diode structure. Resulting holes flow into the p+-type first diode node 602 biased at −2 V, and resulting electrons flow into the n-type second diode node 604 biased at 0 V. The gate structure 608 is biased at 10 V. In FIG. 11A , the charge storage structure 606 stores relatively more negative net charge by the diode structure junction between the p+-type first diode node 602 and the n-type second diode node 604 . In FIG. 11B , the charge storage structure 606 stores a relatively more positive net charge by the diode structure junction between the p+-type first diode node 602 and the n-type second diode node 604 . Greater band bending in the diode structure occurs in FIG. 11B than in FIG. 11A , and greater band-to-band sensing current flows in FIG. 11B than in FIG. 11A .
[0068] In other embodiments, the more heavily doped node is the second node of the diode structure, and the less heavily doped node is the first node of the diode structure substantially surrounded by the combined charge storage and dielectric structure.
[0069] FIGS. 12A and 12B are simplified diagrams of neighboring gated diode nonvolatile memory cells, with and without interconnected second nodes. In FIG. 12A , neighboring gated diode nonvolatile memory cells respectively have second nodes 1204 and 1205 . Both second nodes 1204 and 1205 of the neighboring gated diode nonvolatile memory cells extend beyond the oxide which isolates the upper portions of the second nodes 1204 and 1205 from each other, and connect into a common node structure 1214 . This common node structure is treated as a same bit line used by both neighboring gated diode nonvolatile memory cells. In FIG. 12B , both second nodes 1204 and 1205 of the neighboring gated diode nonvolatile memory cells do not extend beyond the oxide which isolates the second nodes 1204 and 1205 from each other. Each of the second nodes 1204 and 1205 is treated as a distinct bit line, and the two second nodes 1204 and 1205 are not treated as a same bit line.
[0070] FIGS. 13A and 13B are simplified diagrams of an array of gated diode nonvolatile memory cells with interconnected second node columns, performing band-to-band sensing. The first node columns of the diode structures substantially surrounded by the combined charge storage and dielectric structures are n-type, and the second node columns of the diode structures are p-type. Neighboring second node columns of the diode structures extend beyond the oxide which isolates the upper portions of the second node columns from each other, and connect into a common bit line structure. In FIG. 13A , the first node columns of the diode structures are shown with bit line labels DL 1 to DL 6 , the second node columns of the diode structures are shown with the bit line label CL, and the word lines are shown with word line labels WL 1 to WL 6 . In FIG. 13B , voltages are applied to the diode columns and the word lines. The first node column DL 3 is biased at 2 V, and the remaining first node columns are biased at 0 V. The second node columns are biased at 0 V. The word line WL 5 is biased at −10 V, and the remaining word lines are biased at 0 V. A band-to-band sensing operation is thereby performed on the gate diode memory cell at the intersection of word line WL 5 and the first node column DL 3 . By measuring the current flowing through the first node column DL 3 or the second node columns CL, the charge storage state of the charge storage structure of that gate diode memory cell is determined.
[0071] FIGS. 14A and 14B are simplified diagrams of an array of gated diode nonvolatile memory cells without interconnected second node columns, performing band-to-band sensing. Unlike the interconnected common bit line structure of the second node columns shown in FIGS. 13A and 13B , in FIGS. 14A and 14B neighboring second node columns of the diode structures are treated as distinct bit lines. In FIG. 14A , the second node columns of the diode structures are shown with bit line labels CL 1 to CL 6 . In FIG. 14B , voltages are applied to the diode columns and the word lines. The first node column DL 3 is biased at 2 V, and the remaining first node columns are biased at 0 V. The second node columns are biased at 0 V. The word line WL 5 is biased at −10 V, and the remaining word lines are biased at 0 V. A band-to-band sensing operation is thereby performed on the gate diode memory cell at the intersection of word line WL 5 and the first node column DL 3 /second node column CL 3 . By measuring the current flowing through the first node column DL 3 or second node column CL 3 , the charge storage state of the charge storage structure of that gate diode memory cell is determined.
[0072] FIGS. 15A and 15B are simplified diagrams of an array of gated diode nonvolatile memory cells with interconnected second node columns, performing band-to-band sensing, where the doping arrangement of the diode structures is different from FIGS. 13A , 13 B, 14 A, and 14 B. In FIGS. 15A and 15B , the first node columns of the diode structures substantially surrounded by the combined charge storage and dielectric structures are p-type, and the second node columns of the diode structures are n-type. Like FIGS. 13A and 13B , neighboring second node columns of the diode structures extend beyond the oxide which isolates the upper portions of the second node columns from each other, and connect into a common bit line structure. In FIG. 15A , the first node columns of the diode structures are shown with bit line labels DL 1 to DL 6 , the second node columns of the diode structures are shown with the bit line label CL, and the word lines are shown with word line labels WL 1 to WL 6 . In FIG. 15B , voltages are applied to the diode columns and the word lines. The first node column DL 3 is biased at −2 V, and the remaining first node columns are biased at 0 V. The second node columns are biased at 0 V. The word line WL 5 is biased at 10 V, and the remaining word lines are biased at 0 V. A band-to-band sensing operation is thereby performed on the gate diode memory cell at the intersection of word line WL 5 and the first node column DL 3 . By measuring the current flowing through the first node column DL 3 or the second node columns CL, the charge storage state of the charge storage structure of that gate diode memory cell is determined.
[0073] FIGS. 16A and 16B are simplified diagrams of an array of gated diode nonvolatile memory cells without interconnected node columns, performing band-to-band sensing, where the doping arrangement of the diode structures is like FIGS. 15A and 15B . Unlike the interconnected bit line structure of the second node columns shown in FIGS. 15A and 15B , in FIGS. 16A and 16B neighboring second node columns of the diode structures are treated as distinct bit lines. In FIG. 16A , the second node columns of the diode structures are shown with bit line labels CL 1 to CL 6 . In FIG. 16B , voltages are applied to the diode columns and the word lines. The first node column DL 3 is biased at −2 V, and the remaining first node columns are biased at 0 V. The second node columns are biased at 0 V. The word line WL 5 is biased at 10 V, and the remaining word lines are biased at 0 V. A band-to-band sensing operation is thereby performed on the gate diode memory cell at the intersection of word line WL 5 and the first node column DL 3 /second node column CL 3 . By measuring the current flowing through the first node column DL 3 or second node column CL 3 , the charge storage state of the charge storage structure of that gate diode memory cell is determined.
[0074] FIGS. 17A and 17B are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which electron tunnel injection is performed as in FIG. 6A , but on selected cells. In FIG. 17A , the electron tunnel injection mechanism moves electrons from the gate structure 608 biased at −10 V to the charge storage structures 606 and 607 . The first diode nodes 602 and 603 are biased at 10 V or are floating, and the second diode nodes 604 and 605 are biased at 10 V. In FIG. 17B , the first diode node 602 is biased at 10 V or is floating, but the first diode node 603 is biased at −10 V. The electron tunnel injection mechanism selectively moves electrons from the gate structure 608 biased at −10 V to the charge storage structure 606 but not to the charge storage structure 607 . In other embodiments, the electron tunnel injection mechanism moves electrons from the first diode node to the charge storage structure as in FIG. 6B , but on selected cells. In other embodiments, the hole tunnel injection mechanism moves holes from the gate structure to the charge storage structure as in FIG. 8A , but on selected cells. In other embodiments, the hole tunnel injection mechanism moves holes from the first diode node to the charge storage structure as in FIG. 8B , but on selected cells.
[0075] FIGS. 18A , 18 B, and 18 C are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which band-to-band hot hole injection is performed as in FIG. 9B , but on selected cells. In FIG. 18A , the band-to-band hot hole injection mechanism moves holes from the diode structure to the charge storage structure 606 . The p-type second diode nodes 604 and 605 are biased at 0 V, the gate structure 608 is biased at −10 V, and electrons of the resulting electron-hole pairs flow into the n+-type first nodes 602 and 603 biased at 5 V. In FIG. 18B , the first diode node 602 is biased at 5 V, but the first diode node 603 is biased at 0 V. The band-to-band hot hole injection mechanism selectively moves holes from the diode structure to the charge storage structure 606 but not to the charge storage structure 607 . FIG. 18C also shows band-to-band hot hole injection being performed selectively on the diode structure formed by the first diode node 602 and the second diode node 604 , but not on the diode structure formed by the first diode node 603 and the second diode node 605 , as in FIG. 18B . However, in FIG. 18C , the first diode node 603 is biased at 5 V and the second diode node 605 is biased at 5 V. Because a sufficient reverse bias is still absent in the diode structure formed by the first diode node 603 and the second diode node 605 , the band-to-band hot hole injection mechanism is still absent in this diode structure. In other embodiments, the band-to-band hot hole injection mechanism selectively moves holes from the diode structure with a p-type first diode node and a n+-type second diode node to the charge storage structure as in FIG. 9A , but on selected cells. In other embodiments, the band-to-band hot electron injection mechanism selectively moves electrons from the diode structure with a p+-type first diode node and an n-type second diode node to the charge storage structure as in FIG. 7B , but on selected cells. In other embodiments, the band-to-band hot electron injection mechanism selectively moves electrons from the diode structure with an n-type first diode node and a p+-type second diode node to the charge storage structure as in FIG. 7A , but on selected cells.
[0076] FIGS. 22A and 22B are simplified diagrams of neighboring gated diode nonvolatile memory cells without interconnected second nodes, in which band-to-band sensing is performed as in FIG. 10A and 10B , but on selected cells. In FIG. 22A , the band-to-band hot hole sensing mechanism creates electron-hole pairs in the diode structure formed by the n+-type first diode node 602 biased at 2 V and the p-type second diode node 604 biased at 0 V. Resulting electrons flow into the n+-type first diode node 602 , and resulting holes flow into the p-type second diode node 604 . This band-to-band sensing current indicates the amount of net positive or net negative charge characterizing the charge storage structure 606 . The gate structure 608 is biased at −10 V. In the diode structure formed by the n+-type first diode node 603 biased at 0 V and the p-type second diode node 605 biased at 0 V, a band-to-band sensing current indicating the amount of charge characterizing the charge storage structure 607 does not flow, because a sufficient reverse bias is absent. FIG. 22B also shows band-to-band sensing being performed selectively on the diode structure formed by the first diode node 602 and the second diode node 604 , but not on the diode structure formed by the first diode node 603 and the second diode node 605 , as in FIG. 22A . However, in FIG. 22B , the first diode node 603 is biased at 2 V and the second diode node 605 is biased at 2 V. Because a sufficient reverse bias is still absent in the diode structure formed by the first diode node 603 and the second diode node 605 , the band-to-band sensing mechanism is still absent. In other embodiments, the band-to-band sensing mechanism selectively flows in a diode structure with a p-type first diode node and a n+-type second diode node as in FIGS. 11A and 11B , but on selected cells.
[0077] FIGS. 19A , 19 B, and 19 C are exploded view diagrams of multiple arrays of gated diode nonvolatile memory cells, with different interconnections of the word lines, first node columns, and second node columns, between different arrays. Each of the vertically displaced arrays is like the array shown in FIGS. 16A and 16B . Although the multiple arrays displaced vertically from one another by isolation oxide 1904 are part of the same integrated circuit, the multiple arrays are shown in exploded view to show the labels for all word lines and bit lines of the multiple arrays.
[0078] In FIG. 19A , the word lines of different arrays 1900 and 1902 are interconnected. The word lines of array 1900 and the word lines of array 1902 are both labeled WL 1 to WL 6 . However, the first node columns and second node columns of different arrays are isolated from each other. The first node columns of array 1900 are labeled DL 1 to DL 6 , and the first node columns of array 1902 are labeled DL 7 to DL 12 . The second node columns of array 1900 are labeled CL 1 to CL 6 , and the second node columns of array 1902 are labeled CL 7 to CL 12 .
[0079] In FIG. 19B , the word lines of different arrays 1910 and 1912 are isolated from each other. The word lines of array 1910 are labeled WL 1 to WL 6 , and the word lines of array 1912 are labeled WL 7 to WL 12 . However, the first node columns and second node columns of the different arrays 1910 and 1912 are interconnected. The first node columns of array 1910 and array 1912 are both labeled DL 1 to DL 6 , and the second node columns of array 1910 and array 1912 are both labeled CL 1 to CL 6 .
[0080] In FIG. 19C , the word lines of different arrays 1920 and 1922 , and the first node columns and second node columns of different arrays 1920 and 1922 , are isolated from each other. The word lines of array 1920 are labeled WL 1 to WL 6 , and the word lines of array 1922 are labeled WL 7 to WL 12 . The first node columns of array 1920 are labeled DL 1 to DL 6 , and the first node columns of array 1922 are labeled DL 7 to DL 12 . The second node columns of array 1920 are labeled CL 1 to CL 6 , and the second node columns of array 1922 are labeled CL 7 to CL 12 .
[0081] In other embodiments, the multiple arrays have interconnected second node columns, such that a particular array of the multiple arrays has a common bit line structure for the second node columns of that array, or alternatively, for all of the arrays. In other embodiments, the first node columns are n-type and the second columns are p-type.
[0082] FIG. 20 is a simplified diagram of an integrated circuit with an array of gated diode nonvolatile memory cells and control circuitry. The integrated circuit 2050 includes a memory array 2000 implemented using gate diode nonvolatile memory cells, on a semiconductor substrate. The gated diode memory cells of array 2000 may be individual cells, interconnected in arrays, or interconnected in multiple arrays. A row decoder 2001 is coupled to a plurality of word lines 2002 arranged along rows in the memory array 2000 . A column decoder 2003 is coupled to a plurality of bit lines 2004 arranged along columns in the memory array 2000 . Addresses are supplied on bus 2005 to column decoder 2003 and row decoder 2001 . Sense amplifiers and data-in structures in block 2006 are coupled to the column decoder 2003 via data bus 2007 . Data is supplied via the data-in line 2011 from input/output ports on the integrated circuit 2050 , or from other data sources internal or external to the integrated circuit 2050 , to the data-in structures in block 2006 . Data is supplied via the data-out line 2015 from the sense amplifiers in block 2006 to input/output ports on the integrated circuit 2050 , or to other data destinations internal or external to the integrated circuit 2050 . A bias arrangement state machine 2009 controls the application of bias arrangement supply voltages 2008 , such as for the erase verify and program verify voltages, and the arrangements for programming, erasing, and reading the memory cells, such as with the band-to-band currents.
[0083] FIGS. 21A-21H illustrate a sample process flow for multiple arrays of gated diode nonvolatile memory cells. FIG. 21A shows a structure with a p-type polysilicon layer 2112 on an oxide layer 2104 on a silicon substrate 2102 . In FIG. 21B , sacrificial oxide 2116 is formed and nitride 2118 is formed. Shallow trench isolation is performed, resulting in multiple p-type polysilicon structures 2113 . In FIG. 21C , the sacrificial oxide 2116 and nitride 2118 are removed. The multiple p-type polysilicon structures 2113 are implanted, resulting in p-type second nodes 2114 and n+-type first nodes 2121 of the gated diode nonvolatile memory cells. In FIG. 21D , the combined charge storage and dielectric structure 2123 and gate polysilicon 2132 are formed, completing the first array of gated diode nonvolatile memory cells. In FIG. 21E , another layer of oxide 2104 and another layer of p-type polysilicon 2112 are formed. In FIGS. 21F-21H , the steps of FIGS. 21B-D are substantially repeated to form another array of gated diode nonvolatile memory cells that is displaced vertically from the first array.
[0084] While the present invention is disclosed by reference to the technology and examples detailed above, it is to be understood that these examples are intended in an illustrative rather than in a limiting sense. It is contemplated that modifications and combinations will readily occur to those skilled in the art, which modifications and combinations will be within the spirit of the invention and the scope of the following claims.
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A memory integrated circuit has memory arrays that are vertically layered. These memory arrays include word lines and bit lines. Intersections between the word lines and the bit lines include a diode and a memory state storage element. The diode and the memory storage element are connected in between a word line and a bit line. The diode at the intersections includes a first diode node and a second diode node. Various aspects of the memory integrated circuit are electrically interconnected in various ways, such as corresponding word lines, corresponding first diode nodes, or corresponding second diode nodes of different memory arrays being electrically interconnected. Various aspects of the memory integrated circuit are isolated in various ways, such as word lines, first diode nodes, or second diode nodes of different memory arrays being isolated.
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FIELD OF THE PRESENT INVENTION
[0001] The present invention relates generally to nonwoven, natural-fiber fabrics, and specifically to a nonwoven fabric of hydrodynamically entangled waste cotton fibers, which fabric is suited to form, among other things, bags for containing cotton bales.
BACKGROUND OF THE PRESENT INVENTION
[0002] Cotton fiber, a so-called “natural fiber” because it is taken from a plant instead of from a synthetic source such as petrochemicals, is widely used in making fabrics of various types. Before cotton can be used as a fabric, it must undergo a series of processing steps. The cotton plant produces bolls of raw cotton, which are typically mechanically harvested and delivered to a gin, where foreign material such as dirt, plant matter, and insect parts are removed, and where the fiber is separated from the seeds embedded within it.
[0003] The cotton fiber then undergoes successive processes, such as picking and combing, to clean the fiber further and to cause the individual fibers to begin to cohere, or align. Picked cotton fiber destined to become yarn for weaving or knitting is then laid down into a lap. Carding further refines the cotton fiber and begins the process of removing short-staple fibers, which are considered to be too short to be commercially useful in a yarn. Longer fibers generally provide greater resistance to breaking (in a yarn) or tearing (in a woven or knitted fabric). Short-staple, or “waste cotton,” fibers have typically been regarded as not usable in yams and fabrics, and so have been used only for their absorptive capabilities, rather than for their tensile strength, in disposable products such as diapers, sanitary napkins, cigarette filters, and the like.
[0004] Because ginned cotton is fairly lightweight, it is useful to compress it into bales of a convenient size for transportation. Once cotton has been compressed, however, it is necessary to hold it in a compressed condition. Historically, this was accomplished by placing bands around the bale and wrapping the bale in burlap or in a woven or knitted fabric. A more modem method is to wrap the bale in polyethylene film or in woven polypropylene, typically in a bag form, after banding. Wrapping the bale also keeps dirt and foreign matter from contaminating the ginned cotton. Though covering the bale is a necessary step, these coverings create an additional expense for the cotton processor. Consequently, it is desirable to use a material that may be obtained inexpensively, in order to reduce processing costs.
SUMMARY OF THE PRESENT INVENTION
[0005] Briefly summarized, the present invention provides for a non-woven fabric comprises hydrodynamically entangled waste cotton fibers to form a binderless integrated web. Hydrodynamic entanglement, also known as hydroentanglement or hydroneedling, is a process that is well known in the art of textile manufacturing. Hydrodynamic entanglement is usually accomplished by feeding a thick batt of fibers through a series of fine jets of water at water pressures ranging from 10 to 600 bar or more. Energy transferred from the jets of water serves to compact or punch down the batt of fibers, to cause the fibers to cohere, and to entangle the fibers. Often, and especially in the case of natural fibers, a thermoplastic material is intermixed with the fibers to enable them to be thermally bonded, thereby increasing the strength of the fabric. The end result is a non-woven fabric of a fairly uniform density and strength. Hydrodynamic entanglement is typically used to entangle so-called “endless” fibers—for instance, synthetic fibers that are extruded from molten plastic and have a far greater fiber length than natural fibers. One common use for hydroentangled fiber fabrics is for surgical gowns and drapes; because of the relatively inexpensive manufacturing process, such fabrics are disposable and thus ideal for such “single-use” applications.
[0006] Although hydrodynamic entanglement is well known for synthetic fibers and usable for long-staple natural fibers, heretofore the process has not been used to process waste cotton fibers into usable fabric, nor has the process been thought to be capable of effectively forming usable fabric from waste cotton fibers. An object of the present invention is, therefore, to provide for a fabric comprising waste cotton fibers that have been hydrodynamically entangled. As used herein, the term “waste cotton fibers” is intended to mean cotton fibers predominantly of a staple fiber length less than about 1⅛ inches, which are primarily unsuitable for spinning into a usable yarn, although longer fibers may be used without departing from the scope of the invention.
[0007] It is another object of the present invention to provide for a fabric that does not require a thermoplastic bonding agent in order to form an integrated web of waste cotton fibers, because of the expense associated with providing and interspersing such an agent within the batt.
[0008] It is still another object of the present invention to provide for a bag, suitable for containing and protecting a bulk material—such as ginned and baled cotton—which is formed from fabric comprising a binderless cohesively integrated web of hydrodynamically entangled waste cotton fibers, and which may be provided at a substantially smaller cost than traditional bags.
[0009] It is a further object of the present invention to provide for the combination of a cotton bale and a cover for the bale, the cover comprising a fabric that includes a cohesively integrated web of hydrodynamically entangled waste cotton fibers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Further features, embodiments, and advantages of the present invention will become apparent from the following detailed description with reference to the drawings, wherein:
[0011] [0011]FIG. 1 is a schematic representation of a hydrodynamic needling machine and waste cotton being processed thereon;
[0012] [0012]FIG. 2A is a partially schematic side view of a batt of waste cotton fibers, pre- and post-entanglement;
[0013] [0013]FIG. 2B is a large-scale schematic perspective view of a cohesively integrated web of hydrodynamically entangled waste cotton fibers;
[0014] [0014]FIG. 2C is a photograph of a web as in FIG. 2B;
[0015] [0015]FIG. 3 depicts a bag and a bulk material in combination; and
[0016] [0016]FIG. 4 depicts a cotton bale and cover for the bale.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0017] Referring now to FIG. 1, a hydrodynamic needling machine 1 (also known as a hydrodynamic entanglement machine) is schematically depicted. Hydrodynamic needling machines are well known in the art of textile manufacturing. One such machine is manufactured by Fleissner GmbH & Co. Maschinenfabrik of Egelsbach, Germany, under the trademark AQUAJET, and Fleissner, U.S. Pat. No. 5,960,525, issued Oct. 5, 1999, teaches such a device.
[0018] The hydrodynamic needling machine 1 generally comprises a pair of porous conveyor belts 10 , a plurality of water jets 12 , and one or more perforated needling drums 14 . A non-integrated batt of waste cotton fibers 16 , varying in thickness between ⅛″ and 5″, depending on the desired thickness of the resulting fabric, is fed from a conveyor 18 of line 20 , which may be a carding line or an air-laying line, and onto lower conveyor belt 10 . Batt 16 is conveyed in the direction of arrow A to a hydroneedling stage and held between the two conveyor belts 10 , at 11 , which belts serve to advance the fabric through the hydroneedling stage without stretching the web. It may be desirable to wet the batt before the hydroneedling stage to reduce the loft of the batt, particularly for batts of higher loft.
[0019] At the hydroneedling stage, batt 16 , having been compressed somewhat between the two conveyor belts 10 , is held against needling drum 14 and subjected to a plurality of pressurized water jets 12 . Water from the jets 12 traverses porous upper conveyor belt 10 , impinges upon batt 16 , traverses porous lower conveyor belt 10 , and is drawn off through perforations in needling drum 14 . As water passes under pressure through batt 16 , hydrodynamic energy transforms batt 16 in at least two ways. First, batt 16 is further compressed to a degree in accordance with the water pressure. Second, the individual fibers of batt 16 are made to cohere (mutually align) by entanglement with each other. Because of the regularized and coherent application of hydrodynamic energy to batt 16 , the resulting coherently integrated web is of substantially uniform thickness, texture, and strength, making it suitable for use as a fabric. After hydroneedling, batt 16 is conveyed in the direction of arrow B to a finishing stage.
[0020] Because cotton is a highly absorptive material, a portion of the water used during hydrodynamic entanglement is absorbed within the cotton. Therefore, following the hydroneedling process, it is helpful to extract a portion of the water from the web in order to speed drying. Batt 16 , now a fabric, is carried in the direction of arrow C through water extraction zone 22 . After the excess water has been extracted, the fabric may be conveyed through an optional treatment zone 24 , for instance, for adding a waterproofing chemical or a UV inhibitor to the fabric. Following optional zone 24 , the fabric enters drying zone 26 , where the fabric is dried to the necessary extent. Following drying, the fabric may be conveniently wound onto rolls for a subsequent sewing operation, according to manufacturing needs.
[0021] Referring now to FIGS. 2 A- 2 B, fabric 30 is shown in comparison to batt 16 . In FIG. 2A, batt 16 , in its pre-hydroneedling state, is schematically depicted in a side view, and fabric 30 , in a post-hydroneedling state, is depicted in a partial side view, in order to demonstrate both that the hydroneedling process works to compress batt 16 to a great degree and that the resulting fabric 30 comprises fibers that are mutually coherent and entangled (as can be seen from the pattern). Those skilled in the art will recognize that FIG. 2A does not illustrate any particular scale, as various thicknesses of batt 16 can produce a variety of thicknesses of fabric 30 , depending upon the water pressure applied during hydroneedling.
[0022] In FIG. 2B, a fabric 30 comprising a cohesively integrated web of hydrodynamically entangled waste cotton fiber is depicted in a large scale schematic perspective view. As can be seen from the figure, the waste cotton fibers have been entangled to form within fabric 30 a substantially uniform and regularized web pattern. Because the fibers have been entangled to a degree that is commensurate with their length, the resulting fabric is sufficiently strong and resilient to allow it to serve as a bag or a cover for a bulk material, such as a cotton bale, even if that bulk material is in a compressed state and is susceptible of some expansion against the resistance of the bag or cover.
[0023] [0023]FIG. 2C is a photograph of a fabric as represented in FIG. 2B. The flecks visible in the photograph constitute foreign matter, which may comprise dirt, insect matter, plant matter, or other non-fiber matter, and which need not be fully removed prior to processing of the waste cotton fibers to form the fabric of the present invention.
[0024] [0024]FIGS. 3 and 4 depict two possible useful configurations for the fabric as described above and as depicted in FIGS. 2 A- 2 B. FIG. 3 depicts a bag 40 for a bulk material, such as cotton (not shown). FIG. 4 depicts a cotton bale 42 and a cover 44 for the bale, which cover 44 comprises a hydrodynamically entangled fabric according to the present invention. Compression bands 46 provide protection against undesired decompression. Because baled cotton has undergone an extensive and expensive ginning operation to remove non-fibrous matter from the cotton fiber, it is likewise desirable to maintain bale 42 in a substantially clean state, which purpose is served by the cover 44 of the present invention. Cover 44 may also serve to contain the bale if some of compression bands 46 break.
[0025] Although simple applications are depicted in FIGS. 3 and 4, those persons skilled in the art to which the present invention pertains will recognize that a wide variety of configurations is possible, and that the uses of the fabric of the present invention are not limited to bagging or covering applications or to any particular configuration of the fabric.
[0026] Those skilled in the art of manufacturing fabrics will also recognize that fabrics of differing weights, textures, and strengths are desirable for different applications, and further that the fabric of the present invention may be manufactured according to desired characteristics dependent upon the particular application, by altering the parameters of manufacture. Indeed, the interplay between different manufacturing parameters results in particular characteristics of the finished fabric. The thickness of the fabric may be adjusted by adjusting the loft or, correspondingly, the weight of the entering batt, while maintaining water pressure at a chosen level. The strength of the fabric may be adjusted by adjusting the loft or weight of the entering batt and by adjusting the water pressure, or by utilizing a drum of a different perforation configuration to adjust the level of entanglement. The width of the entering batt determines the width of the resulting fabric, and the texture of the resulting fabric is generally dependent upon the drum configuration. Although a wide range of variations is possible, these various embodiments are nevertheless well within the scope of the present invention because they share a common core internal structure: they are cohesively integrated webs of hydrodynamically entangled waste cotton fibers.
[0027] The typical operating ranges for manufacturing the fabric of the present invention are as follows, although these or other methods of manufacturing the fabric of the present invention may permit or even require values outside of these ranges without departing from the scope of the present invention. Therefore, these values are intended to be illustrative rather than limiting. The loft of the entering batt generally varies between ⅛″ and 5″, with a batt weight of between 50 g/m 2 and 200 g/m 2 . Generally, a minimum of 2 water injectors is required, although present machinery allows for as many as 14 injectors and there is, theoretically, no upper limit on the number of injectors. Water pressures of up to 600 bar are available with present machinery, although higher pressures might be achievable and useful for particular applications; the selected water pressure is highly dependent upon the weight of the material being processed, since a major component of the manufacturing process is the compaction of the entering batt.
[0028] In view of the aforesaid written description of the present invention, it will be readily understood by those persons skilled in the art that the present invention is susceptible of broad utility and application. Many embodiments and adaptations of the present invention other than those herein described, as well as many variations, modifications, and equivalent arrangements, will be apparent from or reasonably suggested by the present invention and the foregoing description thereof, without departing from the substance or scope of the present invention. Accordingly, while the present invention has been described herein in detail in relation to preferred embodiments, it is to be understood that this disclosure is only illustrative and exemplary of the present invention and is made merely for purposes of providing a full and enabling disclosure of the invention. The foregoing disclosure is not intended nor is to be construed to limit the present invention or otherwise to exclude any such other embodiments, adaptations, variations, modifications and equivalent arrangements, the present invention being limited only by the claims appended hereto and the equivalents thereof.
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A nonwoven fabric includes a cohesively integrated web of hydrodynamically entangled short-staple or “waste cotton” fibers. A batt of waste cotton fibers is hydrodynamically needled by high-pressure streams of water. The hydrodynamic energy of the streams causes the fibers to cohere and to become mutually entangled, which in turn results in a fabric of sufficient strength to be used for, among other things, a bag for a bulk material and particularly a bag or cover for a cotton bale.
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BACKGROUND OF THE INVENTION
Games simulating putting and devices adapted for putting practice are known. The devices adapted for putting practice have generally been intended for use on a rug or other available practice surface, while the games simulating putting have commonly been arranged on table top surfaces or resilient surfaces allowing for play with conventional golf playing implements or more toy-like playing implements.
U.S. Pat. No. 4,108,440 to Delaplaine is directed to a golf putting game provided in a mat of foam resilient material. The mat has holes cut in it to form putting cups and is also marked with areas indicating tees. The holes and teeing areas are marked with appropriate indicia indicating the sequence of play for the golf game. Further, the mat is reversible to provide a different course layout on each side.
U.S. Pat. Nos. 713,253 and 720,191, both issued to Taylor, show a golf game in which a course is provided on the surface of a game board with sides. The game board is covered with fuzzy material such as flock or felt. The game includes multiple holes cut out of the game board and tee grounds which are marked on the surface of the board. The patents disclose the use of a ball covered with a fuzzy material, smooth or serrated.
U.S. Pat. No. 3,604,710 to Jacobs is directed to an indoor golf putting game where the greens and playing surfaces are constructed from carpet laid upon a foundational material which may be cement, wood, or other suitable material. The holes for this game are cut through the carpet and foundational material. Different elevations for the playing surface and greens may be produced by placing material between the upper playing surface and the foundational material. The game also includes markers which indicate the teeing ground and the number for the hole being played. These markers are portable and may be moved toward or away from the hole to vary the length of a particular putt.
The games associated with the above patents have a playing surface or mat for playing the games and holes permanently cut out or fixed in the playing surface. The coarse layout does not change because the holes are permanently fixed to their respective locations in the coarse. What is needed is a putting game for playing on a suitable surface having holes which may be selectively positioned on the playing surface to alter the playing coarse layout.
SUMMARY OF THE INVENTION
The limitations of previously known golf games have been overcome by a game made in accordance with the principles of the present invention. Generally, the golf game of the present invention comprises a mat and a plurality of detachable disks representing holes so the detachable disks may be selectively positioned about the mat to change the layout of a simulated course.
More particularly, the mat of the present invention has a playing surface simulating a natural grass surface. The game also includes a plurality of detachable or portable disks which may be selectively positioned on the surface of the mat. The disks have an inlet for receiving a ball. Preferably, the disks are marked with indicia indicating the appropriate sequence of play. The game preferably includes a tee mounted to the mat for striking the ball therefrom. The tee may be affixed or selectively attachable to the mat. The portable disks are selectively moved about the mat altering a coarse layout.
In another embodiment of the invention, the mat is marked with obstacles simulating hazards during play. The surface of the mat may be artificial plastic grass, felt, flock, carpet, or any other woven surface simulating a natural grass surface. The inlet for the disks preferably joins with a recess which accepts and retains a ball being played. The ball of the present invention may be a marble, golf ball, or similarly sized rounded object.
Most preferably, four disks having a recess for receiving the ball are positioned on the mat presenting both diagonal and straight line shots across the mat to a disk. The disks are positioned at the comers of a rectangular mat.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a player using the game of the present invention;
FIG. 2 is a plan view of the playing surface of the mat and the selected positions of holes used in the putting game of the present invention;
FIG. 3 is a cross sectional view taken along line 3--3 of FIG. 2;
FIG. 4 is a cross sectional view taken along line 4--4 of FIG. 2; and
FIG. 5 is a perspective view of a preferred embodiment of a detachable disk used in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
A golf game made in accordance with the principles of the present invention is shown in FIG. 1. The game 8 preferably includes a mat 10 having a playing surface 11 to simulate a natural grass putting surface and portable disks 12, 13, 14 and 15 for simulating holes of a putting green. The shape of the mat 10 may be any shape desired although a rectangular shape is most convenient because it will easily roll into a sleeve for storage or when not in use. Preferably, a teeing disk 17 is also mounted to the surface 11 of mat 10. Surface 11 may be felt, plastic grass, carpet or any other surface conducive for putting a rounded object. Preferably, the disks and teeing area are removably attached to mat 10. The disks may be a piece of wood or may be made of any other suitable material such as plastic, cardboard, or the like which can be easily configured to simulate a hole and be detachably secured to mat 10. Disks 12-15 (FIG. 2) are marked with indicia which indicate the sequence in which the holes are to be played. The disks are preferably formed with an inlet 24 and a recess 25 to receive and hold a ball or other round object.
Referring to FIG. 3, teeing area 17 is attached to mat 10. Although other materials and other shapes may be used to form tee 17, tee 17 is preferably a rounded piece of wood having one or more dimples 19 in its upper surface for receiving and holding rounded object 20 until it is struck. Object 20 is preferably a large marble, although other sizes and types of rounded objects are contemplated by this invention and can be placed on dimple 19 of tee 17, including regulation golf balls. Preferably, a golf club (putter) sized for children is used with game 8 to stroke the marble or ball 20 during play although regulation sized clubs may be used. The disks are also provided with dimples 23 to provide a tee ground for playing the next hole in sequence.
Disks 12-15 may be mounted to mat 10 by a variety of methods. For example, as shown in FIG. 4, a mechanical fastener, such as staples, may be used to secure the disks to mat 10. Another type of mechanical fastener is a hook and loop fastener 30 attached to the underside of a disk as shown in FIG. 5. The fastener 30 grips surface 11 to detachably secure a disk to mat 10. Fastener 30 may cover the entire underside of a disk or it may be one or more strips mounted to a disk underside. Alternatively, the disks may be detachably mounted to mat 10 by using double-sided tape or the like.
To play game 8, a player places a rounded object 20 on a dimple 19 of tee ground 17 and strokes object 20 towards disk 12 marked with the indicia "1". To "hole" object 20, the object must pass through inlet 24 so it comes to rest inside recessed opening 25 of disk 12. After a player holes object 20 in recess 25, the object is placed in dimple 23 of disk 12 and struck towards the next higher numbered disk, in this case disk 13 with the indicia "2". This sequence continues until all of the holes have been played. The disks representing the holes of game 8 are preferably arranged so that disks 12 and 13 are placed at the diagonals of rectangular mat 10 and disks 14 and 15 are placed on the crossing diagonal of mat 10. Tee ground 17 is placed approximately half way between disks 13 and 15. Thus, the shots to holes "2" and "4" are along a diagonal across mat 10 while the shots to holes "1" and "3" are shorter shots generally aligned with one side of mat 10. Alternatively, object 20 may be returned to tee area 17 after completion of each hole. This method of play provides "dog leg" shots as shown in FIG. 2. Game 8 may also include variations such as marking or mounting obstacles on mat 10 to simulate water hazards, sand traps, or the like. After all of the "holes" have been played, the player with the lowest number of total strokes wins.
The present invention has been described in detail above for purposes of illustration only and is not intended to be limited by this description or otherwise to exclude any variation or equivalent arrangement that would be apparent from or reasonably suggested by the foregoing disclosure to those skilled in the art.
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A golf game is disclosed which has disks for simulating holes which may be selectively positioned about the surface of a mat to alter the course layout. The mat may be marked with obstacles to simulate playing hazards. Additionally, a teeing disk may also be provided. The disks are preferably provided with fasteners to temporarily secure the disks to the mat for play. The fastener may be hook and loop, adhesive strip or a staple.
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FIELD OF THE INVENTION
[0001] This invention relates generally to methods and apparatus for facilitating the sampling of packaged standard solutions by online total organic carbon (TOC) analyzers, such as those used in the pharmaceutical industry. Such methods and apparatus improve the productivity and reliability of tests that are performance and/or regulatory-driven, such as in calibration procedures and in carrying out the System Suitability Test. The methods and apparatus of this invention can also generally be applied to improving the productivity of related tests of multiple standard solutions and/or calibration procedures with analyzers of various types that sample liquids for continuous analysis.
BACKGROUND OF THE INVENTION
[0002] The United States Phannacopoeia (USP) and the European Pharmacopoeia (EP) have established various requirements for testing TOC analyzer systems to establish their suitability for use in qualifying pharmaceutical water quality. One of those specific requirements, which relates to the methods and apparatus of this invention, is known as the System Suitability Test (SST). This invention, however, also has general utility in connection with other tests that involve multiple standard solutions and/or calibration procedures that require using multiple standard solutions in analyzers used for continuous process analysis.
[0003] The SST consists of multiple analyses of the contents of the different sample vials containing samples R w , R s and R ss as follows: R w —reagent water that is alto used to make the other two standards; R s —a relatively easy-to-oxidize organic compound in the reagent water; and R ss —a relatively difficult-to-oxidize organic compound in the reagent water. Each sample vial contains approximately 30 cc of the solution, and multiple measurements are made from each vial. All three vials are analyzed in succession, the analyzer is returned to online operation, and a results report is automatically generated. The present state of the art in this field, (i.e., without this invention), provides for manual insertion and removal of each vial into and from the analyzer during the test, and then manually reconfiguring the hardware (e.g., the operating valves) to return the analyzer to online operation. The analysis of each vial can take from 30 to 40 minutes, resulting in a large time commitment for the user/operator, who must return to the analyzer at least three times to switch from one vial to the next, or to switch from the last vial back to online operation.
[0004] A sampling device currently in use, which is generally regarded as the leader among current pharmaceutical TOC analyzers, is called the Integrated Online Sampler (IOS), as described at least in part in U.S. Patient Nos. 5,837,203; 5,976,468; and 6,271,043. This device allows the user to easily switch from online water analysis to grab-sample analysis of sample/calibration vials. The IOS apparatus, however, is a completely passive, non-powered device, which requires manual operation of valves by the user, and does not incorporate any information-management functions. Furthermore, the above referenced patents teach that valving will add contamination resulting in an error when conducting low-level TOC measurement.
[0005] Liquid autosamplers have been used with TOC analyzers to provide some level of automation, such as with respect to the ability to sequence through multiple standards or samples without continuous human intervention. Such autosamplers are not commonly used with online analyzers, however, due to cost, adaptation, interface and logistical problems. As one simple example, an online analyzer is usually mounted to a wall in a factory, which would make the interface town autosampler impractical. Since SST protocols are performed relatively infrequently, dedication of an entire autosampler system (which is generally quite expensive) to a given online TOC analyzer is neither economical nor practical.
[0006] Representative of pertinent prior art in the fluid sampling field and in related technological areas, such as memory control and venting systems for fluid sampling applications, are the following U.S. patents, each of which is incorporated herein by reference: U.S. Pat. Nos. 5,837,203 (Godec '203); 5,976,468 (Godec '468); 6,271,043 (Godec '043); 5,869,006 (Fanning '006); 6,135,172 (Féré '172); 6,152,327 (Rhine '327); 6,330,977 (Hass '977); 6,564,655 (Austen '655); 6,613,224 (Strand '224); 6,649,829 (Garber '829); 6,743,202 (Hirschman '202); and 6,841,774 (Weiss '774).
[0007] For example, the Austen '655 patent is directed to an “Analytical Sampling Device” for automatically taking a known volume of liquid from a source and passing liquid from the sample through a solid phase extraction unit, in combination with information reading and control systems. This system is intended to provide portable equipment for conducting on-site batch groundwater analyses instead of having to freeze and transport groundwater samples to a laboratory for subsequent testing. This invention does not teach or suggest an automated standards sampling apparatus for periodically testing the accuracy of an online analyzer that is continuously monitoring the purity of a flowing liquid according to prescribed testing protocols involving the use of multiple standards solutions.
[0008] The Godec '203, Godec '468 and Godec '043 patents, as mentioned previously, are directed to integrated online sampling comprising apparatus and methods for supplying a portion of a fluid stream and, alternately, a fluid of known composition and concentration to an analyzer. The fluid stream is directed along a flow path through a housing containing a sampling needle, which has an inlet in the fluid flow path and an outlet in fluid communication with the analyzer. When desired, a tube or vial containing a known fluid may be inserted into the housing containing the sampling needle, so that the inlet of the sampling needle is in the known fluid whereby the known fluid is supplied to the analyzer. A second needle provides ventilation to the vial of known fluid to prevent the formation of a vacuum as the known fluid is drained from the vial.
[0009] Comparable to the present invention, there Godec patents teach online sampling in conjunction with periodic calibration/verification of the associated analyzer unit. In contrast to the present invention, however, the referenced Godec patents do not teach automatically regulating online sampling/analyzer calibration using automated valves, memory storage devices, meeting standards protocols requiring delivery of a controlled sequence of multiple and different standard solutions to the analyzer, automatic monitoring of the standards being used and associated information recording, or using a keyed vial set assembly to eliminate orientation errors when inserting a vial set into the sampling apparatus.
[0010] The Fanning '006 patent pertains to a device that fills wells of “cards” and then optically analyzes each well in multiple cards. This device is especially designed to fill, incubate and analyze microbiological samples. The device is not used to calibrate or verify performance of an analyzer. It does not provide a method for removing fluid from the cards but rather performs optical analyses of the contents without removing them from the card. This invention, however, does use a “machine-readable memory storage device” to keep track of the cards within the machine. Bar codes are used on the individual cards, and sets of cards are kept in “cassettes” which use “memory buttons” or “touch buttons” (made by Dallas Semiconductor) to track all the cards in the cassette. This apparatus also provides for automated dilution of samples. It does not, however, relate to on-line sampling.
[0011] The Hass '977 patent teaches a medical application for an electronic token system (using “iButtons®” or some equivalent physical realization of the tokens) wherein each token could be used to identify the liquid contents of a single tube sampled by a syringe. In medical applications, the sampled liquid might be blood or therapeutic drugs. This patent also describes how a computer could be used to communicate with the tokens via an RS-232 port, for example to acquire information about the contents of the tubes. However, this invention does not elaborate further on possible uses of such electronic tokens to identify fluid samples (singly or in aggregate); and, in particular, the patent does not teach or suggest an automated standards sampling apparatus for periodically testing the accuracy of an online analyzer that is continuously monitoring the purity of a flowing liquid according to prescribed testing protocols involving the use of multiple standards solutions.
[0012] The Strand '224 patent describes a liquid chromatography column that has a built-in memory storage device to identify the column for a specific analytical method. Such applications include the validation of the data on the memory storage device during the manufacture of a cartridge. This patent, however, does not relate to multiple samples or, in this particular case, to multiple columns. The patent does mention encryption of the data stored in the cartridge, but it does not pertain to on-line sampling or calibration applications. In essence, this patent teaches providing a “smart” component for an analysis system rather than providing a “smart” set of analytes.
[0013] The Garber '829 patent describes RFID-outfitted fluid couplings. The “smart” couplings can be connected, and, if they are intended to be compatible with the flow of fluid, they can be enabled (by a solenoid valve or pump, for example). This patent, however, does not pertain to on-line sampling, calibration, one-time-use standards, or a single memory storage device identifying the contents of multiple standards.
[0014] The Garber '829 patent also teaches about use of a short-range wireless communication system built into mechanically mating fluid couplings. Such system can inform a fluid control device about whether or not the fluid couplings are matched to insure that the fluid would be transmitted only if it was judged to be acceptable in some sense, such as in composition or according to expiration date. However this invention teaches exclusively about the use of wireless communication means (such as RFD modules) to ensure that a mismatch will be sensed remotely before the fluid coupling is completed. This patent does not teach or suggest about the use of a direct electrical connection between halves of the coupling, made after the fluid coupling has been completed, as in the present invention. Furthermore, the Garber '829 patent does not teach or suggest an automated standards sampling apparatus for periodically testing the accuracy of an online analyzer that is continuously monitoring the purity of a flowing liquid according to prescribed testing protocols involving the use of multiple standards solutions.
[0015] The Hirschman '202 patent relates to syringes for injecting fluid, such as contrast agents, into human subjects. The syringes of this invention are equipped with memory storage devices that can be programmed to hold information about the contents of a syringe, such as volume available, flow rate, pressure, and limits of piston travel. The “smart” syringe would be placed in an injector, which reads the information from the syringe's memory storage device and delivers the contents in accordance with the data. This patent, however, does not relate to on-line sampling applications.
[0016] The Weiss '774 patent describes a multi-stream valve for a mass spectrometer inlet. The valve selects flowing streams of gaseous analyte. This patent, however, does not relate to liquid sampling or memory storage devices.
[0017] The Féré '172 patent pertains entirely to the design of a needle for piercing rubber stoppers or septa in the tops of test tubes containing samples to be extracted, especially Vacutainer-style (Vacutainer is a trade name of the BD Diagnostics Corporation), in which a vacuum is inside the tube. The needle design provides a novel shape to prevent coring of the septum and plugging of the needle. The needle of this patent has grooves cut into its exterior, which grooves act as integral “vent needles” which relieve pressure differences once the needle is fully inserted into the test tube. This needle design is used to remove, for example, blood samples from a test tube with sub-ambient pressure inside. This patent, however, does not pertain to on-line sampling, memory storage devices, stream selection or calibration.
[0018] The Rhine '327 patent pertains only to the delivery of reagents, chemicals, detergents and the like—not to the delivery of calibration standards. This patent discloses a novel sealing mechanism that allows air exchange into a sealed container holding a liquid without liquid leakage. This patent does not, however, teach anything about memory storage devices or on-line sampling of a liquid stream requiring analysis.
[0019] In contrast to a conventional liquid autosampler, the automated standards sampling apparatus of this invention provides automated information management features, can readily switch between vial sampling and online sampling, and is fully integrated to the TOC analyzer to perform all liquid sampling functions. While extra hardware and software might, at some considerable expense, be added to a conventional autosampler system to provide, for example, bar code scanning of vial information and automated valving to switch back to online measurements, the resulting system would still lack a high and coherent degree of system integration as is required for convenient and reliable System Suitability Testing in an industrial factory environment, for example.
[0020] Among other advantages, the present invention reduces the operator time commitment to a single interaction which sets into motion the entire multi-step SST, at the conclusion of which (if the SST is successfully passed) the analyzer is automatically returned to online analysis, thereby minimizing the amount of time during which the analyzer is off-line and the process liquid quality is not being monitored.
[0021] In addition to human and equipment timesavings, this invention also improves the reliability of System Suitability Testing. Without this invention, the user must verify that each standard solution is viable—i.e., that its expiration date has not yet passed. The user must also transcribe certain information from the vials to written report records of the test, ensure that the proper set of standards is being used for the test, and ensure that the standards are analyzed in the proper sequence. These potential sources of error in performing the conventional SST can result in a failed SST, at which point the entire process must be repeated. In contrast, this invention automatically transfers vial information to the analyzer, and software associated with the analyzer ensures the proper sequencing of the vials for analysis and prevents out-of-date standards from being analyzed.
[0022] The invention also incorporates automated valving, preferably fabricated using substantially inert materials, that, unlike earlier sampler valving designs, does not introduce levels of contamination into samples being analyzed sufficiently high to interfere with accurate low-level TOC measurement.
[0023] The improved reliability, inertness of materials, convenience and productivity of the present invention also apply to oilier tests that may be performed with multiple standards, including tests for Accuracy/Precision/Verification, Calibration, and Linearity. In each case, using the present invention, the TOC analyzer is given the vial information electronically, which thereby ensures proper sequencing of the vials and recording of information about the vials.
OBJECTS OF THE INVENTION
[0024] Accordingly, a principal object of the present invention is to provide methods and related automated standards sampling apparatus for switching a TOC analyzer from an online sampling mode to processing several standard solutions automatically, and then returning the TOC analyzer to the online sampling mode.
[0025] Another object of the present invention is to provide a system of managing information for individual standards and sets of standards, and to minimize potential errors that might be introduced as a result of manual transcription of identification and other such information from labels on sample vials to written reports, analyzing standards that have expired, and/or analyzing vial sets in an improper sequence for a given protocol.
[0026] Still another object of this invention is to provide methods and related apparatus whereby a “grab” sample may be taken from any source for analysis, wherein such “grab” sampling is fully integrated with an automated standards sampling system for switching a TOC analyzer from an online sampling mode to processing several standard solutions automatically, and then returning the TOC analyzer to the online sampling mode.
[0027] Yet another object of this invention is to provide a keyed vial set assembly adapted to mate with the automated standards sampling apparatus of this invention whereby a physical feature of the “keyed” assembly, e.g., enlarged spacing between two adjacent vials (such as between the first and second vials) prevents mistakes such as inserting the vial set assembly backwards.
[0028] Still another object of this invention is to provide an automated valving system, preferably fabricated of substantially inert materials, to further eliminate or at least minimize introduction of contamination into the sampling systems of this invention.
[0029] These and other objects and advantages of this invention will be apparent from the following detailed description with reference to the attached drawings.
SUMMARY OF THE INVENTION
[0030] The automated standards sampling apparatus which is a preferred embodiment of the present invention comprises an integrated sampling system in combination with an online TOC analyzer. An external view of such a compact, integrated system is shown in FIG. 5 . As shown schematically in FIGS. 6 and 7 , individual vials can be sampled, or sets of vials that have been prepackaged and contain electronic information can be automatically sampled according to the System Suitability Test or another such sampling protocol. During manufacture of vial sets for use with the sampling system of this invention, multiple quality-assurance steps may be taken to ensure that the electronic data programmed into the memory storage system, for example an iButton®-based system or other non-volatile memory storage device, is accurate. The physical design of a preferred embodiment of a vial set for use in this invention is such that improper insertion of a standard vial by a user into the automated standards sampling apparatus of this invention is prevented.
[0031] In general, to perform a given protocol in accordance with this invention, a user directs the TOC analyzer to begin the desired testing protocol, and then the user inserts a suitable vial set into the associated sampling apparatus. No additional user interaction with the sampling apparatus is required. The analyzer and the automated standards sampling apparatus act in conceit to analyze each of die vials' contents, in the proper sequence, and while also ensuring vial viability, and then (if the system passes the testing protocol) to return to monitoring online liquid quality, if the user has selected that option beforehand. The user can also instinct the system to output a formal report of the test results) which explicitly lists the details of each of the standard vials that have been analyzed, including, for example, manufacturer's lot or batch designator, expiration date, vial contents and results of the analyses. After vial sampling is complete, the user should, at a convenient time, ordinarily remove the vial or vial set from connection to the sampling apparatus to limit the potential for biological growth to occur near the sampling needles.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] FIG. 1 is a schematic front view of a preferred embodiment of an automated standards sampling apparatus according to this invention showing the key functional components.
[0033] FIG. 2 is a schematic right-side view of the same assembly shown in FIG. 1 .
[0034] FIG. 3A schematically illustrates a preferred embodiment of a “keyed” vial set assembly (with enlarged spacing between the first and second vials of the set) according to this invention, this assembly being adapted for use with an automated standards sampling apparatus such as that shown in FIGS. 1 and 2 .
[0035] FIG. 3B schematically illustrates a bottom view of the vial set assembly seen in FIG. 3A specifically showing the piercable septum at one end of each standards vial.
[0036] FIG. 4 schematically illustrates a similar view of the vial set assembly as shown in FIG. 3A , but with the front portion of the vial set housing—for example, comprising two injection-molded (typically plastic) shells—removed to expose the interior region and to illustrate the upper ends of the several vials, how the vials engage with the housing, and the positioning of the memory storage device.
[0037] FIG. 5 schematically illustrates a preferred invention embodiment wherein an automated standards sampling apparatus 50 according to this invention is integrated with an online TOC analyzer 52 to form a compact analysis system as a single, easily transportable unit for use in an industrial manufacturing environment.
[0038] FIG. 6 is a schematic diagram representative of the fluidic circuit within an automated standards sampling apparatus according to this invention.
[0039] FIG. 7 is a schematic diagram representative of the electrical interconnections between components of an automated standards sampling apparatus according to this invention, and also between the automated standards sampling apparatus and an associated online TOC analyzer, for example as in the integrated analysis system unit shown in FIG. 5 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0040] FIG. 1 is a schematic front view of one preferred embodiment of an automated standards sampling apparatus according to this invention. The sampling apparatus as shown in FIG. 1 includes a vial set receiving structure 11 sized, shaped, spaced and oriented to receive a standards vial set as discussed hereinafter. In the embodiment illustrated in FIG. 1 , the vial set receiving structure comprises a plurality of interconnected, open-ended tubular elements or vial chambers (reference numeral 26 in FIG. 2 ), each for receiving a standards vial, oriented in a straight line and such that their respective central axes are substantially parallel.
[0041] The spacing between adjacent vial chambers of the vial set receiving structure is, preferably, not completely uniform. Thus, as seen in FIG. 1 , the spacing between the first (left end) vial chamber and the second vial chamber (second to left) is greater than the spacing between the second and the third vial chambers and also greater than the spacing between the third and the fourth (right end) vial chambers. This configuration of the vial chambers provides a physical “key” feature to insure that a vial set is correctly inserted into the vial set receiving structure.
[0042] The top ends of the vial chambers remain open to receive the plurality of vials that constitute a standards vial set. The number of vial chambers should be at least as great as the number of vials in a vial set intended for use with this apparatus. The bottom end of each vial chamber is fitted with a needle holder assembly 12 that holds a sample needle 18 and a vent needle 18 a in a coaxial configuration oriented substantially vertically and having a tip portion configured to pierce a piercable septum that seals an end of each standards vial, as discussed further hereinafter.
[0043] A contact element 10 , such as an electrical contact, designed to provide an interface with an electronic memory storage device or a comparable element having information perceiving, storage, and communicating capability, is also located in the vial set receiving structure as shown in FIG. 1 in the intentionally enlarged space between the first and second vial chambers. In a preferred invention embodiment, the a commercially available iButton® element, which would be incorporated into the standards vial set as described hereinafter.
[0044] Sample needle tubing 22 extends between a lower outlet end of each sample needle 18 and an inlet to a central or hub valve such as stream selection valve 14 . From stream selection valve 14 , a fluid sample is passed to the online sampling block 24 , as described further hereinafter.
[0045] FIG. 1 also shows an assembly 16 comprising an interface board, a single board computer, and an interface element connecting the interface board to the electronic memory storage device of a vial set assembly when the vial set assembly is positioned in the vial set receiving structure. The interface board facilitates downloading and decrypting relevant information from the vial set and communicating such information to the TOC analyzer, as hereinafter described.
[0046] The function of vial chamber drain 20 as shown in FIG. 1 is to pass any vial contents that might accidentally spill to a waste/drain connector 49 , as shown in FIG. 2 .
[0047] FIG. 2 is a schematic right-side view of the assembly shown in FIG. 1 , which shows the right-end vial chamber 26 (which receives the fourth of the four standards vials as shown in FIGS. 3A , 3 B and 4 ). FIG. 2 also better illustrates certain additional elements of the automated standards sampling apparatus of this invention. Thus, FIG. 2 shows the analyzer inlet line 34 , the waste line 32 for waste coming from the analyzer, and the vent drain connector 36 . Also seen in FIG. 2 is the (preferably magnetic) flow switch 38 , the flow-controlling needle valve 28 , the online sample inlet 30 , and the waste/drain connector 49 , the purposes and functions of which are explained hereinafter.
[0048] One or more assembled vial set(s) in accordance with this invention, such as that shown in FIGS. 3A , 3 B, and 4 , contains all of the standard solutions required to perform a given protocol—for example, a System Suitability Test. The standards vials are permanently contained in the vial set assembly 40 (comprising the vials and a vial set housing) to guarantee sequence integrity. All relevant information pertaining to each of the individual standards vials, and information pertaining to the set as a whole, is preferably stored on a suitable electronic memory storage device which is incorporated into the vial set assembly 40 . In alternative invention embodiments, however, other types of electronic and/or magnetic and/or light reading, coding, sensing or other information-perceiving and communicating systems, for example bar coding in combination with a bar code reader, could be substituted for the memory storage device in this invention. In one preferred embodiment of this invention, the memory storage device is a commercially available device which is known as an iButton®—a robust package containing non-volatile random access memory (NVRAM) which is manufactured by Dallas Semiconductor.
[0049] In another preferred embodiment of this invention, the vial set assembly 40 is “keyed” to the automated standards sampling apparatus by means of a physical feature, such as irregular spacing between the vials, to prevent an orientation or similar error during insertion of a vial set assembly into the sampling apparatus. For example, as shown in FIGS. 1 , 3 A, 3 B and 4 , the spacing between vials 1 and 2 can be made larger than the spacing between other adjacent vials to prevent accidentally inserting the vial set into the sampling apparatus backwards (i.e., with vial 4 in the position where vial 1 should be).
[0050] The iButton® memory storage device provides significant benefits for a user relative to the practice of this invention. It can be programmed to contain information about an entire Vial Set (e.g., the information shown below in Table 1) as well as information about each individual vial within the Vial Set (e.g., the information shown below in Table 2).
[0000]
TABLE 1
Vial Set Information
Part number.
The name of the vial set.
The expiration date for the vial set.
[0000]
TABLE 2
Individual Vial Information
Part number.
Lot number.
A field indicating the type of standard.
The expiration date for this particular vial.
The concentration of the solution in the vial.
[0051] When a vial set equipped with an electronic memory storage device, such as the iButton®, is inserted into an integrated analysis system in accordance with this invention, the analyzer unit of the system reads the information from the iButton® into the analyzer. This allows the analyzer to verify that the proper vial set has been installed for the selected protocol. It can also check the expiration date and can warn the user if any of the vials are beyond an expiration date. This checking/verification process prevents wasted time and money, which might otherwise occur if the wrong vial set were installed.
[0052] The information from the iButton® is stored with the results of the analysis in the analyzer. Subsequent reports from the analyzer can display the results and the information obtained from the iButton® This allows independent reviewers to verify that the proper standards were used in producing the data for the report. The data contained in the iButton® is encrypted so the analyzer can verify its validity. This system also provides a traceable link from the factory, to the analyzer, and finally to the report.
[0053] FIG. 6 is a schematic diagram that is representative of a fluidic circuit within an automated standards sampling apparatus according to this invention to show fluid flow pathways in greater detail than was possible in FIGS. 1 and 2 . FIG. 6 schematically illustrates four vial chambers 61 a , 61 b , 61 c and 61 d , which generally correspond to the vial chambers 26 in FIGS. 1 and 2 , except that FIG. 6 does not show irregular spacing between these chambers because such a physical “key” feature is not relevant to a fluid flow diagram.
[0054] Each of the vial chambers 61 a , 61 b , 61 c and 61 d has a coaxial sample and vent needle combination (generally corresponding to 18 / 18 a in FIG. 1 ), i.e., 62 a , 62 b , 62 c and 62 d , respectively, positioned centrally inside the vial chamber so as to pierce the piercable septum of the corresponding standards vial when a vial set assembly is put in place. Fluid sample lines 63 a , 63 b , 63 c and 63 d , respectively coming from needles 62 a , 62 b , 62 c and 62 d , connect respectively to one of the multiple fluid inlets of the stream selection valve ( 14 in FIG. 1 ). Fluid waste lines 64 a , 64 b , 64 c and 64 d , respectively coming from the bottoms of vial chambers 61 a , 61 b , 61 c and 61 d , connect with a drain chamber 25 located within or adjacent to the online sampling block ( 24 in FIG. 1 ); and, from drain chamber 25 the waste fluid is passed by a waste/drain connector 49 to a waste drain 27 . An online fluid line 15 a connects the stream selection valve 14 and the sampling block 24 . A sample fluid line 17 carries a fluid sample from the stream selection valve 14 to an inlet of an associated TOC analyzer (not shown in FIG. 6 ).
[0055] During ordinary operation, an online fluid sample is continuously withdrawn from a flowing stream of primary fluid, passed by means of an online sample inlet 65 through a filter 66 , into the online sampling block 24 , through a needle valve 28 within sampling block 24 , then to a flow controller or switch 38 . From flow controller 38 , the online-fluid sample is passed via line 15 a to stream selection valve 14 , and thence via line 17 to the TOC analyzer for continuous online monitoring of the primary fluid. Excess primary fluid (that not required by the TOC analyzer) flows through waste line 15 b to drain chamber 25 , and then through waste/drain connector 49 to waste drain 27 .
[0056] During a periodic calibration of the TOC analyzer, however, the online fluid sample is directed from flow controller 38 through waste line 15 b to drain chamber 25 instead of to stream selection valve 14 . During such a calibration or system suitability test, in place of the online fluid sample, standard samples are withdrawn sequentially from the set of standards vials positioned in the vial chambers 61 a , 61 b , 61 c and 61 d , and passed via stream selection valve 14 to the associated TOC analyzer. At the conclusion of such a calibration or system suitability test, the flow of online fluid sample from flow controller 38 to stream selection valve 14 is resumed. Using programmable software according to this invention, all of this sequence of steps can automatically be carried out on a regular basis, while simultaneously recording all pertinent information.
[0057] FIG. 7 is a schematic diagram that is representative of an electrical circuit interconnecting components of an automated standards sampling apparatus according to this invention to show electrical interconnections in greater detail than was possible in FIGS. 1 and 2 . FIG. 7 schematically illustrates the key electrical connections between various components of an automated standards sampling apparatus ( 50 in FIG. 5 ) of this invention, and also between the sampling apparatus 50 and an associated TOC analyzer ( 52 in FIG. 5 ).
[0058] As seen in FIG. 7 , a single board computer 71 is electrically connected by means of a communications bus 72 to an interface board 73 (in FIG. 1 , these three elements are combined in a single package identified by reference numeral 16 ). The interface board 73 includes electrical wires 73 a for establishing an electrical connection to the electrical contacts ( 10 in FIGS. 1 and 3A ) of an electronic memory storage device ( 44 in FIG. 4 ), preferably the iButton® contacts of an iButton® unit, when a vial set assembly including the memory storage device is positioned in the vial set receiving structure ( 11 in FIG. 1 ).
[0059] A second communications bus 74 electrically connects interface board 73 to stream selection valve ( 14 in FIG. 1 ), and a 24 VDC power line 75 also runs from interface board 73 to stream selection valve 14 . The sampling apparatus 50 as depicted in the electrical circuitry illustration of FIG. 7 further shows the flow controller or switch ( 38 in FIG. 6 ).
[0060] As shown in FIG. 7 , there are several electrical connections between the automated standards sampling apparatus 50 and the TOC analyzer 52 . A 24 VDC power line 78 a and a power-on signal line 78 b connect TOC analyzer 50 to interface board 73 . Additionally, switch cable line 76 connects flow switch 38 to TOC analyzer 50 . Also, an RS-232 cable 79 connects single board computer 71 and TOC analyzer 50 . A more detailed description of how these various elements cooperate appears hereinafter.
[0061] Thus, in a preferred invention embodiment, a single board computer (SBC) 71 , in combination with suitable software designed or adapted to perform the appropriate information reading/storage, sequencing and control operations, which is part of the automated standards sampling apparatus of this invention, is used to process communications between the analyzer 52 and the sampling apparatus 50 (for example, as illustrated by the electronic circuitry shown in FIG. 7 ). The SBC is responsive to RS-232 commands from the analyzer. The commands are converted to electrical signals and sent to the interface board 73 where they control the hardware components of the sampling apparatus. The SBC can read the iButton® information and command one or more valve/fluid flow control devices of the sampling apparatus, for example the stream selection valve 14 ( FIG. 1 ) to change to a new position. The stream selection valve 14 selects one of the sampling apparatus standards vials or the external water stream as the liquid source for the associated TOC analyzer. Designing customized software or adapting off-the-shelf software to perform the necessary information reading/storage, sequencing and control operations of this invention would be a matter of routine development work for one of ordinary skill in this field working with the teachings of this invention.
[0062] When the vial set is inserted into the vial chambers 26 ( FIG. 2 ), the iButton® makes electrical contact by means of an element known as a 1-wire interface to gold-coated, spring-loaded contacts 10 ( FIG. 1 ) that are wired to the interface board (as seen in FIG. 7 ). This electrical connection enables the TOC analyzer to download and decrypt all of the relevant information from the vial set, through the interface board and SBC 16 ( FIG. 1 ).
[0063] As the vials of vial set assembly 40 are inserted into the vial chambers 26 ( FIG. 2 ), sets of coaxial sample and vent needles 18 / 18 a ( FIG. 1 ) pierce the respective septa (as seen in FIG. 3B ) sealing the mouths of the several sample vials, thereby forming liquid-tight seals. Pump units within the TOC analyzer draw fluid from the particular vial selected by the position of the rotor in the stream selection valve 14 ( FIG. 1 ), via the sample needle associated with the particular vial. The vent needle associated with the particular vial allows the resulting vacuum within the vial to be relieved, via a conduit connecting to the vent drain connector 36 ( FIG. 2 ).
[0064] In the event that one or more of the sample vials' contents accidentally spill into the associated vial chamber 26 (which might occur, for example, if the user had inadvertently loosened one or more of the screw caps that seal the vials), then this fluid is directed through the vial chamber drain 20 ( FIG. 1 ), and it exits the system via the waste/drain connector 49 ( FIG. 2 ). This feature is also useful for draining any liquid that may get into the vial chamber 26 during the course of regular maintenance and cleaning.
[0065] During online analysis, sample liquid enters the online sampling block 24 ( FIG. 1 ) via the online sample inlet 30 ( FIG. 2 ). The total flow rate through the online sampling block 24 may be manually adjusted using the flow-controlling needle valve 28 ( FIG. 2 ) or a suitable flow control device. Downstream of valve 28 is a magnetic piston, which rises when liquid is flowing. The flow switch 38 ( FIG. 2 ) detects the presence of the piston in the raised position, indicating that sample liquid is flowing through the system, and this information is used by the TOC analyzer for the benefit of providing warnings as appropriate to the user.
[0066] Internal surfaces of the apparatus elements of this invention which come into contact with any sample prior to analysis, such as tubing and valving, are preferably fabricated of substantially inert materials to minimize contamination. For example, tubing, preferably stainless steel tubing, conducts sample liquid from the online sampling block 24 through the stream selection valve 14 and into the analyzer inlet 34 . Stainless steel is preferably selected as a material for fabricating tubing, valve components, and the like, for purposes of this invention, for its very low contribution of total organic carbon, inorganic carbon and conductive species to the sample liquid, which is important for accuracy when a TOC analyzer is to be used in highly sensitive and precise applications, for example in pharmaceutical water systems. Plastic tubing may be used, on the other hand, to conduct waste streams out of the system.
[0067] The stream selection valve 14 comprises one common port selectively connected to one of five inlet connections, thereby enabling the system to select either one of four sample vials or online liquid for analysis by the TOC analyzer. The valve 14 preferably uses materials selected for extremely low carbon contribution and conductive species contribution to the conducted water under operational wetted conditions.
[0068] In still another invention embodiment, it will be apparent to one skilled in this art that the methods and apparatus as described above (and as shown in the drawings) can also be readily adapted and utilized to periodically take a “grab” sample from any source for analysis instead of operating in the online analysis mode or the standards solution analysis mode.
[0069] The present invention has been described in detail with reference to preferred embodiments thereof, and although specific terms are employed in describing this invention, they are used and are to be interpreted in a generic and a descriptive sense only and not for purpose of limitation. Accordingly, it will be understood to those of ordinary skill in the art that various changes, substitutions and alterations in form and details may be made without departing from the spirit and scope of the present invention as set forth in the following claims.
[0070] Having described the invention, what is claimed is:
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An automated standards sampling apparatus ( 50 ) and method for using such, apparatus are described. The apparatus can be integrated with a liquid analyzer to form a compact, integrated liquid analysis unit. When used in combination with a specially adapted vial se of standard liquids, the apparatus provides a system for automated, substantially error-free periodic calibration and accuracy verification for an online TOC analyzer ( 52 ). The automated standards sampling apparatus of this invention facilitates the easy introduction of known concentrations of standard solutions and “grab” samples into online TOC analyzers to satisfy regulatory compliance, calibration, and validation requirements. The automated standards sampling apparatus of this invention also provides substantially improved reliability, higher productivity and better performance when running the critical and regulatory driven System Suitability Test than does any conventional sampling equipment, and it is likely to find wide use in a variety of industrial applications other than its principal intended use in the pharmaceutical industry.
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REFERENCE TO RELATED APPLICATION
[0001] The present application is a divisional of U.S. patent application Ser. No. 11/497,526, filed Aug. 2, 2006, pending, which claims the benefit of U.S. Provisional Application No. 60/704,453, filed Aug. 2, 2005, whose disclosure is hereby incorporated by reference in their entireties into the present disclosure.
FIELD OF INVENTION
[0002] The present invention relates to a cleaning, drying, coating, baking and etching apparatus for the “Flat Panel Display” (FPD) glass industry, architectural window elements, solar elements, as well as the precision panel substrate elements, film substrate industry, integrated circuit, and panel circuit boards of the semi-conductor industry, also as such other like devices and substrates arise, the usefulness of the present invention in those applications will be readily apparent.
DISCUSSION OF THE RELATED ART
[0003] In the FPD industry ever larger sheets of glass are being employed in the manufacture of Flat Panel Displays. The processing of these sheets is expensive in that their increasing size makes handling difficult regarding the brittle nature of the glass, due to its thin cross section—precluding anything but the gentlest method of transference. Because the required surface finish is intolerant of any type of defect or contamination manufacturers are increasingly moving towards non-contact conveyance of the panels in handling and processing in order to increase the yield rate. The manufacturing process of the substrate sheets of glass require many operations before they can be integrated with other components. In order for the substrates to perform properly, they must be processed to a high degree of accuracy. This would include cleaning from contamination, streaking and marks, drying, and either coating any number of different ways, or etching to induce desired patterning properties.
[0004] Because the handling and processing of FPD glass is so similar to wafers and circuit boards and other elements inherent in the semi-conductor industry, it is anticipated by the inventor that this method and/or apparatus and invention is directly transferable and translatable to the semiconductor industry and its attendant requirements of manufacturing production. Also the usefulness of the invention when processing flexible film substrates should be readily apparent.
[0005] Cleaning
[0006] In the process of cleaning substrates, traditionally the method utilized in the semi-conductor area, as well as the FPD industry—substrates are held in place while nozzles pass over the surface dispensing water in copious amounts with various cleaning solutions. The force of the cleaning solution spraying on the substrate is increased in order to attempt to use the viscous shear of the water due to its surface tension in order to loosen particles or contaminants adhered to the glass. The process of cleaning is open and dependant upon the level of cleanliness within the clean room, since any particles falling in the air will land and possibly mar the surface. Also, the cleaning solution can be sprayed and or applied via foam rollers which are also used to gently scrub the glass via contact. See U.S. Pat. No. 5,675,856 Itzkowitz, herein used as a reference. This induces errors into the glass surface, though small, due to its contact nature; however this is occasionally desirable due to the polishing effect thereby created. However, due to the atmosphere of the clean room having a very low level of humidity the process engenders streaking due to the cleaning solution drying on the glass surface prior to being rinsed, creating undesirable glass streaks and further issues with glass quality which degrade quality.
[0007] When cleaning semiconductor silicon wafers, a similar process is employed in that nozzles are passed over the substrate surface dispensing copious amount of water and cleaning solution in an effort to dislodge particulate contamination. However, since the wafers are round, the disc is spun, in order to create a centrifugal force and fling the water off the surface in an effort to use the viscous shear effect of the water on the substrate as it is forced to slide over the surface. This process also experiences the same elemental problems as the cleaning process described above, in that the clean room environment has very low humidity, causing quick drying and the creation of streaks on the substrate surface. Also, the water being flung off the surface of the wafers edge impinges the retaining wall of the wafer enclosure, atomizing the water droplets, and causing them to reattach to the wafer surface subsequently drying and causing water spots. This process of utilizing water essentially poured over the surface is not entirely efficacious, allowing streaks, spots and other visual defects to remain. This causes serious problems within the production framework, causing slowdowns and lost revenue due to production delays.
[0008] Etching
[0009] In the manufacture of precision tolerance substrates including the FPD glass industry as well as the semi-conductor industry the need arises to remove material and or to chemically change the surface quality or thickness of the substrate. The use of etchants of various sorts and types is a viable means of changing the substrate surface and or chemically removing material for thickness qualifications. The handling of chemicals is difficult since the substrates involved require careful support as well as the fact that etchants are chemically reactive and so often caustic and dangerous to administer and contain. Conventionally, the most useful method of applying etchings is by soaking the substrate in a container having an etchant and applying a force. There are inherent problems in this method in that the impurities within the etchant are allowed to remain on the surface of the substrate so that the surface of the substrate requires further remediation to correct what the etching process produces. A methodology to further improve upon this process is to set the substrate in a container having an etchant and then direct bubbles generated from an outside source onto the surface of the substrate that is immersed in the etchant, thereby using the force of the bubbles to clean and etch the surface of the substrate as in U.S. Pat. No. 6,281,136 B1 Kim enclosed herewith as reference. This process is time consuming and difficult to apply the bubbles evenly since there is no way to constrain the force of the bubbles uniformly, thereby the surface of the substrate is left with varying thicknesses which can cause further quality issues regarding the end product of the process.
[0010] Another problem inherent in the process of etching is the transference of the substrate into the tank with the etchant, the subsequent handling of the substrate and the etchant material, and the overall environment created with tanks, sprays and the necessary equipment required to process said steps effectively within the clean room environment.
[0011] Another method for Etching is the impingement of the substrate through some means as sand, glass beads or baking soda. This process engenders the need for further cleaning.
[0012] Drying & Baking
[0013] During a cleaning process involving water upon a substrate or device requiring such high tolerances as are required in the FPD and semiconductor industries the substrate will need to be dried. Critical to this process is no remaining moisture on the surface, and also to insure that there is no streaking and or impurities remaining on the surface of the substrate due to their presence in the cleaning solution which has then evaporated away, leaving them behind. Further, there are some processes within the aforementioned industries that require a baking process. This entails a higher order of heat and or application of radiant heat and light to enhance a process, or complete a curing of a coating, or similar elements.
[0014] Conventional drying for FPD glass involves heating and placing the substrate within a chamber and causing the substrate to dwell there, while a heat source is applied to remove any moisture. Problems associated with un-even heating arise in that if the heat source is not applied evenly to the substrate surface, warping and or variations in the surface quality can occur, as well as areas where there is more rapid evaporation of the rinse water from the cleaning process, leaving behind streaks and or water spots.
[0015] Still further, baking presents problems to the cleanliness of the clean room environment, since the presence of high heat sources can create unwanted particulate and contamination in clean room environments through the opening and closing of the chamber used to heat the substrates.
[0016] Within the semi-conductor industry discreet chambers are used where the wafers can be dried, or baked. The substrate must be moved to those chambers Likewise in the FPD market, drying is usually accomplished as part of the cleaning process in separate drying and baking chambers.
[0017] Coating
[0018] Various means of coating are employed in industry. A common method for coating is to pass the substrate beneath a curtain of material which deposits a material upon the substrate in an even thickness, or to have a type of “Shower head” which deposits an even layer of material on the substrate. This is unsatisfactory since the thickness of the coating and the processing parameters need to be controlled for precision applications, also since the size of the apparatus required for ever larger generations of glass is prohibitive, since such equipment must be operated in a clean room environment. Substrates can be dipped and or sprayed as well—neither of which is suitable for FPD glass, or semi-conductor industry products due to handling issues.
SUMMARY OF THE INVENTION
[0019] Accordingly, the present invention is directed to a method and apparatus utilizing the viscous shear force of aerostatic or hydrostatic fluids for cleaning, drying, baking, and etching glass substrate and semiconductor industry flat panel substrates that substantially obviates one or more of the problems due to limitations and disadvantages of the related art.
[0020] An object of the present invention is to provide a method and apparatus for cleaning, drying, coating, baking, and etching glass and semi-conductor substrates having a thin thickness and semi-uniform surface contained within an apparatus that allows for in-line processing and or controlled mini-environments for especially large panels.
[0021] Additional features and advantages of the invention will be set forth in the description which follows and in part will be apparent from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
[0022] Cleaning
[0023] In order to achieve these and other advantages and in accordance with the purpose of the present invention, in the preferred embodiment and broadly described, the apparatus for cleaning contains two horizontal inline and vertically opposed porous media air or fluid bearings, substantially wider and longer than the selected substrate, with a plurality of holes and gas passages through which air or fluid can be forced from behind the porous media from within the housing used to fixture the porous media, the porous media being sealed on its edges to maintain the fluidic pressure behind it, so that air or the desired fluid only flows through the porous media face. The method of constraining the substrate could possibly be achieved through the use of orifice, capillary, and step type bearings, using any number of different types of fluids.
[0024] Through another means, not here detailed, the FPD glass or such other substrate is propelled through the processes in such a manner that does not interfere with the various processes mentioned or interfere with the quality of said substrate in the final state of its manufactured embodiment.
[0025] The opposed bearings are situated each horizontally and vertically opposed to one another and parallel to one another in such a way so as to create a thin gap large enough to allow the substrate plate to pass between them. With the substrate inserted between the parallel porous bearings a thin gap is then created between the substrate and the porous media itself. Air or fluid, in this case air is forced from the porous media through a plurality of holes and impinges against and upon the substrate, from both opposing sides, causing the substrate to remain static between the two bearings in a non-contact disposition to the porous media. Should there be a displacement of the substrate, towards one or the other bearings—there is a natural equalizing force enacted, in that the gap that has grown larger now represents a lower pressure, consequently the gap that is now smaller creates a larger pressure, thereby forcing the substrate back into equilibrium. Since the pressure is then equal on both sides of the substrate, there is no deflection or danger of breaking the fragile substrate; however this pressure on the substrate is greater than atmospheric, causing air to flow out the thin gap between the substrate and porous media. This flow displaces loose particles and dust, and prevents further contamination from entering the area between the porous media.
[0026] Some distance into the apparatus, there are two sets of grooves recessed in the bearings perpendicular to the substrate motion and substantially spanning the full width of the substrate. The second set of grooves supplying a water or surfactant, solvent, de-ionized water, or some other such cleaning solution onto the substrate—with equal and opposed pressure to one another so that the pressure on the substrate is equal on both sides. These grooves act as hydrostatic bearings and operate on the cleaning solution itself insuring that the substrate is completely without contact except for the cleaning solution. The first set of grooves having a substantially lower pressure than the second set, causing the cleaning solution to be forced from the second groove back against the direction of the substrate motion into the first groove. Because the cleaning solution is being forced to flow along the substrate, in the opposite direction of substrate movement, through a very small cross section being formed by the distance between the substrate and the porous media, there is a substantial amount of force being applied to the surface of the substrate via the fluid. This substantial force uses the viscous shear of the cleaning solution and the high pressure gradients produced by the thin cross section of gap between the substrate and the porous media bearings to affect a cleaning action. Since the first groove has a substantially lower pressure than the second groove, the cleaning solution is completely evacuated by the substantially lower pressure groove, essentially removing the excess cleaning solution from the groove, and also the substrate. Very little actual cleaning solution is required and it is constrained by the seals formed via the porous media bearings, insuring that no particulation or contamination is allowed into the process from externally, as well as insuring that there is no leakage of cleaning solution or contaminates from within the cleaning apparatus to the clean room environment.
[0027] In another embodiment, an ultrasonic head can be mounted in-between the first axial groove, and the second. The land formed by the head of the ultrasonic cleaner will be immersed in the cleaning solution that is being forced from the second axial groove, back into the first. The water contact allows the ultrasonic head to induce a vibratory action that aides in the cleaning of particulate from the substrate surface. The head is completely enclosed, and in close contact, so along with the viscous shearing action of the cleaning solution the substrate, an ultrasonic wave form is emanated from the head in close proximity, focusing directly on the substrate surface, further aiding in the cleaning action.
[0028] A further embodiment is for the application of semi-conductor industry substrates, namely silicon wafers. The processes described for FPD glass are substantially similar to semi-conductor wafers. However wafers are traditionally circular in shape, which prove difficult to process across straight lands, and grooves. For that reason, a particular embodiment of the present invention entails creating a significantly curved series of grooves and lands, substantially similar to the radius of the wafer to be processed. In this way, the curved leading edge of the wafer will experience the forces inherent in the process simultaneously. It is perceived that this will accommodate the specific requirements of the wafer industry, and experimentation with various radii can be adapted to suit a viable process.
[0029] Still a another benefit to the described invention is the fact that the cleaning solution can be recycled, and re-used, saving money and time. However a further benefit is the fact that caustic cleaning agents and the like require local, state, and Federal monitoring and inventory, so that processors must give an account of the disposition of cleaning agents. With the current described process completely self contained, and all the cleaning agents accounted for, compliance with regulation is perceived by the inventor as significant improvement on the current art.
[0030] Drying
[0031] In another aspect to the cleaning process described above and substituting cleaning solution for hot air. The pre-heated dry air is forced to impinge upon the substrate, flowing towards the lower pressure axial groove previously illustrated. The flow of the heated dry air, or some other fluid or gas, is against the direction of the movement of the substrate, thereby utilizing the viscous shear of the fluid to effectively push any residue or moisture still remaining on the glass, from say, the cleaning process—back towards the lower ambient pressure axial groove. The process can be repeated as required within the apparatus to insure complete drying of the substrate.
[0032] Chemical Etching
[0033] In another aspect, utilizing the above process—a chemical caustic etchant material can be substituted for the cleaning solution. The size of the gap between the hydrostatic bearing, which is a bearing that can be used for fluid or for gas, and the glass can be modulated, and the pressure differential between the axial grooves can be adjusted to decrease or increase the flow rate of the etchant to achieve the desired chemical surface changes to the substrate. Depending on the particular type of etchant, and the desired through put of the apparatus, the length between the first and second axial grooves can be adjusted to allow for more contact time of the etchant and the substrate. There can also be modulated cleaning steps after the etchant has been supplied as desired. Nozzles can be strategically placed within the axial grooves in order to induce a pattern as may be desired.
[0034] The benefits of such a process are the etchant is kept contained within the apparatus, insuring that there is no caustic material leaked or spilled, fumes are contained, and a minimal amount of etchant is required in order to affect the same surface properties which previously required significant amounts of fluid to obtain. The cost savings is manifest in the attendant equipment, containment, and associated handling details being significantly reduced. Also, the amount of chemical etchant introduced into the process, and contained can be carefully monitored, the etchant being fully contained within the apparatus the reporting requirements of state, local and federal agencies can be more easily affected. The volume of etchant being carefully monitored, the material can be readily recycled and or filtered and cleaned in order to reduce the amount of etchant requiring replacement due to evaporation, or spillage and loss.
[0035] Coating
[0036] In another aspect, similar to the cleaning process described above and substituting a coating agent to be applied, panels can be accurately coated with minimal cost and tighter constraints on contaminants, as embodied in U.S. patent application Ser. Nos. 11/274,513—Devitt “Non-Contact Porous Air Bearing and Glass Flattening Device” and 60/625,583—Devitt “Non-Contact vacuum preloaded porous air bearings for creating conveyors to support, transport or process thin materials and work pieces used in manufacturing displays”
[0037] In this method the air supplied to the hydrostatic bearings is temperature-controlled in preparation for a coating supplied by an axial slit type applicator. The hydrostatic bearing on the top surface of the substrate is configured with numerous evenly placed holes along grooves longitudinally along the bearings, in the direction of the substrate processing direction. The holes supply a vacuum force which is substantially greater than the weight of the substrate, effectively pulling the glass against the hydrostatic bearing lands for a precise gap between the bearing and the substrate. This enables the substrate to be introduced to the slit coater with micron level precision in the distance to the slit coater. This distance from the substrate to the coating orifice is important with certain types of coatings and insures an accurate thickness layer is applied. After the coating head, there are no longer any vacuum grooves in the hydrostatic bearing which is holding the glass up against it; in fact the preferred embodiment is to have nothing near the substrate coating, so effectively a space is created within the apparatus, allowing the substrate coating to dry. The substrate is transported by a lower hydrostatic bearing which supports the substrate as it is “handed off” from the upper hydrostatic bearing, through the coater, then to be supported by the lower hydrostatic bearing. This allows the coating to dry properly as well as avoid transcription effects which can occur should there be any temperature variations on the surface of the substrate during and after the coating process. The apparatus could then conceivably incorporate various drying and baking or further etching elements in order to enhance the coating performance.
[0038] In still another embodiment, in an arrangement similar to the cleaning process, the substrate is constrained hydrostatically via the coating material to be applied with said coating material forced from a higher pressure groove between the gap in the substrate and porous material, against the direction of the substrate travel into a lower pressure groove. The thickness of the gap between the porous media and the substrate can be adjusted to modulate the allowable amount of coating to be applied to the substrate.
[0039] Baking
[0040] In yet another embodiment to the process similarly described above under Drying, there are no axial grooves in the hydrostatic bearings, merely a cutout similar to that described above in the application of coating utilizing Constant vapor deposition. However here there is simply a high heat source specifically for the purpose of baking the substrate, whether to cure a coating, prepare the substrate for some other process requiring high heat, or for further processes inherent in the manufacturing process. The high heat source can, as described above, be situated on both sides of the substrate—above and below, and can be of numerous different means, including but not limited to radiant heat, infra-red drying, and plasma radiation.
[0041] Combination of Stages
[0042] Within the manufacturing arena, floor space of machinery used to process the FPD sheets or substrates within a clean room environment is costly due to the necessary processes required in maintaining such an environment. Any way to minimize the amount of floor space required is advantageous. For this reason, a further aspect of the apparatus is the inline coordination and inclusion of each element described above, the resulting savings in floor space within the clean room environment is substantial thereby realizing a large cost savings. Also the process is internal to the apparatus realizing significant benefits for the prevention of contamination of the clean room from any attendant aspects of any of the processes, as each stage can be performed on the substrate immediately after the previous one, insuring no contamination of the substrate passing from one operation to another.
[0043] Prior to this invention each step is performed separately, within the particular process's own arena on the manufacturing line, thereby requiring significant floor space and the attendant conveyance equipment required to safely transport the substrate between the manufacturing processes. A further aspect of the preferred embodiment entails the processing of substrates and especially large substrates in processes as described above but in an immediately sequential fashion. This includes individually sequential ordering but also is to include simultaneous processing, so that a substrate conceivably could have the 5 (or more) processes, isolated from each other, being performed at once. Such improvements are perceived by its inventor as a significant enhancement in a growing industry which can potentially realize large cost savings while improving overall processes parameters at the same time. The process times may have to be harmonized and more substrate area may be required for exclusion zones but the advantages are still compelling.
[0044] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are intended to provide a further detailed explanation of the invention as claimed but do not constitute the entirety of potential embodiment.
BRIEF DESCRIPTION OF THE DRAWINGS
[0045] FIG. 1 is a schematic view of a cleaning/drying/etching operation showing the vertically opposed hydrostatic bearings, the substrate, and the attendant pressures from orifices.
[0046] FIG. 2 is a schematic view of a multiple of cleaning/drying/etching operation for a solid substrate showing the vertically opposed hydrostatic bearings, in an immediately sequential embodiment.
[0047] FIG. 3 is a schematic view of a flexible substrate or web of material, and the attendant pressures of areas within an apparatus, however the support apparatus is curved, and the substrate is a web of continuous material.
[0048] FIG. 4 is a schematic view of a flexible substrate or web of material in a cleaning/drying operation that is an immediately sequential embodiment and/or simultaneous.
[0049] FIG. 5 is a schematic view of a further embodiment of a flexible substrate or web of material in a cleaning/drying operation that is separate, yet immediately sequential and/or simultaneous.
[0050] FIG. 6 is a schematic view of a further embodiment of a flexible substrate or web material in a cleaning/drying/coating separate utilizing a minor array of axially placed grooves for treating the top and bottom surfaces of a moving web or flexible substrate simultaneously.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0051] As will be understood by those skilled in the art, the present invention may be embodied in other specific forms or configurations without departing from the essential characteristics or spirit and scope thereof. Accordingly, the foregoing description is intended to be illustrative, but not limiting, of the scope of the invention which is set forth in the following claims. Thus it is intended that the present invention cover the modifications and variations of this intention provided they come within the scope of the appended claims and their equivalents.
[0052] Cleaning—Flat Substrate
[0053] Referring to FIG. 1 an upper hydrostatic or aerostatic bearing 5 is vertically disposed opposite a lower hydrostatic bearing 4 between which is supported a glass or other type of substrate 3 . The bearing lands are charged with a fluid or air through passages 11 , 10 supplied in the apparatus housings 26 at a pressure of anywhere between a few inches of water (less than 1 Psi) to 1000's of pounds per square inch or Psi, but for this embodiment, roughly 30 Psi. The bearings 5 , 4 are so disposed around the substrate 3 in such a way as to form narrow gaps 25 , 24 which cause equal pressure build up from the bearings, displacing the substrate to a plane, or line that is approximately an equal distance between the two bearings, creating a non-contact situation. This equilibrium is maintained by the hydrostatic bearings 4 , 5 since if there is a displacement of substrate 3 downward, away from bearing 5 , the gap formed 24 between the substrate 3 and the bearing grows, hence there is a decrease in pressure since the fluid will escape via the easiest path which is now the larger gap. The corresponding decrease in gap 25 beneath substrate 3 causes an increase in pressure in the gap since there is less room for the air or gas to escape, thereby forcing the substrate 3 upwards. This in turn causes a type of equilibrium that is self stabilizing between the higher pressure bearing lands and the substrate 3 keeping gaps 24 , 25 even. This is well known in the art—see U.S. Pat. No. 5,104,237 Slocum. A set of low pressure grooves 6 , 7 are then axially displaced within the apparatus equally disposed on both sides of the substrate. These two grooves are at a substantially lower pressure, conducted by channels 12 , 13 , than the hydrostatic bearing pressure 11 , 10 , possibly even near vacuum, or at a few inches of water in measurable pressure. A middle land is then formed with hydrostatic bearings 9 , 8 which have significantly the same narrow gap as bearings 5 , 4 further indicated by 25 , 24 . The pressure supplied 14 , 15 to these two bearings, 9 , 8 can be lower, higher, or substantially the same as the pressures 11 , 10 found on the first two bearings, 5 , 4 , or in this embodiment, approximately 20 Psi. The relationship between hydrostatic bearings drop in output pressure in relation to input pressure is well known in the art. Hydrostatic bearings 9 & 8 in relation to the drop of input pressure via channels 14 , 15 as related to the pressure on the bearing surface, means the input pressure needs to be substantially higher than that which is seen on the surface of the bearing. The amount of restriction of the bearing material can be adjusted, as this translates directly to the amount of gap 24 , 25 between bearing surface 9 , 8 in relation to substrate 3 as a function of area and pressure. In order to obtain the desired functionality, this restriction in the bearing can be adjusted as needed at the time of apparatus manufacture. See U.S. Pat. No. 6,163,033 Smick. Further along the direction of substrate travel 27 , is a further set of axially disposed grooves 20 , 21 vertically oriented above one another. These grooves, 20 , 21 are pressurized via channels 16 , 17 without restriction in this example at a pressure of 20 Psi. Also within these grooves 20 , 21 a cleaning solution 22 , 23 is supplied through orifices 29 , 28 which feed into channels 16 , 17 and become entrained in fluid supplied to grooves 20 , 21 . The cleaning solution is forced out of grooves 20 , 21 at a pressure slightly higher than 20 Psi. Hydrostatic bearings 1 , 2 placed directly after grooves 20 , 21 in the direction 27 of substrate travel, are pressurized 18 , 19 at anywhere from 30 Psi or significantly higher than the pressure supplied 16 , 17 to grooves 20 , 21 . The subsequent pressure differential forces cleaning solution 22 , 23 against the direction 27 of the substrate, through the narrow gaps 31 , 30 created between the substrate 3 and hydrostatic bearings 8 , 9 , which can be fluid or gas in application. The viscosity of the cleaning solution acts in a shearing action and cleans the substrate 3 of contaminates. The cleaning solution 22 , 23 is then forced, via the pressure differential of lands 8 , 9 into the lower ambient grooves of 6 , 7 , urged by the low pressure from 12 , 13 conducted to the groove. The cleaning solution is then removed to a separate container (not shown) and filtered (not shown). The solution is kept within the apparatus, and contained. A solution may be introduced through 16 , 17 without modification or the additions from a duct like 28 , 29 . Successive cleaning stations can be instituted for different cleaning operations. Also surfactants, various solvents, and de-ionized water can be utilized. In another embodiment the cleaning solution can be supplied via bearings 8 , 9 creating effectively hydrostatic bearings. The solution 22 , 23 applying equal pressure on either side of the substrate 3 , effectively supporting said substrate in a non-contact orientation. The solution 22 , 23 is then forced against the direction 27 of the substrate 3 from the higher pressure of axially disposed grooves 20 , 21 via pressure supplied 16 , 17 which may in this instance be substantially greater than the pressure of the narrow gap 30 , 31 formed between hydrostatic bearing lands 8 , 9 . The solution 22 , 23 is forced along the substrate 3 under pressure, thereby scouring the surface of said substrate 3 and removing all debris, oils etc in a cleaning operation. The cleaning fluid 22 , 23 is then forced into axial groove 6 , 7 and removed via the low pressure ports 12 , 13 and then removed to a separate container (not shown) and filtered, recycled (not shown) or disposed of. The substrate 3 is then removed via support of hydrostatic bearings 1 , 2 which hold said substrate in a further non-contact orientation. Refer to U.S. Ser. No. 60/625,583—Devitt “Non-Contact vacuum preloaded porous air bearings for creating conveyors to support, transport or process thin materials and work pieces used in manufacturing displays”
[0054] In a further embodiment of FIG. 1 , an ultrasonic (<500 kHz) or megasonic (>500 kHz) head is mounted (not shown) substantially within bearings 9 , 8 (or grooves 20 , 21 ) which in this instance is being used as a hydrostatic bearing, with cleaning solution 22 , 23 or water being forced out of the bearing, and applying a force on substrate 3 . The megasonic cleaning head being recessed within the bearing land 8 , 9 or groove 6 , 7 and having its surface substantially co-linear and parallel to substrate 3 in the land, very close gaps are able to be maintained, in this instance, equal to thin gaps 24 , 25 . Since there is a cleaning fluid in-between bearing 8 , 9 and substrate 3 —the megasonic wave force is applied, both pulsed and continuous type, through the cleaning medium which in turn acts on substrate 3 , forming a wave (not shown) which when it impinges substrate 3 , forces the cleaning solution 22 , 23 to pull away from the surface, thereby forming extremely small cavitation bubbles, which burst causing the viscous force of the bubble to affect cleaning, thereby performing a further cleaning action on said substrate, as already known in the art. Since there is equal force applied from both sides to substrate 3 , said substrate remains in a non-contact orientation. In still a further embodiment, bearings 8 , 9 are not hydrostatic, but rather aerostatic, and the cleaning solution 22 , 23 is supplied via axial grooves 20 , 21 —and the ultrasonic heads mounted within bearings 8 , 9 come in contact with cleaning solution 22 , 23 and allow ultrasonic wave forms to be applied to the substrate 3 at a close distance, and safely in relation to the substrate.
[0055] A further embodiment of the cleaning method and apparatus constitutes a multiple stage 5 , or immediately successive and or simultaneous operations. FIG. 2 illustrates the above detailed and previously explained cleaning operation 9 , 8 on substrate 1 with an immediate and simultaneous drying, cleaning, etching, coating or any other type of action that benefits from a viscous shear type affect 20 , 25 performed on the same substrate 1 successively, or simultaneously as shown presently in much the same manner as described above in Cleaning, or some as yet invented method unknown presently in the art. The two processes are separated by hydrostatic bearings 14 , 15 maintaining gaps 3 , 4 between the substrate and bearing surfaces. The separation of the two processes 8 , 9 and 20 , 25 can be of any desired length, given the operating parameters required. Hydrostatic bearings 14 , 15 supplied by channels 13 , 12 generate sufficient pressure to prevent cleaning agent 10 , 11 from migrating in direction 2 of substrate travel into chambers 16 , 17 of the next operation—but instead to be driven by the lower ambient pressure of chambers 6 , 7 and evacuated via channels 30 , 31 . Throughout the two processes, the substrate 1 is maintained in a non-contact orientation maintaining gaps 3 , 4 between substrate 1 and the successive hydrostatic bearing lands. The substrate 1 is then conveyed via hydrostatic bearing lands 18 , 19 into axially displaced vertically disposed relative to one another, chambers 22 , 21 which supply the etchant, forced hot air, coating material etc via channels 26 , 27 at a pressure greater than that exists in the hydrostatic bearings 18 , 19 thereby forcing the second operation material 20 , 25 through the narrow gap 3 , 4 maintained between the substrate 1 and hydrostatic bearings 18 , 19 against substrate 1 direction 2 creating a viscous shear that acts on substrate 1 for a desired effect. Subsequently, hydrostatic bearings 24 , 23 supplied via channels 28 , 29 continue to maintain gap 3 , 4 with substrate 1 via a compatible fluid to the given application, whether it be air, hydrogen, etchant nitrogen, or cleaning fluid. The substrate 1 can then be conveyed into a further operation (not shown) or out of the machine as a finished piece. The substrate can then be successively rinsed via the same method within the apparatus either simultaneously via further axial grooves in a similar manner, or within a further apparatus (not shown in Fig.).
[0056] Drying—Flat Substrate
[0057] In the application of drying a substrate, a similar embodiment to the cleaning operation described above, is utilized as in FIG. 1 . The substrate 3 passes between a hydrostatic bearing 5 which is vertically disposed opposite a lower hydrostatic bearing 4 between which is carried a glass or other type of substrate 3 . The bearings are charged with a gas or air through grooves 11 , 10 supplied in the apparatus housing 26 at a pressure of roughly 30 pounds per square inch, or Psi. The bearings 5 , 4 are so disposed around the substrate 3 in such a way as to form narrow gaps 25 , 24 which create equal pressure build up from the bearings, displacing the substrate into the center of the two bearing lands, creating a non-contact situation, as described above. A set of pressure grooves 6 , 7 are then axially displaced within the apparatus equally disposed on both sides of the substrate. These two grooves are at a substantially lower pressure 12 , 13 than the hydrostatic bearing pressure 11 , 10 , possibly even vacuum. A middle land is then formed with hydrostatic bearings 9 , 8 which have significantly the same or slightly larger narrow gap as bearings 5 , 4 further indicated by 25 , 24 . The pressure supplied 14 , 15 to these two bearings, 9 , 8 may be moderately lower than the pressures 11 , 10 found on the first two bearings, 5 , 4 approximately 20 Psi. Further along the direction of substrate travel 27 , are a further set of axially disposed grooves 20 , 21 vertically oriented above one another. These grooves, 20 , 21 are pressurized via channels 16 , 17 at a pressure of 20 Psi. Also within these grooves 20 , 21 a medium which may be heated 22 , 23 is supplied through orifices 16 , 17 and/or 29 , 28 which are placed along the grooves (not shown). The heated, or dry air is forced out of grooves 20 , 21 at a pressure slightly higher than 20 Psi. Hydrostatic bearings 1 , 2 placed directly after grooves 20 , 21 in the direction 27 of substrate travel, are pressurized 18 , 19 at or significantly higher than the pressure supplied 16 , 17 to grooves 20 , 21 . The subsequent pressure differential forces the heated and dry air 22 , 23 against the direction 27 of the substrate, through the narrow gaps 31 , 30 created between the substrate 3 and hydrostatic bearings 8 , 9 . The force of the heated dry air 22 , 23 being forced between thin gap 30 , 31 acts in a shearing action and cleans the substrate 3 of water or cleaning fluid remaining from a previous cleaning operation (not shown in this embodiment) drying the glass. The heated dry air 22 , 23 is then forced, via the pressure differential of lands 8 , 9 into the lower ambient grooves of 6 , 7 , urged by the low pressure 12 , 13 of the groove. The heated dry air is then removed possibly to a separate filter (not shown) and vented (not shown) in an appropriate manner. The heated exhaust can be kept within the apparatus, thereby maintaining clean room environment integrity and the effluent contained. Successive drying stations can be instituted for different drying operations. In yet another embodiment the drying operation can be supplied via bearings 8 , 9 creating effective hydrostatic bearings. The heated fluid, namely air, but possibly other fluid types, 22 , 23 applying equal pressure on either side of the substrate 3 , effectively supporting said substrate in a non-contact orientation. The heated dry air 22 , 23 is then forced against the direction 27 of the substrate 3 from the higher pressure of axially disposed grooves 20 , 21 via pressure supplied 16 , 17 which may in this instance be substantially greater than the pressure of the narrow gap 30 , 31 formed between hydrostatic bearing lands 8 , 9 which is typically 50% of input pressure. The heated dry air 22 , 23 is forced along the substrate 3 under pressure, thereby fully removing from the surface of said substrate 3 all moisture or liquid fluids. The heated dry air 22 , 23 is then forced into axial groove 6 , 7 and removed via the low pressure ports 12 , 13 and then removed to a separate container (not shown) and possibly vented. The substrate 3 is then removed via support hydrostatic bearings 1 , 2 which hold said substrate in a further non-contact orientation. After being cleaned and dried, the substrate 3 is maintained in a non-contact orientation allowing it to remain free from contaminates, foreign debris, and or marks from handling. Additional grooves may be employed to improve the drying action.
[0058] Etching—Flat Substrate
[0059] In still another embodiment, using FIG. 1 utilizing the now described cleaning/drying method; chemical etchant is substituted for the cleaning solution/heated dry air 22 , 23 . The etchant is kept contained, evacuated from the apparatus through chambers 6 , 7 under lower pressure 12 , 13 and contained in an apparatus (not shown) to be filtered, re-charged, and possibly re-utilized within the apparatus, saving etchant and allowing the apparatus to operate safely within a clean room environment. Still another detail within this embodiment is that the chemical etchant solution or gas can be supplied via bearings 8 , 9 creating effective hydrostatic bearings. The chemical etchant solution 22 , 23 applying equal pressure on either side of the substrate 3 , effectively supports said substrate in a non-contact orientation. The solution or gas 22 , 23 is then forced against the direction 27 of the substrate 3 from the higher pressure of axially disposed grooves 20 , 21 via pressure supplied 16 , 17 which may in this instance be substantially greater than the pressure of the narrow gap 30 , 31 formed between hydrostatic bearing lands 8 , 9 . The solution or gas 22 , 23 is forced along the substrate 3 under pressure, thereby scouring the surface of said substrate 3 and chemically modifying the surface of the substrate 3 as is desired for specific manufacturing processes. The hydrostatic bearing lands 8 , 9 can be so situated to be modified vertically relative to one another and to substrate 3 , thereby changing the gap created 30 , 31 between the hydrostatic bearings 8 , 9 and the substrate 3 itself, allowing modulation of the pressure created between the lands 8 , 9 and the substrate 3 , as is desirable within the chemical etching process. The speed with which the substrate 3 is moved through apparatus 26 can be modulated as well, in order effect the desired chemical etching process. Subsequently the chemical etching fluid or gas 22 , 23 is then forced into axial groove 6 , 7 and removed via the low pressure ports 12 , 13 and then removed to a separate container (not shown) and filtered (not shown). It is possible that multiple or additional lands and grooves could help isolate different processes and may be added as needed, or they may be employed for multiple and immediately sequential processes as shown in FIG. 2 . The substrate 3 is then removed via support hydrostatic bearings 1 , 2 which hold said substrate in a further non-contact orientation to insure proper process parameter remain valid. The substrate 3 can then be moved to further cleaning/drying/baking/CVD/PVD operations.
[0060] Cleaning—Flexible Substrate.
[0061] In a further embodiment, utilizing FIG. 3 , similar to the above described cleaning process, a flexible substrate 3 is fed into a gap between curved hydrostatic bearings 4 , 5 . The web is carried via the impingement of air or fluid upon the web via a porous media in the bearing in which 60 Psi of air or other gas or fluid 7 so that there is no contact between the web substrate 3 and the bearings 4 . The web 3 is constrained on its other surface through an hydrostatic bearing 5 under a pressure of 60 Psi via internal grooves 6 within apparatus 17 , so that there is no contact with web substrate 3 and bearing 5 , leaving a thin gap 1 between the web and the hydrostatic bearing. Bearing 5 is curved in a way to match the radius of bearing 4 , forming an annulus so that thin gap 1 remains substantially consistent traversing the face of bearing 5 . A similar gap 2 is formed between the web and the curved hydrostatic bearing 4 , and it is likewise substantially maintained through the radius of bearing 4 , forming an annulus so that thin gap 1 remains substantially consistent traversing the face of bearing 4 . Immediately adjacent to hydrostatic bearing 5 , in the direction of web travel 18 , is an axial groove 8 which is under vacuum or near 0 Psi via a channel 9 connected to some type of vacuum producing device (not shown). Immediately adjacent to channel 9 , in the direction of web substrate 3 travel 18 is a hydrostatic bearing 10 fed through a channel 11 in the apparatus 17 with 20 Psi. This bearing 10 is substantially curved to match the surface of the web substrate 3 which is riding on curved bearing 4 , so much so that thin gaps 1 , 2 remain substantially consistent. Immediately adjacent to hydrostatic bearing 10 , in the direction of web substrate travel 18 is axial groove 12 . This groove 12 is pressurized via tube 13 with 20 Psi. Immediately adjacent to groove 12 in the direction of web substrate travel 18 is hydrostatic bearing 15 , pressurized by tube 16 with 60 Psi. Bearing 15 is substantially curved to match the surface of the web substrate 3 which is riding on curved bearing 4 , so much so that thin gaps 1 , 2 remain substantially consistent.
[0062] In the cleaning application, groove 12 is pressurized via channels 13 at a pressure of 20 Psi. Also within these grooves 12 a cleaning solution 14 is supplied through orifices which are axially placed along the width of the groove 12 (not shown). The cleaning solution is forced out of grooves 12 at a pressure slightly higher than 20 Psi. Hydrostatic bearing 10 placed directly after groove 12 in the direction 27 of substrate travel, are pressurized 16 at 60 Psi or significantly higher than the pressure supplied 13 to groove 12 . The subsequent pressure differential forces cleaning solution 14 against the direction 18 of the substrate, through the narrow gaps 1 , 2 created between the substrate 3 and hydrostatic bearing 10 The viscosity of the cleaning solution acts in a shearing action and cleans the substrate 3 of contaminates. The cleaning solution 14 is then forced, via the pressure differential of land 10 into the lower ambient groove of 8 , urged by the low pressure 9 of the groove. The cleaning solution is then removed to a separate container (not shown) and filtered (not shown). The solution is kept within the apparatus, and contained. Successive cleaning stations can be instituted for different cleaning operations. Also surfactants, various solvents, and de-ionized water can be utilized. In another embodiment the cleaning solution can be supplied via bearing 10 and passage 11 creating effective hydrostatic bearings. The solution 14 applying equal pressure on the top side of the substrate 3 , effectively supported via bearing 4 with an equal pressure in a non-contact orientation. The solution 14 is then forced against the direction 18 of the substrate 3 from the higher pressure of axially disposed groove 12 via pressure supplied 13 which may in this instance be substantially greater than the pressure of the narrow gap 1 , 2 formed between hydrostatic bearing lands 10 , 4 and web substrate 3 . The solution 14 is forced along the substrate 3 under pressure, thereby scouring the surface of said substrate 3 and removing all debris, oils etc in a cleaning operation. The cleaning fluid 14 is then forced into axial groove 8 and removed via the low pressure port 9 and then removed to a separate container (not shown) and filtered (not shown). The substrate 3 is then removed via support hydrostatic bearings 4 , 15 which hold said substrate in a further non-contact orientation, until it can be led to another process, stage, or further bearing apparatus. The web substrate can then be led to another non-contact web apparatus which is oriented in a minor fashion, and the opposite side of the web can be treated. One skilled in the art can easily imagine complimentary lands and groove in the outer diameter of four exactly opposite embodiments, as noted in the Rigid embodiment.
[0063] In a further embodiment of FIG. 3 , an ultrasonic (<500 kHz) or megasonic (>500 kHz) head is mounted (not shown) substantially recessed within bearing 10 which in this instance is being used as a hydrostatic bearing, with cleaning solution 14 or water being forced out of the bearing, and applying a force on substrate 3 . The ultrasonic cleaning head being recessed within the bearing 10 and having its surface co-linear and substantially curved to match the surface of the web substrate 3 which is riding on curved bearing 4 , so much so that an annulus is formed, and thin gaps 1 , 2 remain substantially consistent in relation to substrate 3 . Since there is a cleaning fluid in-between bearing 10 and substrate 3 —the ultrasonic wave force is applied, both pulsed and continuous type, acting through the cleaning medium which in turn acts on substrate 3 , thereby forming a wave (not shown) which when it impinges substrate 3 , forces the cleaning solution 14 to pull away from the surface, thereby forming extremely small cavitation bubbles, which burst causing the viscous force of the bubble to affect cleaning (as known in the art), performing a further cleaning action to said substrate surface. Since there is equal force applied from both sides to substrate 3 , said substrate remains in a non-contact orientation. In still a further embodiment, bearings 10 are not hydrostatic, but rather aerostatic, and the cleaning solution 14 is supplied via axial grooves 12 , 8 —and the ultrasonic head mounted within bearings 10 comes in contact with cleaning solution 14 and allow ultrasonic wave forms to be applied to the substrate 3 . As noted in the Rigid substrate type embodiment, a further cleaning apparatus can be situated in mirror arrangements, so as to treat the other side of flexible web substrate 3 .
[0064] Drying—Flexible Substrate
[0065] In yet another embodiment referencing FIG. 3 , forced hot air can be substituted for the cleaning solution 14 . In the drying application, groove 12 is pressurized via channels 13 at a pressure of 20 Psi. Also within the groove 12 a heated dry stream of air 14 or some other gas, such as carbon dioxide, nitrogen, etc heated via numerous different means not here detailed, is supplied through orifices which are axially placed along the width of the groove 12 (not shown). The heated dry air is forced out of groove 12 at a pressure slightly higher than 20 Psi. Hydrostatic bearing 10 placed directly after groove 12 in the direction 27 of substrate travel, is pressurized 16 at 60 Psi or significantly higher than the pressure supplied 13 to groove 12 . The subsequent pressure differential forces heated dry air 14 against the direction 18 of the substrate, through the narrow gaps 1 , 2 created between the substrate 3 and hydrostatic bearing 10 The force of the pressure differential forces the heated dry air to act in a shearing action and cleans the substrate 3 of contaminates. The cleaning solution 14 is then forced, via the pressure differential of land 10 into the lower ambient groove of 8 , urged by the low pressure 9 of the groove. The heated dry air is then removed via venting external to the apparatus 17 or to some other desired location (not shown). The heated dry air is retained within the apparatus, and contained, preventing moisture or humid air from escaping the apparatus 17 and potentially contaminating a clean room environment. Successive drying stations can be instituted for different drying operations. In another embodiment the heated dry air can be supplied via bearing 10 and passage 11 creating a further drying condition. The heated dry air 14 applying equal pressure on the top side of the substrate 3 effectively supported via bearing 4 with an equal pressure in a non-contact orientation. The heated dry air 14 is then forced against the direction 18 of the substrate 3 from the higher pressure of axially disposed groove 12 via pressure supplied 13 which may in this instance be substantially greater than the pressure of the narrow gap 1 , 2 formed between bearing lands 10 , 4 and web substrate 3 . The heated dry air 14 is then forced along the substrate 3 under pressure, thereby scouring the surface of said substrate 3 and removing all liquid in a drying operation. The heated dry air 14 is then forced into axial groove 8 and removed via the low pressure port 9 and vented (not shown). The substrate 3 is then removed via support hydrostatic bearings 4 , 15 which hold said substrate in a further non-contact orientation, until it can be led to another process, stage, or further bearing apparatus. It should be noted that the drying operation can occur without the use of heat, simply the shearing force of air applied against the substrate, as it transitions the narrow gaps of the bearing lands. The web substrate can then be led to another non-contact web apparatus which is oriented in a minor fashion, and the opposite side of the web can be treated if required.
[0066] Etching—Flexible Substrates
[0067] In still another embodiment, using FIG. 3 utilizing the now described cleaning/drying method; chemical etchant is substituted for the cleaning solution/dry air 14 . The etchant is kept contained, evacuated from the apparatus through chambers 8 under lower pressure 9 and contained in an apparatus (not shown) to be filtered, re-charged, and possibly re-utilized within the apparatus, saving etchant and allowing the apparatus to operate safely within a clean room environment. Also, the etchant is able to be tracked as far as its disposition to comply with various State, Local and Federal regulations. Still another detail within this embodiment is that the chemical etchant solution can be supplied via bearing 10 and 4 creating an effective hydrostatic bearing. The chemical etchant solution 14 applying pressure on the top side of the substrate 3 , is effectively matched via hydrostatic bearing 4 supporting said substrate in a non-contact orientation. The solution 14 is then forced against the direction 18 of the substrate 3 from the higher pressure of axially disposed groove 12 via pressure supplied 13 which may in this instance be substantially greater than the pressure of the narrow gap 1 , 2 formed between hydrostatic bearing lands 10 , 4 . The solution 14 is forced along the substrate 3 under pressure, thereby scouring the surface of said substrate 3 and chemically modifying the surface of the substrate 3 as is desired for a given manufacturing processes. The now hydrostatic bearing land 10 can be so situated to be modified vertically relative to bearing 4 and to substrate 3 , thereby changing the gap created 1 , 2 between the hydrostatic bearings 10 , 4 and the substrate 3 itself, allowing modulation of the pressure created between the lands 10 , 4 and the substrate 3 , as is desirable within the chemical etching process. The speed with which the substrate 3 is moved through apparatus 26 can be modulated as well, in order effect the desired chemical etching process. Subsequently the chemical etching fluid 14 is then forced into axial groove 8 and removed via the low pressure port 9 and then removed to a separate container (not shown) and filtered (not shown). The substrate 3 is then removed via support hydrostatic bearings 15 , 4 which hold said substrate in a further non-contact orientation to insure proper process parameters remain valid. The substrate 3 can then be moved to further cleaning/drying/baking/CVD operations, successively, sequentially or independently, as is desired for a given process.
[0068] Combination of Stages—Flexible Substrates
[0069] As can be seen by FIG. 4 a multi stage process method and is incorporated into the previously described Flexible Substrate—cleaning embodiment detailed above into apparatus 11 . Substrate web 1 traveling in direction 2 is born via hydrostatic bearing 3 creating gaps 4 , 5 which are consistently maintained throughout the course of the substrates processing, remaining non contact and substantially uniform in height in relation to other bearings and lands. The substrate is constrained via hydrostatic bearing 6 and conveyed into chamber 7 where cleaning, etching, baking, drying operation 8 is performed via the narrow gap formed by substrate 1 and bearing land 9 , while material 8 is forced in the opposite direction of substrate 1 travel 2 , via pressure from chamber 12 while supplied via channel 10 with either the cleaning solution, etchant, etc. Further in direction of substrate 1 travel 2 is a hydrostatic bearing 13 land, immediately positioned next to chamber 12 supplied via channel 14 at a pressure that is greater than that supplied to chamber 12 , insuring that there is no transcription, or transference of material 8 in the direction of substrate 1 travel 2 . This higher pressure, possibly 60 Psi, but conceivable higher, or lower as required for a given process creates a seal all while maintaining gap 4 between the substrate 1 and bearing land 13 . Immediately sequential, but possibly further along in direction of substrate 1 travel 2 is another axial disposed chamber, or groove, or feature, in which a second operation is performed on the same web of substrate 1 . The operation 15 can be further cleaning, etching, baking, coating, drying, or any other conceivable process, embodied in the same manner as previously described, via hydrostatic bearing 18 constraining substrate 1 and forming a narrow gap 4 in which material 15 is forced opposite to substrate 1 travel 2 utilizing the viscous shear affect in a thing gap cross section, while maintaining a non-contact orientation of substrate 1 . Chamber 20 being at a lower pressure than chamber 19 , as has been previously described, above.
[0070] FIG. 5 , Flexible Substrate—cleaning, 2 is coupled simultaneously with Coating—Flexible substrates 5 , upon the same web of flexible substrate 4 . The cleaning process 3 is followed immediately after with the drying process 6 on the substrate 4 in direction 1 . As may be deduced from the art any type of process may be substituted for the drying 6 process, such as etching, coating, baking, or even further cleaning. As should be apparent to one skilled in the art, multiple stages of various different processes may be utilized in the present disclosure simultaneously, or independently, or in multiple configurations for the purpose of manufacturing flexible web utilizing cleaning, etching, drying, baking, coating etc. It may also be readily observed that the patentee desires to anticipate further developments in the art of flexible substrates that are currently not invented, and should be considered as a possible further manufacturing or processing step by those familiar with the art regarding the proposed apparatus and or method in simultaneous fashion or successively, as well as in this patent regarding successive and simultaneous processing of flexible substrates through gaps employing the viscous shear affect of the various fluids used in the process.
[0071] In FIG. 6 , a minor type arrangement is detailed showing a viscous shear fluid 7 being exerted on the underside of flexible substrate or web 3 simultaneously as a fluid 14 , heated air, cleaning fluid, etc. is being exerted on the top surface of flexible substrate 3 . Hydrostatic bearing lands 10 , 23 maintain the substrate 3 in equilibrium through precise control of pressure via channels 11 , 22 , with fluids 14 , 7 evacuated via the now described lower pressure axial chambers 8 , 20 . The substrate is then contained and further carried via hydrostatic lands 5 , 4 . As has been described previously, numerous fluid, heating, cleaning combinations may be performed via this embodiment.
[0072] Summation
[0073] It will be readily apparent to those skilled in the art that various modifications and variations can be made in the apparatus for cleaning, drying, baking, and etching glass substrate and semi-conductor industry wafers of the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention cover the modifications and variations possible of this invention in method and or apparatus provided they come within the scope of the claims and appended claims and their equivalents.
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A method and apparatus for cleaning, drying, coating, baking etching and deposition of surfaces on glass substrate as it transitions thru and between small gaps between hydro-static porous media bearings. Due to the non-contact nature of the device extremely high pressures can be induced upon the work piece through various fluids without damage to the substrate, allowing the system to utilize the viscous nature of fluids to accomplish the desired cleaning, drying, coating, etching or baking. The process also allows for simultaneous and immediately sequential ordering of processes.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present patent application claims the benefits of priority of U.S. patent application Ser. No. 13/750,881, entitled “CANNULATED TELESCOPIC FEMORAL NECK SCREW DEVICE AND RELATED FIXATION METHOD” and filed at the United States Patent and Trademark Office on Jan. 25, 2013.
FIELD
[0002] The present document generally relates to a screw assembly system and method for the fixation of fractures along the femoral neck, and in particular to an improved cannulated bone screw assembly that enables the implant to be used for the fixation of bone fractures through the physeal plate (growth plate).
BACKGROUND
[0003] Cannulated screws have been used for internal fracture fixation, and a single screw placement through the femoral neck has become the preferred treatment for fractures through the physeal plate. Fractures through the physeal plate are more commonly referred to as Slipped Capital Femoral Epiphysis.
[0004] Generally, such a fixation device comprises a hollow shaft having a predetermined cross-section and provided with threaded sections beginning at the medial end of the device spanning a predetermined length of the shaft. The fixation device is placed parallel to the neck of the femur and secures the fracture with compressive force applied by the spherical lateral screw head at the lateral cortex. The prior art typically describes a variety of screw systems comprising different shaft diameters, shaft lengths, thread pitches and thread lengths in order to offer a fixation device for all possible locations and extents of the fracture sites. The general configuration of cannulated screws is well illustrated in U.S. Pat. No. 7,207,994. Such described screws are non self-adjustable in length and, therefore incapable of providing a surgical fixation to stabilize fractured bones during the healing process without disrupting the normal bone growth particularly in pediatric patients.
[0005] In another example described in U.S. Published Patent Application No. 20070260248, an adjustable feature is incorporated into the screw allowing extension of the shaft length along a predetermined range. The screw has an outer member and an inner member connected together by a spring-like component. Once the shaft length is selected and the device is stabilized in said position, the device is inserted into the prepared canal of the femoral neck to fixate the bone segments, just as previously described for cannulated screws, in order to promote healing.
[0006] Other prior art include an intramedullary nail described as an adjustable solution for long bone fixation in U.S. Pat. No. 6,524,313. However, no prior art device has shown adjustable screw solutions for this regard. Therefore, there is a need in the art for an extendable screw system for surgical fixation of femoral neck fractures in pediatric patients.
[0007] Given the present design of cannulated screws used for the fixation of femoral neck fractures, including Slipped Capital Femoral Epiphysis, the compressive loads created by the medially threaded shafts and the lateral spherical screw heads inhibit the normal growth in young patients. Premature closure of the physeal plate is a reoccurring condition widely documented in the literature as a result of pinning and fixation via cannulated screws. Telescoping devices such as the Fassier-Duval Intramedullary Nail, whose fixation features do not thread into the physeal plate, have shown successful internal fixation of fractures and osteotomies in long bones without compromising the integrity of the physeal plate and thus allowing the continuation of normal patient growth.
SUMMARY
[0008] In one aspect, a cannulated screw assembly is provided that is self-extendable in length for surgical fixation of fractured femoral necks or slipped femoral epiphysis in a young patient.
[0009] In another aspect, a cannulated screw assembly is provided which requires minimally invasive instrumentation and a relatively straightforward surgical technique.
[0010] Hence, in accordance with one aspect of the screw assembly, a screw assembly for fixation of femoral neck fractures may include a telescopic assembly having two opposed ends and including a male component and a female component. The interconnected components permit axial movement of each end relative to each other. Anchorage of the female and male components is achieved through screw-type fixation of each end of the telescoping screw to the lateral cortex of the femur and the head of the femur. The smooth shaft design and lack of compression element allow free longitudinal extension of the length of the screw so that the screw is extendable as the bone heals and normal patient growth occurs.
[0011] According to one embodiment of the screw assembly with a beveled head design, the screw assembly is provided with an elongated tube having one end formed with an external self-tapping thread that has a diameter greater than the external diameter of the tube, and a cannulated rod having one end formed with an external self-tapping thread as large as the external diameter of the tube. The cannulated rod is adapted for insertion through a drilled canal into the bone until the self-tapping end is anchored in the medial end of bone (the epiphysis of the femoral head) and the rod spans the fracture site. The elongated tube is adapted for insertion into the bone, over the cannulated rod, until the external fixation thread at the lateral end of the tube is anchored within the lateral cortex of the bone. The screw assembly creates a stable fixation and inhibits radial displacements of the fractured segments of the bone while permitting longitudinal extendibility as the bone structures heals and normal patient growth occurs.
[0012] This embodiment of the screw assembly provides a relatively easy method of implantation because anchorage of the screw assembly is as would be anchorage of a single cannulated screw, wherein the action is achieved through rotating the respective rod and tube components until the threads anchor in the bone structures with the use of detachable driving tools. The position of the screw assembly is final when beveled head is parallel to surface of the lateral cortex.
[0013] According to another embodiment with a triblobe design, the screw assembly is provided with a male component with an elongated rod having one end formed with an external self-tapping thread that has a diameter greater than the external diameter of the tube, and a female component having one end formed with an external self-tapping thread that is the same diameter as the tube. The female component is adapted to be inserted through a drilled canal into the bone until the self-tapping end is anchored in the medial end of bone (the epiphysis of the femoral head) and the rod spans the fracture site. The male component is adapted to be inserted into the bone, inside the female component, until the external fixation thread at the lateral end of the rod is anchored within the lateral cortex of the bone.
[0014] An additional characteristic of this embodiment is to provide a cannulated screw assembly for surgical fixation of fractures bones which prevents rotational instability of the femoral epiphysis by preventing the rotation of the male and female components along the central axis. Rotation is hindered by interlocking of a non-circular feature (e.g. one or more flat surfaces, trilobe, cloverleaf, etc.) on the outer surface of the male component and the inner surface of the female component. The male component must be placed into the female component according to the specific mating pattern dictated by the interlocking feature on the components of the assembly. The screw assembly inhibits both radial displacements of the fractured segments of the bone and axial rotation of the segments around the axis of the screw assembly, while permitting longitudinal extendibility as the bone structures heal and normal patient growth occurs.
[0015] Moreover, the screw assembly provides a relatively easy method of implantation because the design allows anchorage of the screw assembly as would the anchorage of a single cannulated screw. The male and female components are assembled as per presented in the embodiment in order to screw in simultaneously both medial and lateral threading through a simple continuous rotation action with the use of a driving tool detachably connected to the male component, which in turn serves as the driving tool for the female component. Device position is final when all threads on tube have fully tapped into bone beyond the physeal plate within the femoral epiphysis.
[0016] In all embodiments, the screw assembly has a unique feature of self-adjustment in length after its implantation to provide a stable fixation of the fractured bone segments without the use of compressive forces to promote healing without disrupting normal patient growth, which is particularly advantageous when the screw assembly is used in children. In addition, rotational stability can be achieved by the incorporation of a non-circular design feature to block rotation between male and female components. Furthermore, retrieval features incorporated into the lateral ends of the embodiments of the present invention allow retention of the screws during insertion and removal procedures. Finally, a cap-like component completes the screw assembly, which inserts into the proximal end of the screw assembly at the lateral cortex in order to prevent bone in-growth for eased retrieval of the screw assembly once the fracture site is healed or patient growth is complete.
[0017] Additional objectives, advantages and novel features will be set forth in the description which follows or will become apparent to those skilled in the art upon examination of the drawings and detailed description which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 is a perspective view of a first embodiment of a screw assembly having a trilobe configuration;
[0019] FIG. 2 is a side view of the screw assembly;
[0020] FIG. 3 is an exploded view of the screw assembly showing the female component, male component and cap;
[0021] FIG. 3A is an end view of the male component;
[0022] FIG. 4 is partially exploded side view of the screw assembly with the male component, female component, and cap;
[0023] FIG. 5 is a perspective view of the female component;
[0024] FIG. 5A is a cross-sectional view along line 5 A- 5 A of FIG. 5 ;
[0025] FIG. 6 is a side view of the female component;
[0026] FIG. 7 is a perspective view of the male component
[0027] FIG. 7A is a cross-sectional view along line 7 A- 7 A of FIG. 7 ;
[0028] FIG. 8 is a side view of the male component;
[0029] FIGS. 9A and 9B are perspective views of the cap;
[0030] FIG. 10 is a perspective view of a second embodiment of the screw assembly having a double flat configuration;
[0031] FIG. 11 is a side view of the screw assembly shown in FIG. 10 ;
[0032] FIG. 12 is an exploded view of the screw assembly shown in FIG. 10 illustrating the female component, male component and cap;
[0033] FIG. 12A is an end view of the male component shown in FIG. 12 ;
[0034] FIG. 13 is a partially exploded side view of the screw assembly shown in FIG. 10 with the male component, female component, and cap;
[0035] FIG. 14 is a perspective view of the female component shown in FIG. 10 ;
[0036] FIG. 14A is a cross-sectional view taken along line 14 A- 14 A of FIG. 14 .
[0037] FIG. 15 is a side view of the female component shown in FIG. 10 ;
[0038] FIG. 16 is a perspective view of the male component shown in FIG. 10 ;
[0039] FIG. 16A is a cross-sectional view of the male component along line 16 A- 16 A of FIG. 16 ;
[0040] FIG. 17 is a side view of the male component shown in FIG. 10 ;
[0041] FIG. 18 is a perspective of a third embodiment of the screw assembly having a beveled head configuration;
[0042] FIG. 19 is a side view of the screw assembly shown in FIG. 18 ;
[0043] FIG. 20 is an exploded view of the screw assembly shown in FIG.
[0044] FIG. 21 is a partially exploded side view of the screw assembly shown in FIG. 18 with the male component and female component;
[0045] FIG. 22 is a perspective view of the female component shown in FIG. 18 ;
[0046] FIG. 22A is a cross-sectional view taken along line 22 A- 22 A of FIG. 22 ;
[0047] FIG. 23 is a side view of the female component shown in FIG. 18 ;
[0048] FIG. 24 is a perspective view of the male component shown in FIG. 18 ;
[0049] FIG. 24A is a cross-sectional view taken along line 24 A- 24 A of FIG. 24 ; and
[0050] FIG. 25 is a side view of the male component shown in FIG. 18 ;
[0051] FIGS. 26A-26G illustrate one method for using the screw assembly shown in FIG. 1 .
[0052] Corresponding reference characters indicate corresponding elements among the view of the drawings. The headings used in the figures should not be interpreted to limit the scope of the claims.
DETAILED DESCRIPTION
[0053] Referring to the drawings, various embodiments of the screw assembly are illustrated and generally indicated as 100 , 200 and 300 in FIGS. 1-25 .
[0054] In one embodiment shown in FIGS. 1-9 , the screw assembly, designated 100 , may include a hollow female component 102 configured to receive a male component 104 with a cap 105 that engages one end of the male component 104 . Specifically, the male component 104 is freely slidable relative to female component 102 along longitudinal axis 900 ( FIG. 1 ), which allows the screw assembly 100 to lengthen over time along axis 900 and accommodate the natural growth of the growth plate as the fracture heals over a period of time.
[0055] Referring to FIGS. 1 and 4 , the female component 102 defines circular-shaped hollow shaft 107 that defines an elongated trilobe-shaped channel 118 therein configured to accommodate a trilobe-shaped shaft 106 of the male component 104 such that the trilobe-shaped shaft 106 of the male component 104 may freely slide relative to the elongated trilobe-shaped channel 118 of the female component 102 .
[0056] Referring to FIGS. 5 and 5A , the circular-shaped hollow shaft 107 of the female component 102 further defines a proximal end opening 110 in communication with the elongated trilobe-shaped channel 118 . In addition, the female component 102 further include a medial threaded portion 108 , having a cancellous profile, that defines an axial opening 111 in communication with an interior cannulated section 114 . The other end of the interior cannulated section 114 is in communication with the far end of the elongated trilobe-shaped channel 118 such that fluid flow communication is established between the axial opening 111 and the proximal end opening 110 . In one embodiment, the inner diameter of the cannulated section 114 is less than the inner diameter of the elongated trilobe-shaped channel 118 . As shown, one embodiment of the medial threaded portion 108 may define a self-tapping cut-out feature 121 that facilitates entry of the female component 102 into the bone as shall be described in greater detail below. As further shown, an internal threaded portion 112 is defined adjacent to the proximal end opening 110 for engaging with a removal device (not shown) with matching thread.
[0057] As shown in FIGS. 7 , 7 A and 8 , the male component 104 includes a trilobe-shaped shaft 106 having a substantially three-sided cross-sectional configuration sized and shaped to be disposed within the elongated trilobe-shaped channel 118 when the male component 104 is engaged to the female component 102 . The male component 104 defines a far end opening 113 along a trilobe-shaped end 136 of the elongated trilobe-shaped shaft 106 and a lateral threaded portion 116 at the opposite end of the elongated trilobe-shaped shaft 106 . The lateral threaded portion 116 features a flat head configuration at the free end thereof that positions the lateral threaded portion 116 , whose diameter is larger than the trilobe-shaped shaft 106 . In addition, the lateral threaded portion 116 defines a self-tapping feature 120 formed along the lateral threaded portion 116 .
[0058] As shown in FIG. 7A , the far end opening 113 is in communication with a cannulated section 119 which forms a channel along the length of the elongated trilobe-shaped shaft 106 . In addition, a drive feature 122 communicates with the opposite end of the cannulate section 119 through an internal threaded section 115 formed adjacent the drive feature 122 , whose combination is used to retain and drive the assembled male and female components simultaneously into the bone ( FIG. 26A ).
[0059] Referring to FIG. 3A , the trilobe-shaped shaft 106 includes a first trilobe portion 130 , a second trilobe portion 132 , and a third trilobe portion 134 that collectively form a non-cylindrical cross-sectional configuration that prevents rotation of the female component 102 relative to the male component 104 . As noted above, the trilobe-shaped shaped shaft 106 is freely slidable along longitudinal axis 900 of the screw assembly 100 , while the non-circular shape of the trilobe-shaped shaft 106 prevents rotational movement of the female component 102 relative to the male component 104 along rotational direction 902 (e.g. in either the clockwise or counter-clockwise rotational directions). Although the embodiment of the male component 104 shown in FIGS. 1-8 defines a three-sided trilobe-shaped cross-sectional configuration, other types of non-cylindrical cross-sectional configurations may be used to define the shaft 106 , such as triangular, square, rectangular, or oblong-shaped cross-sectional configurations that allows sliding movement of the male component 104 , but prevents rotational movement of the female component 102 relative to the male component 104 . In this mating engagement between the female component 102 and the male component 104 , the drive mechanism 10 is able to drive both female and male components 102 and 104 into the bone.
[0060] Referring to FIGS. 9A and 9B , the cap 105 may be used to seal off the recessed drive feature 122 of the male component 104 . As shown, the cap 105 includes a semi-spherical shaped cap portion 126 that defines a recess 125 configured to connect with a drive and removal tool 11 with a matching profile. The cap portion 126 communicates with a cylindrical-shaped middle portion 128 with an external threaded portion 124 that extends axially from the middle portion 128 . As shown in FIG. 4 , the external threaded portion 124 of the cap 105 is configured to engage and retain the proximal end internal threads 115 defined by the male component 104 .
[0061] During manufacture, the following dimensions may be used for one embodiment of the screw assembly 100 , although other suitable dimensions may be used for other embodiments. Referring to FIGS. 2 and 6 , the screw assembly 100 may have a length 500 of between 60 mm to 102 mm in 2 mm increments, while the female component 102 may have a length 502 of between 52 mm to 92 mm in 4 mm increments and a width 504 of 6.5 mm to 7.3 mm. As shown in FIG. 8 , the male component 104 may have a length 506 of between 48 mm to 50 mm and a width 508 at the head 508 of between 8.0 mm to 9.0 mm.
[0062] In a second embodiment shown in FIGS. 10-17 , the screw assembly, designated 200 , may include a hollow female component 202 configured to receive a male component 204 with a cap 205 that engages the male component 204 in similar fashion as cap 105 . As shown in FIG. 12A , the male component 204 includes a double flat shaped shaft 206 having opposing sides 232 and 236 as well as opposing sides 230 and 234 that collectively define either a generally squared-shaped or rectangular-shaped cross sectional configuration. Similar to screw assembly 100 , the non-cylindrical shape of the double flat shaped shaft 206 for the male component 204 functions in a similar manner as the trilobe-shaped shaft 106 of male component 104 to prevent rotational movement 906 of the female component 202 relative to the male component 204 while allowing free sliding movement along longitudinal axis 904 of the screw assembly 200 .
[0063] Referring to FIGS. 14 and 15 , the female component 202 includes a cylindrically-shaped elongated hollow body 207 having a proximal end opening 210 at one end and an external threaded portion 208 at the opposite end thereof. In one embodiment, the external threaded portion 208 may have a cancellous-shaped profile having a diameter substantially equivalent to the diameter of the cylindrically-shaped elongated hollow body 207 for providing increased mechanical properties under weight bearing conditions. In addition, the external threaded portion 208 includes a self-tapping feature 221 that facilitates entry of the female component 102 into the bone and an axial opening 211 .
[0064] As shown in FIG. 13 , the axial opening 211 is in communication with a cannulated section 214 formed through the external threaded portion 208 of the female component 202 . In addition, the cannulated section 214 is in communication with an elongated channel 218 formed through the cylindrically-shaped elongated hollow body 207 that is configured to receive the male component 204 therein. In one embodiment, the elongated channel 218 defines a double-sided cross sectional configuration having the same cross sectional configuration as the double sided-shaped shaft 206 . As further shown, a left handed internal threaded section 212 is formed proximate the proximal end opening 210 and is configured to mate with a removal instrument (not shown) for ease of retrieval of the female component 202 .
[0065] Referring to FIGS. 13 , 16 , 16 A and 17 , the male component 204 defines a medial threaded portion 216 having a flat head with a self tapping feature 220 formed along the medial threaded portion 216 . In one embodiment, a drive feature 222 forms a hexagonal-shaped recess in communication with a proximal end internal threaded portion 215 configured to engage an external threaded portion 224 of the cap 205 when the cap 205 is engaged into the male component 204 . The combination of the drive feature 222 and the internal threaded portion 215 is used to retain and drive the assembled male and female components 202 and 204 into the bone ( FIG. 26A ). In addition, the male component 204 includes an axial opening 213 in communication with cannulated section 219 that forms an elongated channel between the axial opening and the drive feature 222 . As shown, the cap 205 is similar in construction as cap 105 having a middle portion 228 in communication with a cap portion 226 having a recess 225 .
[0066] During manufacture, the following dimensions may be used for one embodiment of the screw assembly 200 , although other suitable dimensions may be used for other embodiments. Referring to FIG. 11 , the screw assembly 200 may have a length 700 of between 60 mm to 102 mm in 2 mm increments. As shown in FIG. 15 , the female component 202 may have a length 702 of between 50 mm to 90 mm in 4 mm increments and a width 704 of between 6.5 mm and 7.3 mm. As shown in FIG. 17 , the male component 204 may have a length 706 of between 48 mm to 50 mm and a width 708 of between 8.0 mm to 9.0 mm
[0067] In a third embodiment shown in FIGS. 18-25 , the screw assembly, designated 300 , may include a hollow female component 302 configured to receive a male component 304 . As shown in FIGS. 22 , 22 A, and 23 , the female component 302 defines a hollow cylindrical shaft portion 306 having a far end opening 310 formed at one end and a lateral beveled end portion 308 at the opposite end thereof. The hollow cylindrical shaft portion 306 allows for ease of insertion of the screw assembly 300 into the bone and eliminates disruption of the physeal plate as not sharp features are inserted into the physeal plate. The far end opening 310 is in communication with an elongated channel 320 formed along the cylindrical shaft portion 306 .
[0068] As shown in FIG. 22A , an internal drive feature 322 is formed at the proximal end inside the lateral beveled end portion 308 and forms a hexagon-shaped recess. The drive feature 322 is configured to receive a portion of the drive mechanism 10 ( FIG. 26A ) for insertion through a bone. As further shown, a left-handed internal threaded portion 324 is formed between the drive feature 322 and a cannulated section 326 . The left-handed internal threaded portion 324 facilitates retention of the screw assembly 300 for ease of removal, while the cannulated section 326 for guided insertion of the component into the bone using a cannulated rod (not shown). The lateral beveled end portion 308 has a diameter larger than the hollow shaft portion 306 for better retention of the screw assembly 300 in the bone.
[0069] Referring to FIG. 19 , the lateral beveled end portion 308 defines a beveled profile that positions the cortical profiled threads of the lateral beveled end portion 308 fully within the lateral cortex, flush against the bone surface, thereby eliminating exposure of the threads outside the bone.
[0070] As shown in FIGS. 20 , 24 , 24 A, and 25 , the male component 304 defines a hollow cylindrical shaft portion 307 with a medial threaded portion 316 having a cancellous profile formed at one end of the shaft portion 307 and an external drive feature 312 formed at the opposite end thereof. The medial threaded portion 316 defines a self-tapping feature 318 that facilitates entry of the male component 304 into the bone. In some embodiments, the medial threaded portion 316 has a diameter larger than the diameter of the cylindrical shaft 307 . As shown, an axial opening 313 is formed proximate the medial threaded portion 316 and is in communication with an elongated channel 325 at one end thereof. The external drive feature 312 forms an opening 315 that communicates with the opposite end of the elongated channel 325 . As such, the male component 304 is fully cannulated to insert over a standard guide wire (not shown). In addition, the hollow cylindrical shaft portion 307 defines a left-handed retrieval threaded section 314 formed proximate the external drive feature 312 .
[0071] As shown in FIG. 20 , the male component 304 may freely slide relative to the female component 302 . In this embodiment, no cap is required to be engaged to the male component 304 .
[0072] During manufacture, the following dimensions may be used for one embodiment of the screw assembly 300 , although other suitable dimensions may be used for other embodiments. Referring to FIG. 19 , the screw assembly 300 may have a length 800 of between 60 mm to 100 mm in 2 mm increments. As shown in FIG. 23 , the female component 302 may have a length 802 of between 50 mm to 80 mm in 4 mm increments and a width 804 at the shaft of between 8.0 mm to 9.0 mm. As shown in FIG. 25 , the male component 304 may have a length 806 of 50 mm, a width 808 at the shaft of between 5.0 mm and 5.8 mm and a width 808 at the head of between 6.5 mm to 7.3 mm.
[0073] Referring to FIGS. 26A-26G , one method of using the screw assemblies 100 and 200 is illustrated. However, for ease of description only the use of screw assembly 100 will be described herein since the method of use is the same for both embodiments. Referring to FIGS. 26A-26C , the male component 104 received within the female component 102 is inserted through the physeal plate using a drive mechanism 10 until the lateral threaded portion 116 of the male component 104 is fully disposed within the lateral cortex. In this arrangement, the male component 104 is fully received within the female component 102 such that the cylindrical shaft 106 is fully disposed within the female component 102 . As shown in FIGS. 26D-26F , the cap 105 is attached to the lateral threaded portion 116 using the driving mechanism 11 which seals off both the male component 104 and female component 102 within the lateral cortex. As shown in FIG. 26G , the free sliding engagement between the female component 102 and the male component 104 allows the cylindrical shaft 106 to gradually extend from the female component 102 as the physeal plate grows over time as the fracture heals.
[0074] It should be understood from the foregoing that, while particular embodiments have been illustrated and described, various modifications can be made thereto without departing from the spirit and scope of the invention as will be apparent to those skilled in the art. Such changes and modifications are within the scope and teachings of this invention as defined in the claims appended hereto.
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A screw assembly and method developed for the fixation of femoral neck fractures without interruption of the growth process is disclosed. The screw assembly includes a male component that is attached to the lateral cortex and a female component that is attached at the proximal epiphysis. Anchorage of the components is achieved through screw-type fixation. The screw has a built-in feature that allows for free extension of its length as the fracture site or the slipped capital physeal plate heals and normal patient growth continues. Stable fixation and rotational stability are created at the fracture (slip) site while avoiding compression forces, thus avoiding premature closure of the physeal plate.
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This application is a continuation-in-part of co-pending application Ser. No. 07/552,936 filed Jul. 16, 1990, now U.S. Pat. No. 5,096,960.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a novel composition of matter for reducing cosolvent quantities in water-borne resins. Particularly, this invention relates to a novel composition of matter that has been found to give good film forming characteristics from cosolvent/aqueous media and improved impact resistance. More particularly, this invention relates to a novel water-borne composition that can be reacted to higher molecular weight than standard trimellitic anhydride resins without gelling. The invention composition permits the use of less amounts of environmentally dangerous cosolvents in an aqueous alkyd system.
2. Description of the Prior Art
In water-borne alkyd coatings, the reduction of organic cosolvents is important since they contribute to the amount of volatile organic compounds (VOC's) in the system. Historically, the use of trifunctional acids such as trimellitic anhydride has been the preferred method of solubilizing preformed alkyd resins into an aqueous medium. Alkyd resins are presynthesized to an acid number of about ten and then further reacted with trimellitic anhydride to an acid number of about 45 to 50 to form resins that may be neutralized with base to provide water soluble resins (Amoco Technical Bulletin GSTR 21).
A main deficiency of this technology is the need for a relatively large amount of organic cosolvent in the mixture to maintain solubility. The organic cosolvents that are commonly employed include acetone, butanol, secondary butanol, cyclohexanone, ethylene glycol monobutyl ether, and methyl isopropyl ketone. The chief characteristic of these solvents is that they are at least partially water soluble and have the ability to interact with the water-borne resin to maintain its solubility. Although these water/cosolvent/resin compositions give reasonable properties, the fact that relatively large amounts of cosolvent must be employed means that a large amount of organic material escapes into the environment during processing and application leading to pollution. Although alternative systems to alkyds exist, such as epoxies and acrylics, these latter suffer from deficiencies such as very high price and relative difficulty in application in the case of epoxies and poorer properties with an acrylic.
Therefore, it is the object of this invention to have an alkyd composition that addresses environmental concerns by effectively reducing the amount of cosolvent in the system. In addition, organic cosolvents are frequently expensive and any means of reducing their presence would lead to lowered costs for a paint.
SUMMARY OF THE INVENTION
The object of this invention is met by the use of maleinized fatty acid, preferably maleinized oleic, linoleic, or linolenic, more preferably oleic, in water-borne alkyds in lieu of aromatic triacids (e.g., trimellitic anhydride). The maleinized fatty acid substitution gives systems which may be formulated with less cosolvent than their aromatic counterparts. This finding is significant since it would provide a means of both reducing the amount of volatile organic material in the system and reducing costs for paint manufacturers.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Water-borne alkyd paint systems frequently contain water-soluble organic cosolvents. Included in this list of potential cosolvents are such materials as:
butanol
secondary butanol
cyclohexanone
acetone
methyl isopropyl ketone
methyl isobutyl ketone
ethyleneglycolmonobutyl ether
ethylene glycol monomethyl ether
ethylene glycol monoethyl ether
propylene glycol monobutyl ether
This list is intended to be representative and it will be obvious to those skilled in the art that a variety of other solvents and combinations thereof can be used. Therefore, other solvents or combinations which reduce viscosity can be considered part of this invention when used with the described composition of matter below. This invention describes an effective means of reducing the amount of cosolvents such as those listed above while still obtaining good film-forming characteristics. Most water-borne alkyd based paints require the use of a trifunctional acid or acid-anhydride to obtain sufficient acidity for neutralization and subsequent solubilization in water. The trifunctional materials currently employed are well suited to the requirements of water-borne alkyds except they require a significant amount of cosolvent to maintain solubility and give good film forming characteristics. Most formulations appear to be based on trimellitic anhydride since it has the very highly reactive anhydride linkage which can be reacted with the residual hydroxyls in the alkyd system. Presumably, other aromatic or aliphatic triacids could be used but they are not as reactive as trimellitic anhydride and can give gelation in the alkyd since they have similar reactivity in their carboxylic acid groups. For the purpose of describing this invention, trimellitic anhydride is considered as the comparative prior art trifunctional material since it is the most readily available commercial product (Amoco Chemicals) and also has the desired reactivity in the anhydride linkages.
It has been discovered that use of acid-anhydrides derived from the reaction of maleic anhydride with either oleic, linoleic, or linolenic acids serve a similar function as trimellitic anhydride in regards to reacting with the hydroxyls of an alkyd system and providing adequate acidity for neutralization and solubilization. The oleic acid adduct is most preferred in this invention since it combines more readily with the initial alkyd resin than, for example, the linoleic or linolenic adducts. Significantly, these materials, when used according to the descriptions of this invention, can substantially reduce the viscosity of resins in cosolvent media when substituted for aromatic moieties at the same solids level. Film properties are not seriously affected. An alternative embodiment is to formulate the resins to similar viscosities. The maleinized fatty acid derived resins require less solvent. This finding is unexpected since the trifunctional materials, either aromatic or aliphatic, traditionally serve only to couple the main polymer backbone of the alkyd resin and are present in relatively small quantities. Therefore, larger quantities of material would be expected to be needed to obtain the large viscosity decreases observed. In fact, molecular weights of alkyd resins synthesized from fatty acid derived materials are frequently higher than corresponding resins obtained from aromatic trifunctional materials; higher molecular weights would be expected to give larger viscosities. Indeed, it is possible to react the maleinized fatty acid resins to a lower acid (higher molecular weight) value than the trifunctional aromatic moieties and still maintain good solubility characteristics. Viscosity data for the different resins at different solids levels are given in Table I.
TABLE I______________________________________Representative Viscosity Values at Different PercentSolids Loadings for Alkyd Resins Trimellitic Maleinized Anhydride Fatty Acid% Solids Resin Resin______________________________________75 13600 623280 41200 1636085 83000 34800______________________________________
At eighty percent solids the maleinized fatty acid (MFA), in this case maleinized oleic, has a slightly larger viscosity than the trimellitic anhydride (TMA) system at 75% solids; both viscosities are considered within the range of workable water borne systems (up to about 50,000 centipoise). At 85% solids the viscosity of the TMA resin is too large to be workable whereas at this solids level the MFA resin is still able to be handled. Results of formulating these different resins into aqueous solutions are shown below in Table II (final solids of systems are approximately 35%).
TABLE II______________________________________Appearance of Aqueous Formulations of Alkyds Trimellitic Maleinized Anhydride Fatty Acid% Solids Resin Resin______________________________________75 clear clear80 cloudy clear85 cloudy cloudy with ppt.______________________________________
At higher solids content based on initial formulation with organic cosolvent, it is evident that resins based on MFA give better solubility characteristics than TMA based resins. Although partially soluble resins (cloudy) might give good films in these cases, clarity of the solution generally correlates with film quality as judged by levelling and dry times. Thus, TMA resins, when drawn down to films do not give good levelling properties when formulated at either 80 or 85% solids in initial organic cosolvent. MFA resins, on the other hand, give good results when formulated from either 75 or 80% solids; with 85% solids reasonable properties were obtained although film leveling was of slightly poorer quality than at higher volatile organic content (lower solids) levels. Since the MFA based resins may be effectively used at an 80% solids level in initial organic cosolvent, it is possible to reduce the amount of cosolvent in the system and still obtain desired good film forming properties compared with trimellitic anhydride. In going from 75% to 80% solids the amount of solvent is reduce by 20% (20 % VOC/25% VOC=80% of the original VOC).
Physical properties of the different resins described above are shown in Table III. Data indicate that the physical properties of the systems are essentially equal; this similarity exists for the TMA resin at 75% solids, and the MFA resins at both 75 and 80% solids. One significant difference between the systems is the impact resistance; those resins containing the MFA have considerably higher impact resistance than those with TMA. This is yet another added benefit of using MFA in lieu of TMA in water dispersible alkyd systems.
TABLE III__________________________________________________________________________Properties of Alkyds Dry Pencil Sward ImpactEntry Description Time Hardness Hardness Front Reverse Flexibility Adhesion__________________________________________________________________________1 TMA-75% Solids 1 hr. F 72 160 170 >32% 95% (4B) 2 TMA-80% Solids Precipitation/viscosity problems3 TMA-85% Solids Could not adequately film form4 ENE-75% Solids 5 hr. 2B 36 160 160 >32% 100% (5B)5 ENE-80% Solids 5 hr. B 26 160 160 >32% 100% (5B)__________________________________________________________________________
A resin typical of this invention consists of a drying oil fatty acid consisting of, but not limited to:
Pamolyn 200 (80% linoleic acid; 20% oleic acid - Hercules)
tung oil fatty acid
linseed oil fatty acid
soya fatty acid
tall oil fatty acid
safflower fatty acid
The proportion of fatty acid present in the alkyd is between 20 to 80% by weight and preferably between 35 and 65% by weight. Alternatively, corresponding glycerides of the above materials may be used as will be obvious to those skilled in the art.
Also, a difunctional acid is used in the first stage of synthesis of the resin. This difunctional acid may be taken from any one or a combination of the following. This list is not intended to be limiting:
isophthalic acid
phthalic anhydride
terephthalic acid
isomeric naphthalene dicarboxylic acids
The diacids are present at between 10% and 50% by weight and preferably between 20% and 40% by weight.
In addition, a trifunctional alcohol is used in the reaction of first stage alkyd resin. This trifunctional alcohol may be taken from the list of materials below, but is not limited by them:
trimetholylpropane
trimetholylethane
glycerol
Triols are present at levels of between 2% and 40% of the alkyd weight and preferably between 5% and 35% by weight.
Finally, during the synthesis of the first stage alkyd resin a difunctional alcohol is used. Suitable diols are indicated, but not limited by:
neopentyl glycol
butanediol
hexanediol
cyclohexane diols
ethylene glycol
propylene glycol
Diols may be used in weight proportions between 2% and 40% and preferably between 5% and 35% by weight. Tetraols (4 OH's), pentaols (5 OH's), and hexaols (6 OH's) are also known and may be used in substitution for the above triols and diols when substituted on an equivalent weight basis.
When the above reactants are combined in suitable proportions and reacted they form a first stage resin which in a second stage reaction with either trimellitic anhydride or maleinized fatty acid give the final desired alkyd resin. The amount of maleinized fatty acid employed is from about 5% to about 35%, preferably from about 15% to about 25%, by weight of the first stage resin. Suitable proportions of the components may be calculated according to well known alkyd formulating equations by those skilled in the art. A description of these calculations is also given in Alkyd Resin Technology - Formulating Techniques and Allied Calculations, T. C. Patton, Interscience Pub., 1962, pp. 100-102. This final alkyd resin is subsequently solubilized by neutralization into an aqueous medium with a volatile amine which includes, but is not limited to, ammonia, ammonium hydroxide, methyl amine, dimethyl amine, trimethyl amine, dimethyl ethanolamine, ethyl amine, and dimethyl amine.
The film-forming compositions described herein also may be used in fully formulated paints. The use of the water-borne alkyds in paints may be accomplished by combining alkyd resin (preferably at 80% solids) with a pigment additive for color, such as titanium dioxide. To this combination may be added a suitable chemical dryer combination, such as a cobalt dryer and a manganese dryer. In addition, a drying promoter, such as Activ 8® (a 1,10-phenanthroline based drying promoter by Mooney Chemicals), may also be added. Also, a surface leveling agent, such as Bykanol 301® (a polymeric silicone reagent by Byk-Chemie), may be added to enhance wetting properties. Bykanol 301 is used to lower resin solution surface tensions and enhance wettability.
These examples are representative of the practice of this invention:
EXAMPLE 1
The following example is a typical first stage resin commercial formulation.
Pamolyn 200 (Hercules, linoleic acid) is combined with trimethylolpropane, and neopentyl glycol in a resin kettle or other suitable flask. After heating to melting with sparging (nitrogen), the isophthalic acid is added and heating is continued at a temperature of about 240° C. until an acid number of below 10 is obtained. The amounts of various components that are necessary for the first step of this sequence are shown below (based on parts by weight):
______________________________________Materials Parts by Weight______________________________________Pamolyn 200 366.8Trimetholylpropane 202.8Neopentyl Glycol 115.5Isophthalic Acid 307.2______________________________________
This first stage resin may then be used when combined with an acid-anhydride (or corresponding triacid) to generate the desired final second stage resin for use in water-borne paints.
EXAMPLE 2
The resin described in Example 1 was taken at 170° C. and reacted with 101.7 parts of trimellitic anhydride. This mixture was allowed to reach an acid number of between 45 to 50 and diluted with solvent in the following manner:
The reaction mixture was cooled to about 150° C. and a suitable amount of ethylene glycol monobutyl ether (EGMBE) was added so that it will constitute 40% of the 25% volatile material in the system. This amount may be calculated by the following equation: ##EQU1## After addition of the EGMBE the resin solution was further cooled to below 100° C. and then a suitable amount of secondary butanol was added so that it will constitute 60% of the 25% material in the system. This amount may be calculated by an equation similar to the one shown in step 3.
EXAMPLE 3
The resin of Example 2, at 75% solids (25.6 parts by weight) was diluted with water (43.9 parts) and 28% ammonium hydroxide (1.15 parts). To this was added suitable driers such as cobalt, calcium and zirconium to give effective curing; optionally, anti-skinning agents may be employed if needed. Finally, pigment (titanium dioxide, 17.3 parts) and additional secondary butanol (2.1 parts), EGMBE (1.4 parts) and deionized water (7.5 parts) were added. Pigmentation is not necessary in order to study the film properties. Finally, the resin pH is adjusted to 8.5. Drawn down films of about 1 mm thickness were prepared from this final aqueous solution. All testing was done on this type film.
EXAMPLE 4
A resin was synthesized and formulated in a fashion analogous to Example 2 above except that instead of TMA, maleinized fatty acid was employed. The difference incorporated in this procedure in contrast to Example 2 was that 195.1 parts by weight of MFA were used instead of 101.7 parts by weight of TMA during the synthesis of the resin.
MFA resins were generally reacted to a slightly lower acid number of between 32-42. Although good films are still obtained at higher acid values of between 45 to 50 the lower acid number resins have higher molecular weight distributions and require less neutralizing ammonia. Resins reacted below an acid number of about 32 generally are not as soluble as desired in the final formulation and the risk of gelation during reaction is greatly increased.
Use of this slightly different procedure resulted in resins with comparable properties to the TMA based systems.
EXAMPLE 5
In a fashion analogous to Example 3,the resin described in Example 4 was solubilized in water with the exception that it is necessary to neutralize this material to a pH of about 10 to insure long-term shelf life. This distinguishes the invention resins from the prior art resins and indicates the uniqueness of the claimed composition. Generally accepted formulation techniques would only call for a resin to be neutralized to a pH of between 8.5 and 9.5. With the invention resin, only at a higher pH of from about 9.5 to about 11.0, is stability obtained.
The use of the water-borne alkyds in paints is described in the following example.
EXAMPLE 6
Fifty-nine grams of alkyd resin at 80% solids (prepared as in Example 4) were combined with 12.4 grams of titanium dioxide. To this combination was added a suitable chemical dryer combination. For example, 0.30 gram of a 6% active cobalt dryer plus 0.23 gram of an 8% manganese dryer plus 0.15 gram of Activ 8 drying promoter was found to give good drying properties. In addition, a surface leveling agent (Bykanol 301) was added to enhance wetting properties of drawn down films.
The above formulation was placed in a small ball mill and rolled for 12 to 15 hours to obtain a smooth white pigmented paint. Films were drawn down at 0.004 inch wet and allowed to dry. Dry times were typically two to five hours, and smooth durable films were obtained.
This example effectively demonstrates how the alkyd compositions in this patent may also be used in paints.1 The use of other pigments besides titanium dioxide would be evident to those skilled in the art.
While the invention has been described and illustrated herein by reference to various specific materials, procedures and examples, it is understood that the invention is not restricted to the particular materials, combinations of materials, and procedures selected for that purpose. Numerous variations of such details can be employed, as will be appreciated by those skilled in the art.
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Water-borne alkyd resin compositions are disclosed comprising maleinized fatty acid. Substitution of the aromatic triacid component of the composition with the maleinized fatty acid permits a reduction in the amount of organic cosolvent employed to solubilize the resin in the water. Alkyd resin containing paint formulations also are disclosed.
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This is a Divisional Application of U.S. patent application Ser. No. 09/045,889 filed Mar. 23, 1998 now abandoned and Provisional Application No. 60/043,875 filed Apr. 10, 1997 and U.S. Provisional No. 60/059,730 filed Sep. 23, 1997.
FIELD AND BACKGROUND OF THE INVENTION
The present invention relates to the modulation of electromagnetic radiation and, more particularly, to a mechanical valve, and an array of such valves, for regulating the flow of radiation by selectively blocking the radiation.
Transmissive devices for modulating the flow of electromagnetic radiation, such as visible, infrared and ultraviolet radiation, are known. The simplest such devices are mechanical shutters. These devices have the advantage of being broad band, inasmuch as the materials used are opaque, in the thicknesses typically used, over a very wide spectral range; but typically these devices are too large to allow spatial modulation of the radiation on a short length scale approaching the wavelength of the radiation. In addition, their mechanical inertia places a lower bound on the time scale of this modulation. Spatial modulation on a short length scale, and temporal modulation on a short time scale, typically require the manipulation, by electrical, magnetic or electronic means, of the optical properties of substances such as liquid crystals. These optical properties generally are strong functions of wavelength, and so restrict the operation of such devices to particular spectral bands.
Reflective devices for fine spatial and temporal modulation of electromagnetic radiation over a relatively wide spectral range are known. These devices include, for example, the deformable mirror device described in U.S. Pat. No. 5,083,857 to Hornbeck. These devices typically consist of arrays of reflectors, each reflector corresponding to one pixel of a display. Such devices are inherently reflective, rather than transmissive, because the control electronics that addresses and activates each individual pixel is located behind the pixel, and would block the transmission of electromagnetic radiation across the pixel. Systems including such devices are inherently less compact than systems based on transmissive devices, because the light to be modulated must be directed at the device at an angle different from that at which the modulated, reflected light leaves the device.
There is thus a widely recognized need for, and it would be highly advantageous to have, a transmissive device, for fine spatial and temporal modulation of electromagnetic radiation, that operates over a wide spectral range.
SUMMARY OF THE INVENTION
According to the present invention there is provided a radiation valve including: (a) a substrate transparent to the radiation; and (b) a first planar member, at least partly flexible, opaque to the radiation, rigidly attached to the substrate, and operative to alternately assume an open orientation and a closed orientation with respect to the substrate, more of the radiation transiting the substrate when the first planar member is in the open orientation than when the first planar member is in the closed orientation.
According to the present invention there is provided a device for modulating radiation, including: (a) a substrate transparent to the radiation and having a surface; (b) a plurality of valves on the surface, each of the valves including a first at least partly flexible planar member that is opaque to the radiation, rigidly attached to the surface, and operative to alternatively assume an open orientation and a closed orientation with respect to the surface, more of the radiation transiting the substrate when the first planar member is in the open orientation than when the first planar member is in the closed orientation, the valves being arranged in at least one row and at least one column on the surface; and (c) for each of the at least one row, a mechanism for inducing the first planar member of at least one of the valves of the row to assume the orientations.
According to the present invention there is provided a display for displaying a pattern of spatially and temporally modulated radiation, including: (a) an array of a plurality of valves, in a common plane, for alternately transmitting and blocking the radiation, the valves being arranged in at least one row and in at least one column in the common plane; and (b) a control mechanism, for opening and closing the valves in accordance with the pattern, positioned laterally apart from the array of valves.
According to the present invention there is provided a method of modulating radiation, including the steps of: (a) providing a radiation modulator including: (i) a substrate transparent to the radiation and having a surface, and (ii) at least one valve on the surface, each of the at least one valve including a first, at least partly flexible planar member and a second, at least partly flexible planar member, the planar members being opaque to the radiation, rigidly attached to the surface, and operative to alternately assume an open orientation and a closed orientation with respect to the surface; (b) directing the radiation at the radiation modulator; and (c) for each of the at least one valve, alternately inducing the first planar member and the second planar member to both assume the open orientation and to both assume the closed orientation, more of the radiation transiting the substrate when both the planar members are in the open orientation than when both the planar members are in the closed orientation.
According to the present invention there is provided a method of fabricating a mesoscale device having a wall perpendicular to a substrate, including the steps of: (a) depositing photoresist on the substrate in a pattern including at least one surface substantially perpendicular to the substrate; (b) directing a first substantially parallel beam of atoms of a first deposant species at the at least one surface at a first oblique angle to the at least one surface, thereby depositing the wall of the first deposant species on the at least one surface; and (c) removing the photoresist.
According to the present invention there is provided a method of fabricating a mesoscale device including a substrate and a body, the body including at least two layers substantially perpendicular to the substrate, including the steps of: (a) depositing a first wall on the substrate, the first wall including a first surface substantially perpendicular to the substrate, the wall constituting a first of the two layers; and (b) directing a substantially parallel beam of atoms of a deposant species at the first surface at an oblique angle to the first surface, thereby forming a second of the two layers.
According to the present invention there is provided a method of modulating radiation to display successive frames of pixels, each of the frames having a duration, each of the pixels having an intensity, the method including the steps of: (a) providing an array of a plurality of valves, in a common plane, for alternately transmitting and blocking the radiation, the valves being arranged in a plurality of rows and in a plurality of columns in the common plane, each of the pixels corresponding to at least one of the valves; (b) directing the radiation at the array of valves; and (c) for each of the pixels, opening at least one of the at least one valve corresponding to the pixel for a fraction of the duration of the frame of the each pixel in accordance with the intensity of the each pixel.
According to the present invention there is provided a mesoscale device including: (a) a substrate; and (b) at least one wall, substantially perpendicular to the substrate, having a height of at least about 5 microns and a thickness of at most about 1 micron.
According to the present invention there is provided a mesoscale device including: (a) a substrate; and (b) a layer, above the substrate, at least about 5 microns thick and including at least one gap having a width of at most about 1 micron.
According to the present invention there is provided a three dimensional display for presenting an illusion of parallax to a first and second eye of a user, including: (a) a source of light; (b) an array of a plurality of valves, in a common plane, for alternately transmitting and blocking the light; (c) a mechanism for directing the light via a first subset of the valves towards the first eye of the user; and (d) a mechanism for directing the light via a second subset of the valves towards the second eye of the user.
As used herein, the term "radiation" includes all forms of radiation, both particles and waves, to which the principles of the present invention are applicable. Thus, for example, the term "radiation", as used herein, includes, but is not limited to, electromagnetic radiation and acoustic radiation. The illustrative examples herein are directed towards electromagnetic radiation, and primarily towards visible and infrared radiation. The radiation may be collimated or uncollimated, coherent or incoherent.
As used herein, the term "transparent", used in connection with a substrate, means that the radiation can propagate through the substrate. In the case of a substrate transparent to electromagnetic radiation, such as visible light or infrared light, the substrate need not be homogeneous. The index of refraction of the substrate may vary continuously. There may be discrete regions of different indices of refraction in the substrate, and some of these regions may be holes in the substrate occupied by vacuum or air.
As used herein, the term "opaque" refers to a material through which the radiation does not propagate. This material may absorb the radiation, may reflect the radiation, or may absorb a portion of the radiation while reflecting another portion of the radiation.
As discussed in more detail below, the scope of the present invention includes an innovative method for fabricating mesoscale devices, including the step of directing a parallel beam of atoms of a deposant species at a substrate. As used herein, the term "mesoscale" refers to devices whose components whose length scales are on the order of about 0.1 micron to about 100 microns and which generally are fabricated by photolithography. Familiar examples of such devices include integrated chips. Note that the defining length scales refer to the components, and not to the devices themselves, which, in the present context, may be several tens of centimeters across.
As used herein, the term "deposant species" refers to a chemical element, alloy or compound deposited on a substrate by processes commonly used in photolithography, for example, vacuum evaporation and sputtering. As used herein, the term "atom" includes both neutral atoms and ions. The beam of deposant atoms need not be homogeneous. For example, in the deposition of a layer of silica, the beam includes both silicon atoms and oxygen atoms.
The principle of the present invention is illustrated in FIGS. 1 and 2. FIG. 1 is a perspective view of a basic valve 10 of the present invention. Perpendicular to a surface 13 of a transparent, electrically insulating substrate 12 are mounted two thin rectangular leaves 14 and 16 made of an opaque, electrically conducting material. Leaves 14 and 16 are mutually parallel, as shown. Leaf 14 is rigidly mounted on a transparent, electrically conducting pad 20. Similarly, leaf 16 is rigidly mounted on a transparent, electrically conducting pad 22. Pads 20 and 22 are separated from each other by a transparent, electrically insulating layer 24, preferably of the same material as substrate 12. The upper portion of the side 15 of leaf 14 that faces leaf 16 is covered with a barrier 18 of an electrically insulating material.
It is to be understood that the terms "transparent" and "opaque" are relative to the wavelength of radiation that valve 10 is intended to modulate. For example, for the modulation of visible light, leaves 14 and 16 typically are made of aluminum, substrate 12 typically is made of silica glass, and pads 20 and 22 typically are made of indium tin oxide.
Leaves 14 and 16 are thin enough to be elastically flexible along at least part of their length in the direction perpendicular to side 15. The orientations of leaves 14 and 16 as they bend towards and away from each other are parametrized by the distance d between the tops of leaves 14 and 16. Appropriate electrical voltages are applied to pads 20 and 22 to induce leaves 14 and 16 to bend together or apart by electrostatic attraction. FIG. 2 is a schematic plot of the equilibrium value of d as a function of the difference V between a voltage applied to pad 20 and a voltage applied to pad 22. When no voltage difference is applied, d is equal to d max , the separation of the bases of leaves 14 and 16. As V increases from 0, leaves 14 and 16 bend towards each other and d decreases, until point A on the curve is reached, at a critical voltage difference V CR at which the curve of d vs. V has a local maximum. At this point, leaves 14 and 16 snap together, as shown by the upper arrow, reducing d to the thickness l of insulating barrier 18. Note that in the absence of barrier 18, leaves 14 and 16 would discharge and snap apart. If V now is decreased, leaves 14 and 16 stay together until V is reduced to the threshold value V TH corresponding to d=l. At this point leaves 14 and 16 snap apart, as shown by the lower arrow. Thus, valve 10 is a bistable device that can be opened by setting V equal to a value V 1 less than V TH , closed by setting V equal to a value V 2 greater than V CR , and maintained in either orientation by setting V equal to a bias value V BIAS that is between, preferably halfway between, V TH and V CR .
The mode of operation described above is a digital mode, in which valve 10 alternately occupies one of two discrete states, open and closed. Valve 10 also can be operated in an analog mode, in the distance range A<d≦d max , to achieve a continuous range of partial blockage of radiation.
A single valve 10 provides temporal modulation of radiation that is normally incident on surface 13 from either side of substrate 12: when valve 10 is open, the radiation passes between leaves 14 and 16, and when valve 10 is closed, leaves 14 and 16 block the radiation. Preferably, the material of leaves 14 and 16 reflects the radiation, rather than absorbing the radiation. This has two beneficial effects. First, valve 10 can be used in either a transmissive mode or in a reflective mode. In the transmissive mode, the radiation target is on the other side of valve 10 from the radiation source. Radiation traverses valve 10 to reach the target when valve 10 is open, but not when valve 10 is closed. In the reflective mode, the radiation target is on the same side of valve 10 as the radiation source. Radiation is reflected from valve 10 to the target when valve 10 is closed, but not when valve 10 is open. Second, valve 10 can be used to modulate intense radiation without overheating. It is clear that an array of valves 10 can be arranged in rows and columns on surface 13 to provide spatial modulation as well. In such an array, pads 20 are sections of row control lines and pads 22 are sections of column control lines.
It will be readily appreciated that the present invention may be scaled to accommodate many different types of electromagnetic radiation for a host of applications. In a digital display panel based on an array of valves 10, the pixel size, determined by the distance d max , may be as small as several microns or as large as several centimeters. By making leaves 14 and 16 sufficiently thick, and applying correspondingly increased voltages to pads 20 and 22, valve 10 can be used to modulate x-rays.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is herein described, by way of example only, with reference to the accompanying drawings, wherein:
FIG. 1 is a perspective view of a valve of the present invention;
FIG. 2 illustrates the principle of the present invention;
FIG. 3 is a partial plan view of a valve array of the present invention;
FIG. 4 is a partial schematic diagram of the valve array of FIG. 3;
FIG. 5 shows a monochrome display pixel including valves of the present invention;
FIG. 6 shows a color display pixel including valves of the present invention;
FIGS. 7A-7F and 8A-8D show steps in the fabrication of the valve array of FIG. 3;
FIGS. 9A-9E show steps in the fabrication of a variant of the valve array of FIG. 3;
FIGS. 10A-10C show mesoscale structures of the present invention that cannot be fabricated by conventional photolithography;
FIG. 11 is a schematic illustration of a high definition television screen based on the valve array of FIG. 3
FIG. 12 is a schematic illustration of a three dimensional display based on the valve array of FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is of a valve, and an array thereof, which can be used to modulate radiation both spatially and temporally.
The principles and operation of a radiation valve array according to the present invention may be better understood with reference to the drawings and the accompanying description.
Referring now to the drawings, FIGS. 3 and 4 are partial illustrations of an array 30 of radiation valves of the present invention. FIG. 3 is a plan view. FIG. 4 is a corresponding schematic diagram. Shown in FIGS. 3 and 4 are four valves 32a through 32d, each with four leaves. Valve 32a includes leaves 14b, 16a, 16b and 14c. Valve 32b includes leaves 14d, 16c, 16d and 14e. Valve 32c includes leaves 14h, 16e, 16f and 14i. Valve 32d includes leaves 14j, 16g, 16h and 14k. Leaves 14a, 14f, 14g and 14l are parts of neighboring valves that are not shown in their entirety in FIG. 3. Leaves 14a through 14f are mounted on a row control line 26a. Leaves 14g through 141 are mounted on a row control line 26b. Leaves 16a, 16b, 16e and 16f are mounted on a column control line 28a. Leaves 16c, 16d, 16g and 16h are mounted on a column control line 28b. Row control lines 26a and 26b are orthogonal to column control lines 28a and 28b. Row control lines 26a and 26b are formed directly on substrate surface 13. Column control lines 28a and 28b are formed above, and are electrically insulated from, row control lines 26a and 26b. In FIG. 3, valve 32c is shown closed, and valves 32a, 32b and 32d are shown open.
The valves of array 30 are addressable in any desired combination, and so can be opened and closed in any desired combination, by applying appropriate voltages to the row and column control lines. Consider, for example, the method used to keep open valves 32a and 32d while closing valves 32b and 32c. Let Δ=(V 2 -V 1 )/4, and start with all four valves open. Apply a voltage of -Δ to row line 26a, a voltage of 0 to row line 26b, a voltage of V BIAS +Δ to column line 28a and a voltage of V BIAS to column line 28b. The resulting voltage differences are: for valve 32a, V BIAS +2Δ; for valve 32b, V BIAS +Δ; for valve 32c, V BIAS +Δ; and for valve 32d, V BIAS . Valve 32a closes, while the other three valves remain open. Next, apply a voltage of 0 to row line 26a, a voltage of -Δ to row line 26b, a voltage of V BIAS to column line 28a and a voltage of V BIAS +Δ to column line 28b. The resulting voltage differences are: for valve 32a, V BIAS ; for valve 32b, V BIAS +Δ; for valve 32c, V BIAS +Δ; and for valve 32d, V BIAS +2Δ. Valve 32d closes, while valves 32b and 32c remain open. Because the voltage difference applied to valve 32a is between V TH and V CR , valve 32a remains closed. In general, any desired configuration of open and closed valves is obtained by opening all the valves, which can be done by grounding all the row control lines and applying a voltage of V BIAS -2Δ to all the column lines; and then successively applying a voltage of -Δ to each row line while grounding the other row lines and applying a voltage of V BIAS +Δ to all the column control lines whose valves are to be closed in the target row. This voltage application scheme is illustrative. Those skilled in the art will be able to readily develop equivalent schemes.
One straightforward application of the present invention is in a flat panel display. Each pixel of the display is composed of one valve, or several contiguous valves. FIG. 5 shows schematically a pixel 34 of a monochromatic display. Pixel 34 is composed of sixteen valves 36a through 36p. A 16 level gray scale is obtained via spatial modulation by opening any number of valves between none and all for the duration of one frame of the display. One particularly convenient way of selecting valves to open and close is to represent the intensity as a four-digit binary number and to assign specific groups of valves to the first, second, third and fourth digits, with the relative areas of the groups being in accordance with the significance of the corresponding digits. For example, valves 36a through 36h are assigned to the first digit, valves 36i through 36l are assigned to the second digit, valves 36m and 36n are assigned to the third digit and valve 36o is assigned to the fourth digit. If "1" means open and "0" means closed, and if the 16 levels of a gray scale are represented by binary numbers from 0000 and 1111, then, with valve 36p open, any one of the 16 levels is accessed by opening or closing the valves corresponding to each digit. In addition, closing all 16 valves provides a 17th level.
Alternatively, the valves of a single pixel may have different areas. For example, pixel 34 can be composed of 5 valves: a first valve having eight times the area of valves 36 and occupying the area of valves 36a through 36h, a second valve having four times the area of valves 36 and occupying the area of valves 36i through 36l, a third valve having twice the area of valves 36 and occupying the area of valves 36m and 36n, and valves 36o and 36p as before. The first valve is assigned to the first digit of the four-digit binary number that represents the intensity, the second valve is assigned to the second digit of the binary number, the third valve is assigned to the third digit of the binary number, and valve 36o is assigned to the fourth digit of the binary number.
As another alternative, a 16 level gray scale is obtained via temporal modulation, specifically, pulse width modulation, by opening valves 36 for between 1/16 and all of the duration of a single frame. Temporal and spatial modulation can be combined to produce a 256-level gray scale. Doubled resolution can be obtained by frame averaging, using the fact that the perceived gray level of a pixel in two successive frames is the average of the actual gray levels of the pixel in the two frames.
FIG. 6 shows schematically a pixel 38 of a color display. Pixel 38 includes three groups of valves. Valves 40a through 40l are backed by red filters. Valves 42a through 42l are backed by green filters. Valves 44a through 44l are backed by blue filters. Arbitrary hues and intensities are obtained by opening and closing the appropriate valves for varying lengths of time during a single frame.
As is well known in the art, a color display can be achieved by other means. For example, an array of valves 34 can be used in a projector with a rotating color wheel that includes a red filter, a green filter and a blue filter. The wheel is rotated so that red light is directed at valves 34 for the first third of the duration of each frame, green light is directed at valves 34 for the middle third of the duration of each frame, and blue light is directed at valves 34 for the last third of the duration of each frame.
The above description relates to a transmissive-mode flat panel display. A monochromatic reflective-mode flat panel display is operated in the manner described above in connection with FIG. 5, except that the roles of closed valves 36 and open valves 36 are interchanged, so that the greater the number of valves 36 that block and reflect incident light, and the longer these blocking valves 36 are closed, the more intense is pixel 34.
To achieve 600 dpi resolution, pixels 34 and 38 should be about 40 microns on a side. This gives a lateral dimension for valves 36 of about 10 microns by 10 microns, and for valves 40, 42 and 44 of about 6 microns by 6 microns. In a projector, valves 36, 40, 42 and 44 typically are on the order of 5 to 10 microns on a side. In a flat panel display having pixels 34 or 38 that are 280 microns on a side, valves 36, 40, 42 and 44 are correspondingly larger.
Array 30 is fabricated by standard methods, such as are used to fabricate microelectronic devices, with one additional innovative process step.
The first step is the deposition of row lines 26 on surface 13 of substrate 12, as shown from above in FIG. 7A and from the side, along cut B--B, in FIG. 7B. The second step is the deposition of insulating strips 46 orthogonal to row lines 26 and column lines 28 above insulating strips 46, as shown from above in FIG. 7C and from the side, along cut B--B, in FIG. 7D. The third step is the deposition of a layer 20 to 30 microns deep of photoresist 48 with rectangular holes 50 oriented as shown with respect to row lines 26 and column lines 28, as shown from above in FIG. 7E and from the side, along cut B--B, in FIG. 7F.
The next steps, in which leaves 14 and 16 are deposited, are illustrated in FIGS. 8A through 8D, which are enlarged views of the portion of FIG. 7F that is enclosed in a dashed box. FIGS. 8A and 8B show a hole 50 bounded by vertical surfaces 52 and 53 of photoresist 48. Hole 50 constitutes a gap between vertical surfaces 52 and 53 that is free of photoresist. A layer 58 of aluminum is deposited on surface 53 by directing a parallel beam of aluminum atoms at holes 50 at an oblique angle α from the vertical, so that the photoresist adjacent to surface 52 shadows beam 54, preventing deposition at the bottom of hole 50 to the left of surface 53. This is done by conventional vacuum evaporation. See, for example, Handbook of Thin Film Technology (L. I. Maissel and R. G. Lang, editors, McGraw Hill, 1970): Chapter 1, "Vacuum evaporation", pages 1-3 and 1-55; Chapter 7, "Generation of patterns in thin films", page 7-1. After a thickness of aluminum between about 50 nanometers and about 100 nanometers is deposited to form layer 58, a layer 60 of between about 250 nanometers and about 400 nanometers of amorphous silica is deposited over layer 58, and another layer 62 of between about 50 nanometers and about 100 nanometers of aluminum is deposited over layer 60. Like layer 58, layers 60 and 62 are deposited by directing parallel beams of the deposited material at holes 50 at an oblique angle slightly different from α. At the end of the fabrication process, layers 58 and 62 will be leaves 14.
The same process is used to deposit a 50 to 100 nanometer thick layer 64 of aluminum, a 250 to 400 nanometer thick layer 66 of amorphous silica, and another 50 to 100 nanometer thick layer 68 of aluminum on surface 52, by directing parallel beams 56 of the deposited material at surface 52 at an oblique angle β, as illustrated in FIG. 8B. The result of this deposition is illustrated in FIG. 8C. At the end of the fabrication process, layers 64 and 66 will be leaves 16. Photoresist 48 now is removed, to leave layer sandwiches 58-60-62 and 64-66-68 as freestanding vertical walls. This process for forming a freestanding vertical wall on a substrate also is within the scope of the present invention. Amorphous silica is deposited around and above the freestanding walls and etched back to the level shown in FIG. 8D. The remaining amorphous silica 70 serves to anchor the resulting leaves 14 and 16. Note that this etchback also removes most of the amorphous silica of layers 60 and 66. Finally, the oblique deposition process is used, at a steep angle, to deposit amorphous silica contact barriers 18 towards the top of the outside surface of either the left leaf of each pair of leaves 14 and 16, as shown in FIG. 8D, or of the right leaf of each pair. In this final step, each pair of leaves 14 or 16 serves to shadow the pair of leaves immediately to its right or left.
FIGS. 9A through 9E show steps in the fabrication of a variant of array 30. FIG. 9A corresponds to FIG. 7E and shows that in this variant, there are no column lines 28 deposited directly above insulating strips 46, and photoresist 48 is deposited as parallel walls perpendicular to row lines 26, with gaps 50' separating the walls of photoresist 48. The walls of photoresist 48 have sides 52' and 53' that are perpendicular to surface 13 of substrate 12. FIG. 9B shows a cut along one of surfaces 52' after the deposition thereon of aluminum layer 64', which corresponds to aluminum layer 64 of FIG. 8C. Layer 64' is deposited through a mask, leaving gaps above row lines 26 through which surface 52' is exposed. The thin portions of layer 64' that are separated from row lines 26 by insulating strip 46 will be sections of a column line 28'. FIG. 9B also shows that in this variant, substrate 12 includes holes 11 opposite the eventual locations of the valves. FIG. 9C shows a similar cut along one of surfaces 53' after the deposition thereon of aluminum layer 58', which corresponds to aluminum layer 58 of FIG. 8C. Like layer 64', layer 58' is deposited through a mask, leaving gaps above row lines 26 through which surface 53' is exposed. FIG. 9D corresponds to FIG. 8D, and shows that at the end of fabrication, layer 64' has become a leaf 16' of one pair of leaves 16', and layer 58' has become a leaf 14' of another pair of leaves 14'. FIG. 9E is a plan view of a portion of this variant of array 30 at the end of fabrication. The common root of each leaf pair 16' is a portion of a column line 28'.
The masks through which layers 58' and 64' are deposited may be conventional photolithography masks. Alternatively, the masks may be provided by forming the walls of photoresist 48 with appropriate cutouts.
Note that in this variant of array 30, column lines 28' are deposited, along with leaves 16', on surfaces 52' of the walls of photoresist 48 instead of directly on surface 13 of substrate 12. In both this variant and the first variant, row lines 26 and column lines 28 or 28' are elongated parallelepipeds, with their long dimensions as long as surface 13 of substrate 12. Row lines 26 and column lines 28 have their short dimensions perpendicular to surface 13 and their intermediate dimensions parallel to surface 13. Column lines 28' have their short dimensions parallel to surface 13 and their intermediate dimensions perpendicular to surface 13. In FIG. 9E, the double-headed arrow shows the intermediate dimension of one of row lines 26. In FIG. 9D, the double-headed arrow shows the intermediate dimension of a column line 28'.
It will be appreciated that the techniques used to fabricate valve array 30 are applicable to the fabrication of mesoscale devices generally, and in particular to the fabrication of walls, perpendicular to substrates such as substrate 12, that are too thin or too high to be fabricated by prior art photolithography methods. FIGS. 10A through 10C are illustrative cross sections through structures that cannot be fabricated by prior art photolithography methods but can be fabricated by the method of the present invention. FIG. 10A shows walls 84, perpendicular to a surface 82 of a substrate 80, and having heights h of 5 microns and thicknesses t of 1 micron. FIG. 10B shows a layer 86 of thickness h of 5 microns above substrate 80, with gaps 88 in layer 86 of width t of 1 micron. Such extreme aspect ratios are not attainable using prior art photolithography methods. FIG. 10C shows double-layered walls deposited on substrate 80. Uniform layers 90 may be deposited either by photolithography or by the method described above of depositing photoresist walls on substrate 80, depositing layers 90 obliquely on the photoresist walls, and removing the photoresist. Layers 92, whose thicknesses increase with distance from substrate 80, are deposited on layers 90 by using layers 90 to shadow the gaps therebetween and continuously increasing the oblique angle at which the deposant of layers 92 is directed at substrate 82.
FIG. 11 shows, schematically, a high definition television screen 78 fabricated as a four-part flat panel display of the present invention. Each independently operated portion 76 of television screen 78 includes an array 72 of valves of the present invention, similar to array 30 described above, and associated control electronics 74 for selective application of activation voltages to the row lines and column lines of array 72. Upper left portion 76a includes valve array 72a and control electronics 74a. Upper right portion 76b includes valve array 72b and control electronics 74b. Lower left portion 76c includes valve array 72c and control electronics 74c. Lower right portion 76d includes valve array 72d and control electronics 74d. Because arrays 72 are fabricated using the same methods as are used to fabricate integrated circuits, television screen 78 can be fabricated as an integrated device. For special applications, control electronics 74 include read only memory areas that are loaded, at fabrication, with application-dependent data and/or random access memory areas that can be programmed by users with application-dependent data. For example, in high definition television screen 78, the read-only memory is programmed with color parameters conforming to either the European standard or the American standard, so that valves analogous to valves 40, 42 and 44 can be opened and closed accordingly.
The protocol for opening and closing the valves of arrays 72 takes advantage of the mechanical properties of the valves. Valves fabricated as described above typically take about 5 microseconds to close, but only about 1.5 microseconds to open. In one of flat panel display portions 76, even if there is only one valve per pixel, setting all 540 lines independently of each other would require 540×6.5 microseconds=3.51 milliseconds. This is too long to achieve 16 gray scale level in a 16.6 millisecond (1/60 second) frame. Therefore, each flat panel display portion 76 is operated by operating all 540 lines independently, in 16 subframes per frame. In the first subframe, all the lines are closed successively. After each line is closed, and before the next line is closed, the valves, of the line that has just been closed, that correspond to pixels whose gray scale level=full illumination, are opened. As noted above, this takes 3.51 milliseconds. In each remaining subframe, the lines are scanned, and, in each line, all the valves that should be opened for the remaining duration of the entire frame are opened. For example, in the second subframe, all valves corresponding to pixels whose gray scale level=15/16 of full illumination are opened. Each of subframes 2 through 16 takes only 1.5×540 microseconds=0.81 milliseconds, so that the total time needed to display one frame is 15.66 milliseconds.
Control electronics 74 can be configured and used for other applications. For example, a device including array 72 and control electronics 74 can be used as a shutter in a slide projector or a movie projector, with control electronics 74 included in a feedback circuit that monitors the screen illumination and regulates the opening of the valves of array 72 to keep the screen illumination uniform. Similarly, in a projector that projects an image of a color display, if the display is created using a device similar to high definition television screen 78, color fidelity can be corrected by a similar feedback circuit that includes control electronics 74. The fact that control electronics 74 is displaced laterally from valve arrays 72 has the advantage, in applications such as projectors, of keeping control electronics 74 away from the intense incident light, thereby making it easier to keep control electronics 74 from overheating.
FIG. 12 shows schematically the use of an array 94 of interleaved valves 96r and 96l of the present invention as a component of a three-dimensional display, to provide the illusion of parallax to a user 90. Light 104 from a source 102 is collimated by a collimator, represented by convex lens 100, and directed at array 94. Array 94 includes, for each valve 96r or 96l, a refractive optical element 98r or 98l, specifically, a prism. Prisms 98r refract light 104 towards the right eye 92r of user 90. Prisms 98l refract light 104 towards the left eye 92l of user 90. Valves 96r are opened and closed in accordance with the display to be projected to right eye 92r. Valves 96l are opened and closed in accordance with the display to be projected to left eye 92l. For simplicity, only one row of array 94 is shown, it being understood that array 94 includes many such rows to project in dependent two-dimensional images at eyes 92r and 92l. Also for simplicity, all valves 96r and 96l are shown open. The leaves of valves 96r and 96l are moved in a direction perpendicular to the plane of FIG. 12 to open and close valves 96r and 96l.
While the invention has been described with respect to a limited number of embodiments, it will be appreciated that many variations, modifications and other applications of the invention may be made.
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A radiation valve includes a transparent substrate and at least one opaque flexible planar member, rigidly attached to the substrate, that alternately assumes a closed orientation relative to the substrate to block the radiation and an open orientation relative to the substrate to pass the radiation. Preferably, the valve includes two parallel electrically conducting planar members that are perpendicular to the substrate when the valve is open. The valve is closed by imposing a voltage difference on the two planar members to snap their tops together. An array of such valves can be controlled to modulate the radiation temporally and spatially, for applications such as flat panel displays. This array is fabricated by steps including the formation of temporary surfaces perpendicular to the substrate; depositing a deposant at an oblique angle to the substrate, the temporary surfaces shadowing each other so that the deposant is deposited only on the temporary surfaces to form the planar members; and removing the temporary surfaces, leaving behind only the planar members.
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BACKGROUND OF THE INVENTION
This invention relates generally to nonwoven tubular filters. In one aspect, the invention relates to the manufacture of nonwoven tubular filters in which nonwoven fibers are deposited on a rotating mandrel. In another aspect, the invention relates to the withdrawal of the tubular filter formed on a rotating mandrel.
Nonwoven fabric, particularly meltblown fabric, have long been used as filters. Because of the microsize of the filters (i.e. microporosity) and the random collection of the fibers, the meltblown fabrics exhibit excellent properties of filtration at reasonable pressure losses. Meltblown fabrics are generally made by forming a web which can be readily converted to a plainer filter. For example U.S. Pat. 4,714,647 discloses the manufacture of meltblown filters, wherein fibers of the same composition but different sizes are collected on a horizontal plane and used as a multi-layered filter.
It is difficult to convert meltblown webs into tubular filters because of the need for tubular filters to be continuous without a bonding seam. For example, if the web disclosed in U.S. Pat. Nos. 4,714,647 were rolled into a tube, a seam would be required to secure the inner and outer edges to the tube body.
Efforts have been made to form the meltblown web directly into a tube continuously on a mandrel. For example, in U.S. Pat. Nos. 3,933,557 and 4,032,688,meltblown fibers are deposited onto a rotating mandrel forming a tube which is continuously withdrawn and cut to proper length for the filter. The meltblowing die is positioned at an angle with respect to the axis of the mandrel so that a variation in density of the fibers is achieved as the tube moves longitudinally on the mandrel through the zone of fiber deposition.
U.S. Pat. Nos. 4,112,159 and 4,116,738 also disclose the deposition of meltblown fibers onto a rotating mandrel. The apparatus disclosed in these patents, however, deposit the fibers onto a core so that the final tubular filter comprises the core and the fibers wound about the core.
U.S. Pat. No. 4,021,281 discloses the deposition of meltblown fibers onto a rotating drum to form a relatively large diameter tube which is then flattened thereby forming a two-layer web. The web then is wound about a core material forming a tubular filter. The filter, however, is not continuous.
U.S. Pat. No. 4,594,202 discloses an apparatus for forming tubular filters by depositing meltblown fibers onto a drum which are then rolled onto a mandrel.
As discussed in U.S. Pat. No. 4,714,647, in many filters it is desirable to have a variable fiber size gradient across the filter. The fiber size gradient across the filter (i.e. in the direction of fluid flow) combines the filtration efficiency of each filtration layer. As described in U.S. Pat. 4,714,647, the first layer comprises meltblown fibers having large fiber size, the intermediate layers have medium fiber size, and the-final layer has small fiber size. The pore size is a function of fiber size so that the filtration of the laminate described above would result in the separation of large particles in the first layer, medium size particles in the second layer, and finally the smallest particles in the final layer.
The same filtration principles would apply in tubular filters. However, it has been difficult to provide a continuous filter having a fiber size gradient across the radius of the filter.
SUMMARY OF THE INVENTION
The method and apparatus of the present invention produces a seamless, continuous nonwoven tube which is ideally suited for tubular filter application.
In a preferred embodiment, the tube or tubular filter produced by principles of the present invention comprises a multi-layer tube, with each layer having different characteristics, dimensions, or properties. For example, the tube may have a fiber size gradient differing radially between the layers.
The apparatus of the present invention briefly comprises a die having a row of orifices, divided into at least two side-by-side groups; a rotating mandrel positioned in alignment with the row of orifices to receive and wind up the filaments extruded therefrom; and means for extruding polymer through the orifices of each group at a different rate. Preferably, such means comprises two pumps (one for each orifice group).
In operation of the apparatus, the rate of polymer passing through each orifice group may be varied so that the filaments from one group collected on the mandrel therefrom are different in size from the filaments of the other group or groups. This produces a multi-layered tubular filter wherein each layer may be varied to enhance filtration, as by providing a fiber size gradient along the radius of the tube.
The method carried out by the apparatus includes the steps of meltblowing filaments from a first row of orifices onto a rotating mandrel to form a first layer thereon, meltblowing filaments from a second row of orifices onto the first layer of filaments to form a composite of two layers, and continuously withdrawing the composite from the mandrel. Composites of more layers may be formed by adding third or fourth groups in the orifice row. The process may be carried out by a single die constructed to permit separate control of polymer throughput or composition extruded through selected groups of orifices of the die. The process forms a novel multilayer tube wherein the filaments of each layer have different properties or dimensions.
Another important feature of the present invention is the mandrel assembly for continuously discharging the nonwoven tube. The mandrel assembly comprises two concentric, corotating shafts. The outer shaft is hollow and has a smooth surface for receiving and winding up filaments extruded from the majority of the orifices. The inner shaft is concentrically mounted in the outer Shaft and has an end portion extending axially outwardly therefrom. The end portion is threaded and is positioned to receive and wind up filaments extruded from a minor portion of the orifices. The inner shaft (including the threaded end portion) is driven at a slightly higher rpm than the outer shaft so that the tube of filaments collected and wound about the mandrel, by action of the threads engaging the inner surface of the filament tube, is moved along the mandrel and discharged off the distal end of the inner shaft.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of the apparatus constructed according to the present invention.
FIG. 2 is an end view of the apparatus shown in FIG. 1 from the perspective indicated by the plane of 2:2 of FIG. 3.
FIG. 3 is a top plan view of the apparatus shown in FIG.1
FIG. 4 is an enlarged view of the die body and pump assembly shown in FIG. 3, with portions cut away.
FIG. 5 is an enlarged, partially sectional view, of the die assembly shown depositing webs of various sizes onto a rotating mandrel.
FIG. 6 is a cross-sectional view of a tubular filter having a fiber size gradient across the radius thereof.
FIG. 7 is a sectional view showing the mandrel and drive mechanism.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to FIG. 1, the apparatus for manufacturing meltblown tubular filters comprises meltblowing system 10, a mandrel assembly 11, and a cutting and collecting assembly 12.
Briefly, the mandrel assembly is provided with a rotating mandrel 13 which is positioned in longitudinal alignment with the die of the meltblowing system 10. Fibers 14 extruded from the die are deposited and wound around the rotating mandrel 13 forming a tube 16 of random fibers. The tube 16 is moved across the length of the meltblowing die in alignment with the row of fibers 14 causing the tube 16 to grow in diameter as additional fibers are wound thereabout. The full diameter tube 16 is driven off the end of the mandrel 13 and cut to the proper filter length forming tubular filter 18. The filters 18 may be collected in suitable container 19. The main components may be mounted on a frame 21.
Details of the present invention will be described with reference to the Meltblowing System 10, the Mandrel Assembly 11, and the Cutting and Collecting Assembly 12.
Meltblowing System
With reference to FIG. 2, the meltblowing system 10 comprises a plurality of meltblown units, each of which includes die assembly 22, a pump assembly 23, a pump manifold 24, a drive shaft 26, an electric motor 27, motor controls 28, and a sensor assembly (e.g. tachometer) 29. The drive shaft 26 may also include an electromagnetic clutch 31 and coupling 32. Hot air through lines 33a and 33b, each of which may include an in-line heater. 34a and 34b, is delivered to opposite sides of the die assembly 22. The rotating mandrel 13 is positioned below the die assembly 22 for receiving the meltblown fibers discharged therefrom to form tube 16.
In FIGS. 3 and 5, the different meltblowing units of the system 10 are designated by different letters with the same reference numeral for the corresponding part described above. For example, pump 23A is driven by motor 27A through shaft 26A. The pump 23A feeds polymer melt to a longitudinal portion of die assembly 22 designated 22A (see FIG. 5).
Although the present invention is described with reference to three die assembly units 22A, 22B, and 22C, the die assembly 22 may include a plurality of units ranging from 2 to 100, preferably 2 to 50, most preferably 2 to 20. (The dashed lines in FIG. 5 indicate the separate die assembly units 22A, 22B, and 22C.)
FIG. 4 depicts only one of the meltblowing units or component thereof of the meltblowing system, and is described without reference to the letters (i.e., A-C). It should be understood, however, that each meltblowing unit has components corresponding to those depicted in FIG. 4, unless otherwise indicated.
With reference to FIGS. 2 and 3, the melt-blowing system 10 operates as follows: polymer melt is delivered to the apparatus through lines 36a and 36b into manifold 37. The manifold 37 contains passages (described below) which conduct the polymer melt to each of the pump assemblies 23A-23C, and from there to the separate die units 22A-22C of the die assembly 22 where the melt is extruded as a plurality of side-by-side fibers 14 (best seen in FIG. 5). Converging hot air delivered to the die via air conduits 33a and 33b contacts the extruded fibers 14 and stretches them into microsized fibers. These fibers collect on the rotating mandrel 13 in a random manner forming a nonwoven seamless tube 16. (The terms "filaments" and "fibers" as used herein are interchangeable.)
As described in detail below, the rotating mandrel 13 causes the nonwoven tube 16 formed thereon to move parallel to the die 22 under each unit 22A, 22B, and 22C. Thus, the initial annular deposits of the meltblown fibers onto the mandrel 13 will have the characteristics of the fibers exiting unit 22A, and the second annular layer deposited on the first annular layer will have the characteristics of the fibers received from unit 22B, and finally the outermost annular layer will have the characteristics of the fibers received from unit 22C.
An important feature of the present invention is the variability of each of the layers. By controlling the extrusion conditions (e.g. polymer throughput of each unit) or varying the equipment (e.g. size of orifices of each unit), the properties of the layers may be determined. Also, the present invention contemplates the selective addition of additives such as powders, liquids, etc. to one or more of the polymer streams flowing through each unit. It is also within the skill of the art based on the present disclosure to modify the manifold 37 so that units can be fed with one or more of a different polymer than the other unit or units. Thus the tubular filter will have distinct radial layers which have different properties than the other layers. This permits the tailoring of the tubular filter for a variety of different filtering conditions.
As best seen in FIG. 2, the meltblowing die assembly 22 comprises an elongate die body 39, a die tip assembly 41 connected to the bottom of the die body 39. The die body and die tip components, as well as other parts of the system exposed to the high meltblowing temperatures may be machined from steel or steel alloys.
Referring to FIG. 4, the die body 39 has formed therein intersecting polymer flow passages 42 and 43 for each unit. Passage 42 is aligned with a polymer flow passage in the pump manifold 24 and passage 43 extends vertically in body 39, exiting at the underside thereof and serves to conduct polymer to the die tip assembly 41 as described below.
The manifold 24 and die body 39 may be provided with electric heaters (not shown) to heat and maintain the polymer passing therethrough at the desired temperature.
Returning to FIG. 2, the die tip assembly 41 is made up of three parts: (1) a transfer plate 46, (2) a die tip 47, and (3) air plates 48a and 48b. The transfer plate 46 may be bolted to the underside of the die tip 47 and this assembly bolted to the die body 39.
The transfer plate 46 extends substantially the entire length of the die body 39 (see FIG. 5) and has formed therein a polymer passage 51 (disclosed as 51A, 51B, and 51C) for each of the meltblowing units 22A-22C. The flow passage 51 exits into an elongate groove (semicircular in cross-section) formed in the underside of the transfer plate 46, which in combination with a similar groove formed in the upper side of the die tip 47 defines an elongate chamber 52 for each unit (i.e. 52A, 52B, and 52C).
The die tip 47 has formed therein a nose section 53 of triangular cross section which is flanked by elongate flanges 56 and 57 (see FIG. 2). The nose section 53 terminates in an apex 58, through which are drilled a plurality of orifices 59 (see also 59A-59C in FIG. 5). Channel 61 interconnects chamber 52 of each unit with a linear portion of the orifices 59. Thus, chamber 52A is in fluid communication with orifices 59A through channel 61A. Chambers 52B and 52C similarly are interconnected with orifices 59B and 59C, respectively, through channels 61B and 61C. The orifices 59 are aligned in a row along the apex 58. It is preferred that the orifices 59 are equally spaced along the full length of apex 58 as illustrated in FIG. 5.
Air plates 48a and 48b are mounted on the die body 39 as described in detail in U.S. patent application Ser. No. 757,848, filed Sep.11, 1991, now U.S. Pat. No. 5,236,641, the disclosure of which is incorporated herein by reference. The air plates 48a and 48b are adjustable, thereby permitting the adjustment of the dimensions referred to in the art as setback and air gap.
The inner surface of each air plate 48a and 48b is tapered and in combination with the flanking surfaces of the triangular nose section 53 define converging air passage 38a and 38b. The setback and air gap determine the geometry of air passages 38a and 38b.
Air passages 62a and 62b conduct hot air from lines 33a, 33b to air passages 38a and 38b, respectively. The air lines 33a and 33b are connected to the longitudinal mid-section of each air passage 62a and 62b.
Referring to FIGS. 2 and 5, polymer flow through each die assembly unit 22A, 22B, and 22C is via passages 42 and 43 of each unit, through passage 51 of transfer plate 46, into chamber 52, through channel 61 and, finally, through orifices 59; whereas, air from the inlet pipes 33a and 33b flows through passages 62a and 38a on one side of the orifices 59, and passages 62b and 38b on the other side, exiting as converging air sheets at apex 58 on opposite sides of the extruded fibers 14. The polymer flow paths through the meltblowing units 22A, 22B and 22C are parallel and independent of each other.
The hot air delivered to opposite sides of the die assembly 22 by lines 33a and 33b may include an in-line electric air heater 34a and 34b (see FIG. 1) which may be of the same construction as described in U.S. Pat. No. 5,145,689, the disclosure of which is incorporated herein by reference. Alternatively, the hot air may be provided by an electric or gas furnace. A compressor or blower (not shown) may be used to deliver air at the desired pressure (2 to 20 psi) to the inlet of die assembly 22.
The die body 39, transfer plate 46 (see FIG. 5), and die tip 47, as well as the air plates 48a and 48b are of the same general length, traversing the full length of the row of orifices 59. The die body 39, while being of unitary construction may be viewed as separate side-by-side sections provided with flow passages 42A, 42B, and 42C and 43A, 43B, and 43C. Likewise, the die tip assembly 41 may be viewed as separate side-by-side units having inlets 51A, 51B, and 51C feeding end-to-end chambers 52A, 52B, and 52C, respectively, which in turn feed orifices 59A, 59B, and 59C through passages 61A, 61B, and. 61C, respectively. Each side-by-side unit as described above operates independently from the other units. Thus, polymer entering passage 43A is extruded through orifices 59A only, 43B through 59B only, and 43C through 59C only.
While the polymer flow is through separate meltblowing units 22A, 22B and 22C in the system, only one air delivery system is provided. The air flow is through two main passages which converge from opposite sides of the nose piece 53 as described above in relation to FIG. 2. The air passages are not divided into units but extend substantially the entire length of the die.
As shown in FIG. 4, the die inlet polymer flow passage 42 (shown in FIG. 5 as 42A, 42B, and 42C for a die with multiple units 22A, 22B, and 22C, respectively), is fed by pump 23. The polymer flow to and from the pump 23 of each unit is provided by passages formed in the header manifold 37 and pump manifold 24. Polymer is delivered to a passage 66 in header manifold 37 which distributes the flow to a plurality of flow passages 67 of the header manifold 37. Manifold 24 has formed therein a pump suction passage 68 which registers with header manifold passage 67a and the inlet of pump 23. A pump outlet passage 69 extends from the outlet of the pump 23 to register with inlet passage 42 of die body 39.
The polymer flows into the header manifold 37 from lines 36a and 36b (see FIG. 3) and is distributed through header passage 66 to unit feed passages 67, one for each pump assembly 23A, 23B, and 23C. Polymer is fed to pumps 23A-23C through passage 68, and discharged from the pumps through passages 69, respectively, to die body inlet passages 42A-42C and outlet passages 43A-43C, respectively. The header passage 66 may be provided with a porous filter.
It should be noted that the header passage 66 may be constructed to feed only one or two of the distribution passages 67 and other polymer connections can be used to feed a different polymer or polymer formulation. For example, line 36a can be connected to passage 66 which feeds only distribution passage 67 for passage 42A and line 36b can feed passages 42B and 42C. The tubular filter made from this system would consist of one seamless annular layer of one polymer fiber and two seamless annular layers of a different polymer.
The pump 23 of each meltblowing unit may be any positive displacement pump as depicted in FIG. 4 which provides a fluid output rate proportional to drive shaft rotation rate. The preferred positive displacement pump is a gear pump which comprises a driven gear 71 keyed to shaft 26, and an idler gear (not shown). The gears are mounted in a suitable housing 70, the interior chamber 72 of which is in fluid communication with suction passage 68 and outlet passage 69. Rotation of the gears pumps polymer entering from passage 68 around the periphery of chamber 72 into outlet passage 69. Conventional packing and bearings may be employed in the gear pump.
As shown in FIG. 2, the drive shaft 26 is driven by a variable speed motor 27 through gear box 73. The drive shaft 26 may also include a coupling 32 and electromagnetic clutch 31. The clutch 31 is a safety device to prevent damage to the motor if the pump 23 fails. The output shaft 26 extends through the gear box 73 terminating in pump speed sensor gear 74. It is preferred that the electric motor 27 be variable speed and have an rpm output between 1500 to 2000, and that the gear box 73 have a gear reduction ratio of 20 to 1. An electric motor that has proven successful in the apparatus of the present invention is manufactured by Baldor. This 1725 rpm motor with gear reducer box provides an output range of 0 to 104 rpm. A sensor probe 29 such as a proximity switch or digital pulse encoder is used to detect the rpm of shaft 26 via gear 74. Each motor 27A-27C controls polymer throughput through its respective unit, independent of the other units. Motor controller 28 with input from the sensor 29 provide means for controlling motor rpm and hence polymer throughput through each unit, independent of the other units. As seen in FIG. 3, each unit includes a separate sensor 29A-29C and controller 28A-28C.
Although an almost infinite number of combinations and sizes of the meltblowing system components described above are possible, the following indicates the typical and preferred ranges.
______________________________________ MOST PRE- PREFERRED BROAD FERRED RANGE RANGE RANGE (BEST MODE)______________________________________Length of Die 1-150 4-150 6-150(inches)Number of Units 2-100 2-50 2-20Length of Units 0.5-12.0 1-8 1.5-3.0(inches)Orifice Diameter 0.010-0.080 0.010-0.040 0.015-0.030(inches)Orifices/inch 10-50 15-40 20-30Gear Pump Capac- 1-20 2-12 4-10ity (for each Unitlbs/hr)Polymer Flow Rate 1-20 2-12 4-10(per unit lbs/hr)Polymer Flow Rate 0.8-3 0.9-2 1.0-1.6(per orificegrams/min)Air Gap (inches) .010-.200 .020-.150 .040-.120Set Back (inches) .010-.200 .020-.150 .040-.120Air Capacity 5-30 10-25 15-20(SCFM/inch)______________________________________
The apparatus of the present invention, because of the simple configuration of dividing the row of orifices into a plurality of groups, offers the advantage of providing the filter with small graduation of fiber size differences. For 2 to 100 orifice groups (preferably 2 to 50) groups, for example, the differences in average fiber size diameter can be small, differing by at least 10%. For fewer groups, the size difference should be at least 20%.
The meltblowing system of the present invention has been described in somewhat simplified form for clarity. In practice, many of the components illustrated as unitary bodies, such as die body and manifolds, may be made in two or more parts to facilitate assembly. Also, the system may include hoods or housings for safety and operation protection.
Details of the complete meltblowing system are described in U.S. patent application Ser. No. 757,848, referred to above.
FIG. 5 illustrates schematically the deposition of polymer fiber 14 extruded from each die unit 22A, 22B, and 22C onto a rotating mandrel 13. The fibers are wound around the mandrel 13 forming a tube 16 which, by means described below, is moved in succession under orifices 59A, 59B, and 59C. The unique construction of the meltblowing system 10 permits the fibers extruded from each die assembly unit 22A, 22B, and 22C to form annular layers of different properties or characteristics. For example, in one embodiment the orifices 59A may be larger than the orifices 59B which in turn are larger than the orifices 59C. The filter tube 16 made from this construction (as shown in FIG. 6) has an inner annular portion 76A of large fibers (e.g. from 3.0 to 10 microns) and the middle annular portion 76B of intermediate sized fibers (e.g. from 2 to 5 microns), and an outer annular portion 76C of small diameter fibers (e.g. from 0.75 to 3 microns. The average fiber sizes thus range from 0.75 to 10 microns. The size differences in the layers may be varied in any order. Generally, the average fiber size in one layer should be between 1.1 to 3, preferably 1.5 to 2 times that of the average fiber size of an adjacent layer. Size differentiation between layers 76A, 76B, and 76C may also be achieved by varying the polymer throughput through each unit by operation of pumps 23A, 23B and 23C. In this embodiment polymer throughput through unit 22A would be greatest, producing the largest fiber diameter for layer 76A, with pumps 23B and 23C being progressively less producing medium fiber size for layer 76B and smallest fibers for layer 76C.
Other variations of the filter tube construction are possible with the present meltblowing system and are described below under "Operation".
Mandrel Assembly
As indicated above, the mandrel assembly 11 provides rotating mandrel 13 for forming the meltblown tube and advancing it linearly underneath and parallel to the row of orifices 59 as fibers are deposited and wound thereon.
As best seen in FIGS. 3 and 7, the rotating mandrel 13 comprises an outer shaft 81, an inner shaft 82, and a threaded screw take-off shaft 83 secured to and in axial alignment with the inner shaft 82 as at 84. The inner shaft 82 and screw take-off 83 rotate as a unit and are journaled to rotate relative to outer shaft 81 by bearing 86.
The outer shaft 81 is journaled in outer shaft bearing housing 87 by spaced apart bearings 88 and 89. An end of the outer shaft 81 extends a short distance out of housing 87 and is keyed to pulley 91.
The inner shaft 82 extends without interference through the outer shaft 81, including housing 87, through pulley 91 and is journaled to its own housing 92 by spaced apart bearings 93 and 94. Shaft 82 extends through housing 92 and is keyed to pulley 96. The inner shaft 82 and screw take-off 83 are rotatable independently of outer shaft 81. As shown in FIG. 7, the take-off screw 83 is threaded and the outer periphery of shaft 81 is smooth. The outer diameter of shaft 81 is approximately equal to the outer diameter of the threads of shaft 83.
Referring to FIG. 3, pulley 96 is driven by motor 97 through belt 98 which drivingly connects pulley 96 and motor pulley 99. Similarly pulley 91 is driven by motor 101 through belt 102 trained around motor pulley 103 and shaft pulley 91.
The motors 97 and 101 may be variable speed D.C. motors and the pulley sizes are selected so that the shafts 81 and 82 are driven at an rpm of between 200 to 2000. Independent controls (not shown) are provided for each motor 97 and 101 to provide for independent rpm control of the motors and hence the shafts.
Although the size (diameter) of the shafts 81 and 83 can vary within a relatively wide range, the following dimensions are suitable for making filters having a core opening of 0.75 to 4 inches.
______________________________________ Broad Preferred Range (in.) Range (in.)______________________________________Shaft 81 - Diameter 0.5-20 1-5Length 3-60 5-30Screw Take-off 83Diameter 0.75-20 1-5Length 1-20 1.5-15______________________________________
The screw 83 is threaded in relation to its direction of rotation to force tube 16 to move to the right as disclosed in the drawings.
The length of shaft 82 and screw take-off 83 are sized in proportion to the length of the row of orifices 59. As a general rule, more than 50% and up to 75% of the orifice row is traversed by the smooth shaft 81 and about 25% to 50% of the orifices row 59 is traversed by the screw take-off 83. The outer end of the screw 83 extends well beyond the die assembly 22 to permit cutting of the tube 16 to the proper length without interfering with the tube formation. The components of the mandrel assembly described above may be mounted on frame 21.
Although the preferred mandrel assembly 11 is as described above, other mandrel assemblies may be used in connection with certain aspects of the present invention. For example, the assembly disclosed in U.S. Pat. No. 3,933,557 comprising external rollers may be used, the disclosure of which is incorporated herein by reference.
Tube Cutting and Collection Assembly:
As schematically illustrated in FIG. 1, the cutting assembly 12 comprises a rotating blade 17 mounted on the shaft of motor 106. The motor 106 may be mounted on the frame 21 to permit adjustment of the blade 17 and permit movement of the motor and blade in a vertical plane to cut tubular lengths 18 from the tube 16 being discharged off screw 83.
The blade is preferably composed of steel or tungsten and is rotated at from 1000 to 3000 rpm. The blade 17 motor 106 are pivotable or otherwise movable as by a hydraulic ram to cause the blade to move in a vertical plane and sever the filter tube 18 from tube 16 as illustrated in FIG. 1. The tube 18 may be collected in a container 19 as schematically illustrated in FIG. 1. More sophisticated collection methods of course may be employed such as conveyors.
Operation:
The operation of the apparatus described above will be described with reference to the following example.
A meltblowing system 10 comprising die assembly 22 having three units was mounted on frame 21 in relation to the mandrel assembly 11 and cutting assembly 12. The dimensions and construction of the meltblowing system were generally within the most preferred ranges recited above. The meltblowing system was movably mounted on tracks (not shown) secured to the frame to permit its withdrawal and access to the die assembly 22 for repair, maintenance, and adjustment.
The row of orifices need not be parallel to the mandrel, but should lie in the same vertical plane and are positioned from 2 to 20 inches above the mandrel 13.
The die assembly 22 may be fed by a conventional extruder in a conventional hook-up to lines 36a and 36b or it may be fed by the polymer delivery system disclosed in U.S. Pat. No. 5,061,170.
Any polymer capable of being meltblown may be used. The typical meltblowing web forming resins include a wide range of polyolefins such as propylene and ethylene homopolymers and copolymers. Specific thermoplastics include ethylene acrylic copolymers, nylon, polyamides, polyesters, polystyrene, poly-(methyl-methacrylate), polytrifluoro-chloroethylene, polyurethanes, polycarbonates, silicone sulfide, and poly(ethylterephthalate), pitch, and blends of the above. The preferred resin is polypropylene. The above list is not intended to be limiting, as new and improved meltblowing thermoplastic resins continue to be developed. Hot melt adhesives may also be used.
The operating temperature of the meltblowing system will, of course, depend on the resin employed, but for PP (MFR of 800), they may be as follows:
Polymer temperatures: 475° to 520° Fahrenheit
Air temperatures: 500° to 750° Fahrenheit.
The mandrel assembly 11 included 1 inch diameter outer shaft 81, 11/4 inch diameter (threaded section) screw shaft 83 and a 5 thread inch pitch. The motor rpms and pulley ratios were sized to rotate the shafts 81 and 83 at 900 rpm and 1000 rpm, respectively, during operation.
The mandrel 13 was placed under the row of orifices at a distance of 12 inches, and the cutting blade 17 was positioned to cut filter lengths of 10 inches off tube 16.
The pumps 23A, 23B, and 23C were each driven at a rate to provide a flow through orifices as follows:
______________________________________Orifices 59A 0.5 Gr./orificeOrifices 59B 0.8 Gr./orificeOrifices 59C 1.5 Gr./orifice______________________________________
This produced variable fiber size of each annular layer A, 76B, and 76C as follows (for radially inward flow filter):
______________________________________ Average Fiber Diameter (microns)______________________________________Inner Layer 76A 1.8Middle Layer 76B 3Outer Layer 76C 5______________________________________
Upon startup shaft 81 and screw 83 were rotated at the same rpm to initiate tube formation thereon. When a sufficient tube 16 was formed, the screw take-off 83 was driven slightly faster (approximately 15%) than shaft 81. The screw take-off 83 engaging the interior of the tube drives the tube to the right as viewed in FIG. 1. As the full diameter tube 16 is withdrawn, the thinner tube portion forming under orifices 59 are pulled along the smooth shaft 81. The diameter of tube 16 is thus increased as it moves progressively under orifices 59A, 59B, and 59C. The diameter of each annular layer 76A, 76B, and 76C can be controlled by the rpms of shaft 81 and screw take-off 83 as well as the polymer flow through orifices 59A, 59B, and 59C.
The final size and composition of the filter tube 18 will depend upon the intended use of the filter and can vary within wide limits. The following ranges and compositions are merely presented as representative examples:
______________________________________Annular Radial Length Average FiberThickness (Inches) (Inches) Diameter (microns)______________________________________Layer 76A 0.5 to 1.5 4-12 1 to 10Layer 76B 0.25 to 1.5 4-12 2 to 10Layer 76C 0.25 to 1.5 4-12 3 to 10______________________________________
It should be observed that the transition from the layer-to-layer (e.g. 76A and 76B) as the tube 16 moves from orifices 59A to 59B is extremely smooth because of the in-line deposition of the fibers. In addition, it is well known in the art that nonwoven fabrics are held together by a combination of filament entanglement and inter-filament bonding while still in the molten state during deposition. In nonwoven tubes constructed according to present invention, there is no distinct transition from layer-to-layer in terms of the filament entanglement and bonding. There is, however, a measurably distinct transition in average filament diameter from layer-to-layer. The resulting tube 16 and filter 18 exhibit excellent structural integrity and minimal delamination.
The above description of the operation is given in reference to a specific filter. It is to be understood that wide variations in the tubular filter composition and dimensions are possible. For example, a number of layers may be made by simply increasing the number of meltblowing units in the die. Also, different polymers may be used in each unit so that the final tubular filter may contain multiple layers of different fiber sizes and/or compositions. Also, the variations of polymer flow or polymer description through each unit may be in any order.
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An apparatus and method for producing a meltblown continuous and seamless nonwoven tube is described. The apparatus comprises a meltblowing die for extruding two groups of polymer thermoplastic filaments onto a rotating mandrel to form a multilayer layer tube thereon. The tube is withdrawn from the mandrel by a rotating screw. The present apparatus is capable of producing nonwoven tubes having variable fiber diameters and/or composition in the radial direction, making them ideally suited for filtration purposes.
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BACKGROUND OF THE INVENTION
The present invention relates to lubricating devices. More particularly, it relates to lubricating devices which are capable of dispensing very accurate quantities of special lubricants at very low flow rates for lubricating tools and work pieces during machining operations.
SUMMARY OF THE INVENTION
As is known, during machining operations large amounts of heat are generated by the friction between the tool and work piece. If not effectively dealt with, this heat is highly undesirable since it leads to the early dulling or failure of the tool; or it may render the tool inoperable in other ways, such as by welding to it chips of metal formed during the machining operations.
One conventional way of solving the problem of excessive heat buildup during machining operations is to apply special lubricants to the tool and work piece which are so effective at reducing the friction between the tool and work piece that the heat generated during machining operations is reduced to acceptable levels. Said special lubricants are applied at very low flow rates to the tool and work piece; and are essentially consumed during the machining operations.
Some examples of said special lubricants are Boelube brand lubricant and Accu-Lube brand lubricant; both of which are liquids at room temperature. Boelube comprises high carbon (long carbon chain) fatty alcohols and is manufactured by the Orelube Corporation located in Plain View, N.Y. Accu-Lube comprises fractions of fatty acids and fatty alcohols, and is sold by Lubricating Systems, Inc. of Kent, Wash.
Although the exact flow rates of said special lubricants will vary somewhat depending on the particular special lubricant being used, on the particular machining operation being conducted, on the hardness and metal from which the work piece is made, on the particular machine tool being used, etc., typically such flow rates will be in the range of from about 0.10 to about 10.0 cc's (cubic centimeters) per minute.
However, the use of such very low flow rates of said special lubricants does present several problems. For example, since said special lubricants are typically very expensive, it will be appreciated that if the flow rate of said special lubricants is higher than is required for effective machining operations, costly wastage will occur. On the other hand, if the flow rate is too low, loss of the tool, and possibly the work piece, may result. Accordingly, extremely precise metering of such very low flow rates is imperative.
In addition, since the exact flow rates of said special lubricants which are needed will vary according to the particular special lubricant being used, the particular machining operations being performed, the particular machine tool being used, the hardness and type of the metal from which the work piece is made, etc., it is essential that it be possible to achieve very small changes in the already very low basic flow rate of said special lubricants which is consistent with superior tool life and operation.
Further, it is necessary that the lubricating apparatus which delivers such very low flow rates of said special lubricants be highly reliable. This is because if it fails to continuously deliver the precise flow rate of said special lubricants which is required, loss of the tool, and possibly the work piece, will occur shortly after the flow of said special lubricants is too low or is interrupted.
Accordingly, one of the objects of the present invention is to provide a highly reliable, precision, very low flow rate lubricator for machining operations. Another object of the present invention is to provide such a lubricator which has the further capability of having its flow rates selectively adjustable in minute amounts for the optimum minimum delivery of said special lubricants to the tool and work piece.
In basic form, the lubricator of the present invention comprises a precision, positive displacement, pneumatic injection pump which delivers an output pulse of lubricant to a lubricant output tube in response to each input air pulse which is delivered to it. The lubricant output tube is adapted to convey the lubricant output pulses to the machine tool where they are then applied to the tool and work piece by any suitable conventional means.
The lubricator of the present invention may be provided with two internal check valves. One check valve achieves one of the objects of the present invention, which is to prevent back flow of lubricant from the lubricator into the lubricator's source of lubricant during the pumping stroke of the lubricator's piston. The other check valve achieves another of the objects of the present invention, which is to prevent back flow of lubricant from the lubricator's lubricant output tube into the lubricator during the return stroke of the lubricator's piston.
The lubricator of the present invention may also be provided an adjustable stop which controls the travel of the lubricator's piston, and which thus controls the amount of lubricant pumped by each pumping stroke of the piston. Preferably, the adjustable stop is provided with positive stops for its minimum and maximum adjustments, which achieves another of the objects of the present invention, namely, to prevent the user from endlessly turning the adjustable stop in either direction with no further actual adjustment in amount of lubricant pumped by the piston.
Since many machine tools incorporate a pneumatic chip blower and may use compressed air to apply said special lubricants to the tool and work piece, a further object of the present invention is to conveniently supply both said special lubricants and compressed air to the machine tools. To this end, the lubricator of the present invention may be internally arranged so that its lubricant output tube and its atomizing air output hose are coaxially arranged, with its lubricant output tube running inside of its atomizing air output hose.
In addition, the lubricator may include needle valve means for selectively varying the amount of atomizing air which it delivers to its atomizing air output hose. Naturally, if only lubricant is needed by a particular machine tool, the flow of compressed air from the lubricator can be cut off by using the lubricator's needle valve means or by cutting off the lubricator's source of compressed air. Similarly, if only compressed air is needed by a particular machine tool, the flow of lubricant from the lubricator can be cut off by using the adjustable stop for the lubricator's piston, by cutting off the lubricator's source of input air pulses, or by cutting off the lubricator's source of lubricant.
A further object of the present invention is to provide a lubricator which can simultaneously supply lubricant and compressed air to more than one machine tool; with the amount of lubricant and compressed air being supplied to each machine tool being independently controllable This object is achieved by providing the lubricator with stackable valve bodies; with each valve body being used to supply lubricant and atomizing air to its respective machine tool. The valve bodies are constructed so that the lubricator's input lubricant, input air pulses and input compressed air are shared by all of the valve bodies; whose air relief means are in fluid communication with each other.
It should be understood that the foregoing is intended to be a brief, not an exhaustive, summary of the objects, features, advantages and characteristics of the present invention, since these and further objects, features, advantages and characteristics of the present invention will be directly or inherently disclosed to those skilled in the art to which it pertains by the following, more detailed description of the present invention.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a partially exploded, perspective view of the present invention;
FIG. 2 is a bottom plan view of the invention's upper plate;
FIG. 3 is a bottom plan view of the invention's lower plate;
FIG. 4 is a top plan view of the invention's valve body;
FIG. 5 is a bottom plan view of the invention's valve body;
FIG. 6 is a partial cross-sectional view taken generally along line 6--6 of FIG. 1, with some parts shown in elevation;
FIG. 7 is a partial cross-sectional view taken generally along line 7--7 of FIG. 6, with some parts shown in elevation; and
FIG. 8 is a cross-sectional view taken generally along line 8--8 of FIG. 6, with some parts shown in elevation.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Construction of the Invention
Turning now to FIG. 1, the lubricator of the present invention is shown generally designated at 10. In basic form, lubricator 10 comprises an upper plate 12, a valve body 14 and a lower plate 16 which are assembled together with a pair of assembly bolts 18. Bolts 18 pass through bolt holes 20, 22 in upper plate 12 and valve body 14, respectively, and are screwed into threaded bores 24 in lower plate 16. Upper and lower plates 12, 16 and valve body 14 can be made from any strong, crack resistant metal or plastic Due to its complexity, valve body 14 is preferably injection molded from plastic or die cast from metal in order to help minimize its cost.
As seen in FIGS. 1 and 2, upper plate 12 includes a threaded lubricant input bore 25, which is adapted to be connected by any conventional means to a source of lubricant. Each of upper plate 12's bolt holes 20 is sized to receive the head of its respective bolt 18 within it; and includes an internal shoulder 27 (see FIG. 2), which acts as a stop for its respective bolt 18 when the bolt's head is flush with upper plate 12's top surface.
Referring now to FIGS. 1 and 3, it is seen that lower plate 16 has a threaded atomizing air input bore 26 with an O-ring recess 28 for O-ring 30; a threaded piston air pulse input bore 32 with an O-ring recess 34 for O-ring 36; a threaded piston air relief bore 38 with an O-ring recess 40 for O-ring 42; and a blind bore 44 which forms an O-ring recess for O-ring 46. Rubber O-rings 30, 36, 42 and 46 form seals between corresponding portions of the top of base plate 16 and the bottom of valve body 14.
Lower plate 16's threaded atomizing air input bore 26 is adapted to be connected by any conventional means to a compressed air source. The pressure of the compressed air delivered to lubricator 10 from the compressed air source will be selected by the particular user in accordance with his needs and the particular machine tool being used. However, typically, a machine tool's chip blower and lubricant atomizer or applicator use compressed air having pressure of about 80 pounds per square inch (psi).
Lower plate 16's threaded air pulse input bore 32 is adapted to connected to any conventional source of pulses of compressed air, such as an air logic device made by Crouzet Division Aerospatial, 62-64 Emile Zola Avenue, Paris, France 75115 under part number 81 532 001 for the air logic device's base, and part number 81 506 820 for the air logic device's main body. Said air logic device is designed to operate with an input air pressure of 42 to 120 psi and will, in response to its input air, deliver output pulses of compressed air with an air pulse frequency which is selectively adjustable from 0 to 180 air pulses per minute. Because said air logic device will generate its output air pulses with an input air pressure of 42 to 120 psi, the device is relatively immune to the changes in air pressure typically encountered in a manufacturing facility's installed compressed air system, thus enhancing the reliability of lubricator 10.
Lower plate 16's threaded piston air relief bore 38 can either communicate directly with the atmosphere, or, if desired, it can be connected to any conventional conduit means so that it communicates with the atmosphere at a location which is remote from lubricator 10.
The top of lower plate 16 has a peripheral locating shoulder 48 which mates with a corresponding peripheral locating recess 50 (see FIG. 5) in the bottom of valve body 14, for accurate registration of lower plate 16 and valve body 14 with respect to each other when lubricator 10 is assembled.
Referring now to FIGS. 1 and 4, it is seen that valve body 14 includes a vertical atomizing air input bore 52 with an 0-ring recess 54 for 0-ring 56; a vertical lubricant input bore 58 with an 0-ring recess 60 for 0-ring 62; a vertical piston air relief bore 64 with an 0-ring recess 66 for 0-ring 68; and a vertical piston air pulse input bore 70 with an 0-ring recess 72 for 0-ring 74. Rubber 0-rings 56, 62, 68, 74 form seals between corresponding portions of the top of valve body 14 and the flat, smooth bottom of upper plate 12. The top of valve body 14 includes a locating shoulder 76 whose purpose will be described below. When lubricator 10 is assembled, there is fluid communication between valve body 14's bore 58 and upper plate 12's bore 25. When lubricator 10 is assembled, upper plate 12's smooth, flat bottom surface acts as a plug for the upper ends of valve body 14's bores 52, 64, 70. Alternatively, an air relief bore could be provided in upper plate 12 which was in fluid communication with valve body 14's vertical piston air relief bore 64.
Referring now to FIG. 5, it is seen that the bottoms of the valve body 14's atomizing air input bore 52, lubricant input bore 58, piston air relief bore 64 and piston air pulse input bore 70 are each provided with a flat 0-ring seal surface 77 for their respective 0-rings 30, 46, 42 and 36. When lubricator 10 is assembled, there is fluid communication between valve body 14's bores 52, 64, 70 and lower plate 16's bores 26, 38, 32, respectively; while lower plate 16's blind bore 44 acts to plug the lower end of valve body 14's bore 58.
Alternatively, when lubricator 10 has only one valve body 14, upper and lower plates 12, 16 could be eliminated. In such an event, one end of valve body 14's bores 52, 58, 64, 70 would be plugged by any suitable conventional means; and other end of valve body 14's bores 52, 58, 64, 70 would be connected by any suitable conventional means to a compressed air source, to a lubricant source, to the atmosphere, and to an input air pulse source, respectively.
Naturally, upper plate 12's lubricant input bore 25 and lower plate 16's blind bore 44 could be interchanged. Similarly, one or more of lower plate 16's bore's 26, 38, 32 could be located in upper plate 12; and for each bore which was so located in upper plate 12, lower plate 16 would be modified to act as a plug for valve body 14's corresponding bore 52, 64, 70, respectively.
As was mentioned above, in basic form, lubricator 10 comprises an upper plate 12, a valve body 14 and a lower plate 16, all of which are assembled together with a pair of bolts 18. However, it is within the scope of the present invention for two or more valve bodies 14 to be used, with the valve bodies 14 being stacked on top of each other between upper and lower plates 12, 16. For example, if two valve bodies 14 were used, then the peripheral locating shoulder 76 in the top of the lower valve body 14 would be fitted into the peripheral locating recess 50 in the bottom of the upper valve body 14 for accurate registration of the two valve bodies 14 with respect to each other. As many valve bodies 14 can be stacked on top of each other between upper and lower plates 12, 16 as is desired.
If two or more valve bodies 14 are used, each lower valve body 14 is provided with a set of 0-rings 56, 62, 68, 74 to provide a seal between its bores 52, 58, 64, 70 and the corresponding bores 52, 58, 64, 70 in the adjacent valve body 14 above it. In addition, assembly bolts 18 would be selected to have a length sufficient to hold top plate 12, valve bodies 14 and bottom plate 16 assembled together. If two or more valve bodies 14 are used, there is fluid communication between their respective bores 52, 58, 64, 70.
Turning now to FIG. 6, it is seen that a horizontal, longitudinal main bore 78 extends the complete length of valve body 14. The right hand portion of main bore 78 defines a lubricant pumping chamber 102, a piston air relief chamber 104 and a piston air pulse input chamber 106. Air relief chamber 104 is in fluid communication with vertical piston air relief bore 64; and air pulse input chamber 106 is in fluid communication with vertical air pulse input bore 70.
As seen in FIGS. 1 and 6, the right hand portion of main bore 78 carries a piston assembly 80 and a stop assembly 82.
Piston assembly 80 comprises a piston return spring 84, a piston lubricant seal (a rubber 0-ring) 86, a brass piston 88 and a rubber piston air seal 90. As seen in FIGS. 1 and 6, piston 88 is a one-piece member comprising, from left to right, a piston shaft 92 having an annular recess 94 for lubricant seal 86; an annular shoulder 96; and a piston head 98 having an annular recess 100 for piston air seal 90. Piston lubricant seal 86 and piston air seal 90 are assembled to piston 88 by passing them over piston shaft 92 and piston head 98, respectively, until they are seated in their respective annular recesses 94, 100.
As seen in FIG. 6, piston return spring 84 is located in piston air relief chamber 104. Alternatively, piston return spring 84 could be suitably sized to fit inside, and could be located inside, lubricant pumping chamber 104.
Referring again to FIGS. 1 and 6, it is seen that stop assembly 82 comprises an adjustable brass stop 110, a stop seal (a rubber 0-ring) 112, and a brass stop nut 114. Stop 110 is a one-piece member comprising, from left to right, a stop shaft 118 which butts against piston 88's head 98; an annular shoulder 120; a neck 122 having an annular recess 124 for stop seal 112; and a threaded head 126 which screws into stop nut 114. Stop seal 112 is assembled to stop 110 by passing it over stop neck 122 until it is seated in its annular recess 124. Stop 110 and stop nut 114 are assembled together by screwing stop 110's threaded head 126 into stop nut 114.
In order to assemble valve body 14, piston assembly 80, and stop assembly 82 together, piston spring 84 is first inserted over piston 88's shaft 92 until it butts against piston shoulder 96. Then piston 88 (with its lubricant seal 86, air seal 90 and spring 84) is inserted into main bore 78 until it is positioned as seen in FIG. 6. Last, stop nut 114 (with its stop 110 and stop seal 112) is screwed all of the way into the right hand end of main bore 78 until it makes sealing contact with valve body 14's annular ridge seal 122, as is also seen in FIG. 6.
Referring now to FIGS. 6 and 8, a horizontal, transverse lubricant input bore 128 provides fluid communication between vertical lubricant input bore 58 and main bore 78. Lubricant input bore 128 includes an enlarged portion in which is located a conventional lubricant input check valve comprising check ball 130 and check spring 132. After check ball 130 and check spring 132 are inserted into transverse lubricant input bore 128, they are held in place by plug 134 which is secured in lubricant input bore 128 by any conventional means, such as by gluing or by a tight, leak proof friction fit. Alternatively, a conventional check valve, which served the same purpose as said lubricant input check valve, could be located outside of lubricator 10 between the lubricant source and upper plate 12's lubricant input bore 25.
Referring now to FIGS. 1 and 6, it is seen that the left hand portion of main bore 78 carries an atomizing air/lubricant output assembly 136. Atomizing air/lubricant output assembly 136 comprises an atomizing air output hose 138, a lubricant output tube 140, a barb fitting 142, a lubricant output seal 144, and a conventional lubricant output check valve comprising a lubricant output check spring 146 and a lubricant output check ball 148. Alternatively, a conventional check valve, which served the same purpose as said lubricant output check valve, could be located outside of lubricator 10 in or at the end of its lubricant output tube 140.
In order to assemble valve body 14 and atomizing air/lubricant output assembly 136 together, lubricant output check ball 148 and lubricant output check spring 146 are first inserted into main bore 78 until they are located as seen in FIG. 6. Next, rubber or soft plastic lubricant output seal 144 is inserted into main bore 78 until it is located as seen in FIG. 6, where it is held in place by a snug, leak proof friction fit. Then lubricant output tube 140 is inserted into lubricant output seal 144, as seen, where it is held in place by a snug, leak proof friction fit. Next, barb fitting 142 is passed over lubricant output tube 140 and is then screwed into the left end of horizontal, transverse bore 78 until it makes sealing contact with valve body 14's ridge seal 150, as seen. Barb fitting 142's threads are straight rather than tapered, in order to help prevent valve body 14 from being split when barb fitting 142 is screwed into it. A seal between barb fitting 142 and valve body 14 is provided by valve body 14's ridge seal 150, rather than by any tapering of barb fitting 142's threads. Last, atomizing air output hose 138 is passed over lubricant output tube 140, and is then passed over and secured to barb fitting 142 as seen.
As best seen in FIGS. 6 and 7, the left hand portion of main bore 78 defines an atomizing air chamber 153; and as best seen in FIGS. 1, 6 and 7, valve body 14 defines a transverse, horizontal atomizing air bore 152 which is in fluid communication with vertical atomizing air input bore 52 and atomizing air chamber 153. The internal diameter of the bore in barb fitting 142 is sized considerably larger than the outside diameter of lubricant output tube 140; in order to permit the free flow of atomizing air from atomizing air chamber 153 to atomizing air output hose 138 through barb fitting 142.
Referring now to FIGS. 1 and 7, atomizing air chamber 153 carries an atomizing air needle valve assembly 154 which comprises a brass needle valve nut 156, a brass needle 158 and a needle valve seal (a rubber 0-ring) 160. Needle valve assembly 154 is generally of conventional construction.
Needle 158 has an annular recess 162 for needle valve seal 160, and has a threaded head 164. Needle valve seal 160 is assembled to needle 158 by passing it over needle 158 until it is seated in its needle valve recess 162. Needle 158 is assembled to needle nut 156 by screwing its head 164 into needle nut 156. Valve body 14 and needle valve assembly 154 are then assembled together by screwing needle nut 156 (with its needle 158 and needle valve seal 160) into atomizing air chamber 152 until it makes sealing contact with valve body 14's ridge seal 166, as seen.
OPERATION OF THE INVENTION
Before lubricator 10 is ready for operation, certain connections need to be made.
A source of lubricant is connected to top plate 12's threaded lubricant input bore 25. Since lubricant input bore 25 is in fluid communication with the vertical lubricant input bore 58 of each valve body 14, input lubricant is thereby provided to each valve body 14.
A source of compressed air pulses is connected to bottom plate 16's threaded air pulse input bore 32. Since air pulse input bore 32 is in fluid communication with the vertical air pulse input bore 70 in each valve body 14, compressed air pulses are thereby provided to each valve body 14.
Bottom plate 16's threaded piston air relief bore 38 may be permitted to vent directly to the atmosphere; or if remote venting is desired, an air relief line may be connected to bottom plate 16's threaded piston air relief bore 38. Since piston air relief bore 38 is in fluid communication with each vertical piston air relief bore 64 in each valve body 14, piston air relief is thereby provided for each valve body 14.
A source of pressurized atomizing air is connected to bottom plate 16's threaded atomizing air input bore 26. Since atomizing air input bore 26 is in fluid communication with the vertical atomizing air input bore 52 in each valve body 14, atomizing air is thereby provided for each valve body 14.
Once the above connections have been made, lubricator 10 is then primed by allowing it to run for a short time until air bubble free lubricant flows out of the free end of lubricant output tube 140. Once lubricator 10 has been primed, its operation is as follows.
Referring now to FIG. 6, upon the delivery of a compressed air pulse to valve body 14's air pulse input chamber 106 from the source of pressurized air pulses via air pulse input bore 70, the compressed air pulse acts on piston air seal 90 and piston head 98. This forces piston 88 to move to the left and compress piston return spring 84. As piston 88 moves to the left, it forces lubricant out of lubricant pumping chamber 102, thereby forcing check ball 148 to open and permit lubricant to be forced through lubricant output tube 140. While this is happening, back flow of lubricant from the central portion of main bore 78 into vertical lubricant input bore 58 through horizontal transverse lubricant input bore 128 is prevented by check ball 130 and check spring 132, as best seen in FIG. 8. As piston 88 is being forced to the left by the input air pulse, the air in air relief chamber 104 which is compressed by piston 88 exits chamber 104 through vertical piston air relief bore 64, to vent, directly or indirectly, to the atmosphere.
When the input air pulse is over, piston return spring 84 forces piston 88 to move to the right to its starting position. As piston 88 starts to move to the right, check spring 146 forces check ball 148 closed, thereby preventing any back flow of lubricant from lubricant output tube 140 into main bore 78 of valve body 14. As piston 88 is moving to the right, a negative pressure is formed in lubricant pumping chamber 102 which immediately sucks check ball 130 open, thereby permitting lubricant from vertical lubricant input bore 58 to be sucked into lubricant pumping chamber 102 through transverse lubricant input bore 128. As piston 88 is moving to the right, a negative air pressure is formed in air relief chamber 104, thereby sucking air into chamber 104 from vertical piston air relief bore 64. As piston 88 is moving to the right, it also compresses the air in air pulse input chamber 106 and forces it out of chamber 106 through vertical air pulse input bore 70. The source of compressed air pulses which is connected to vertical air pulse input bore 70 is preferably constructed so that, between delivering air pulses to input bore 70, it vents to the atmosphere the air which is forced out of chamber 106 by piston 88.
The amount of lubricant which is pumped by each pumping stroke of piston 88 is governed by how far piston 88 travels in response to each input air pulse. In turn, the amount of travel of piston 88 is governed by the adjustment of stop 110.
Referring now to FIG. 6, as stop 110's threaded head 126 is screwed clockwise, the left end of stop 110's shaft 118, which butts against piston 88's head 98, forces piston 88 to the left. As stop 110's threaded head 126 is screwed clockwise further and further, the left end of piston 88's shoulder 96 will eventually be forced into contact with piston stop shoulder 108 of main bore 78. This results in zero travel of piston 88 and no lubricant being pumped by piston 88. Thus, piston stop shoulder 108 and piston 88 act, in effect, as a fixed positive stop for the clockwise adjustment of stop 110; while piston stop shoulder 108 acts as a fixed positive stop for the lower pumping limit for each pumping stroke of piston 88, which is zero.
If stop 110's threaded head 126 is then screwed counterclockwise, the travel of piston 88 is thereby permitted to increase in direct proportion to how far threaded head 126 is screwed counterclockwise. Thus, the amount of lubricant pumped by each pumping stroke of piston 88 is also thereby permitted to increase in direct proportion to how far threaded head 126 is screwed counterclockwise. As stop 110's threaded head 126 is screwed counterclockwise more and more, further movement of stop 110 will eventually be prevented when its shoulder 120 contacts the left end of stop nut 114. Thus, stop nut 114 acts as a fixed positive stop for the counterclockwise adjustment of stop 110; meaning that it acts as a fixed positive stop for the upper pumping limit of each pumping stroke of piston 88.
Thus, it is seen that the adjustment by stop 110 of both the upper and lower pumping limits for each pumping stroke of piston 88 is subject to positive stops. This is desirable since it prevents the possibility that stop 110 could be turned endlessly in either direction without any actual adjustment of the amount of lubricant being pumped by lubricator 10.
As was discussed above, the exact flow rates of said special lubricants which the user will require lubricator 10 to deliver to the tool and work piece will vary according to the particular special lubricant being used, the particular machining operation being performed, the particular machine tool being used, the hardness and type of the metal from which the work piece is made, etc. However, lubricator 10 will typically be required to provide substantially continuous flow rates of said special lubricants in the range of from about 0.10 to about 10.0 cc's per minute. Although, as mentioned above, the source of compressed air pulses can provide 0 to 180 compressed air pulses per minute; it is preferred that it be adjusted to deliver from about 20 to about 60 compressed air pulses per minute, so that lubricator 10 will deliver lubricant substantially continuously to its lubricant output tube 140.
When the typical flow rates of lubricant and preferred number of air pulses per minute which were mentioned above are used, the amount of lubricant which lubricator 10 will deliver to its lubricant output tube 140 for each pumping stroke of its piston 88, will range from about 0.0017 cc's to about 0.5 cc's per minute. It is preferred that pumping chamber 102, piston assembly 80 and stop assembly 82 be sized and arranged so that the amount of lubricant pumped by each pumping stroke of piston 88 can be varied by as little as about 0.0001 cc, or less. It is also preferred that lubricator 10 provide lubricant to lubricant output tube 140 at pressures of up to about 10,000 psi. This is done by suitably selecting the pressure of the input compressed air pulses, and by suitably selecting the size of lubricator 10's pumping chamber 102 and piston assembly 80. The valve body 14 illustrated in the figures is about four inches long, about 1 and 1/2 inches wide and about 1 and 1/4 inches thick; with its various components being sized accordingly.
Turning now to FIGS. 6 and 8, the rate of flow of atomizing air from vertical atomizing air input bore 52 through horizontal atomizing air bore 152 to atomizing air chamber 153 and atomizing air output hose 138 is governed by needle valve assembly 154. If threaded needle valve head 164 is screwed clockwise as far as it will go, then the left end of needle 158 will plug horizontal atomizing air bore 152, thereby cutting off the flow of atomizing air to atomizing air chamber 153 and atomizing air output hose 138. If threaded needle valve head 164 is then screwed counterclockwise, the rate of flow of atomizing air through horizontal atomizing air bore 152 to atomizing air chamber 153 and atomizing air output hose 138 is thereby permitted to increase in direct proportion to how far threaded needle valve head 164 is screwed counterclockwise. Although the pressure and rate of flow of the atomizing air delivered by lubricator 10 to atomizing air output hose 138 will depend upon the needs of the user, typically the atomizing air will be delivered by lubricator 10 at pressures of about 80 psi and at flow rates of up to about 3 to 4 cubic feet per minute (cfm). Since the pressure of the atomizing air which is delivered by lubricator 10 is essentially the same as the pressure of the input compressed air which is provided to lubricator 10, it is apparent that by suitably selecting the pressure of the input compressed air to lubricator 10 the user can control the pressure of the atomizing air which is delivered by lubricator 10. If a greater flow rate of atomizing air is needed, then the size of all of the components through which the atomizing air passes in lubricator 10 can be increased accordingly.
In view of the foregoing, these and further modifications, adaptations and variations of the present invention will now be apparent to those skilled in the art to which it pertains, within the scope of the following claims. It is understood that the foregoing forms of the invention were described and/or illustrated strictly by way of non-limiting example.
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A precision, highly reliable, positive displacement, pneumatic lubricant for pumping lubricant to a tool and work piece during machining operations; and for delivering compressed atomizing air thereto. The lubricator pumps lubricant substantially continuously at highly accurate, very low flow rates which can be minutely varied according to the needs of the user. The lubricator's piston delivers one pulse of lubricant for each input air pulse which is supplied to the lubricator from a source of input air pulses. The lubricator includes internal check valves for preventing back flow of lubricant into the lubricator's source, and for preventing back flow of pumped lubricant into the lubricator. The lubricator has an adjustable stop which controls the stroke of its piston, and which thus controls the amount of lubricant which is pumped by each pumping stroke of its piston. The lubricator also has positive stops for the maximum and minimum adjustment of its adjustable stop. The positive stops prevent endless turning of the lubricator's adjustable stop in either direction with no change being made in the amount of lubricant pumped by each pumping stroke of its piston. The lubricator's valve body is made stackable so that one lubricator may comprise several valve bodies; each valve body being able to independently deliver lubricant and atomizing air to its respective tool and work piece through coaxial atomizing air/lubricant output lines. If the lubricator has more than one valve body, their lubricant input means, air pulse input means, air relief means, and compressed air input means are in fluid communication with each other.
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This application is a divisional application of application Ser. No. 08/952,445 filed Nov. 18, 1997, now U.S. Pat. No. 6,368,833, which is a 371 national phase filing of International Application Ser. Number PCT/US97/17614 filed Sep. 29, 1997, which is a continuation-in-part application of application Ser. No. 08/722,713 filed Sep. 30, 1996, now abandoned.
BACKGROUND OF THE INVENTION
The present invention is directed to a novel esterolytic enzyme, novel genetic material encoding that enzyme and esterolytic proteins developed therefrom. In particular, the present invention provides an esterase derived from Aspergillus , a DNA encoding that esterase, vectors comprising that DNA, host cells transformed with that DNA and a protein product produced by such host cells.
Xylan, next to cellulose, is the most abundant renewable polysaccharide in nature. It is the major hemicellulosic component in plants and is located predominantly in the secondary cell walls of angiosperms and gymnosperms. The composition and structure of xylan are more complicated than that of cellulose and can vary quantitatively and qualitatively in various woody plant species, grasses, and cereals. Xylan is a heteropolymer in which the constituents are linked together not only by glycosidic linkages but also by ester linkages. Ferulic acid is the most abundant hydroxycinnamic acid found in plants and is known to be esterified to arabinose in wheat bran, wheat flour, barley straw, maize, sugar-cane bagasse, rice straw and other monocotyledons and also found esterified to galactose residues in pectins of sugar beet, spinach and other dicotyledons. p-Coumaric acid is also linked in a similar fashion in monocots. The presence of these phenolic acids has been shown to limit cell-wall biodegradation and play significant roles in cell wall extension and stabilization through cross-linking heteroxylan chains by forming phenolic dimers via plant peroxidases and/or photodimerization initiated by sunlight. Further, phenolic acids have been shown to function as cross-links between cell wall polysaccharides and the phenylpropanoid lignin polymer. The covalent attachment of lignin to wall polysaccharides and the crosslinking of xylan chains within hemicellulose limit overall polysaccharide bioavailability resulting in significant amounts of undigested fiber in animal feedstuffs, poor bioconversion of agricultural residue into useful products and incomplete processing of grains.
Enzyme hydrolysis of xylan to its monomers requires the participation of several enzymes with different functions. These are classified in two groups based on the nature of the linkages that they cleave. The first group of enzymes is hydrolases (EC 3.2.1) involved in the hydrolysis of the glycosidic bonds of xylan. These include endo-xylanases (EC 3.2.1.8) which randomly dismember the xylan backbone into shorter xylooligosaccharides; β-xylosidase (EC 3.2.1.37) which cleave the xylooligosaccharides in an exo-manner producing xylose; α-L-arabinofuranosidase (EC 3.2.1.55); and α-glucoronidase (EC 3.2.1.1) which remove the arabinose and 4-O-methylglucuronic acid substituents, respectively, from the xylan backbone. The second group includes enzymes that hydrolyze the ester linkages (esterase, EC 3.1.1) between xylose units of the xylan polymer and acetyl groups (acetyl xylan esterase, EC 3.1.1.6) or between arabinosyl groups and phenolic moieties such as ferulic acid (feruloyl esterase) and p-coumaric acid (coumaroyl esterase).
Faulds et al., reported two forms of ferulic acid esterase isolated from Aspergillus niger . The different esterases were distinguished on the basis of molecular weight and substrate specificity (Faulds et al., Biotech. Appl. Biochem., vol. 17, pp. 349-359 (1993)). Brezillon et al. disclosed the existence of at least two cinnamoyl esterases which were believed to be distinct from the ferulic acid esterases shown in the prior art (Brezillon et al., Appl. Microb. Biotechnol., vol. 45, pp. 371-376 (1996)). A ferulic acid esterase called FAE-III was isolated from Aspergillus niger CBS 120.49 and shown to act together with xylanase to eliminate nearly all of the ferulic acid and low molecular mass xylooligosaccharides in a wheat bran preparation; ferulic acid was also removed without the addition of xylanase, albeit at a lower level. Faulds et al. further isolated and partially characterized FAE-III from Aspergillus niger CBS120.49 grown on oat spelt xylan (Faulds et al., Microbiology, vol. 140, pp. 779-787 (1994)) and showed it to have a pI of 3.3, a molecular weight of 36 kD (SDS-PAGE) and 14.5 kD (Gel Filtration method), a pH optimum of 5 and a temperature optimum of 55-60° C.; microcrystalline cellulose binding was also detected. The authors theorized that FAE-II may be a proteolytically modified FAE-III. Recently, the various known ferulic acid esterases derived from Aspergillus niger have been distinguished based on their distinct substrate specificity and it was noted that FAE-II and FAE-III were unable to release ferulic acid from sugar beet pulp (Brezillon et al., supra).
Nonetheless, despite the characterization work which has been directed to Aspergillus niger esterases, the art remains in need of additional esterases for its various applications. Further, those of skill in the art have thus far failed to discover a nucleotide sequence which can be used to produce more efficient genetically engineered organisms capable of expressing such esterases in large quantities suitable for industrial production. However, a pressing need exists for the development of an esterase expression system via genetic engineering which will enable the purification and utilization of working quantities of relatively pure enzyme.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide for novel esterase proteins and DNA encoding such proteins.
It is an object of the present invention to provide for a method of isolating DNA from many different species, which DNA encodes protein having esterase activity.
It is a further object of the present invention to provide for an esterase which is produced by a suitable host cell which has been transformed by the DNA encoding the esterolytic activity.
The present invention provides for a purified 38 kD esterase which is derived from Aspergillus niger . Further, a DNA sequence coding for the 38 kD esterase comprising a DNA as shown in FIGS. 4A-4E (SEQ. ID NO: 27); a DNA which encodes the amino acid sequence also shown in FIGS. 4A-4E (SEQ. ID NO: 28); a DNA which encodes an esterase which comprises an amino acid segment which differs from the sequence in FIGS. 4A-4E, provided that the DNA encodes a derivative of the 38 kD esterase specifically described herein; and a DNA which encodes an esterase that comprises an amino acid segment which differs from the sequence in FIGS. 4A-4E, provided that the DNA hybridizes under low-stringency conditions and/or standard stringency conditions, as defined below, with a DNA comprising all or part of the DNA in FIGS. 4A-4E are provided. The present invention further encompasses vectors which indude the DNA sequences described above, host cells which have been transformed with such DNA or vectors, fermentation broths comprising such host cells an esterase proteins encoded by such DNA which are expressed by the host cells. Preferably, the DNA of the invention is in substantially purified form and is used to prepare a transformed host cell capable of producing the encoded protein product thereof. Additionally, polypeptides which are the expression product of the DNA sequences described above are within the scope of the present invention.
The enzyme of the instant invention has application as a supplement to an animal feed; in a process for treating fabric; to improve the mechanical properties of dough and the end product of baking of foods; in the modification of polysaccharides to give novel properties, e.g., gums; and in the processing grains. Further, the enzyme also has application in processing of plant materials for the release of free phenolic groups for use as an antioxidant, photoprotector, anti-inflammatory and/or anti-microbial agent which find use in personal care products such as cosmetics and as an aid in the conversion of chemical feed stocks to valuable specialty chemicals, food additives and flavorings.
An advantage of the present invention is that a DNA has been isolated which provides the capability of isolating further DNAs which encode proteins having esterolytic activity.
Another advantage of the present invention is that, by virtue of providing a DNA encoding a protein having esterolytic activity, it is possible to produce through recombinant means a host cell which is capable of producing the protein having esterolytic activity in relatively large quantities.
Yet another advantage of the present invention is that commercial application of proteins having esterolytic activity is made practical.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a western blot following SDS-PAGE gel showing the fragmentation of FAE under denaturing conditions.
FIGS. 2A-2B illustrate the DNA sequence (SEQ. ID NO:25) with deduced introns and amino acid sequence (SEQ. ID NO:26) of a 650 base pair fragment corresponding to the gene encoding a 38 kD esterase isolated from Aspergillus niger.
FIG. 3 illustrates a restriction map of a DNA fragment containing the gene encoding the 38 kd esterase.
FIGS. 4A-4E illustrate the complete DNA (SEQ. ID NO:27), with highlighting to point out the signal sequence, intron and various restriction endonuclease sites, and amino acid sequence (SEQ. ID. NO:28) corresponding to the gene encoding the 38 kD esterase isolated from Aspergilius niger.
FIG. 5 illustrates the DNA sequence of the gene encoding the 38 kD esterase (SEQ. ID. NO:29).
FIG. 6 illustrates a southern blot gel showing hybridization between a DNA probe derived from the 38 kD esterase of the invention and several other filamentous fungi (“gel 1”).
FIG. 7 illustrates a southern blot gel showing hybridization between a DNA probe derived from the 38 kO esterase of the invention and several other filamentous fungi (“gel 2”).
DETAILED DESCRIPTION OF THE INVENTION
“Esterase” or “esterolytic activity” means a protein or peptide which exhibits esterolytic activity, for example, those enzymes having catalytic activity as defined in enzyme classification EC 3.1.1. Esterolytic activity may be shown by the ability of an enzyme or peptide to cleave ester linkages, for example, feruloyl, coumaroyl or acetyl xylan groups, from organic compounds in which they are known to exist, e.g., primary and secondary cell walls. Preferably, the esterase comprises an esterolytic activity which cleaves the ester linkage of phenolic esters such as: [5-O-((E)-feruloyl)-α-L-arabinofuranosyl] (1→3)-O-β-D-xylopyranosyl-(1→4)-D-xylopyranose (also known as FAXX); [5-O-((E)-feruloyl)-α-L-arabinofuranosyl] (1→3)-O-β-D-xylopyranose (also known as FAX); O-β-D-xylopyranosyl-(1→4)-O-[5-O-((E)-feruloyl)-α-arabinofuranosyl-(1→3)]-O-β-D-xylopyranosyl-(1→4)-D-xylopyranose (also known as FAXXX); [5-O-((-p-coumaroyl)-α-L-arabinofuranosyl] (1→3)-O-β-D-xylopyranosyl-(1→4)-D-xylopyranose (also known as PAXX); [5-O-((E)-p-coumaroyl)-α-L-arabinofuranosyl] (1→3)-O-β-D-xylopyranose (also known as PAX): O-β-D-xylopyranosyl-(1→4)-O-[5-O-((E)-p-coumaroyl)-α-arabinofuranosyl-(1→3)]-O-β-D-xylopyranosyl-(1→4)-D-xylopyranose (also known as PAXXX) and other ester linked phenolic oligosaccharides as are known in the art. Such esterases are generally referred to as ferulic acid esterase (FAE) or enzymes having feruloyl esterase activity. It has surprisingly been discovered that an esterase having ferulic acid esterase activity which may be purified from Aspergillus niger , as described herein, and having an amino acid sequence as shown in FIGS. 4A-4E, further has activity on sugar beet pulp and also proteolytic and lipolytic activity. Thus, according to a particularly preferred embodiment of the present invention, an esterase and/or a DNA encoding that esterase is provided which esterase also has lipolytic and/or proteolytic activity. Accordingly, the esterase of the proteolytic and lipolytic activity. Thus, according to a particularly preferred embodiment of the present invention, an esterase and/or a DNA encoding that esterase is provided which esterase also has lipolytic and/or proteolytic activity. Accordingly, the esterase of the invention having measurably significant esterolytic activity on feruloyl and coumaroyl esters also has proteolytic and lipoolytic activity.
Preferably, the esterase and/or DNA encoding the esterase according to the present invention is derived from a fungus, more preferably from an anaerobic fungus and most preferably from Aspergillus spp., e.g., Aspergillus niger . Thus, it is contemplated that the esterase or the DNA encoding the esterase according to the invention may be derived from Absidia spp.; Acremonium spp.; Actinomycetes spp.; Agaricus spp.; Anaeromyces spp.; Aspergillus spp., including A. auculeatus, A. awamori, A. flavus, A. foetidus, A. fumaricus, A. fumigatus, A. nidulans, A. niger, A. oryzae, A. terreus and A. versicolor; Aeurobasidium spp.; Cephalosporum spp.; Chaetomium spp.; Coprinus spp.; Dactyllum spp.; Fusarium spp., including F. conglomerans, F. decemcellulare, F. javanicum, F. lini, F. oxysporum and F. solani; Gliocladium spp.; Humicola spp., including H. insolens and H. lanuginosa; Mucor spp.; Neurospora spp., including N. crassa and N. sitophila; Neocallimastix spp.; Orpinomyces spp.; Penicillium spp; Phanerochaete spp.; Phlebia spp.; Piromyces spp.; Pseudomonas spp.; Rhizopus spp.; Schizophyllum spp.; Streptomyces spp; Trametes spp.; and Trichoderma spp., including T. reesei, T. longibrachiatum and T. viride ; and Zygorhynchus spp. Similarly, it is envisioned that an esterase and/or DNA encoding an esterase as described herein may be found in bacteria such as Streptomyces spp., including S. olivochromogenes ; specifically fiber degrading ruminal bacteria such as Fibrobacter succinogenes ; and in yeast including Candida torresii; C. parapsilosis; C. sake; C. zeylanoides; Pichia minuta; Rhodotorula glutinis; R. mucilaginosa ; and Sporobolomyces holsaticus.
According to a preferred embodiment of the invention, the esterase is in a purified form, i.e., present in a particular composition in a higher or lower concentration than exists in a naturally occurring or wild type organism or in combination with components not normally present upon expression from a naturally occurring or wild type organism.
“Expression vector” means a DNA construct comprising a DNA sequence which is operably linked to a suitable control sequence capable of effecting the expression of the DNA in a suitable host. Such control sequences may include a promoter to effect transcription, an optional operator sequence to control such transcription, a sequence encoding suitable ribosome-binding sites on the mRNA, and sequences which control termination of transcription and translation. Different cell types are preferably used with different expression vectors. A preferred promoter for vectors used in Bacillus subtilis is the AprE promoter; a preferred promoter used in E. coli is the Lac promoter and a preferred promoter used in Aspergillus niger is glaA. The vector may be a plasmid, a phage particle, or simply a potential genomic insert. Once transformed into a suitable host, the vector may replicate and function independently of the host genome, or may, under suitable conditions, integrate into the genome itself. In the present specification, plasmid and vector are sometimes used interchangeably. However, the invention is intended to include other forms of expression vectors which serve equivalent functions and which are, or become, known in the art. Thus, a wide variety of host/expression vector combinations may be employed in expressing the DNA sequences of this invention. Useful expression vectors, for example, may consist of segments of chromosomal, non-chromosomal and synthetic DNA sequences such as various known derivatives of SV40 and known bacterial plasmids, e.g., plasmids from E. coli including col E1, pCR1, pBR322, pMb9, pUC 19 and their derivatives, wider host range plasmids, e.g., RP4, phage DNAs e.g., the numerous derivatives of phage λ, e.g., NM989, and other DNA phages, e.g., M13 and filamentous single stranded DNA phages, yeast plasmids such as the 2μ plasmid or derivatives thereof, vectors useful in eukaryotic cells, such as vectors useful in animal cells and vectors derived from combinations of plasmids and phage DNAs, such as plasmids which have been modified to employ phage DNA or other expression control sequences. Expression techniques using the expression vectors of the present invention are known in the art and are described generally in, for example, Sambrook et al., Molecular Cloning: A Laboratory Manual, Second Edition, Cold Spring Harbor Press (1989). Often, such expression vectors including the DNA sequences of the invention are transformed into a unicellular host by direct insertion into the genome of a particular species through an integration event (see e.g., Bennett & Lasure, More Gene Manipulations in Fungi, Academic Press, San Diego, pp. 70-76 (1991) and articles cited therein describing targeted genomic insertion in fungal hosts, incorporated herein by reference).
“Host strain” or “host cell” means a suitable host for an expression vector comprising DNA according to the present invention. Host cells useful in the present invention are generally procaryotic or eucaryotic hosts, including any transformable microorganism in which expression can be achieved. Specifically, host strains may be Bacillus subtilis, Escherichia coli, Trichoderma longibrachiatum, Saccharomyces cerevisiae or Aspergillus niger , and preferably Aspergillus niger . Host cells are transformed or transfected with vectors constructed using recombinant DNA techniques. Such transformed host cells are capable of both replicating vectors encoding esterase and its variants (mutants) or expressing the desired peptide product.
“Derivative” means a protein which is derived from a precursor protein (e.g.; the native protein) by addition of one or more amino acids to either or both the C- and N-terminal end, substitution of one or more amino acids at one or a number of different sites in the amino acid sequence, deletion of one or more amino acids at either or both ends of the protein or at one or more sites in the amino acid sequence, or insertion of one or more amino acids at one or more sites in the amino acid sequence. The preparation of an enzyme derivative is preferably achieved by modifying a DNA sequence which encodes for the native protein, transformation of that DNA sequence into a suitable host, and expression of the modified DNA sequence to form the derivative enzyme. The derivative of the invention includes peptides comprising altered amino acid sequences in comparison with a precursor enzyme amino acid sequence (e.g., a wild type or native state enzyme), which peptides retain a characteristic enzyme nature of the precursor enzyme but which have altered properties in some specific aspect. A “derivative” within the scope of this definition will retain generally the characteristic esterolytic activity observed in the native or parent form to the extent that the derivative is useful for similar purposes as the native or parent form. However, it is further contemplated that such derivatives may have altered substrate specificity, e.g., greater or lesser affinity for a specific substrate such as feruloyl, cinnamoyl or coumaroyl groups, or modified pH, temperature or oxidative stability. The derivative of the invention may further be produced through chemical modification of the precursor enzyme to alter the properties thereof.
Hybridization is used herein to analyze whether a given fragment or gene corresponds to the esterase described herein and thus falls within the scope of the present invention. The hybridization assay is essentially as follows: Genomic DNA from a particular target source is fragmented by digestion with a restriction enzyme(s), e.g., EcoRI, HindIII, PinAI, MluI, SpeI, BglII, Ppu10I, MfeI, NcoI, BlnI, EagI and XmaI (supplied by New England Biolabs, Inc., Beverly, Mass. and Boehringer Mannheim) according to the manufacturer's instructions. The samples are then electrophoresed through an agarose gel (such as, for example, 0.7% agarose) so that separation of DNA fragments can be visualized by size. The gel may be briefly rinsed in distilled H 2 O and subsequently depurinated in an appropriate solution for 30 minutes (such as, for example, 0.25M HCl) with gentle shaking followed by denaturation for 30 minutes (in, for example, 0.4 M NaOH) with gentle shaking. The DNA should then be transferred onto an appropriate positively charged membrane, for example the Maximum Strength Nytran Plus membrane (Schleicher & Schuell, Keene, N.H.), using a transfer solution (such as, for example, 0.4 M NaOH). After the transfer is complete, generally at about 2 hours or greater, the membrane is rinsed and air dried at room temperature after using a rinse solution (such as, for example, 2×SSC[2×SSC=300 mM NaCl, 30 mM trisodium citrate]). The membrane should then be prehybridized (for approximately 2 hours or more) in a suitable prehybridization solution (such as, for example, an aqueous solution containing per 100 mls: 20-50 mls formamide, 25 mls of 20×SSPE (1×SSPE=0.18 M NaCl, 1 mM EDTA, 10 mM NaH 2 PO 4 , pH 7.7) 2.5 mls of 20% SDS, 1 ml of 10 mg/ml sheared herring sperm DNA and 21.5 ml distilled H 2 O). As would be known to one of skill in the art, the amount of formamide in the prehybridization solution may be varied depending on the nature of the reaction obtained according to routine methods. Thus, a lower amount of formamide may result in a more complete gel in terms of identifying hybridizing molecules than the same procedure using a larger amount of formamide. On the other hand, a strong hybridization band may be more easily visually identified by using more formamide.
The DNA probe derived from the sequence in FIGS. 4A-4E or 5 should be isolated by electrophoresis in 1% agarose, the fragment excised from the gel and recovered from the excised agarose. This purified fragment of DNA is then random prime 32 P labeled (using, for example, the Megaprime labeling system according to the instructions of the manufacturer (Amersham Intemational plc, Buckinghamshire, England)). The labeled probe is denatured by heating to 95° C. for 5 minutes and immediately added to the prehybridization solution above containing the membrane. The hybridization reaction should proceed for an appropriate time and under appropriate conditions, for example, for 18 hours at 37° C. with gentle shaking. The membrane is rinsed (for example, in 2×SSC/0.3% SOS) and then washed with an appropriate wash solution and with gentle agitation. The stringency desired will be a reflection of the conditions under which the membrane (filter) is washed.
Specifically, the stringency of a given reaction (i.e., the degree of homology necessary for successful hybridization) will depend on the washing conditions to which the filter from the Southern Blot is subjected after hybridization. “Low-stringency” conditions as defined herein will comprise washing a filter from a Southern Blot with a solution of 0.2×SSC/0.1% SDS at 20° C. for 15 minutes. “Standard-stringency” conditions comprise a further washing step comprising washing the filter from the Southern Blot a second time with a solution of 0.2×SSC/0.1% SDS at 37° C. for 30 minutes.
FIGS. 5 and 6 illustrates the amino acid sequence and DNA sequence of a novel esterase derived from Aspergillus niger . The isolated esterase has a molecular weight of about 38 kD (as shown on SDS-PAGE), a pI of about 2.8 (as shown on IEF), a pH optimum of about 5.1 on methyl ferulate, a temperature optimum of about 55° C. and activity on coumaroyl and feruloyl esters, and sugar beet pulp. The FAE gene shown in FIG. 5 (SEQ. ID NO: 27) is approximately 2436 base pairs in length including deduced intron sequence and, if expressed, will encode the herein identified esterase from Aspergillus niger (hereinafter the “38 kD esterase”). For the purposes of the present invention, the term “38 kD esterase” means an esterase derived from Aspergillus niger corresponding to the esterase specifically exemplified herein. The DNA provided in FIG. 5 or 6 will be useful for obtaining homologous fragments of DNA from other species, and particularly from anaerobic fungi, which encodes an enzyme having esterolytic activity.
The DNA sequences of the present invention may be expressed by operatively linking them to an expression control sequence in an appropriate expression vector and employed in that expression vector to transform an appropriate microbial host according to techniques well established in the art. The polypeptides produced on expression of the DNA sequences of this invention may be isolated from the fermentation of animal cell cultures and purified in a variety of ways according to well established techniques in the art. One of skill in the art is capable of selecting the most appropriate isolation and purification techniques.
The esterase isolated according to the present invention is useful in applications in which it is desired to remove phenolic constituents of xylan oligosaccharides. For example, esterases may be applied to improve animal, and possibly human, nutrition as the digestibility of forage cell walls appears to be dependent on the phenolic content of the forage. Furthermore, esterases could be applied in the pulp and paper industry as hydrolysis of phenolic ester linked moieties from lignin may contribute to solubilization of the lignin and also may contribute to hydrolysing lignin/hemicellulose linkages. Esterases may be of potential use in the synthesis of carbohydrate derivatives and in the bioconversion of agricultural residue to fermentable sugars and free phenolic acid useful as an antioxidant, photoprotectant and/or antimicrobial in foods and personal care products; as a feed stock for conversion to flavors (such as vanillin) biopolymers, and valuable chemicals. Esterases have also been implicated in the finishing of textile fibers (see e.g., PCT Publication No. 96/16136). The activity of esterases toward multiple substrates present in many dirt based stains, their activation by surfactants and specificity toward phenolics suggests that esterases may also be of value in detergents. The availability of relatively large quantities of esterase facilitated by the present invention will enable the development of additional valuable applications.
The invention will be explained further below in the accompanying examples which are provided for illustrative purposes and should not be considered as limitative of the invention.
EXAMPLES
Example 1
Purification and Isolation of Peptides Comprising Ferulic Acid Esterase Activity and Design of Degenerate DNA Fragments for PCR
A fermentation broth from Aspergillus niger was filtered (0.8 μm) and 10 ml transferred into a centrifuge tube (50 ml) at room temperature. Saturated (NH 4 ) 2 SO 4 was added to give a final concentration of 60%. The solution was mixed and stored for approximately one hour at 4° C. then centrifuged at 1500×g for 20 minutes at 4° C. The supernatant was removed and the pellet resuspended in distilled water. Four tubes prepared as above were combined and diluted to approximately 200 ml with ammonium sulfate (2 M) to give a final concentration of 1.2 M ammonium sulfate, the pH was adjusted to pH 7.4 by the addition of Tris-HCl (200 mM).
The enzyme sample was chromatographed by hydrophobic interaction chromatography (Poros® HPEM phenyl ether, Perseptive BioSystems, perfusion chromatography, 12×30 cm). The column was connected to a BioCad® Perfusion Chromatography Workstation (Perseptive BioSystems) and equilibrated with 5 column volumes Tris-HCl (50 mM, pH 7.4) plus 1.2 M ammonium sulfate. The sample (205 ml) was applied to the column and separated at a flow rate of 30 ml/min with a linear gradient from 1.2 M to 200 mM ammonium sulfate over 20 column volumes. Fractions (15 ml) were collected during the gradient phase of the separation and assayed for FAE activity with methyl ferulate by the method of Faulds and Williamson (1994, Microbiology 140: 779-787). Four fractions eluting at 750 mM ammonium sulfate contained 83% of the starting FAE activity. Active fractions were pooled (60 ml), dialysed by ultrafiltration into start buffer for next chromatographic step (10 kDa membrane, 20L of 25 mM sodium acetate buffer pH 5.0). The sample was concentrated to 10 ml in preparation for ion exchange chromatography.
Ion exchange chromatography was performed using a MonoQ strong anion exchanger (MonoQ®, HR 10/10, Pharmacia Biotechnology) connected to BioCAD Perfusion Chromatography Workstation and equilibrated with 25 mM sodium acetate (pH 5.0). The sample (10 ml) was applied to the column and eluted at a flow rate of 5 ml/min with a linear NaCl gradient (0-500 mM) over 15 column volumes. Fractions (5 ml) were collected during the gradient and assayed for FAE activity (activity against feruloyl esters). FAE activity eluted as a single peak at 155 mM NaCl and was collected in one fraction. The sample was concentrated (Centricon, 10 kDa) to 1.5 ml.
High performance size exclusion chromatography (HPSEC) was carried out using two Superdex 75 columns (10/30 HR, Pharmacia Biotechnology) connected in tandem on a BioCAD Perfusion Chromatography Workstation. The columns were equilibrated with 10 column volumes sodium acetate buffer (25 mM, pH 5.0) containing 125 mM NaCl and 0.01% triton X-100. The columns were calibrated for determination using protein standards of known molecular mass (Bio-RAD gel filtration standards, and Sigma gel filtration standards). Samples (500 μl) were applied and separated at a flow rate of 750 μl/min. Fraction (1 ml) were collected. The FAE activity eluted as a single peak corresponding to a molecular mass of about 32 kDa.
Upon native PAGE of a desalted active fraction from HPSEC a single protein band was observed, The isolelectric point of the FAE was determined using Phast gel Dry IEF equilibrated with a solution ampholyte, (20% final concentration, containing a mix of pI 2-4, 80%, pI 3-10 20%) Glycerol (10%) for 1 hour. Separation was performed as per manufacturers recommendation (Pharmacia Biotechnology, Dry IEF instruction bulletin) and stained with coomassie R-250. The sample migrated as a single protein band with an isolelectric point of about 2.8.
Western Blots of the HPSEC FAE sample were performed using PVDF membranes (0.2 μm pore size) a Novex mini-gel apparatus for obtaining N-terminal amino acid sequence by methods recommended by manufacturer. A sample of the FAE in dialysed into buffer (5 mM MES pH 5.8).
The resultant purified protein was placed in an aqueous solution for peptide sequence analysis according to standard methods. Briefly the peptides were digested in solution with the following sequencing grade proteases:
Lys-C—200 μl reaction buffer comprising 100 mM ammonium bicarbonate and 2-4 μg of enzyme, pH 8.0, overnight at 37° C.;
Arg-C—200 μl reaction buffer comprising 20 mM Tris and 4 μg of enzyme, pH 7.5+1.5 mM CaCl 2 +2 mM DTT overnight at 37° C.;
Glu-C—digest buffer for on-blot digests was 50 mM ammonium bicarbonate with 4 μg enzyme, 10% acetonitrile and 1% reduced triton X-100;
CNBr cleavage—was conducted by dissolving enzyme sample in 200 μl of 70% formic acid in water and CNBr crystals added in sufficient quantity to produce methionine cleavage.
The digested peptides were then concentrated to approximately 100 μl and loaded is directly onto a reverse-phase HPLC (Phenomenex Primesphere C18 column, 250×2.0 mm). Reverse phase separations were carried out using Applied Biosystems 140A solvent delivery system. Buffers used were 0.1% TFA in water (A), 70% acetonitrile in water +0.070% TFA (B); flow rate was 150 μl per minute with a gradient as follows: 0 minutes—5% Buffer B, 10 minutes—10% Buffer B, 80 minutes—80% Buffer B, 85 minutes—100% Buffer B, 90 minutes—100% Buffer B.
CNBr digests are treated as follows: water is added to the solution and the whole volume concentrated to 100 μl in a speed-vac. Further water is added to approximately 1 ml and this dried again to about 100 μl. This removes the majority of the formic/CNBr.
Various peptide fragments obtained as described above were analyzed to determine their sequence and for subsequent development of degenerate probes for use in cloning the gene encoding the 38 kD esterase from the genome of the donor organism. Peptide sequence analysis of the 38 kD esterase was problematic due to cycles containing mixed signals indicating the presence of multiple polypeptides in the analyzed sample. Protein sequencing resulted in an N-terminal sequence and several additional peptide fragments as follows:
ASTQGISEDLYSRLVEMATISQAAYXDLLNIP
(SEQ. ID NO:1)
XTVGFGPY
(SEQ. ID NO:2)
FGLHLXQXM
(SEQ. ID NO:3)
XISEDLYS
(SEQ. ID NO:4)
YIGWSFYNA
(SEQ. ID NO:5)
GISEDLYXXQ
(SEQ. ID NO:6)
XISESLYXXR
(SEQ. ID NO:7)
GISEDLY
(SEQ. ID NO:8)
LEPPYTG
(SEQ. ID NO:9)
XANDGIPNLPPVEQ
(SEQ. ID NO:10)
YPDYALYK
(SEQ. ID NO:11)
From these fragments, suitable degenerate probes for hybridization and use as PCR primers were produced and fragments were obtained which were believed to be derived from the gene encoding the 38 kD esterase. However, sequencing of the fragments obtained in this manner (550 and 100 base pairs) showed that the fragments were merely artifacts of PCR and were not of use in cloning the 38 kD esterase. Additional analysis of 2 different probes derived from 2 protein sequences isolated as above resulted in similar lack of success. From these results, it was determined that routine protein purification and peptide sequencing procedures were insufficient to obtain suitable peptide fragments for the preparation of degenerate DNA probes.
The inventors herein hypothesized that a specific property of the protein or the purified protein composition was preventing obtaining purified representative protein. To test this theory, the product protein from above was analyzed via isoelectric focusing gel at pH 2-4 under various conditions. Protein samples taken from purification steps along the purification method described above appeared to be a single band of highly purified protein. A second analysis was performed in which the purified protein was subjected to denaturing conditions of an SDS-PAGE and the results western blotted. As shown in FIG. 1, the resultant protein showed a number of bands indicating either some degeneration of the protein or other compounds hidden during the IEF gel. Sequencing of each of the numerous bands showed that each possessed an identical N-terminal sequence and that proteolysis appeared to be occurring from the carboxy terminal.
From the data, the inventors herein hypothesized that numerous fragments may be appearing due to carboxy terminal proteolytic clipping within the molecule itself upon unfolding of the protein in reduced SDS buffer. Unfolding of the 38 kD esterase may expose the previously internal hydrophobic residues, e.g., tyrosine, tryptophan and phenylalanine, providing a structurally similar substrate to the ester linked feruloyl group which would be recognized in the active site of the 38 kD esterase allowing for hydrolysis peptide. This result was highly unpredictable due to the fact that the heretofore observed enzymatic action of the isolated protein was esterolytic and not proteolytic. In any event, the inventors herein theorized that if protein denaturing conditions (i.e., unfolding of the peptide chain) were avoided, internal clipping may be avoided. To effect this, the purified protein from the anion exchange chromatography step was further chromatographed using high resolution size exclusion chromatography (HPSEC as detailed above).
The HPSEC purified 38 kD esterase was separated by SDS-PAGE and a Western blot onto a PVDF membrane was performed for sequencing “on-blot”. Digests directly from the blots were prepared as follows: neat TFA is added to the blot containing solution to give a final volume containing 50% TFA. This solution is then sonicated for 5 minutes. The liquid (but not the blot pieces) is removed and a solution of 50% acetonitrile in 0.1% TFA is added. The sample is sonicated again for 5 minutes. The liquid was removed and replaced by a final wash of 0.1% TFA in water and a final 5 minutes sonication. All wash solutions were pooled and concentrated down to approximately 100 μl. This method allowed for the polypeptides resulting from enzymatic digests to be collected without further proteolysis by 38 kD esterase immobilized on the membrane. In this way, single polypeptides suitable for sequence analysis were obtained due to 38 kD esterase being immobilized on the PVDF thus preventing carboxy terminal proteolytic clipping and the presence of mixed amino acid signals during each cycle of sequencing.
When this procedure was followed, a number of fragments which were appropriate for the design of degenerate DNA fragments were produced.
Example 2
Isolation of a 650 Base Pair Fragment Corresponding to FAE Gene
Based on the peptide fragments obtained in Example 1 after the protein clipping problem had been solved, the gene encoding the 38 kD esterase was cloned by amplifying the gene from its genome using polymerase chain reaction and appropriately designed degenerate oligonucleotide primers. Primers were designed based upon partial amino acid sequences of fragmented 38 kD esterase protein. Amplification of three fragments from the 38 kD esterase gene was obtained using the following four oligonucleotide primers (the oligonucleotide primers were designed based upon the underlined peptide sequence following the oligonucleotide primers. The following abbreviations were used to identify wobble position alternates: I=inosine, W=A/T, S=C/G, R=A/G, Y=T/C, H=A/T/C, D=A/G/T, X=A/T/G/C.
Sense primer 11:
CGGGAATTCGCIWSIACICARGGXAT
(SEQ ID. NO:12)
Derived from:
ASTQGI SEDLYSRLVEMATISQAAYADLLNIP
(SEQ ID. NO:13)
Sense primer 7:
CGGGAATTCTAYTAYATHGGITGGGT
(SEQ. ID NO:14)
Derived from:
VHGG YYIGWV SVQDQV
(SEQ. ID NO:15)
Anti-sense primer 8:
CGGGAATTCACCCAICCDATRTARTA
(SEQ. ID NO:16)
Derived from:
VHGG YYIGWV SVQDQV
(SEQ. ID NO:17)
Anti-sense primer 2:
CGGGAATTCTTIGGIATICCRTCRTT
(SEQ. ID NO:18)
Derived from:
TDAFQASSPDTTQYFRVTHA NDGIPN L
(SEQ. ID NO:19)
Two primers enabled deduction of putative amplified DNA fragments encoding the 38 kD esterase:
Anti-sense primer 3:
CGGGAATTCATICCRTCRTTIGCRTG
(SEQ. ID NO:20)
Derived from:
TDAFQASSPDTTQYFRVT HANDGI PNL
(SEQ. ID NO:21)
Anti-sense primer 12:
CGGGAATTCGCYTGRAAIGCRTCIGTCAT
(SEQ. ID NO:22)
Derived from:
( M ) TDAFQA SSPDTTQYFRVTHANDGIPNL
(SEQ. ID NO:23)
An EcoRI restriction endonuclease recognition site and a “GC” clamp was included at the 5′ end of all primers to facilitate cloning of amplified fragments into the plasmid vector pUC18. PCR reaction included placing the following into “Hot Start” (Molecular Bio-Products, Inc., San Diego, Calif.) tubes in the order provided:
1 μl 500 ng/μl sense primer
1 μl 500 ng/μl anti-antisense primer
2 μl nucleotide mix (10 mM each dNTP)
5 μl 10×PCR Buffer
41 μl distilled water
Heated at 95° C. for 90 seconds, placed onto ice for 5 minutes.
5 μl 10×PCR Buffer
43 μl distilled water
1 μl Aspergillus niger genomic DNA
1 μl Taq DNA Polymerase (Boehringer Mannheim, 5 U/μl)
Amplification was carried out in a Minicycler Model PTC-150 (MJ Research Inc., Watertown, Mass.). Amplification conditions followed a sequential pattern of: 95° C. for five minutes; 40° C. for 90 seconds; 72° C. for 3 minutes; and 28 cycles of 94° C. for 1 minute 40° C. for 90 seconds, and 72° C. for 3 minutes for 28 cycles. A final extension step of 72° C. at 2 minutes was included.
The primers were used for PCR amplification in the following paired combinations: 11-2, 11-3, 11-8, 11-12, 7-2,7-3 and 7-12. Each primer combination produced multiple DNA bands upon agarose electrophoresis. Major DNA bands for the PCR products of primers pairs 7-2, 7-3 and 7-12 were present at around 350, 350 and 300 base pairs respectively as visualized on a 3% NuSieve (FMC Corp.) agarose electrophoresis gel. Antisense primers 2, 3 and 12 were designed to the same continuous peptide fragment: (M)TDAFQASSPDTTQYFRVTHANDGIPNL (SEQ. ID NO: 24). Anti-sense primers 2 and 3 code for nearly the same stretch of DNA, their 3′ ends being offset by only 6 bases. As antisense primer 12 corresponds to amino acids that are upstream of primers 2 and 3, the 3′ end of antisense primer 12 is offset by approximately 60 base pairs from primers 2 and 3. Therefore, the lengths of the PCR bands were approximately consistent with a continuous stretch of DNA encoding the 38 kD esterase. Additionally the primer pairs 11-2, 11-3 and 11-12 produced bands of approximately 650, 650 and 600 base pairs respectively. These lengths were approximately consistent with amplification of a piece of DNA encoding the 38 kD esterase.
The PCR amplification products were digested with EcoRI, ligated into the cloning vector pUC18 and then transformed into E.coli . The cloned PCR products were sequenced. Sequencing of the product of primers 11-2 revealed a 650 base pair. DNA sequence shown in FIG. 2 (SEQ. ID NO:25) which upon translation codes for 197 amino acids. A total of 155 residues corresponded to nine sequenced peptide fragments of 38 kD esterase protein. A putative 57 base pair intron exists containing splicing sequences of GTATGC at the 5′ site, an internal lariat sequence of CACTAACT, and TAG at the 3′ splice site. Furthermore a product of primers 11-8 when sequenced reveals approximately the first 314 bases (5′-3′) of the 650 base pair 11-2 fragment. A 350 base pair product of primers 7-2 revealed DNA that corresponds in sequence to the second half of the 650 base pair 11-2 fragment.
Example 3
Obtaining Genomic DNA from Aspergillus niger for Cloning
A preserved culture of Aspergillus niger was grown on Potato Dextrose Agar (PDA) at 30° C. Approximately 2 cm 2 of the fungi grown on PDA was inoculated into 50 ml of Yeast Extract Glucose media in a 250 ml baffled flask and incubated at 33° C. in a rotary shaker at a speed of 300 RPM for 24 hours. The mycelia was harvested through miracloth, squeezed dry, immediately frozen in liquid nitrogen and ground with ½ teaspoon of sand in a mortar and pestle for approximately two minutes. The genomic DNA was extracted from the ground mycelia using a modification of Invitrogen's Easy-DNA Genomic Isolation Kit. The ground, frozen mycelia was immediately transferred to a centrifuge tube to which 3.5 mls of Solution A was added, followed by vortexing and a 10 minute incubation at 65° C. Next, 1.5 mls of Solution B was added, followed by vortexing. 5 mls of chloroform was added, followed by vortexing until the viscosity decreased and the mixture was homogeneous. The mixture was centrifuged at 15,000×G at 4° C. for 20 minutes. The upper phase was transferred into a new tube and then precipitated with two volumes of 95% ethanol. The precipitation reaction was incubated on ice for 30 minutes. The precipitation DNA was pelleted by centrifugation at 15,000×G at 4° C. for 15 minutes. The ethanol was removed. The DNA pellet was washed with 25 mls of 70% ethanol and the mixture was centrifuged at 15,000×G at 4° C. for 5 minutes. The 70% ethanol was removed and the pellet allowed to air dry for 5 minutes The extracted DNA was suspended in a volume of 500 μl of TE, RNase was added to a final concentration of 4 μg/ml. This extracted genomic DNA was used in PCR amplification of the DNA fragments encoding 38 kD esterase.
Example 4
Using the Obtained 650 Base Pair Fragment to Isolate DNA Encoding Homologous Enzymes from Aspergillus or Other Species
One particularly effective method of obtaining clones of homologous genomic DNA is by construction and screening of a subgenomic libraries. Briefly, and as described in more detail below, this method involves cutting the genomic DNA to completion with appropriate restriction endonucleases, performing Southern hybridization with the 650 base pair fragment as a probe, ligating the appropriately sized fragments into a plasmid vector, transforming the plasmid into E.coli and then southern probing the colonies with the 650 base pair fragment to obtain a genomic clone. These techniques are known in the art and are described in Current Protocols in Molecular Biology, supra.
To obtain clones of a vector comprising the gene encoding the entire 38 kD esterase protein, Aspergillus niger genomic DNA was prepared as in Example 3. The genomic DNA was fragmented by digestion with a number of restriction enzymes: EcoRI, HindIII, PinAI, MluI, SpeI, BglII, Ppu10I, MfeI, NcoI, BlnI, EagI and XmaI (supplied by New England Biolabs, Inc., Beverly, Mass. and Boehringer Mannheim). The reaction conditions combined 3 μl of genomic DNA, 2 μl of the appropriate 10× restriction endonuclease buffer (according to the manufacturers instructions), 2 μl of restriction enzyme (at 10 units/μl), 13 μl of distilled water; the reaction proceeded at 37° C. for 6 hours. The samples were then electrophoresed through a 0.7% agarose gel so that separation of DNA fragments could be visualized between a size of 1 kb to >12 kb. The gel was briefly rinsed in distilled H 2 O and subsequently depurinated for 30 minutes in a solution of 0.25M HCl with gentle shaking followed by denaturation for 30 minutes in a solution of 0.4 M NaOH with gentle shaking. The DNA was then transferred onto a positively charged Maximum Strength Nytran Plus membrane (Schleicher & Schuell, Keene, N.H.) using a solution of 0.4 M NaOH as transfer solution. After the transfer was complete, >2 hours, the membrane was rinsed in 2×SSC and air dried. The membrane was then prehybridized for 8 hours in a prehybridization solution containing per 100 mls: 50 mls formamide, 25 mls of 20×SSPE (1×SSPE =0.18 M NaCl, 1 mM EDTA, 10 mM NaH 2 PO 4 , pH 7.7), 2.5 mls of 20% SDS, 1 ml of 10 mg/ml, sheared herring sperm DNA and 21.5 mls of distilled H 2 O.
The cloned 650 base pair fragment of Example 2 was used as a hybridization probe of the membrane. The fragment was isolated from the pUC18 plasmid by restriction digestion with EcoRI, electrophoresis in 1% agarose, excision of the fragment from the gel and recovery of the fragment from the excised agarose. This purified 650 base pair fragment of DNA was random prime 32 P labeled using the Megaprime labeling system according to the instructions of the manufacturer (Amersham International plc, Buckinghamshire, England). The labeled probe was denatured by heating to 100° C. for 5 minutes and immediately added to the prehybridization solution containing the membrane. The hybridization reaction proceeded for 18 hours at 37° C. with gentle shaking. The membrane was rinsed in a solution of 2×SSC/0.3% SDS and then washed for 15 minutes in the same solution at 37° C. with shaking. The membrane was further washed with a solution of 0.2×SSC/0.1% SDS at 37° C. for 30 minutes. The membrane was then exposed onto X-Omat AR film (Eastman Kodak Co, Rochester, N.Y.) for 3 hours and developed.
The film developed from the digests prepared as above showed only one band of hybridization per restriction enzyme digestion consistent with hybridization. The EcoRI digestion showed a single band of hybridization at about 5.5 kb in length. Because this hybridized fragment was an excellent candidate fragment to contain a gene corresponding to the entire 38 kD esterase as a result of its size being consistent with a gene encoding a protein of that size, a sub-library was made choosing EcoRI to digest genomic Aspergillus niger DNA to obtain fragment sizes around 5.5 kb in length.
A restriction digest was made on genomic DNA prepared as in Example 3. The reaction included 50 μl of genomic DNA, 50 μl of 10×restriction endonuclease buffer H (Boehringer Mannheim), 25 μl of EcoRI (10 units/μl, Boehringer Mannheim), 375 μl of distilled water. The reaction proceeded at 37° C. for 6 hours. The digestion mixture was electrophoresed through 0.8% agarose. Fragments between a range of approximately 5 kb to 6 kb were cut from the gel in three approximately equal slices. The three pools of DNA fragments contained within the three gel slices each possessed a slightly different range of fragment lengths. The DNA was recovered from the slices of agarose using QIAquick Gel Extraction columns, following the instructions of the manufacturer (Qiagen, Inc., Chatsworth, Calif.). Approximately {fraction (1/10)} of each pool of recovered DNA was electrophoresed in 0.8% agarose and southern hybridized to the 650 base pair fragment as described above. The pool of DNA which gave the strongest hybridization signal was ligated into an EcoRI digested E.coli vector (for example pLITMUS 28, New England Biolabs), which was then transformed into E.coli . The E.coli transformants were plated out on 5 plates at a concentration of 650 base pair fragment as described above. The pool of DNA which gave the strongest hybridization signal was ligated into an EcoRI digested E.coli vector (for example pLITMUS 28, New England Biolabs), which was then transformed into E.coli . The E.coli transformants were plated out on 5 plates at a concentration of approximately 500 colonies per plate (150 mm diameter plate). Colony lifts were performed on the plates using Maximum Strength Nytran Plus membranes. A southern hybridization was performed using the 650 base pair fragment. Four strong hybridization signals were obtained. Colonies putatively corresponding to the four strong hybridization signals were grown up, and their plasmid DNA recovered. Restriction digests on the plasmid DNA were made using restriction enzymes that were chosen based on sites within the 650 base pair fragment. One plasmid restriction digest gave restriction fragments consistent with the known restriction sites within the 650 base pair fragment. Upon DNA sequencing, this clone was revealed to contain the 650 base pair sequence that was obtained through PCR described in example 2. Restriction mapping of this clone reveals the 650 base pair fragment to lie within the approximately 5.5 kb of cloned genomic DNA sequence. Based on this procedure, DNA encoding the entire gene of the 38 kD esterase was isolated corresponding to the sequence provided in FIG. 5 (SEQ. ID. NO:27) encoding a protein having the amino acid sequence of FIG. 5 (SEQ. ID. NO:28).
Modifications of this method which are known to effect similar results would also be effective in obtaining the suitable DNA or clones. Of course, this method is similarly suitable for the identification and cloning of homologous esterase enzymes from species other than Aspergillus niger . For example, as described above, a genomic library could be produced from a suitable microorganism by preparing genomic DNA and cutting with an appropriate restriction endonuclease. The library would then be subjected to Southern Blot hybridization with the 650 base pair fragment described in Example 2 as a probe and suitable hybridizing fragments ligated into a suitable expression vector and transformed into a suitable organism for expression. Suitable techniques for such processes are described in, for example, European Patent No. 215 594 (Genencor).
Example 5
Construction of an Expression System for FAE
Production of FAE was achieved by constructing an expression vector and transforming that vector into Aspergillus . The transformed Aspergillus strain is then grown in appropriate fermentation media. An FAE expression vector is described below. Transformation of Aspergillus is known in the art and is described for example in “Cloning, mapping and molecular analysis of the pyrG (orotidine-5′-phosphate decarboxylase) gene of Aspergillus nidulans ”, B. Oakley et al., Gene, 61 (1987) pp. 385-399.
An FAE expression vector can be constructed in available E.coli plasmids like pNEB193 (New England Biolabs, Beverly, Mass.). Three elements are required for the expression vector. In brief these elements are: The FAE gene with its downstream terminator sequence, the A.niger glucoamylase promoter and the A.nidulans pyrG gene which is used as a selectable marker for transformation. The pyrG gene may be PCR amplified from Aspergillus nidulans FGSC4 obtainable from the Fungal Genetics Stock Center, Department of Microbiology, University of Kansas Medical Center, Kansas City, Kans. 66160-7420 USA. The FAE gene sequence is given in FIG. 6 . The A.niger glucoamylase promoter and the A.nidulans pyrG DNA sequences may be obtained from the GenBank sequence database. The A. nidulans pyrG sequence is disclosed in Oakley et al. The DNA sequence of the A.niger glucoamylase promoter is disclosed in “Regulation of the glaA gene of Aspergillus niger ,” Fowler et al., Current Genetics (1990) 18:537-545. The elements were arranged in the E.coli plasmid in such a way that the glucoamylase promoter drives the expression of the fae1 gene starting from the fae1 start methionine codon (from base 519 in the fae1 gene). This allows the strong glucoamylase promoter to drive expression of the FAE gene product.
Methods for constructing DNA sequences in E.coli plasmids are known in the art. An acceptable method for constructing an FAE expression vector in the vector pNEB193 follows:
(a) PCR is used to amplify the A.nidulans pyrG gene and insert this sequence into pNEB193. This could be accomplished with two primers and suitable conditions to obtain a pyrG fragment of approximately 2.0 kb in size. For example, the upper primer may be:
5′-GGCCTGCAGCCCCGCAAACTACGGGTACGTCC-3′ (SEQ. ID. NO:30) and the lower primer may be:
5′-CGCGCTGCAGGCTCTTTCTGGTAATACTATGCTGG-3′ (SEQ.ID.NO:31)
Aspergillus nidulans genomic DNA may be prepared for amplification as described above. The conditions needed to amplify a 2.0 kb fragment are known in the art, for example they are given in the “Expand High Fidelity PCR System” (Boehringer Mannheim, Indianapolis, Ind.). After amplification of the fragment, it is isolated and then digested with the enzyme PstI. Also the plasmid pNEB193 is digested with PstI. After digestion, the fragment and plasmid are isolated and ligated together.
(b) PCR is used to amplify the A.niger glucoamylase promoter and place this sequence into the plasmid constructed. This could be accomplished using two primers and conditions to obtain a promoter fragment of approximately 1.9 kb in size. As examples of suitable primer, the upper primer could be
5′-GGCTTAATTAACGTGCTGGTCTCGGATCTTTGGCGG-3′ (SEQ.ID.NO:32) and the lower primer could be:
5′-GGGGCGCGCCAGATCTAGTACCGATGTTGAGGATGAAGCTC-3′ (SEQ.ID.NO:33).
While many different strains are suitable for amplification, one particularly useful strain for amplification is A.niger strain ATCC10864 (American Type Culture Collection, Rockville, Md.). The A.niger genomic DNA for amplification may be isolated as described above. After amplification the fragment is isolated and digested with the enzymes PacII and AscI. The plasmid created in (a) above above is also be digested with the enzymes PacII and AscI. The digests of both the amplified fragment and plasmid would be ligated together.
(c) Two fragments of the FAE gene are combined into the plasmid created in (b) utilizing the a 5.5 kb EcoRI fragment comprising the entire FAE gene. The first fragment is created via PCR using the following primers in connection with the 5.5 kb EcoRI fragment of the FAE gene disclosed above as the source to be amplified:
forward primer: 5′-GCCCAGATCTCCGCAATGAAGCAATTCTCCGCCAAACAC-3′ (SEQ.ID.NO:34)
reverse primer: 5′-AATAGTCGACGGAATGTTGCACAGG-3′ (SEQ.ID.NO:35)
This fragment is digested with BglII and SalI to result in a fragment of about 169 base pairs long. The second fragment is made by incubating the 5.5 kb EcoRI fragment of the FAE gene with SalI and EcoRI, the resulting 1.75 kb fragment being isolated. The plasmid created in (b) above is prepared for insertion of the FAE gene by digesting with BglII and EcoRI. The three fragments, the 169 base pair PCR product, the 1.75 kb fragment and the BglII/EcoRI digested step 2 plasmid, are ligated together. This resulting plasmid would be an Aspergillus FAE gene expression vector.
The vector created above would be used to carry out transformation of Aspergillus.
Example 6
Identification of Homologous Genes in Filamentous Fungi
A southern hybridization experiment was performed under hybridization conditions described using 25% formamide in hybridization buffer as defined herein. The 650 base pair FAE gene fragment isolated in Example 2 was used to probe digested genomic DNA from a number of genera. Hybridization bands were obtained with genomic DNA obtained from fungi other than Aspergillus niger implying the existence of homologous esterase genes in these other organisms. Based on the hybridization data, it is believed that the DNA identified in this experiment will code for closely related enzymes with esterolytic activity. The genes for these other homologous enzymes are cloned by the methods described. These cloned genes are then expressed in suitable hosts to produce the encoded enzyme.
The genomic DNA was digested with two restriction enzymes, BglII and Ppu10I, and then electrophoresed through 0.7% agarose in two different gels. Genomic DNA fragment sizes separated on the agarose gel ranged from about 1 kb to about 20 kb. The gels were depurinated and denatured and Southern blotted onto Nytran plus. The membranes were air dried and hybridized with the 650 base pair fragment 32 P labeled. The membranes were washed under low stringency conditions, followed by washing under standard stringency conditions. The membranes were then autoradiographed. The reproduced gels are provided in FIGS. 6 and 7.
gel 1
lane #
endonuclease
DNA source
2
Bgl II digest
Aspergillus niger GCI strain #7
3
Ppu 10 I digest
Aspergillus niger GCI strain #7
4
Bgl II digest
Aspergillus terrus
5
Ppu 10 I digest
Aspergillus terrus
6
Bgl II digest
Trichoderma reesei strain QM6a, ATCC13631
7
Ppu 10 I digest
Trichoderma reesei strain QM6a, ATCC13631
8
Bgl II digest
Acremonium brachypenium , ATCC 32206
9
Ppu 10 I digest
Acremonium brachypenium , ATCC 32206
gel 2
lane #
endonuclease
DNA source
17
Bgl II digest
Aspergillus niger GCI strain #7
18
Ppu 10 I digest
Aspergillus niger GCI strain #7
19
Bgl II digest
Gliocladium roseum
20
Ppu 10 I digest
Gliocladium roseum
25
Bgl II digest
Penicillium notatum
26
Ppu 10 I digest
Penicillium notatum
Bands are apparent in lanes 2, 3, 17 and 18 which correspond to the cloned FAE gene described in this patent. Bands appear in the lanes 2 and 17 BglII digest which may indicate other homologous FAE enzymes present in the Aspergillus niger strain. Two bands are present in lanes 4 and 5 and two bands are present in lane 4, indicating homologous DNA in the Aspergillus terrus . A band is apparent in lane 7 indicating homologous DNA in Trichoderma reesei . A band is apparent in lane 8 indicating homologous DNA in Acremonium brachypenium . A band is apparent in lane 19 indicating homologous Gliocladium roseum . Two bands are present in lanes 25 and 26 indicating homologous DNA in Penicillium notatum.
Example 7
Biochemical Properties and Substrate Specificity of FAE Purified According to Example 1
The 38 kD esterase isolated according to Example 1 was analyzed for biochemical properties. The molecular weight was found to be about 38 kD when measured on SDS-PAGE and 30-32 kD as measured by HPSEL. The pI as measured on isoelectric focusing (IEF) gel was found to be about 2.8. Purified 38 kD esterase was found to be active toward several natural feruloyl and p-coumaroyl esters, cell walls of wheat bran and sugar beet pulp, wheat flour, the pentosan fraction of wheat flour, and ethyl and methyl esters of ferulic and p-coumaric acid. Kinetic data for various substrates is presented in Table 1. The 38 kD esterase showed a pH optimum of 5.1 for methyl ferulate with 83% and 25% maximal activity found at pH 3 and 8, respectively. When the 38 kD esterase was incubated in buffer for 30 minutes without substrate at pH 5.1, the temperature optima was 55° C. With 250 μM methyl ferulate present the optima increases to 65° C. A low K m of the trisaccharide FAXX favors the use of the 38 kD esterase of the present invention in combination with a xylanase that leaves such carbohydrate oligomers preferentially unhydrolyzed when degrading cell walls.
Purified 38 kD esterase was analyzed for a variety of biochemical activities with an API-20 enzyme test strip (BioMerieux Vitek) according to the manufacturers instructions. The results shown in Table 2. Activity was observed on the following substrates. “+++” indicates very strong response, “++” indicates strong response and “+” indicates activity shown towards substrate. “−” means no activity detected.
TABLE 1
Activity of 38kD Esterase On Various
Feruloylated Oligosaccharides
Substrate
K m (mM)
V max (U/mg)
V max /K m
Methyl-FA
2.08
87
41.8
FA
0.125
245
1960.0
FAX
0.078
276
3539.5
FAXX
0.019
498
26210.5
FAX 3
0.052
307
5903.8
TABLE 2
Substrate Specificity For 38kD Esterase
Enzyme Generally Associated
Substrate
Activity
With Activity
2-naphthyl butyrate [pH 6.5]
(+++)
Esterase (C4)
2-naphthyl caprylate [pH 7.5]
(++)
Esterase/Lipase (C8)
2-naphthyl myristate [pH 7.5]
(+)
Lipase (C14)
2-naphthyl phosphate [pH 5.4]
(+)
Acid Phosphotase
Naphthol-AS-BI-phosphate [pH 5.4]
(++)
Phosphohydrolase
6-Br-2-naphthyl-αD-galactopyranoside [pH 5.4]
(+++)
α-galactosidase
2-naphthyl-βD-galactopyranoside [pH 5.4]
(++)
β-galactosidase
2-naphthyl-αD-glucopyranoside [pH 5.4]
(+)
α-glucosidase
6-Br-2-naphthyl-βD-glucopyranoside [pH 5.4]
(+++)
β-glucosidase
2-naphthyl phosphate [pH 8.5]
—
Alkaline Phosphotase
L-leucyl-2-naphthylamide [pH 7.5]
—
Leucine arylamidase
L-valyl-2-naphthylamide [pH 7.5]
—
Valine arylamidase
L-cystyl-2-naphthylamide [pH 7.5]
—
Cysteine Arylamidase
N-glutaryl-phenylalanine-2-naphthylamide
—
Chymotrypsin
N-benzoyl-DL-arginine-2-naphthylamide [pH 8.5]
—
Trypsin
Naphthol-AS-BI-βD-glucuronide [pH 5.4]
—
β-Glucuronidase
6-Br-2-naphthyl-αD-mannopyronoside [pH 5.4]
—
α-Mannosidase
2-naphthyl-αL-fucopyranoside [pH 5.4]
—
α-Fucosidase
Example 8
Activity of the 38 kD Esterase Towards Sugar Beet Pulp Substrate
Sugar beet pulp (100 mg SBP) was incubated together with FAE (1.5 FAXX Units as measured by the method described in McCallum et al., Analytical Biochemistry , vol. 196, p. 362 (1991)) alone and in combination of 50 Units xylanase from Trichoderma longibrachiatum (Irgazyme 4×, available commercially from Genencor International, Inc.) in sodium acetate buffer (100 mM, pH 5.0). The reaction mixtures were continuously inverted at 25° C. during incubation. SBP incubated with (i) buffer alone, (ii) xylanase alone, or (iii) is boiled FAE served as controls. Reactions were halted at 12 and 24 hours by the addition of 1.1 equivalents of HCL. Determination of total ferulic acid content of SBP was determined by saponification with NaOH by the method of Borneman et al., Appl. Microbiol. Biotech . vol. 33, pp. 345-351 (1990). Ferulic acid released by enzymatic treatment was determined by HPLC using authentic ferulic acid standards (Aldrich) by the method of Borneman et al., Anal. Biochem ., vol. 190, pp. 129-133 (1990). Results are shown in table 3.
TABLE 3
Release of ferulic acid from sugar beet pulp
with ferulic acid esterase
Ferulic acid released from sugar beet pulp
Enzyme
12 hrs
24 hrs
treatment
μg
%
μg
%
FAE
15.3
2.7
26.2
4.6
Xylanase
0.5
0.1
0.6
0.1
FAE +
27.1
4.8
49.7
8.7
Xylanase
Buffer Control
0.2
0.04
0.2
0.04
Inactivated
0.2
0.03
0.2
0.04
FAE
Of course, it should be understood that a wide range of changes and modifications can be made to the preferred embodiment described above. It is therefore intended that the foregoing detailed description be understood in the context of the following claims, including all equivalents, which are intended to define the scope of this invention.
35
32 amino acids
amino acid
single
linear
1
Ala Ser Thr Gln Gly Ile Ser Glu Asp Leu Tyr Ser Arg Leu Val Glu
1 5 10 15
Met Ala Thr Ile Ser Gln Ala Ala Tyr Xaa Asp Leu Leu Asn Ile Pro
20 25 30
8 amino acids
amino acid
single
linear
2
Xaa Thr Val Gly Phe Gly Pro Tyr
1 5
9 amino acids
amino acid
single
linear
3
Phe Gly Leu His Leu Xaa Gln Xaa Met
1 5
8 amino acids
amino acid
single
linear
4
Xaa Ile Ser Glu Asp Leu Tyr Ser
1 5
9 amino acids
amino acid
single
linear
5
Tyr Ile Gly Trp Ser Phe Tyr Asn Ala
1 5
10 amino acids
amino acid
single
linear
6
Gly Ile Ser Glu Asp Leu Tyr Xaa Xaa Gln
1 5 10
10 amino acids
amino acid
single
linear
7
Xaa Ile Ser Glu Ser Leu Tyr Xaa Xaa Arg
1 5 10
7 amino acids
amino acid
single
linear
8
Gly Ile Ser Glu Asp Leu Tyr
1 5
7 amino acids
amino acid
single
linear
9
Leu Glu Pro Pro Tyr Thr Gly
1 5
14 amino acids
amino acid
single
linear
10
Xaa Ala Asn Asp Gly Ile Pro Asn Leu Pro Pro Val Glu Gln
1 5 10
8 amino acids
amino acid
single
linear
11
Tyr Pro Asp Tyr Ala Leu Tyr Lys
1 5
22 base pairs
nucleic acid
single
linear
12
CGGGAATTCG CWSACCARGG AT 22
32 amino acids
amino acid
single
linear
13
Ala Ser Thr Gln Gly Ile Ser Glu Asp Leu Tyr Ser Arg Leu Val Glu
1 5 10 15
Met Ala Thr Ile Ser Gln Ala Ala Tyr Ala Asp Leu Leu Asn Ile Pro
20 25 30
25 base pairs
nucleic acid
single
linear
14
CGGGAATTCT AYTAYATHGG TGGGT 25
16 amino acids
amino acid
single
linear
15
Val His Gly Gly Tyr Tyr Ile Gly Trp Val Ser Val Gln Asp Gln Val
1 5 10 15
25 base pairs
nucleic acid
single
linear
16
CGGGAATTCA CCCACCDATR TARTA 25
16 amino acids
amino acid
single
linear
17
Val His Gly Gly Tyr Tyr Ile Gly Trp Val Ser Val Gln Asp Gln Val
1 5 10 15
23 base pairs
nucleic acid
single
linear
18
CGGGAATTCT TGGATCCRTC RTT 23
27 amino acids
amino acid
single
linear
19
Thr Asp Ala Phe Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe Arg
1 5 10 15
Val Thr His Ala Asn Asp Gly Ile Pro Asn Leu
20 25
24 base pairs
nucleic acid
single
linear
20
CGGGAATTCA TCCRTCRTTG CRTG 24
27 amino acids
amino acid
single
linear
21
Thr Asp Ala Phe Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe Arg
1 5 10 15
Val Thr His Ala Asn Asp Gly Ile Pro Asn Leu
20 25
27 base pairs
nucleic acid
single
linear
22
CGGGAATTCG CYTGRAAGCR TCGTCAT 27
28 amino acids
amino acid
single
linear
23
Met Thr Asp Ala Phe Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe
1 5 10 15
Arg Val Thr His Ala Asn Asp Gly Ile Pro Asn Leu
20 25
28 amino acids
amino acid
single
linear
24
Met Thr Asp Ala Phe Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe
1 5 10 15
Arg Val Thr His Ala Asn Asp Gly Ile Pro Asn Leu
20 25
650 base pairs
nucleic acid
single
linear
25
GCCTCTACGC AGGGCATCTC CGAAGACCTC TACAGCCGTT TAGTCGAAAT GGCCACTAT 60
TCCCAAGCTG CCTACGCCGA CCTGTGCAAC ATTCCGTCGA CTATTATCAA GGGAGAGA 120
ATTTACAATT CTCAAACTGA CATTAACGGA TGGATCCTCC GCGACGACAG CAGCAAAG 180
ATAATCACCG TCTTCCGTGG CACTGGTAGT GATACGAATC TACAACTCGA TACTAACT 240
ACCCTCACGC CTTTCGACAC CCTACCACAA TGCAACGGTT GTGAAGTACA CGGTGGAT 300
TATATTGGAT GGGTCTCCGT CCAGGACCAA GTCGAGTCGC TTGTCAAACA GCAGGTTA 360
CAGTATCCGG ACTATGCGCT GACTGTGACG GGCCACAGGT ATGCCCTCGT GATTTCTT 420
AATTAAGTGT ATAATACTCA CTAACTCTAC GATAGTCTCG GAGCGTCCCT GGCAGCAC 480
ACTGCCGCCC AGCTGTCTGC GACATACGAC AACATCCGCC TGTACACCTT CGGCGAAC 540
CGCAGCGGCA ATCAGGCCTT CGCGTCGTAC ATGAACGATG CCTTCCAAGC CTCGAGCC 600
GATACGACGC AGTATTTCCG GGTCACTCAT GCCAACGACG GCATCCCAAA 650
197 amino acids
amino acid
single
linear
26
Ala Ser Thr Gln Gly Ile Ser Glu Asp Leu Tyr Ser Arg Leu Val Glu
1 5 10 15
Met Ala Thr Ile Ser Gln Ala Ala Tyr Ala Asp Leu Cys Asn Ile Pro
20 25 30
Ser Thr Ile Ile Lys Gly Glu Lys Ile Tyr Asn Ser Gln Thr Asp Ile
35 40 45
Asn Gly Trp Ile Leu Arg Asp Asp Ser Ser Lys Glu Ile Ile Thr Val
50 55 60
Phe Arg Gly Thr Gly Ser Asp Thr Asn Leu Gln Leu Asp Thr Asn Tyr
65 70 75 80
Thr Leu Thr Pro Phe Asp Thr Leu Pro Gln Cys Asn Gly Cys Glu Val
85 90 95
His Gly Gly Tyr Tyr Ile Gly Trp Val Ser Val Gln Asp Gln Val Glu
100 105 110
Ser Leu Val Lys Gln Gln Val Ser Gln Tyr Pro Asp Tyr Ala Leu Thr
115 120 125
Val Thr Gly His Ser Leu Gly Ala Ser Leu Ala Ala Leu Thr Ala Ala
130 135 140
Gln Leu Ser Ala Thr Tyr Asp Asn Ile Arg Leu Tyr Thr Phe Gly Glu
145 150 155 160
Pro Arg Ser Gly Asn Gln Ala Phe Ala Ser Tyr Met Asn Asp Ala Phe
165 170 175
Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe Arg Val Thr His Ala
180 185 190
Asn Asp Gly Ile Pro
195
2436 base pairs
nucleic acid
single
linear
27
CCATGGTGGT GTCGATATCG GCAGTAGTCT TTGCCGAAAC GTTGAGGGTT ACAGTGATCT 60
GCGTCGGACA TACTTCGGGG AATCTACGGC GGAATATCAA AGTCTTCGGA ATATCCATAT 120
TGGGAAAGGA CAGAAGCTCC GGGGTAGTTT GATAGATGAG CTCCGGTGTA TTAAATCGGG 180
AGCTGACAGG AGTGAGCGTC ATGTAGACCA TCTAGTAATG TCAGTCGCGC GCAATTTCGC 240
ACATGAAACA AGTTGATTTC GGGACCCCAT TGTTACATCT CTCGGCTACA GCTCGAGATG 300
TGCCTGCCGA GTATACTTAG AAGCCATGCC AGCGTGTTGT TATACGACCA AAAGTCAGGG 360
AATATGAAAC GATCGTCGGA TATTTCTTGT TTTTATCCTA AATTAGTCTT CCAGTGGTCT 420
ATTTAAGAGA TAGATCCCTT CACAAACACT CATCCAACGG ACTTCTCATA CCACTCATTG 480
ACATAATTTC AAACAGCTCC AGGCGCATTT AGTTCAACAT GAAGCAATTC TCCGCCAAAC 540
ACGTCCTCGC AGTTGTGGTG ACTGCAGGGC ACGCCTTAGC AGCCTCTACG CAAGGCATCT 600
CCGAAGACCT CTACAGCCGT TTAGTCGAAA TGGCCACTAT CTCCCAAGCT GCCTACGCCG 660
ACCTGTGCAA CATTCCGTCG ACTATTATCA AGGGAGAGAA AATTTACAAT TCTCAAACTG 720
ACATTAACGG ATGGATCCTC CGCGACGACA GCAGCAAAGA AATAATCACC GTCTTCCGTG 780
GCACTGGTAG TGATACGAAT CTACAACTCG ATACTAACTA CACCCTCACG CCTTTCGACA 840
CCCTACCACA ATGCAACGGT TGTGAAGTAC ACGGTGGATA TTATATTGGA TGGGTCTCCG 900
TCCAGGACCA AGTCGAGTCG CTTGTCAAAC AGCAGGTTAG CCAGTATCCG GACTATGCGC 960
TGACTGTGAC GGGCCACAGG TATGCCCTCG TGATTTCTTT CAATTAAGTG TATAATACTC 1020
ACTAACTCTA CGATAGTCTC GGAGCGTCCC TGGCAGCACT CACTGCCGCC CAGCTGTCGC 1080
CGACATACGA CAACATCCGC CTGTACACCT TCGGCGAACC GCGCAGCGGC AATCAGGCCT 1140
TCGCGTCGTA CATGAACGAT GCCTTCCAAG CCTCGAGCCC AGATACGACG CAGTATTTCC 1200
GGGTCACTCA TGCCAACGAC GGCATCCCAA ACCTGCCCCC GGTGGAGCAG GGGTACGCCC 1260
ATGGCGGTGT AGAGTACTGG AGCGTTGATC CTTACAGCGC CCAGAACACA TTTGTCTGCA 1320
CTGGGGATGA AGTGCAGTGC TGTGAGGCCC AGGGCGGACA GGGTGTGAAT AATGCGCACA 1380
CGACTTATTT TGGGATGACG AGCGGAGCCT GTACATGGTG ATCAGTCATT TCAGCCTCCC 1440
CGAGTGTACC AGGAAAGATG GATGTCCTGG AGAGGGCATG CATGTACGTA TACCCGAAGC 1500
ACACTTTTTC GGTAAATCAG GACATGTAAT AAGTTCCTTC CATGAATAGA TATGGTTACC 1560
CTCACCATAA GCCTTGAGGT TGCCTTTCTC TTTTGATTGT GAATATATAT TTAAAGTAGA 1620
TGACAGATAT CTCTAAACAC CTTATCCGCT TAAACCCATC ATAGATTGTG TCACGTGATA 1680
GACCCCTTGA ATGATGAGCG AAATGTATCA GTCCCGTTTA AATCAAACCC TTTCAGCCTA 1740
GCACAGTCAG AATACACCAA CCCCATTCTA AGGTAGTACT AAATATGAAT ACAGCCTAAA 1800
TGCATCGCTA TATGATCCCA TAAAGAAGCA ACAACCTTTC AGATCTCGTT TTGCGCTGCG 1860
AAGAGCTAGC TCTACCATGG TCTCAATTAT GAGTGGAGCG TTTAGTCTCG TTTAAGCCTA 1920
GCTATCTTAT AAGGACAACA CATGTACATG GGCTTACTTG TAGAGAGGTA GGATCCCGGG 1980
CTTCTTCACA TCTCGAGGAG TTGTCTACAC GTCGCGTCCA TGTCATAAGC CGGTACTCGA 2040
CGTTGTCGTG ACCGTGACCC AGACCCCTGT TGATAGCGTT GAGAAGGCCC TATATTTGAA 2100
TTTCCAATCT CAGCTTTACG AAGATATGCC CATGGTGGAG GGTTAGTAAA CCGATGATGA 2160
TCGTGTGCAG CATGAGATGA GACCGTGGCC AATCCTGTTC AAATGCCAAG ACCCGCCTCC 2220
TACCACATGT AAGGCATCCG TCGGCCGCAC GTTGAATTGT GCAAATGCCG AGATCATAAA 2280
AGCGGCCACA CTTCCACGTC GGTACTGGAT GGGTTGCGCG TGGCCATACT GTGTTTTCCA 2340
TTGCGTGGGT CGTTCGTGTT ACTGCGACGC AGATTCTGTA GGCAAGGCGC AGGGCTCTCT 2400
TCTGAGGTAG AAAACACCCC ATATTAATCT GAATTC 2436
281 amino acids
amino acid
single
linear
28
Met Lys Gln Phe Ser Ala Lys His Val Leu Ala Val Val Val Thr Ala
1 5 10 15
Gly His Ala Leu Ala Ala Ser Thr Gln Gly Ile Ser Glu Asp Leu Tyr
20 25 30
Ser Arg Leu Val Glu Met Ala Thr Ile Ser Gln Ala Ala Tyr Ala Asp
35 40 45
Leu Cys Asn Ile Pro Ser Thr Ile Ile Lys Gly Glu Lys Ile Tyr Asn
50 55 60
Ser Gln Thr Asp Ile Asn Gly Trp Ile Leu Arg Asp Asp Ser Ser Lys
65 70 75 80
Glu Ile Ile Thr Val Phe Arg Gly Thr Gly Ser Asp Thr Asn Leu Gln
85 90 95
Leu Asp Thr Asn Tyr Thr Leu Thr Pro Phe Asp Thr Leu Pro Gln Cys
100 105 110
Asn Gly Cys Glu Val His Gly Gly Tyr Tyr Ile Gly Trp Val Ser Val
115 120 125
Gln Asp Gln Val Glu Ser Leu Val Lys Gln Gln Val Ser Gln Tyr Pro
130 135 140
Asp Tyr Ala Leu Thr Val Thr Gly His Ser Leu Gly Ala Ser Leu Ala
145 150 155 160
Ala Leu Thr Ala Ala Gln Leu Ser Ala Thr Tyr Asp Asn Ile Arg Leu
165 170 175
Tyr Thr Phe Gly Glu Pro Arg Ser Gly Asn Gln Ala Phe Ala Ser Tyr
180 185 190
Met Asn Asp Ala Phe Gln Ala Ser Ser Pro Asp Thr Thr Gln Tyr Phe
195 200 205
Arg Val Thr His Ala Asn Asp Gly Ile Pro Asn Leu Pro Pro Val Glu
210 215 220
Gln Gly Tyr Ala His Gly Gly Val Glu Tyr Trp Ser Val Asp Pro Tyr
225 230 235 240
Ser Ala Gln Asn Thr Phe Val Cys Thr Gly Asp Glu Val Gln Cys Cys
245 250 255
Glu Ala Gln Gly Gly Gln Gly Val Asn Asn Ala His Thr Thr Tyr Phe
260 265 270
Gly Met Thr Ser Gly Ala Cys Thr Trp
275 280
2436 base pairs
nucleic acid
single
linear
29
CCATGGTGGT GTCGATATCG GCAGTAGTCT TTGCCGAAAC GTTGAGGGTT ACAGTGATCT 60
GCGTCGGACA TACTTCGGGG AATCTACGGC GGAATATCAA AGTCTTCGGA ATATCCATAT 120
TGGGAAAGGA CAGAAGCTCC GGGGTAGTTT GATAGATGAG CTCCGGTGTA TTAAATCGGG 180
AGCTGACAGG AGTGAGCGTC ATGTAGACCA TCTAGTAATG TCAGTCGCGC GCAATTTCGC 240
ACATGAAACA AGTTGATTTC GGGACCCCAT TGTTACATCT CTCGGCTACA GCTCGAGATG 300
TGCCTGCCGA GTATACTTAG AAGCCATGCC AGCGTGTTGT TATACGACCA AAAGTCAGGG 360
AATATGAAAC GATCGTCGGA TATTTCTTGT TTTTATCCTA AATTAGTCTT CCAGTGGTTT 420
ATTTAAGAGA TAGATCCCTT CACAAACACT CATCCAACGG ACTTCTCATA CCACTCATTG 480
ACATAATTTC AAACAGCTCC AGGCGCATTT AGTTCAACAT GAAGCAATTC TCCGCCAAAC 540
ACGTCCTCGC AGTTGTGGTG ACTGCAGGGC ACGCCTTAGC AGCCTCTACG CAAGGCATCT 600
CCGAAGACCT CTACAGCCGT TTAGTCGAAA TGGCCACTAT CTCCCAAGCT GCCTACGCCG 660
ACCTGTGCAA CATTCCGTCG ACTATTATCA AGGGAGAGAA AATTTACAAT TCTCAAACTG 720
ACATTAACGG ATGGATCCTC CGCGACGACA GCAGCAAAGA AATAATCACC GTCTTCCGTG 780
GCACTGGTAG TGATACGAAT CTACAACTCG ATACTAACTA CACCCTCACG CCTTTCGACA 840
CCCTACCACA ATGCAACGGT TGTGAAGTAC ACGGTGGATA TTATATTGGA TGGGTCTCCG 900
TCCAGGACCA AGTCGAGTCG CTTGTCAAAC AGCAGGTTAG CCAGTATCCG GACTATGCGC 960
TGACTGTGAC GGGCCACAGG TATGCCCTCG TGATTTCTTT CAATTAAGTG TATAATACTC 1020
ACTAACTCTA CGATAGTCTC GGAGCGTCCC TGGCAGCACT CACTGCCGCC CAGCTGTCTG 1080
CGACATACGA CAACATCCGC CTGTACACCT TCGGCGAACC GCGCAGCGGC AATCAGGCCT 1140
TCGCGTCGTA CATGAACGAT GCCTTCCAAG CCTCGAGCCC AGATACGACG CAGTATTTCC 1200
GGGTCACTCA TGCCAACGAC GGCATCCCAA ACCTGCCCCC GGTGGAGCAG GGGTACGCCC 1260
ATGGCGGTGT AGAGTACTGG AGCGTTGATC CTTACAGCGC CCAGAACACA TTTGTCTGCA 1320
CTGGGGATGA AGTGCAGTGC TGTGAGGCCC AGGGCGGACA GGGTGTGAAT AATGCGCACA 1380
CGACTTATTT TGGGATGACG AGCGGAGCCT GTACATGGTG ATCAGTCATT TCAGCCTCCC 1440
CGAGTGTACC AGGAAAGATG GATGTCCTGG AGAGGGCATG CATGTACGTA TACCCGAAGC 1500
ACACTTTTTC GGTAAATCAG GACATGTAAT AAGTTCCTTC CATGAATAGA TATGGTTACC 1560
CTCACCATAA GCCTTGAGGT TGCCTTTCTC TTTTGATTGT GAATATATAT TTAAAGTAGA 1620
TGACAGATAT CTCTAAACAC CTTATCCGCT TAAACCCATC ATAGATTGTG TCACGTGATA 1680
GACCCCTTGA ATGATGAGCG AAATGTATCA GTCCCGTTTA AATCAAACCC TTTCAGCCTA 1740
GCACAGTCAG AATACACCAA CCCCATTCTA AGGTAGTACT AAATATGAAT ACAGCCTAAA 1800
TGCATCGCTA TATGATCCCA TAAAGAAGCA ACAACCTTTC AGATCTCGTT TTGCGCTGCG 1860
AAGAGCTAGC TCTACCATGG TCTCAATTAT GAGTGGAGCG TTTAGTCTCG TTTAAGCCTA 1920
GCTATCTTAT AAGGACAACA CATGTACATG GGCTTACTTG TAGAGAGGTA GGATCCCGGG 1980
CTTCTTCACA TCTCGAGGAG TTGTCTACAC GTCGCGTCCA TGTCATAAGC CGGTACTCGA 2040
CGTTGTCGTG ACCGTGACCC AGACCCCTGT TGATAGCGTT GAGAAGGCCC TATATTTGAA 2100
TTTCCAATCT CAGCTTTACG AAGATATGCC CATGGTGGAG GGTTAGTAAA CCGATGATGA 2160
TCGTGTGCAG CATGAGATGA GACCGTGGCC AATCCTGTTC AAATGCCAAG ACCCGCCTCC 2220
TACCACATGT AAGGCATCCG TCGGCCGCAC GTTGAATTGT GCAAATGCCG AGATCATAAA 2280
AGCGGCCACA CTTCCACGTC GGTACTGGAT GGGTTGCGCG TGGCCATACT GTGTTTTCCA 2340
TTGCGTGGGT CGTTCGTGTT ACTGCGACGC AGATTCTGTA GGCAAGGCGC AGGGCTCTCT 2400
TCTGAGGTAG AAAACACCCC ATATTAATCT GAATTC 2436
32 base pairs
nucleic acid
single
linear
30
GGCCTGCAGC CCCGCAAACT ACGGGTACGT CC 32
35 base pairs
nucleic acid
single
linear
31
CGCGCTGCAG GCTCTTTCTG GTAATACTAT GCTGG 35
36 base pairs
nucleic acid
single
linear
32
GGCTTAATTA ACGTGCTGGT CTCGGATCTT TGGCGG 36
40 base pairs
nucleic acid
single
linear
33
GGGGCGCGCC AGATCTAGTA CCGATGTTGA GGATGAAGCT 40
39 base pairs
nucleic acid
single
linear
34
GCCCAGATCT CCGCAATGAA GCAATTCTCC GCCAAACAC 39
25 base pairs
nucleic acid
single
linear
35
AATAGTCGAC GGAATGTTGC ACAGG 25
|
A novel DNA is provided which encodes an enzyme having esterolytic activity isolated from Aspergillus . Also provided for is a method of isolating DNA encoding an enzyme having esterolytic activity from organisms which possess such DNA, transformation of the DNA into a suitable host organism, expression of the transformed DNA and the use of the expressed esterase protein in feed as a supplement, in textiles for the finishing of such textiles prior to sale, in starch processing or production of foods such as baked bread.
| 3
|
BACKGROUND
[0001] This invention relates generally to offshore drilling operations.
[0002] Offshore drilling operations may be implemented with a variety of different platforms which may be secured to the seabed floor. These platforms may be effective at shallower depths. At greater depths, such as depths greater than 5000 feet, it is generally desirable to use ships or semi-submersible rigs to conduct such deep water drilling operations.
[0003] These ships or rigs may be precisely positioned at a desired location so that the drilling equipment may be operated to precisely drill wells at desired locations. The ship or rig may be maintained in position under dynamic positioning even in extreme seas. As used herein, a “ship” is a floating platform capable of propulsion on its own or by being pushed, pulled or towed. It includes semi-submersible rigs and self-propelled vessels.
[0004] As a result, a number of exploration wells may be drilled, one after the other, in a deepwater offshore environment, such as the outer continental shelf of the United States, Africa, Asia, or Western Europe. However, the large number of operations that must be performed when successively drilling a number of exploration wells, even in the same area, may be extremely time consuming because of the complexity of deep water operations.
[0005] Conventionally, tubulars must be made up, lowered through extensive sea depths to the seabed floor, used to drill the seabed floor, and then withdrawn to be replaced by other tubulars. As used herein, “tubulars” refers to piping, conduits, conductors, casing, drill strings, and risers. In addition, marine risers must extend ultimately from the ship to the seabed floor and blowout preventers may ultimately be run and installed on the seabed floor for well control reasons. Assembling, positioning, and removing these disparate tubulars generally involve operations that take extensive time periods. The time needed to extend a tubular through 5000 or greater feet of water results in some delay. The time needed to make up tubulars results in additional delay.
[0006] With a conventional ship having a single drilling platform, it is impossible to perform multiple operations in parallel. Thus, the time periods needed to complete each well may be relatively long. Since, generally, these drilling ships are operated on a rental basis, the longer that it takes to drill the well, the more expensive is the resulting well.
[0007] So called dual activity drilling ships are known. In these ships, a pair of derricks may be provided on the ship which provide a structural support for underlying drilling tubulars. The dual derricks may be operated in some degree in parallel. For example, while one operation is occurring on one derrick, other operations may be implemented on another derrick. While such approaches may result in some time savings, there are still some deficiencies in such dual activity approaches.
[0008] Thus, there is a need for even faster ways to drill deep water wells.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a partial, schematic depiction of a drill ship in position at an offshore drill site at an early stage in the well completion process according to one embodiment of the present invention;
[0010] FIG. 2 is a partial, schematic depiction of the drill ship shown in FIG. 1 at a subsequent stage of well completion in accordance with one embodiment of the present invention;
[0011] FIG. 3 is a partial, schematic depiction of the drill ship shown in FIG. 1 at a subsequent stage of well completion in accordance with one embodiment of the present invention;
[0012] FIG. 4 is a partial, schematic depiction of the drill ship shown in FIG. 1 at a subsequent stage of well completion in accordance with one embodiment of the present invention;
[0013] FIG. 5 is a partial, schematic depiction of the drill ship shown in FIG. 1 at a subsequent stage of well completion in accordance with one embodiment of the present invention;
[0014] FIG. 6 is a depiction of the same drill ship after the ship has been moved in accordance with one embodiment of the present invention;
[0015] FIG. 7 is a partial, schematic, enlarged top plan view of the ship shown in FIG. 4 in accordance with one embodiment of the present invention; and
[0016] FIG. 8 is a partial, enlarged, perspective view of a trolley and casing hung off in accordance with one embodiment of the present invention.
DETAILED DESCRIPTION
[0017] Referring to FIG. 1 , a triple activity drilling ship 10 may be a ship capable of drilling operations in deep and ultra-deep water. The ship 10 may also be a semi-submersible rig as well. The ship may be equipped with conventional dynamic positioning controls which enable the ship to be precisely positioned at a precisely determined location. Moreover, the ship may be held precisely in position during drilling operations pursuant to computer control.
[0018] Prior to arriving on the drilling site, tubulars may be readied. For example, a blow out preventer and riser may be assembled, skidded, and tested prior to arrival. Likewise, the 20 inch casing may be assembled prior to arrival as well.
[0019] Initially, as the ship comes on a drilling site, operations are implemented to precisely orient the ship with respect to the seabed floor. Global positioning satellites and other technology may be utilized for this purpose. Some amount of time is needed, prior to initiation of drilling operations, to precisely position the ship at the desired location. During this time, some drilling preparation activities may be accomplished in accordance with some embodiments of the present invention. Tubulars may be made up and readied for use. For example, a 30 inch conductor may be made up and stowed in appropriate tubular holding facilities prior to being actually run into the sea. Likewise, the blow out preventer and riser may be run during the dynamic positioning.
[0020] In some embodiments, a main drilling center 14 and a secondary drilling center 12 may be provided. In some embodiments, the secondary drilling center is adapted for handling lighter tubulars, while the main drilling center is adapted to handle heavier tubulars and drilling the well. In one embodiment, the main and secondary drilling centers may be implemented by hydraulic RAM devices. In other embodiments, derricks or superstructures may be provided. Such derricks or superstructures may provide structural support for the tubulars hung from such derricks.
[0021] In contrast, with a hydraulic RAM system, the tubulars may be supported directly on the ship's deck. This avoids the need for expensive, heavy derricks to support the tubulars. However, in some embodiments, even using a hydraulic system, masts or guides may be provided to guide the tubulars when they are in their uphauled positions.
[0022] Thus, depending on the nature of the centers 12 and 14 , different tubular storage facilities may be utilized. For example, when a derrick system is utilized, the derricks are of sufficient strength that tubulars may be stored by simply leaning them against the insides of the derricks. In other cases, tubular and storage systems, setbacks envelopes, and racks may be provided to hold the assembled or partially assembled tubulars.
[0023] Conventional equipment may be used for advancing, running, withdrawing, lifting, or rotating the tubulars to the seabed and ultimately into the seabed floor. In this regard, hoists, top drives, sheaves, draw works, rotary tables, traveling blocks, motion compensators, hydraulic RAMS, or any other known equipment may be utilized. The hydraulic RAM may support tubulars on the deck, but derricks support tubulars from above the deck. The present invention is in no way limited to any particular equipment.
[0024] As described above, prior to the point when the ship is precisely positioned, some drilling preparatory activities may be completed. In some embodiments, the tubulars may be in the position shown in FIG. 1 at the time when the ship's positioning operation is finally completed. As will be appreciated by those skilled in the art, in this way, substantial activity may be completed prior to the time that drilling may actually begin. This may substantially reduce the overall amount of time needed to complete a given well.
[0025] The ship may include a third activity center in the form of a trip saver trolley 16 . In one embodiment, the trolley 16 may be a Christmas tree trolley. However, any moveable, tubular supporting surface that can support tubulars may be utilized in some embodiments. Underslung trip saver trolleys mounted on rollers that roll over a rail or track may be utilized, as well as overslung trolleys that ride on top of a rail or track.
[0026] In most embodiments, a trolley rail or track allows the trolley to move from a position displaced to the side of the secondary drilling center 12 to a position under or within the secondary drilling center 12 . In this way, tubulars already made up and hung from the trolley 16 may be moved in position for use by the secondary drilling center 12 . This ability to pre-hang tubulars from the trolley 16 may result in significant time savings since it allows tubulars to be made up prior to the time when drilling operations are actually ready to begin and the ship has been accurately positioned in some embodiments.
[0027] Referring to FIG. 1 , initially, a 20 inch casing 18 is made up on the secondary drilling center 12 . Then, the trip saver trolley 16 , positioned astride the secondary drilling center 12 , may be slid into position under the secondary drilling center 12 as indicated in FIG. 2 . The trolley 16 may then latch onto the 20 inch casing 18 and slide it to the left in the direction of the arrow shown in FIG. 2 .
[0028] In some embodiments, the removal of tubulars from one drilling center, such as the drilling center 12 , and their securement on the trolley 16 may be done using conventional equipment such as a running tool. In some embodiments, the tubulars may be lifted onto or off of the trolley 16 .
[0029] In some embodiments, the trolley may have an opening 90 which is sized to mate with components of tubulars such as the casing 18 as shown in FIG. 8 . For example, the 20 inch casing 18 may have an enlarged element, such as a housing 52 , that may be retained atop the trolley 16 . The housing 52 may, for example, be used to latch to the blow out preventer.
[0030] In one embodiment, a split spherical bearing 50 , as shown in FIG. 8 , may be utilized. The split spherical bearing 50 may include portions 50 a and 50 b that are openable in the directions indicated by the arrows B. In other words, the bearing 50 includes two portions which support the casing 18 on the housing 52 . When the bearing 50 is opened, the casing 18 may be lifted from the trolley 16 and moved onto other components. The trolley may include sets of rollers or bearings 30 that slide on a track 28 that extends across the secondary drilling center 12 .
[0031] At the instance illustrated in FIG. 3 , a 30 inch conductor 22 may have been run down to the seabed floor, perhaps without yet contacting the seabed floor SB. The conductor 22 may be supported on a string 20 . This means the 30 inch conductor was already made up with an internal 26 inch drill.
[0032] At the same time, in the main drilling center 14 , a marine riser 24 may be assembled with the blowout preventer 26 secured to its lowermost end as indicated in FIG. 1 . Thus, the blowout preventer 26 has already been skidded, tested, and assembled. Depending on the depth of the sea S, the blowout preventer 26 may be all the way down to a position close to the seabed floor, as shown in FIG. 4 , or it may still be suspended within the sea S, well above the seabed floor, at the time that drilling operations are ready to begin, the ship has been accurately positioned.
[0033] In some embodiments, the blowout preventer 26 may be lowered to the position shown in FIG. 3 , but, in other embodiments, the blowout preventer may not yet have reached a point proximate to the seabed floor at the time the conductor 22 is jetted in. This positioning of the blowout preventer may depend on how skillful the crew is, how long it takes to position the ship, and the depth of water in which the ship is operating among other factors.
[0034] Note that at the point in time shown in FIG. 2 , no contact with the seabed SB has yet been made in some embodiments. This lack of contact enables the ship to be repositioned in the course of the ship positioning operation. Prior to completion of dynamic positioning, the 20 inch conductor may be made up on the secondary drilling center 12 and transferred to and hung off of the trolley 16 . Also, the conductor 22 may be already made up and lowered down to, but not touching, the seabed.
[0035] While the casing 18 is made up on the secondary drilling center 12 , transferred to the trolley 16 , and the conductor 22 is made up and lowered from the secondary drilling center 12 , the marine riser 24 and blowout preventer 26 may be assembled and may be begun to be run to the seabed S from the main drilling center 14 . Thus, it will be appreciated that three different tubulars may be assembled, at least partially in parallel, and partially pre-positioned and preassembled prior to the time that drilling operations can actually begin because the ship is accurately positioned.
[0036] Once the ship is accurately positioned, the running of the blow out preventer and riser may be stopped. Then, the 30 inch conductor 22 may be lowered into contact with the seabed floor SB as shown in FIG. 3 . Then, the 30 inch conductor 22 may be jetted into the seabed in one embodiment. Thereafter, an internal 26 inch drill, within the string 18 , may be operated to drill a 26 inch hole. Of course, these sizes of the tubulars and the holes that are drilled are simply illustrative. Other tubular sizes and hole sizes may be utilized and those skilled in the art will appreciate that only examples are given herein.
[0037] After completion of the 30 inch jet in and the 26 inch hole drilling, the 30 inch conductor 22 and its tubulars 20 may be raised from the secondary drilling center 12 , disassembled, and stored.
[0038] Once the 30 inch conductor is no longer touching the seabed, then the running of the blow out preventer and riser may be resumed.
[0039] As soon as the 30 inch conductor 22 is out of the way, the trolley 16 may be rolled to the right to the position shown in FIG. 4 with the 20 inch casing 18 already fully or at least partially assembled thereunder. The 20 inch casing 18 may then be connected to the secondary drilling center 12 using a running tool or another tool of the type shown in FIG. 8 . The 20 inch casing may then be run into the 26 inch hole and cemented in place.
[0040] At the times shown in FIG. 4 after the 30 conductor 22 is placed onto the seabed floor SB and jetted in, the riser 24 and blowout preventer 26 may be continued to be run into the seabed S. In other words, in embodiments where it was not possible to get the blowout preventer 26 proximate to the seabed floor at the point in time when drilling operations can begin, the downward course of the riser 24 and blowout preventer 26 may be continued thereafter, as possible. Specifically, that downward running of the blowout preventer 26 may be continued while the 30 inch conductor is being jetted in, the 26 inch hole is being drilled, and the 20 inch casing 18 is transferred to the trolley to the secondary drilling center 12 and then run into the seabed and cemented in.
[0041] Thus, operations in the main drilling center 14 with the blowout preventer 26 continue, to the extent necessary and as possible, while other operations are occurring so as to further reduce the overall time of the drilling operation.
[0042] In some embodiments, the riser 24 and blowout preventer 26 may be maintained out of contact with the seabed floor at any time when the 20 inch casing 18 is in contact with the seabed floor. Thus, once the 20 inch casing makes contact with the seabed floor, in those embodiments, the blowout preventer 26 is at all times out of contact with the seabed floor and may not be run in some embodiments.
[0043] Once the 20 inch casing is in place, the tubulars 18 may be released from the seabed, withdrawn, disassembled, and stored, so that the ship 10 may be repositioned. Particularly, the ship may be repositioned in the direction of the arrows shown in FIG. 6 . In some embodiments, it is advantageous to have the trolley 16 , and the drilling centers 12 and 14 aligned along the length of the ship so that the ship may be moved in a normal forward motion direction to reposition the blowout preventer 26 and the riser 24 over the well as indicated in FIG. 6 . Thus, longitudinal conventional forward power may be utilized to reposition the ship and the riser and blowout preventer over the well.
[0044] Once the ship has been positioned accurately, the blowout preventer may be latched on the 20 inch casing already in position. Then, a 17½ inch hole is drilled and the 13¾ inch casing may be run and cemented in position. The 13⅜ inch casing may be assembled on a pipe racker in some embodiments.
[0045] In some embodiments, this results in completion of the well. If subsequent drilling operations are desired, the ship may be repositioned after detaching the riser. For example, in some cases, the ship may be repositioned with the risers still hanging from the ship, as long as the repositioning distance is relatively short. However, in other embodiments, the entire process begins again.
[0046] In the case where production is planned, then the ship can be maintained in position and production may begin.
[0047] Referring to FIG. 7 , in some embodiments of the present invention, the trolley 16 may be mounted on a pair of parallel tracks 28 which extend under the secondary drilling center 12 and to the left thereof. In one embodiment, the trolley 16 may be a conventional Christmas tree trolley which hangs from rollers 30 positioned over the track 28 . However, other arrangements are also possible.
[0048] References throughout this specification to “one embodiment” or “an embodiment” mean that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation encompassed within the present invention. Thus, appearances of the phrase “one embodiment” or “in an embodiment” are not necessarily referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be instituted in other suitable forms other than the particular embodiment illustrated and all such forms may be encompassed within the claims of the present application.
[0049] While the present invention has been described with respect to a limited number of embodiments, those skilled in the art will appreciate numerous modifications and variations therefrom. It is intended that the appended claims cover all such modifications and variations as fall within the true spirit and scope of this present invention.
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A triple activity drilling ship may be provided with two separate drilling centers, each including drilling apparatus. In addition, a trolley that is capable of supporting tubulars may be positioned between a first position within one of said drilling centers and a second position outside that drilling center. As a result, the trolley may be used to hold assembled tubulars while other activities are ongoing in one or more of the drilling centers.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a non-provisional application which claims benefit under 35 USC §119(e) to U.S. Provisional Application Ser. No. 61/421,509 filed Dec. 9, 2010, entitled “CONDENSATION OF GLYCOLS TO PRODUCE BIOFUELS,” which is incorporated herein in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
None.
FIELD OF THE INVENTION
The present disclosure relates to the field of biomass-derived transportation fuels. More specifically, it relates to methods for converting light glycol feeds originating from biomass into polyglycol products suitable for use as a bio-derived fuel or cetane-enhancing fuel additive.
BACKGROUND
There is a great interest in the discovery of alternative sources of fuels and chemicals from resources other than petroleum. Development of non-petroleum-based liquid transportation fuels may provide economic and environmental benefits, while also increasing national security by decreasing reliance on non-domestic energy sources. Biomass, such as plants and animal fats, represent a major alternative source of hydrocarbons that can be converted into fuels. Liquid fuels derived from biomass are rapidly entering the market, driven by both need for increased national energy independence and rapid fluctuations in the cost of petroleum products. In 2007, the Energy Independence and Security Act was passed in the United States, which requires increasing quantities of bio-derived fuels to be produced over time. Similarly, the European Union directive 2003/30/EC promotes the use of biofuels or other renewable fuels. The directive has set a minimum percentage of biofuels to replace diesel or gasoline for transport purposes so, that by the end of 2010 there should be a 5.75% minimum proportion of biofuels in all gasoline and diesel fuels sold. To meet these mandates, it is essential to develop more efficient processes to convert bio-derived compounds into fuels that can fulfill these government mandates, as well as future global energy needs.
The carbohydrates found in plants and animals can be used to produce fuel range hydrocarbons. However, many carbohydrates (e.g., starch) are undesirable as feed stocks for creating biomass-derived fuels due to the costs associated with converting them to a useable form. The chemical structure of some carbohydrates makes them difficult to convert, and conversion processes may produce low yields of desirable products. Carbohydrates that are difficult to convert include compounds with low effective hydrogen to carbon ratios, including carbohydrates such as starches and sugars, and other oxygenates with low effective hydrogen including carboxylic acids and anhydrides, light glycols, glycerin and other polyols and short chain aldehydes. As such, development of an efficient and inexpensive process for converting one or more of these difficult-to-convert biomass feedstocks into a form suitable for use as a fuel additive could be a significant contribution to the art and to the economy.
Glycerol is a significant side-product of the trans-esterification reaction utilized to convert plant oils and animal fats into biofuels, and some work has been done examining ways to utilize glycerol. Karinen, et al. have reported methods for the etherification of glycerol and isobutene, while papers by Frustieri, et al. and Keplacova, et al., both include methods for catalytic etherification of glycerol by tert-butyl alcohol. U.S. Patent App. Pub. US2010/0094062 describes a process for the etherification of glycerol with an alkene or alkyne, followed by nitration of a remaining hydroxyl group. A portion of the process claimed in US2008/0300435 pertains to the dimerization/condensation of alcohols such as pentanol or isopropyl alcohol. However, to date, no methods have demonstrated an efficient process for the etherification of biologically-derived light glycol feedstock, such as ethylene glycol or propylene glycol, that results in a product suitable for subsequent use as a fuel additive.
BRIEF SUMMARY
Towards this goal, we disclose herein a novel process for efficiently converting biomass-derived light glycols, such as ethylene glycol and propylene glycol, into low molecular weight poly-glycol products useful as oxygenated cetane enhancers in transportation fuels. Whereas glycerol is a common byproduct of transesterification processes, light glycol streams are often obtained by the moderate hydrogenolysis of larger biomass-derived oxygenates such as alditols, cleaving backbone carbon-carbon linkages to form this feed. Glycols are easier to utilize as feedstock than their parent alditols in that glycols are liquids at room temperature and may be distilled to remove impurities rather than having to rely on other purification techniques (e.g. ion-exchange for metals removal). In contrast, alditols in the five to six carbon range are solids at room temperature and tend to decompose when heated above their melting points. Unlike some unsaturated biomass derived oxygenates, glycols are stable and may be stored long term without special measures to prevent degradation.
Unfortunately, glycols are not suitable for direct blending into fuels due to miscibility issues. However, converting these glycols to low molecular weight poly-glycols (LMWPG) helps resolve this problem. During the conventional processing of hydrocarbons to produce fuels, removing oxygen involves reacting oxygen containing compounds with hydrogen to produce water. However, the underlying chemistry behind the conversion of the present disclosure involves acid-catalyzed condensation reactions that do not require hydrogen for oxygen removal. This reduces greenhouse gas emissions while also reducing the operational cost associated with production of hydrogen. Some oxygen from the feed is left in the final product resulting in the product maintaining much of the volume of the original starting material. Finally, these condensation reactions may be conducted at much lower temperatures than conventional oxygen removal processes, resulting in further savings.
The present disclosure pertains to using solid acidic catalysts to convert biomass-derived glycols into di-, tri-, and some larger low molecular weight polyglycols (LMWPG), followed by steps to increase miscibility of the LMWPG with liquid hydrocarbon fuels. Derivatives of these LMWPG fall into a category of materials termed oxygenated cetane improvers, which are larger, predominantly linear compounds with oxygen substituted for carbon periodically along the backbone. The oxygen content of oxygenated cetane improvers varies depending on the feedstream used in their formation. However, a National Renewable Energy Laboratory report by Murphy, et al. shows that number of polyglycols have been calculated to possess a high cetane number. In addition, preliminary findings by Tijm, et. al. have shown that several LMWPG, when added to premium diesel fuel at 10-11% (by wt.), reduce particulate emissions during combustion by up to 28% versus unmodified premium diesel.
Certain embodiments of the invention disclosed herein provide a process for converting glycols (such as, for example, ethylene glycol and propylene glycol) into products suitable for use as fuel additives that comprises the steps of: (a) providing a biomass-derived feedstream comprising light glycols, where the glycols contain two, three or four carbon atoms, (b) contacting the feedstream with a first catalyst in a reactor, where the contacting results in an acidic condensation reaction that converts a least a portion of the feedstream to condensation products, and where said condensation products possess at least 4 carbon atoms and one ether functional group, (c) converting at least a portion of the remaining hydroxyl functional groups on the condensation products from step (b) to ether functional groups by combining the condensation products with a second catalyst to produce a liquid hydrocarbon mixture suitable for use as an additive to liquid hydrocarbon fuels, wherein the converting takes place in the presence of an olefin, monofunctional alcohol or mixtures thereof, and wherein the liquid hydrocarbon mixture has increased miscibility in liquid hydrocarbon fuels as a result of step c).
Certain alternative embodiments of the invention disclosed herein provide a process for converting glycols (such as, for example, ethylene glycol and propylene glycol) into products suitable for use as fuel additives that comprises the steps of: (a) providing a biomass-derived feedstream comprising light glycols, where the glycols contain two, three or four carbon atoms, (b) contacting the feedstream with a first catalyst in a reactor, where the contacting results in an acidic condensation reaction that converts a least a portion of the feedstream to condensation products, and where said condensation products possess at least 4 carbon atoms and one ether functional group, (c) reducing at least a portion of the remaining hydroxyl groups on the condensation products by combining the condensation products with a second catalyst in the presence of hydrogen to produce water and a liquid hydrocarbon mixture that is suitable for use as an additive for a liquid hydrocarbon fuel. This liquid hydrocarbon mixture has increased miscibility in liquid hydrocarbon fuels as a result of this reduction step. In certain embodiments, the functions of the first and second catalyst are performed by the same catalyst.
In certain embodiments, the process additionally comprises combining the liquid hydrocarbon mixture of step (c) with a liquid hydrocarbon fuel to produce an improved liquid hydrocarbon fuel, wherein the improved liquid hydrocarbon fuel has improved combustion properties that may include increased cetane number, decreased emissions of environmental pollutants during combustion, or both.
The first catalyst may comprise at least two elements, one selected from Group 4 of the periodic table, and the other selected from Group 6 of the periodic table. Alternatively, the first catalyst may be a microporous molecular sieve selected from the group consisting of crystalline silicoaluminophosphates and aluminosilicates, that has been chemically treated to decrease catalytic activity outside the internal channels of the catalyst. Preferably, the pore diameter of the molecular sieve catalyst restricts the formation of circular products inside its pores.
In certain embodiments, the second catalyst may be an acidic macroreticular ion-exchange resin. In other embodiments, the second catalyst may be a microporous molecular sieve selected from the group consisting of crystalline silicoaluminophosphates and aluminosilicates, that has been chemically treated to decrease catalytic activity outside the internal channels of the catalyst.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG.1 illustrates an acidic condensation of the current disclosure also referred to as etherification.
FIG.2 illustrates outlines how a non-preferred cyclic product (p-dioxane) can be formed from the condensation product of two ethylene glycol molecules.
DETAILED DESCRIPTION
Process conditions for conducting condensation reactions are relatively mild when compared to other industrial processes, such as conventional naphtha hydrodesulfurization, which normally requires temperatures in the range of 285° C. to 370° C. Low temperatures are advantageous since at higher temperature elimination becomes a competing reaction mechanism. Elimination, like condensation, involves the removal of a small molecule from a parent, but there is no coupling associated with the reaction. Elimination results in the production of an unsaturated product (e.g., ethanol to ethylene.) While these limits exist, yields for this process are typically sufficient to operate at the commercial level for chemical production. The acidic condensation of the current disclosure could also be referred to as etherification, and is illustrated in FIG. 1 . Depicted in the first line, the acid catalyst donates a proton to a hydroxyl group of a first glycol molecule. By definition, a glycol is a diol where the two hydroxyl groups are attached to different carbons. Thus, the R groups shown in FIG. 1 represent a hydrocarbon chain comprising a second hydroxyl moiety. Referring to the second line of FIG. 1 , a hydroxyl group from a second glycol molecule to reacts with the electrophilic carbon adjacent to the proton-accepting hydroxyl. Finally, the third line of FIG. 1 depicts removal of a water molecule (and proton) forming an ether bond between the two glycols. Acid-catalyzed condensation of primary alcohols in the homogeneously catalyzed case occurs via an S N 2 mechanism. In this type of mechanism, the transition state involves the attacking nucleophile driving off the leaving group in a concerted mechanism. This acid catalyzed condensation reaction is distinct from the base-catalyzed condensation reaction developed by Guerbet, which instead produces branched, saturated alcohols and not ethers. Examples of the Guerbet condensation reaction being utilized to form saturated branched hydrocarbons are shown in U.S. Pat. No. 7,049,476 and US2008/0302001.
Typical biomass-derived molecules suitable for conversion to LMWPG by the processes described herein include any diol comprising two to four carbon atoms. Examples include ethylene glycol, propylene glycol, 1,3-propanediol, 1,2,-butanediol, 1,3,-butanediol, 2,3-butanediol, and 1,4-butanediol.
As mentioned above, it is possible to convert glycols into di-, tri-, and some larger LMWPG using a solid acidic catalyst. Derivatives of these LMWPG fall into a category of materials termed oxygenated cetane improvers. Oxygenated cetane improvers are larger, predominantly linear compounds with oxygen substituted for carbon periodically along the backbone. The oxygen content of oxygenated cetane improvers varies depending on the feedstream used in their formation. However, a National Renewable Energy Laboratory report by Murphy, et al. shows that number of polyglycols have been calculated to possess a high cetane number. In addition, preliminary findings by Tijm, et. al. have shown that several LMWPG, when added to premium diesel fuel at 10-11% (by wt.), reduce particulate emissions during combustion by up to 28% versus unmodified premium diesel.
The condensation reactions associated with the processes described herein are generally conducted at a temperature ranging from about 100° C. to about 300° C. More preferably, these reactions are conducted at a temperature ranging from about 120° to about 260° C. The condensation reactions are generally conducted at a pressure ranging from about 200 kPa to about 8000 kPa. Preferably, reactions are conducted at a pressure ranging from about 500 kPa to about 5000 kPa. Additionally, condensation reactions of the present disclosure are generally conducted with a feedstream flow rate ranging from about 0.1 h −1 liquid weight hourly space velocity (LWHSV) to about 20 h −1 LWHSV. Preferably, reactions are conducted with a feedstream flow rate ranging from about 0.5 h −1 LWHSV to about 15 h −1 LWHSV.
The condensation catalyst utilized may be any catalyst capable of condensing light glycols to produce LMWPG. Preferably, the catalyst is an acidic catalyst suitable for such reactions, such as tungstated zirconias (for example, WO 3 /ZrO 2 ), metal loaded tungstated zirconias (for example, Pt—WO 3 /ZrO 2 ), heteropoly acids (for example, H 4 SiW 12 O 40 ), supported sulfonic acids (for example, acidic Amberlyst™ ion-exchange resins [Rohm and Haas]). Other catalysts useful for such condensation reactions may include acidic metal oxide catalysts, such as niobium pentoxide. Preferably, the catalyst is a microporous molecular sieve selected from crystalline silicoaluminophosphates and aluminosilicates with a three-dimensional pore structure that selectively favors the production of linear condensation products within the pores of the zeolite, while minimizing production of undesirable cyclic secondary products. Such undesirable products include p-dioxane. FIG. 2 outlines how this non-preferred cyclic product 121 can be formed from the condensation product 115 of two ethylene glycol molecules 101 .
In certain embodiments, the condensation catalyst is a surface-passivated zeolite (such as, for example, H-Y, H-USY, H-mordenite, or H-ZSM-5) that selectively favors the production of linear LMWPG within the internal pores of the zeolite, while further minimizing production of undesirable cyclic secondary products on the zeolite surface. P-dioxane is a bulky, cyclic structure that is less likely to form within the confines of a zeolite channel system at low temperatures. Selectivity toward the formation of LMWPG may be enhanced by surface passivation of the zeolite to block activity outside of the channel system. Methods for surface passivation of zeolites are familiar to those with knowledge in the art, and one example of a zeolite passivation procedure is provided in Example II of the current disclosure. Creating selectivity towards the favored primary poly-glycol product is important for the economic viability of the process at industrial scale, since p-dioxane is unsuitable for blending into fuels, and is a stable product that is difficult to convert back to a form that is useful as a biofuel component.
Following condensation of the light glycol feed to form a LMWPG, in certain embodiments the remaining hydroxyl groups are modified by an additional “capping” step to produce a poly-glycol derivative. This end-capping of the terminal hydroxyl groups may be accomplished by any catalyst capable of catalyzing an etherification reaction between the remaining terminal hydroxyl groups and an olefin. The end product would preferably have increased miscibility in liquid hydrocarbon fuels, and thus, be more suitable for use as a fuel additive. Such capping techniques are understood by individuals having knowledge in the art, and examples of such techniques are provided in the previously mentioned papers by Karinen, et. al., Frustieri, et. al. and Keplacova, et. al.
In certain alternative embodiments, the remaining hydroxyl groups that are present on the LMWPG following condensation of the light glycol feed are instead “capped” by an additional acidic condensation reaction in the presence of a monofunctional alcohol (such as, for example, methanol, ethanol or propanol). This step may be performed with the catalyst of step b), for example, or any other catalyst capable of catalyzing an etherification reaction between the remaining terminal hydroxyl groups of the LMWPG and the monofunctional alcohol. The monofunctional alcohol has only one functional group capable of participating in a further round of etherification, thus effectively preventing further growth of the polymer. The end product would preferably have increased miscibility in liquid hydrocarbon fuels, and thus, be more suitable for use as a fuel additive.
In still other embodiments, the remaining hydroxyl groups that are present on the LMWPG following condensation of the light glycol feed are instead “capped” by mild hydrodeoxygenation (HDO) of the remaining hydroxyl functional groups. It is important that the HDO step be mild so as to not completely remove all oxygen from the LMWPG, as a certain amount of oxygen in the final product is desirable. This HDO step may be catalyzed by any of a number of commercially available catalysts, including commercial hydrotreating catalysts comprising Co and Mo, or Ni and Mo. Procedures for conducting such HDO reactions are commonly known in the art. The end product would preferably have increased miscibility in liquid hydrocarbon fuels, and thus, be more suitable for use as a fuel additive.
EXAMPLES
The following examples are each intended to be illustrative of a specific embodiment of the present invention in order to teach one of ordinary skill in the art how to make and use the invention. They are not intended to limit the scope of the invention in any way.
Example I
Preparation of Catalysts: 40 wt % H 4 SiW 12 O 40 /SiO 2 was prepared by incipient wetness impregnation. H 4 SiW 12 O 40 (Sigma-Aldrich) was dissolved in ethanol and added dropwise to Davicat SI 1103 (320 m 2 /g, −40/+60 mesh.) Samples were sealed for 24 hours and then dried for 12 hours at 90° C. in flowing nitrogen.
1 wt % Pt—WO 3 /ZrO 2 was prepared by precipitation of Zr(OH) 4 followed by the loadings of tungsten and platinum via incipient wetness impregnation. Pt was loaded onto the catalyst using aqueous hexachloroplatinic acid. Catalysts were dried at 150° C. for 6 hours, and calcined at 300° C. overnight in flowing air.
H-MOR (Si/Al=10), NH4-USY (Si/Al=2.6), and TPA-ZSM-5 (Si/Al=15) were obtained from Zeolyst International. Extrudates were crushed and sieved to −20/+40 mesh. Zeolites containing template or in the ammonium form were converted into the acidic form by calcining in a muffle furnace under flowing air prior to use. Excess air was flowed over the catalyst while the samples were heated using a gradual heat/soak temperature profile to a final temperature of 450° C. The final temperature was maintained overnight (>12 hours.)
Example II
Hypothetical Example: Passivation of a Zeolite Catalyst with Either Poly(phenylmethyl)siloxane or Tetraethylorthosilicate: Zeolite catalysts useful in certain embodiments of the invention may be chemically-modified to passivate (i.e., block active sites on) the external surface of the catalyst, thereby increasing selectivity for the production of LMWPG. One examples of how this can be achieved is outlined in U.S. Pat. No. 6,228,789, which pertains to a method for silylation of zeolite catalysts, and is incorporated herein by reference.
A zeolite H-ZSM-5 was contacted to incipient wetness with a 50 wt % solution of poly(phenylmethyl)siloxane (PPMS) in cyclohexane, and the catalyst was not pre-calcined prior to contacting. After loading of the catalyst, it was dried and calcined at 538° C. for 6 hrs. Alternatively, the H-ZSM-5 catalyst was loaded with a 50 wt. % solution of tetraethylorthosilicate (TEOS) under conditions identical to those used for loading with PPMS.
Example III
Catalytic Conversion Test Conditions: Unless otherwise noted, catalysts were tested in a standard, ¾-inch diameter down-flow reactor. A bed of heated glass beads was utilized upstream from the catalyst to preheat the feed to reaction temperature prior to contacting the catalyst. Typically 6 mL of catalyst was diluted in an inert material (alundum) to a constant 13 mL bed volume for screening runs. The reactor was heated using a three-zone Thermcraft™ furnace with independent temperature control for each zone. Liquid feed was delivered to the system by an ISCO™ 1000D syringe pump, and system pressure was controlled by a Tescom™ backpressure regulator. Samples were taken at one hour intervals, and conversion and selectivity percentages (unless otherwise noted) were calculated by averaging data obtained from three different samples taken at different time points.
Catalysts were dried in-situ at the desired operating temperature for a minimum period of 30 minutes in at least 100 sccm H 2 at 2758 kPa psig prior to each run. Pt containing catalysts were reduced for a minimum of 30 minutes at 300° C. and 2758 kPa in 100 sccm of H 2 . Except as noted, runs were performed as follows: Ethylene glycol was obtained from Sigma-Aldrich™ (97% purity) and diluted to 50 vol. % in water, and was fed to the reactor at a constant liquid feed rate of 30 mL/hr. Reactions were typically performed at 200° C., 5.0 h −1 LVHSV, and 2758 kPa. Hydrogen was flowed at 100 sccm during screening runs as some catalysts tested needed spillover hydrogen for activity. Liquid sample collection began 1 hour after starting the feed. Samples were acquired at 1 hour intervals for 5 hours and analyzed on an Agilent™ 7890A gas chromatograph equipped with an Agilent™ HP-5 capillary column, and a flame ionization detector (FID). Ambient temperature non-condensable products were analyzed on-stream using a HP-5 capillary column with FID detection.
Example IV
The tungstated zirconia catalyst Pt—WO 3 /ZrO 2 was prepared as detailed in Example 1, and found to convert 18.5% (w/v) of the feed during the experiment. However, selectivity for the formation of LMWPG was only 1.7% (w/v). Instead, this catalyst produced a relatively large quantity of ethanol from the ethylene glycol feedstock. While not wishing to be limited by theory, it is hypothesized that this ethanol was formed by the intramolecular dehydration of ethylene glycol to form acetaldehyde, followed by reduction of the acetaldehyde at the Pt sites of the catalyst to form ethanol. Alternatively, ethanol may have formed through direct hydrogenolysis at Pt sites.
Example V
A member of the heteropoly acid catalyst family (with the formula H 4 SiW 12 O 40 /SiO 2 ) was tested for its ability to convert the glycol feedstock to LMWPG. At a run temp of 250° C., utilizing undiluted ethylene glycol at a feed rate of 15 ml/hr, this catalyst converted 74.7% of the feedstock (average of samples taken at third and fourth hours), with a selectivity of 20.3% for the formation of LMWPG. However, this catalyst produced a large percentage of p-dioxane product, which is unsuitable for use as a biofuel, or a cetane-increasing fuel additive. p-dioxane is formed from the product of an intermolecular condensation between two ethylene glycols molecules. The primary product of this condensation, diethylene glycol, can undergo intramolecular condensation and circularize to form p-dioxane. This is not desirable, because p-dioxane is not suitable for use as a cetane-enhancing additive, and is a relatively stable product that is difficult to convert into back into a form that can be used as a fuel, or fuel additive.
Example VI
The zeolite catalysts USY, mordenite, and ZSM-5 were obtained and used with similar Si/Al ratios for comparison (the Si/Al ratios were 2.6, 10 and 15, respectively.) The relatively low Si/Al ratios were selected to maximize the acid site quantity for each catalyst. Each zeolite catalyst exhibited conversion of the ethylene glycol feed (See Table 1) to form LMWPG.
TABLE 1
Conversion of ethylene glycol to LMWPG by several zeolite catalysts.
Si/Al
% Selectivity
Catalyst
Ratio
% Conv.
for LMWPG
H-USY
2.6
0.6
58.2
H-MOR (mordenite)
10
4.7
6.2
H-ZSM-5
15
15.8
61.5
Reaction products in addition to LMWPG were observed, including acetaldehyde and p-dioxane. The acetaldehyde was hypothesized to have formed by the intramolecular dehydration of ethylene glycol, while p-dioxane was thought to have formed by the mechanism outlined previously. Interestingly, the USY and ZSM-5 zeolites exhibited higher selectivity for the production of LMWPG than with the other catalysts tested previously.
Example VII
The ZSM-5 zeolite catalyst was selected for further testing to optimize reaction conditions for converting the ethylene glycol feed stock to LMWPG. Conditions of pressure, temperature and flow rate were altered, and the effect on percent conversion and selectivity for the formation of LMWPG is shown in Table 2:
TABLE 2
Conversion of ethylene glycol to LMWPG at various reaction conditions:
%
%
Temp.
Pressure
LWHSV
Run
Conversion
Selectivity
(° C.)
(KPa)
(hr −1 )
1
1.20
71.7
126.5
689
1.5
2
0.14
53.6
126.5
689
15.0
3
0.45
93.2
124.5
2758
1.5
4
0.55
92.8
128
2758
1.5
5
0.21
100
126.5
2758
15.0
6
0.96
87.4
134.5
689
15.0
7
0.11
71.5
149
1724
8.25
8
1.60
85.4
154.5
1724
8.25
9
40.60
62.4
174
689
1.5
10
3.60
42.4
175.5
689
15.0
11
48.90
59.7
177.5
2758
1.5
12
1.80
84.5
174.5
2758
15.0
13
53.30
56.2
183.5
689
1.5
14
5.50
81.0
182
2758
15.0
DEFINITIONS
As used herein, the term “liquid weight hourly space velocity” or “LWHSV” refers to the liquid weight hourly space velocity.
As used herein, the term “cetane” or “cetane number” refers to the cetane number of a fuel as measured by the ASTM (American Society for Testing and Materials) D613 or D6890 standard.
As used herein, the term “transportation fuel” refers to any liquid hydrocarbon mixture used as a fuel for powering engines, including gasoline, diesel and jet fuels.
Further modifications and alternative embodiments of various aspects of the invention will be apparent to those skilled in the art in view of this description. Accordingly, this description is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the general manner of carrying out the invention. It is to be understood that the forms of the invention shown and described herein are to be taken as examples of embodiments. Elements and materials may be substituted for those illustrated and described herein, parts and processes may be reversed and certain features of the invention may be utilized independently, all as would be apparent to one skilled in the art after having the benefit of this description of the invention. Changes may be made in the elements described herein without departing from the spirit and scope of the invention as described in the following claims.
REFERENCES
All of the references cited herein are expressly incorporated by reference. Incorporated references are listed again here for convenience:
1. US2010/0094062 (Rabello; Ferreiral; Menenzes); “Cetane Number Increasing Process and Additive for Diesel Fuel.” 2. US2008/0300435 (Cortright; Blommel); “Synthesis of Liquid Fuels and Chemicals From Oxygenated Hydrocarbons.” 3. US2008/0302001 (Koivusalmi; Piiola; Aalto) “Process for Producing Branched Hydrocarbons.” 4. U.S. Pat. No. 7,049,476 (O'Lenick, Jr.) “Guerbet Polymers” (2006). 5. U.S. Pat. No. 6,228,789 (Wu; Drake) “Silylated Water Vapor Treated Zinc or Gallium Promoted Zeolite and Use Thereof for the Conversion of Non-aromatic Hydrocarbons to Olefins and Aromatic Hydrocarbons” (2001). 6. Klepacova, K., et al., “Etherification of Glycerol and Ethylene Glycol by Isobutylene.” Applied Catalysis A: General 328: 1-13 (2007). 7. Klepacova, K., et al., “tert-Butylation of Glycerol Catalyzed by Ion-Exchange Resins.” Applied Catalysis A: General 294: 141-147 (2005). 8. Karinen, R. et al., “New Biocomponents from Glycerol” Applied Catalysis A: General 306: 128-133 (2006). 9. Frusteri, F., et al., “Catalytic Etherification Of Glycerol By tert-Butyl Alcohol To Produce Oxygenated Additives For Diesel Fuel.” Applied Catalysis A: General 367: 77-83 (2009). 10. Tijm, P. et al., “Effect of Oxygenated Cetane Improver on Diesel Engine Combustion & Emissions” http://www.energy.psu.edu/tecetane.html 11. Murphy, M. et al., “Compendium of Experimental Cetane Number Data” NREL/SR-540-36805 (2004). http://www.nrel.gov/vehiclesandfuels/pdfs/sr368051.pdf
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The present disclosure relates to methods for converting light glycol streams of biological origin into products suitable for use as oxygenated fuel additives. These methods involve the acidic condensation of light glycols to form larger products, termed low molecular weight poly-glycols. The remaining hydroxyl functional groups of the poly-glycol products are then modified to decrease the overall polarity of the products, and improve their suitability for use as an oxygenated fuel additive.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to the infusion of medication contained in a flexible bag, which flows into the veins of a patient via an infusion line, under the effect of gravity, the bag being suspended above the patient.
[0002] More particularly, the invention relates to a bag for medical use for infusing medication by gravity, comprising at least two compartments, one containing medication and the other containing a rinsing solution, and separation/communication means for automatically rinsing the medication bag and infusion line.
[0003] The invention is intended to solve, simply and inexpensively, two major problems encountered with this type of infusion, namely:
the loss of some of the medication: The infusion line has a non-negligible volume, in particular in the case of small infusion bags. The amount of medication remaining in the line plus the residual amount contained in the bag is not infused into the patient who thus does not receive the prescribed dose; the risk of contamination due to the toxicity of the medication: the medication infused may be extremely toxic or allergenic (cancer medication, antibiotics, etc.) and there may be a risk of contamination when the care personnel purges the air from the perfusion line before connecting up to the patient or when disconnecting the infusion line.
[0006] The solution to these two problems consists in rinsing the line before and after infusion and rinsing the bag after infusion using a harmless, inexpensive solution (isotonic sodium chloride for example).
DESCRIPTION OF THE PRIOR ART
[0007] Devices are already known which can at least partially rinse the bag/line, limiting medication loss and the risks for care personnel.
[0008] U.S. Pat. No. 5,242,392 describes an infusion system comprising a chamber for a rinsing liquid connected to the infusion tubing between the medication bag and the injection device and located lower than the medication bag. When the medication has been administered, the rinsing solution rinses the infusion tubing and injection device automatically.
[0009] Patent FR 2 794 983 describes a closed-circuit infusion system comprising at least one medication bag and dispensing and infusion means, associated with a rinsing bag in such a way that the rinsing solution can flow through the dispensing and infusion means, and also selection means allowing the medication and/or the rinsing solution to flow through the dispensing and infusion means.
[0010] Patent FR 2 306 711 describes an infusion device comprising at least two infusion containers suspended at different heights, whose tubes are connected for example using a Y-shaped connection piece, and a valve device with two inlets whose operation is linked to the difference in height between the infusion containers which causes a difference in height between the columns of liquid.
[0011] Documents WO 92/11881, U.S. Pat. No. 4,512,764, WO 95/09020, EP 0 790 064, U.S. Pat. No. 4,623,334 and WO 03/077974 describe infusion or injection systems comprising devices for rinsing the infusion line or injection system.
[0012] These devices do not provide a satisfactory solution to the problems of safety and effectiveness of the infusion systems:
If the bag contains air, it may be completely emptied but a relatively large part of the infusion line will contain air and the line cannot be rinsed since the air contained in the line would be injected in the patient (risk of air embolism). The presence of the nurse is therefore required before the end of infusion in order to carry out rinsing at the exact moment when the bag is completely emptied, before some of the line fills with air. If the bag does not contain air, it cannot be completely emptied and the residual liquid contained in the bag will not be injected into the patient. In this case, the line may be rinsed, but not the bag. In all cases, the intervention of the nurse is required, entailing extra work.
SUMMARY OF THE INVENTION
[0016] The present invention is intended to improve the safety and effectiveness of infusion systems by virtue of a device for automatically rinsing the line and the bag after infusion, without the nurse's intervention.
[0017] The present invention relates to a bag for medical use for infusing medication by gravity, comprising at least two compartments, one containing medication in the form of a solution and the other(s) containing a rinsing solution, and compartment separation/communication means which allow the rinsing solution to enter the compartment containing the medication automatically only after infusion. The rinsing solution completes the infusion, rinsing the medication bag and the infusion line, thus eliminating the risk of contamination and the loss of residual medication in the bag and that contained in the infusion line.
[0018] The basic principle of the invention consists in using the vacuum created in the medication bag at the end of infusion owing to the water column height in the infusion line. This vacuum gradually increases at the end of infusion, as the bag becomes flattened through a “siphon” effect. This vacuum can reach around −100 mb.
[0019] The rinsing liquid, which is at atmospheric pressure, is drawn into the compartment containing the medication, which in turn is at a vacuum pressure with respect to atmospheric pressure.
[0020] The separation/communication means comprise a breakable device between the compartment containing the medication and the compartment (one of the compartments) containing the solution and a device for ensuring automatic communication between the compartment containing the medication and the compartment containing the solution or between the two compartments containing the solution.
[0021] The device for ensuring automatic communication between the compartments may be a communication channel positioned above the level of the liquid in said compartments when the bag is suspended vertically.
[0022] As a variant, the device for ensuring automatic communication between the compartments may be a pressure-threshold valve.
[0023] The compartment or compartments containing the rinsing solution may comprise a narrow area towards the top of the bag.
DESCRIPTION OF THE DRAWINGS
[0024] The attached drawings illustrate the present invention in more detail.
[0025] FIG. 1 shows an infusion bag with two compartments comprising a communication channel.
[0026] FIG. 2 shows an infusion bag with two compartments comprising a pressure-threshold valve.
[0027] FIG. 3 is a cross section through the pressure-threshold valve of FIG. 2 with integrated breakable device in the closed state.
[0028] FIG. 4 shows the same valve in the open state.
[0029] FIG. 5 shows an infusion bag with three compartments comprising a communication channel.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0030] According to a first embodiment of the invention shown in FIG. 1 , use is made of a flexible infusion bag separated into two juxtaposed compartments ( 1 ) and ( 2 ), one ( 1 ) of which contains the medication and the other ( 2 ) the rinsing solution. Compartment ( 1 ) comprises an access ( 4 ) for filling the bag and connecting to the infusion line ( 10 ). Compartment ( 2 ) comprises a narrow area ( 9 ) at the top of the bag and an access ( 5 ) for filling said compartment. The two compartments are separated by a substantially vertical wall ( 7 ) whose upper part comprises a breakable device ( 3 ) designed to ensure the seal between the two compartments when it is intact and to allow communication between the two compartments when it is broken by the nurse by mechanical intervention on the outside of the bag. This device is imperatively placed above the level of the liquids when the bag is suspended.
[0031] Compartments ( 1 ) and ( 2 ) are filled without the addition of air. Said compartments comprise means ( 8 ) and ( 6 ) for preventing the flow path of the liquid from being sealed up completely when the bag flattens. These means ( 8 ) and ( 6 ) may consist for example of a “roughening” of the surface of one of the faces of the bag or a thermoformed channel, which aid the flow.
[0032] According to a second embodiment of the invention shown in FIG. 2 , use is made of a flexible infusion bag separated into two superposed compartments ( 1 ) and ( 2 ). The two compartments are separated by a substantially horizontal wall ( 7 ) whose central part comprises a breakable device ( 3 ) broken by the nurse. In this embodiment, the flow of the rinsing solution from compartment ( 2 ) to compartment ( 1 ) is triggered by a pressure-threshold valve ( 11 ) as a function of the difference in pressure between the compartments ( 1 ) and ( 2 ).
[0033] Compartment ( 1 ) comprises means ( 8 ) for preventing the flow path of the liquid from being sealed up completely when the bag flattens. These means ( 8 ) facilitate the flow between the communication orifice between the two compartments and the access ( 4 ) to the infusion line ( 10 ).
[0034] According to a variant (not shown) of the bag of FIG. 1 or 2 , use is made of two separate bags instead of one bag with two compartments.
[0035] FIGS. 3 and 4 show an example of the pressure-threshold valve used in the bag of FIG. 2 .
[0036] The valve comprises two chambers ( 14 ) and ( 15 ) separated by an elastomer membrane ( 13 ). As shown in FIG. 3 , the seal between the two chambers is ensured by the membrane ( 13 ) being pretensioned on the annular sealing ring ( 17 ). The chamber ( 14 ) is in communication with compartment ( 2 ) containing the rinsing solution via the openings ( 12 ). After the breakable device ( 3 ) is broken, the chamber ( 15 ) is in communication with the compartment ( 1 ) containing the medication.
[0037] As shown in FIG. 4 , when the pressure inside the chamber ( 15 ) becomes negative with respect to the pressure in the chamber ( 14 ), the membrane ( 13 ) detaches from the annular sealing ring ( 17 ), thus allowing the rinsing liquid contained in compartment ( 2 ) to flow into compartment ( 1 ) via the orifice ( 16 ).
[0038] According to a third embodiment of the invention shown in FIG. 5 , use is made of a flexible infusion bag separated into three juxtaposed compartments, allowing rinsing at the beginning and end of infusion. Compartment ( 1 ) contains the medication and is separated from compartments ( 2 ) and ( 2 a ) containing rinsing solution by a substantially vertical wall ( 7 ) whose lower part comprises a breakable device ( 3 ) broken by the nurse.
[0039] Compartments ( 2 ) and ( 2 a ) are separated by a wall ( 20 ) leaving a passage ( 18 ) at the top of the bag which prevents the transfer of the contents from ( 2 ) into ( 2 a ) and/or the contents from ( 2 a ) into ( 2 ) if the bag is suspended vertically and if there is no difference in pressure between said compartments. Compartment ( 2 a ) comprises an access ( 4 ) to the infusion line ( 10 ). The volume of compartment ( 2 a ) is slightly greater than the volume of a standard infusion line (around 10 milliliters).
[0040] The following examples illustrate how the infusion bags of the invention are used.
Example 1
Bag with Two Juxtaposed Compartments (FIG. 1 )
[0041] After the infusion line has been established, the nurse breaks the breakable device ( 3 ) by mechanical intervention on the outside of the flexible bag, to place the compartments ( 1 ) and ( 2 ) in communication without causing transfer since the pressure inside the two compartments is identical. When compartment ( 1 ) is practically empty, its walls collapse. The pressure in compartment ( 1 ) then becomes negative with respect to the pressure in compartment ( 2 ), which flattens, causing the rinsing liquid to rise into the communication channel between the two compartments. The rising liquid then empties into compartment ( 1 ), and then into the infusion line, thus rinsing the medication out of compartment ( 1 ) and the line ( 10 ). The patient will thus receive all the medication and the nurse will handle an infusion line and a bag free of toxic liquid.
Example 2
Bag with Two Superposed Compartments (FIG. 2 )
[0042] The method of example 1 is followed, except that it is the pressure-threshold valve that allows the rinsing solution to flow into compartment ( 1 ) when the pressure in this compartment becomes negative with respect to the pressure in compartment ( 2 ).
Example 3
Bag with Three Juxtaposed Compartments (FIG. 5 )
[0043] Once the bag has been connected up to the infusion line ( 10 ), the air-filled infusion line is in communication with compartment ( 2 a ) which is full of rinsing solution. The nurse starts infusion as usual with the contents of compartment ( 2 a ). After this operation, compartment ( 2 a ) is almost empty.
[0044] The nurse connects the line to the patient, then breaks the breakable device ( 3 ). Compartment ( 1 ) is then in communication with compartment ( 2 a ) and thus with the infusion line ( 10 ). The medication contained in ( 1 ) flows into compartment ( 2 a ) until the heights of liquid in said compartments are equal.
[0045] When compartments ( 1 ) and ( 2 a ) are almost empty, the walls collapse, causing the rinsing solution in compartment ( 2 ) to be sucked into compartment ( 2 a ). After the levels between compartments ( 1 ) and ( 2 a ) have equaled out, which rinses the bottom of the compartment, the rinsing solution flows into the perfusion line ( 10 ).
[0046] The description and figures illustrate various embodiments of the present invention. However, the invention is not limited to the embodiments described and shown but, on the contrary, encompasses all variants.
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The invention relates to a medical bag which is intended for the infusion of a medicament by means of gravity. The inventive bag comprises: at least two compartments, namely a first compartment ( 1 ) containing a medicament in the form of a solution and a second compartment ( 2 ) containing a rinsing solution; and means for separating/communicating the compartments, which prevent the rinsing solution from automatically entering the medicament compartment except at the end of the infusion period. The rinsing solution ends the infusion, by rinsing the medicament bag and the infusion line, such as to prevent any risk of contamination or leakage of residual medicament from the bag or line.
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BACKGROUND OF THE INVENTION
The present invention relates to a rosary card which may be used in both teaching the recital of the rosary and for actual prayer.
By way of background, rosary devices utilized in the past were either relatively expensive, complicated, or cumbersome. Furthermore, insofar as known, prior rosary devices which could actually be used for prayer also did not have instructional information thereon which would enable one to learn the rosary.
SUMMARY OF THE INVENTION
It is one object of the present invention to provide an improved rosary prayer card which can be used for instructing people in the saying of the rosary.
It is another object of the present invention to provide a rosary card which is fabricated from a sheet of planar material and which is of a configuration which can be used in reciting the rosary.
A further object of the present invention is to provide a rosary card which can be produced simply and economically and therefore can be capable of low cost widespread distribution. Other objects and attendant advantages of the present invention will readily be perceived hereafter.
The present invention relates to a rosary card comprising a planar sheet-like body having an outer periphery, and a plurality of protrusions on said outer periphery lying in the same plane as said planar sheet-like body, said protrusions representing various portions of the rosary.
The various aspects of the present invention will be more fully understood when the following portions of the specification are read in conjunction with the accompanying drawings wherein:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of the rosary card of the present invention;
FIG. 2 is a fragmentary cross-sectional view taken substantially along line 2--2 of FIG. 1; and
FIG. 3 is a fragmentary cross sectional view taken substantially along line 3--3 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The rosary card 100 includes a planar sheet-like body 121 having an upper surface 122 and an undersurface 123 and a periphery 124. The planar sheet-like body 121 is fabricated from sheet semi-rigid plastic of the type used for plastic credit cards approximately 0.018 mils thick, but it can be of any desired practical thickness.
By way of introduction, the numerals drawn with a lettering guide may be printed on the card itself as an instructional aid, and those numerals which are drawn freehand with lead lines are for purposes of explaining the various constructional details of rosary card 100.
The following numerals of 1 through 19, inclusive, which represent the steps in reciting the rosary, may be printed on the card itself as shown when it is to be used as an instructional tool, but may be omitted on cards which are to be used for actual prayer. In this regard, a cutout cross C proximate printed numeral 1, which designates the first step in reciting the rosary, is located centrally in body 121 for being felt while making of the sign of the Cross and saying the Apostles' Creed. Next in sequence is a cutout large circle 2' proximate printed numeral 3, which represents the second step in saying the rosary. The large circle 2' is to be felt during the saying of the "Our Father." Thereafter, three smaller circular cutouts 3' are bracketed by the printed numeral 3, which represents the third step in saying the rosary. Cutouts 3' are located in the body of the card and are to be felt during the saying of three "Hail Marys." A card body portion 4' proximate printed numeral 4 is located after the third circular cutout 3' and it is to be felt during the saying of "Glory be to the Father." A large circular cutout 5' proximate printed numeral 5 is positioned after card portion 4' and is to be felt during the announcing of the first mystery and the saying of the "Our Father." Pictures of beads 102, 103 and 104 are located alongside the holes 2', 3' and 5', respectively. The pictures of beads are connected by pictures of a chain (not numbered).
Ten equally spaced protrusions 6' are bracketed by numeral 6, which represents the sixth step in saying the rosary. The ten protrusions 6' are located on periphery 124 and are to be felt during the saying of ten "Hail Marys." These are followed by a straight edge portion 7' next to printed numeral 7 which is to be felt during the saying of "Glory be to the Father." A peripheral protrusion 8' is proximate printed numeral 8, and it is to be felt during the announcing of the second mystery and the saying of the "Our Father."
Ten equally spaced protrusions 9' are bracketed by printed numeral 9, which represents the ninth step in the saying of the rosary. Protrusions 9' are felt during the saying of ten "Hail Marys." An elongated peripheral portion 10' is proximate printed numeral 10 and is felt during the saying of "Glory be to the Father." Thereafter, a single protrusion 11' proximate printed numeral 11 is to be felt during the saying of the third mystery and then the saying of "Our Father." Bead pictures 106, 108, 109 and 111, which are connected by a chain picture (not numbered), are adjacent protrusions 6', 8', 9' and 11', respectively.
The ten protrusions 12' proximate printed numeral 12 and the associated bracket at the lower end of body 121 are felt during the saying of ten "Hail Marys." The protrusion 13' proximate printed numeral 13 is felt during the announcing of the fourth mystery and then saying the "Our Father." The peripheral card portion 14' proximate printed numeral 14 and following the protrusion 13' is felt during the saying of "Glory be to the Father." The ten following protrusions 15' bracketed by printed numeral 15 are felt during the saying of ten "Hail Marys." The peripheral protrusion 16' proximate printed numeral 16 is felt during the announcing of the fifth mystery and then the saying of "Our Father." The straight peripheral portion 17' proximate printed numeral 17 is felt during the saying of "Glory be to the Father." The ten protrusions 18' bracketed by printed numeral 18 are are felt during the saying of ten "Hail Marys," and the straight peripheral portion 19' proximate printed numeral 19 is felt during the saying of "Glory be to the Father." Bead pictures 111, 112, 113, 115, 116 and 118 lie alongside peripheral protrusions designated by printed numerals 11, 12, 14, 15, 16 and 18, respectively, and are connected by a picture of a chain (not numbered).
In addition, a picture of religious figures, namely, the Virgin Mary and Child, can be placed within the portion denoted by the circular border 120, and another picture, namely, Jesus on the Cross, may be placed within the stylized picture of the cross 126. The horizontal lines located between the bottom of cross 126 and the pictures of beads at printed numeral 12 may be filled with necessary script. Suitable script can also appear on the rear face 123 of body 121. This script can be the various prayers and may include instructional material in reciting the rosary.
As noted above, the printed numerals 1-19, inclusive, are for instructional purposes, namely, to represent the steps in reciting the rosary, and these may be omitted on cards used for actual prayer.
It will be appreciated that the protrusions on the edges of the card may be of shapes and sizes other than as shown, and that the card itself may be of any desired size, and that the cut-out area of the cross may be different from that shown.
It can thus be seen that the rosary card of the present invention is manifestly capable of attaining the above objects and while a preferred embodiment of the present invention has been disclosed, it will be appreciated that it is not limited thereto but may be otherwise embodied within the scope of the following claims.
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A rosary card fabricated from a sheet of planar sheet material having protrusions on its outer edges designating the various parts of the rosary and also having cutouts in the card designating other portions of the rosary and also having pictures of beads thereon resembling a rosary and also having various parts designated by numerals as an aid in learning the rosary and also having script thereon for instructions in reciting the rosary.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims priority under 35 USC 119 to Japanese Patent Application No. 2005-032126 filed on Feb. 8, 2005 the entire contents of which are hereby incorporated by reference.
FIELD OF THE INVENTION
[0002] This invention relates to a clutch mechanism of a hydrostatic continuously variable transmission and more particularly a constitution of a spring sheet of a coil spring for pressing a roller bearing member of a centrifugal type governor clutch of the hydrostatic variably transmission.
DESCRIPTION OF BACKGROUND ART
[0003] In the prior art centrifugal type governor clutch, the side part of a cam plate arranged near the end part of a transmission shaft is axially extended to form a cylindrical part and the cylindrical part is directly attached and fixed to a casing of the transmission with bolts. A ring-like spring sheet of an independent component formed as a separate element is fixed to the cylindrical part with a ring-like grip. See, for example, JP-A 070331/2004 ( FIG. 1 ). The number of component elements is increased because the ring-like sheet of such a small parts as described above is troublesome in its manufacturing and assembling and a fixing clip are needed.
SUMMARY AND OBJECTS OF THE INVENTION
[0004] An embodiment of the present invention overcomes the aforesaid problems of the prior art and provides a spring sheet wherein the manufacturing and assembling are simple and the number of component elements is less.
[0005] An embodiment of the present invention overcomes the aforesaid problem by providing a clutch mechanism for a hydrostatic continuously variable transmission in which a hydraulic circuit includes a high pressure oil path for feeding working oil from a hydraulic pump to a hydraulic motor and a low pressure oil path for feeding working oil from the hydraulic motor to the hydraulic pump. The clutch mechanism is positioned between the hydraulic pump and the hydraulic motor in a casing rotated by a driving source within a cylinder integral with a transmission shaft. A clutch valve, arranged in the transmission shaft, is slid by a centrifugal governor. The high pressure oil path and the low pressure oil path are shortened to change-over a transmittance of power wherein the same includes a cam plate member arranged at the end part of the transmission shaft, a roller engaged with said cam plate member and moved in a diametrical outward direction with a centrifugal force, a roller bearing member for receiving a roller pressing force caused by an outward motion of said roller and axially slid, a spring member for biasing the roller bearing member toward the roller, a spring sheet member for supporting the spring member, and the spring sheet member being held by the cam plate member and the casing and supported.
[0006] According to an embodiment of the present invention, the cylindrical part formed by extending the side part of the cam plate member axially is substituted such that the cylindrical part is made as a separate member different from the cam plate member. The spring sheet is integrally formed at the cylindrical part to make the cylindrical spring sheet member with the spring sheet member being held between the cam plate member and the casing of the transmission and fixed with bolts. Accordingly, manufacturing and assembling of the clutch mechanism are easy because there is not provided the spring sheet of a small independent parts and the number of component parts is decreased because the fixing clip is not required.
[0007] Further scope of applicability of the present invention will become apparent from the detailed description given hereinafter. 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.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The present invention will become more fully understood from the detailed description given hereinbelow and the accompanying drawings which are given by way of illustration only, and thus are not limitative of the present invention, and wherein:
[0009] FIG. 1 is a side view of the motorcycle 1 including the power unit 2 of the embodiment of this invention;
[0010] FIG. 2 is a left side view of the power unit 2 mounted in the motorcycle;
[0011] FIG. 3 is a cross sectional cutaway view along lines III-III of FIG. 2 ;
[0012] FIG. 4 is a cross sectional view along IV-IV of FIG.2 ;
[0013] FIG. 5 is a vertical cross sectional view of the static hydraulic continuously variable transmission T;
[0014] FIG. 6 is a cross sectional view of an essential section of the static hydraulic continuously variable transmission T showing the vicinity of the distributor valve 160 ;
[0015] FIG. 7 ( a ) is a frontal view of the cotter pin 151 ;
[0016] FIG. 7 ( b ) is the cross-sectional view along I-I of FIG. 7 ( a );
[0017] FIG. 8 ( a ) is a frontal view of the retainer ring;
[0018] FIG. 8 ( b ) is the cross-sectional view along I-I of FIG. 8 ( a );
[0019] FIG. 9 ( a ) is a frontal view of the C clip;
[0020] FIG. 9 ( b ) is the cross-sectional view along I-I of FIG. 9 ( a );
[0021] FIG. 10 is a vertical cross-sectional view of an essential section of the static hydraulic continuously variable transmission T showing the vicinity of the centrifugal governor clutch C; and
[0022] FIG. 11 is a vertical cross-sectional view of an essential section of the static hydraulic continuously variable transmission T showing the supply passages for the operating fluid and the lubricant fluid.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] FIG. 1 is a side view of the motorcycle 1 containing the power unit 2 of an embodiment of the present invention. A pair of main frames 4 connecting to the head pipe 3 and sloping downwards to the rear are provided together with a pair of sub-frames 5 sloping downwards from the lower section of the head pipe 3 and bending rearwards. The tips of the sub-frames 5 connect to the rear end of the main frame 4 on the motorcycle 1 .
[0024] A power unit 2 , integrating an internal combustion engine 6 and a transmission 7 , is mounted in the largely triangular space formed by the main frame 4 and the sub-frame 5 as seen from the side. A front fork 8 is supported to allow rotation in the head pipe 3 . The steering handle 9 is mounted on the top end of the front fork 8 , and a front wheel 10 is axially supported by the bottom end. A pair of rear forks 11 are supported on their forward end by the rear section of the main frame 4 and are capable of swinging upward and downward. A rear suspension (not shown in drawing) is mounted between the rear end of the main frame 4 and the center section of the rear fork 11 . A rear wheel 12 is axially supported on the rear end of the rear forks 11 .
[0025] The internal combustion engine 6 is a water cooled V-type two-cylinder combustion engine with the cylinders opening in a V-shape towards the front and rear. The crankshaft of the internal combustion engine 6 is perpendicular to the forward direction of the vehicle, and installed facing towards the left and right of the vehicle. The transmission shaft of the transmission 7 is parallel to the crankshaft. The rear wheel drive shaft (not shown in FIG. 1 ) is connected to the connecting shaft 85 ( FIG. 2 ) perpendicular to the output shaft of the transmission, and extends to in the rearward direction of the vehicle, reaching the rotating shaft of the rear wheel 12 and driving the rear wheel 12 .
[0026] An exhaust pipe 13 , connecting to the exhaust port installed facing the front and rear of the two vehicle cylinders, extends forwards of the internal combustion engine 6 , and extends under the transmission 7 extending to the frame rear section. The exhaust pipe 13 is connected to the exhaust muffler 14 . A fuel tank 17 is mounted on the upper section of the (main) frame 4 , and a seat 18 is mounted to the rear. This internal combustion engine 6 is of the water-cooled type wherein cooling water whose temperature rises during the process of cooling the cylinder and oil is cooled in the radiator 19 installed on the front end of the sub-frames 5 .
[0027] FIG. 2 is a left-side view of the power unit 2 mounted on the motorcycle. The arrow F indicates the front during installation in the frame. The front side cylinder 24 F and the rear side cylinder 24 R possess the same internal structure so the cross section of only the rear side cylinder 24 R is shown. The crankcase rear section shows the state with the left crankcase cover removed and shows the positions of the main internal rotating shafts and gears and sprockets.
[0028] FIG. 3 is a cross-sectional view taken along lines III-III of FIG. 2 illustrating the rear side cylinder 24 R and the crankshaft 30 and the transmission shaft 100 of the static hydraulic continuously variable transmission T. The rear side cylinder 24 R is a cylinder holding the piston 33 connecting to the left side crankpin 31 .
[0029] The main components of the power unit 20 in FIG. 2 and FIG. 3 are the crankcase 20 including a left crankcase 20 L and a right crankcase 20 R, a left crankcase cover 21 L, a right crankcase cover 21 R, and a cylinder block 25 , a cylinder head 26 and a cylinder head cover 27 , respectively, installed with the front side cylinder 24 F and the rear side cylinder 24 R. The following description of the cylinder sections is based on the rear cylinder 24 R.
[0030] In FIG. 3 , the crankshaft 30 is supported to allow free rotation by the left side bearing 28 and the right side bearing 29 held in the left/right crankcases 20 L and 20 R. A connecting rod 32 and a piston 33 are connected to the left side crankpin 31 on the crankshaft 30 , and the piston 33 is held to allow sliding movement in the cylinder hole 34 of the cylinder block 25 . A combustion chamber 35 is formed in the section facing the piston 33 of the cylinder head 26 . A spark plug 36 inserts through the wall of the cylinder head 26 , and the spark plug tip enters the combustion chamber 35 with the spark plug rear end being exposed externally.
[0031] In FIG. 2 , an exhaust port 40 and an intake port 41 are connected to the combustion chamber 35 . The exhaust port 40 extends forwards in the front side cylinder 24 , and rearward in the rear side cylinder 24 R. The intake port 41 extends upwards for either cylinder in the space between both cylinders. The exhaust port 40 contains an exhaust valve 42 , and the intake port 41 contains an intake valve 43 . A camshaft 44 is installed inside the cylinder head cover 27 . An exhaust rocker arm shaft 45 , and an intake rocker arm shaft 46 are installed above the camshaft 44 . The exhaust rocker arm 47 and the intake rocker arm 46 installed on the arm shafts are driven by the cam 44 a , 44 b of the camshaft 44 , and press the stem top section of the intake valve 43 and the exhaust valve 42 to drive the each valve to open or close. In FIG. 3 , the camshaft 44 is driven by a camshaft drive chain 51 hooked on the camshaft drive sprocket 50 installed in the crankshaft 30 and the camshaft auxiliary sprocket 49 installed on the end of the camshaft 44 .
[0032] In FIG. 2 , a low-pressure oil pump and a high-pressure oil pump are integrated via an oil pump shaft 91 into an oil pump cluster 90 , at a lower section of the crankcase 20 . The low-pressure oil pump feeds oil towards the internal combustion engine 6 , and the high-pressure oil pump feeds oil towards the static hydraulic continuously variable transmission T. The oil pump cluster suctions oil within the oil pan 92 by way of the lower section oil strainer 92 . The internal combustion engine 6 drives the oil pump cluster 90 via an oil pump drive chain, 96 engaged on the oil pump shaft drive sprocket 95 installed in the crankshaft 30 , and the oil pump auxiliary drive sprocket 94 inserted into the oil pump shaft 91 . An oil cooler 97 and a low-pressure oil filter 98 can be seen on the rear section of the crankcase. The high-pressure oil filter is installed on the right side of the crankcase and is therefore not shown in FIG. 2 .
[0033] In FIG. 3 , the crankshaft output gear 37 , installed on the left end of the crankshaft 30 , functions as a gear in combination with the cam type torque damper 38 , and engages with the transmission input gear 116 installed on the casing 110 of the tilt plate plunger-type hydraulic pump P of the static hydraulic continuously variable transmission T. The crankshaft output gear 37 and the cam type torque damper 38 are installed on a collar 60 spline-coupled to the crankshaft 30 . The crankshaft output gear 37 , mounted for free rotation on the collar 60 , and a recessed cam 37 a with a concave surface in an arc-shape is formed on that side surface. A lifter 61 is inserted on the outer circumferential spline of the collar 60 to allow axial movement. A projecting cam 61 a with an arc-shaped projecting surface is formed on the edge of the same lifter 61 , and this same projecting cam 61 a engages with the recessed cam 37 a . A spring holder 62 is fastened to the edge of the collar 60 with a spline and cotter pin. A flat spring 63 is installed between the spring holder 62 and the lifter 61 , and forces the projecting cam 61 a towards the recessed cam 37 a.
[0034] During operation at fixed speed, the crankshaft 30 torque is transferred in sequence to the collar 60 , the lifter 61 , the projecting cam 61 a , the recessed cam 37 a , and the crankshaft output gear 37 , and the crankshaft output gear 37 rotates along with the crankshaft 30 . When excessive torque is applied to the crankshaft 30 , the projecting cam 61 a slides along the circumference of the cam surface of the recessed cam 37 a , and moves axially opposing the force of the flat spring 63 , absorbing the huge torque and alleviating the impact.
[0035] The crankshaft output gear 37 is a gear for reducing backlash. The crankshaft output gear 37 is comprised of a thick, main gear 64 in the center, and a thin auxiliary gear 65 supported to allow concentric rotation versus the main gear 64 , and an auxiliary gear coil spring 66 for applying a peripheral force via the auxiliary gear 65 on the main gear 64 . The auxiliary gear applies a circumferential (peripheral) force to eliminate the backlash gap that occurs between the main gear and the normal gear, when the backlash reducing gear engages with a normal gear for eliminating looseness (play) and alleviate noise to quiet the mechanism. In the present case, the noise from the crankshaft output gear 37 engaging with the transmission input gear 116 is reduced.
[0036] In FIG. 3 , the static hydraulic continuously variable transmission T is installed rearward of the crankshaft 30 . The static hydraulic continuously variable transmission T is a device combining a centrifugal governor clutch C, tilt plate plunger-type hydraulic pump P, and tilt plate hydraulic motor M via the motor transmission shaft 100 . When the rotation speed of the casing 110 of the tilt plate plunger-type hydraulic pump P exceeds a specified speed, the transmission input gear 116 connects (engages) the static hydraulic continuously variable transmission T due to the centrifugal force effect of the governor clutch C to change the speed. The static hydraulic continuously variable transmission T changes the speed by changing the speed (gear) ratio according to the tilted state of the tilt plate for the tilt plate hydraulic motor M. The rotational force for the change in speed is extracted from the motor transmission shaft 100 that rotates as one piece with the hydraulic pump P and the hydraulic motor M. A motor servomechanism changes the tilt angle of the tilt plate of the tilt plate hydraulic motor M. The structure and effect of the static hydraulic continuously variable transmission T is described later on.
[0037] FIG. 4 is a cross-sectional view taken along lines IV-IV in FIG. 2 . This is the path for transmitting power from the transmission shaft 100 to the connecting shaft 85 . A neutral-drive selector shaft 76 for the neutral-drive selector clutch 75 for selecting the neutral and drive states disposed in parallel with the transmission shaft 100 , is supported via ball bearings in the right crankcase 20 R and the left crankcase 20 L to allow rotation. An output shaft 80 disposed in parallel with the neutral-drive selector shaft 76 , is supported via ball bearings in the right crankcase 20 R and the right crankcase cover 21 R to allow rotation. Further, the connecting shaft 85 perpendicular to the output shaft 80 , is supported by the connecting shaft support section 84 installed near the left edge of the output shaft 80 to allow rotation. The connecting shaft support section 84 is installed on the outer side of the left crankcase 20 L. Also see FIG. 2 .
[0038] In FIG. 4 , a gear 68 is clamped to the transmission shaft 100 . A gear 77 is inserted into the neutral-drive selector shaft 76 to allow rotation versus the shaft. The gear 77 engages with the transmission output gear 65 affixed to the transmission 100 . The swing member 78 including a mesh gear 78 a , adjacently connected to the gear 77 , is inserted to allow sliding motion axially to the neutral-drive selector shaft 76 . The neutral-drive selector clutch 75 includes the neutral-drive selector shaft 76 , the gear 77 , and a swing member 78 ; and cuts off or connects the drive power conveyed from the transmission drive shaft 100 to the output shaft 80 . When the mesh gear 78 a of swing member 78 releases from the gear 77 , the neutral-drive selector clutch 75 sets a neutral state, and slides the swing member 78 . When the mesh gear 78 a engages with the mesh section of the gear 77 , the drive power transmission path is connected, and the drive state is set.
[0039] In FIG. 4 , a gear 79 is inserted on the neutral-drive selector shaft 76 and adjacently contacts the gear 77 on the opposite side of the slide member 78 . A gear 81 is inserted on the right end of the output shaft 80 to engage with the gear 79 of a neutral-drive selector shaft 76 . A bevel gear 82 is formed as one piece with the other end of the output shaft 80 . A bevel gear 86 is formed as one piece on the front end of the connecting shaft 85 , and engages with the bevel gear 82 of the output shaft 80 . A spline 85 a is mounted on the rear end of the connecting shaft 85 for connection to the rear wheel drive shaft. The rotational output power of the static hydraulic continuously variable transmission T is transmitted to the rear wheel transmission shaft by way of the shafts and gears.
[0040] FIG. 5 is a vertical cross-sectional view of the static hydraulic continuously variable transmission T. The static hydraulic continuously variable transmission T is made up of a tilt plate plunger-type hydraulic pump P, a tilt plate plunger-type hydraulic motor M, and a centrifugal governor clutch C. The transmission shaft 100 , functioning as the output shaft for the static hydraulic continuously variable transmission T, is mounted to pass through the center (of transmission T). The left end of the transmission shaft 100 is supported to allow rotation by the ball bearings B 1 , B 2 on the left crankcase cover 21 L, and the right end is supported to allow rotation by the ball bearing B 3 on the right crankcase 20 R.
[0041] The hydraulic pump P includes a pump casing 110 capable of rotating relative to the transmission shaft 100 that is installed concentrically therewith. A pump tilt plate 111 is installed tilted at a specific angle versus the rotating shaft of the pump casing in the interior of the pump casing 110 . A pump cylinder 112 is installed facing this same pump tilt plate 111 with multiple pump plungers 114 installed to slide within the pump plunger holes 113 arrayed in a ring shape enclosing the shaft center within the pump cylinder 112 . One end of the pump casing 110 is supported to allow rotation by the bearing B 2 in the transmission shaft 100 . The other end is supported to allow rotation by the bearing B 4 in the pump cylinder 112 , and is also supported to allow rotation by the bearing B 1 in the left crankcase cover 21 L. The pump tilt plate 111 is installed to be tilted at a specified angle to allow rotation relative to the pump casing 110 by the bearings B 5 , B 6 .
[0042] The transmission input gear 116 affixed by the bolt 115 is installed on the outer circumference of the pump casing. The outer end of the pump plunger 114 engages with the tilt plate surface 111 a of the pump tilt plate 111 projecting outwards, and the inner edge of the pump plunger 114 forms a pump fluid chamber 113 a in the pump plunger hole 113 . A pump passage opening 117 functioning as a dispensing hole with an intake hole being formed on the edge of the pump plunger hole 113 . The pump casing 110 rotates when the transmission input gear 116 is made to rotate, and the pump tilt plate 111 installed inside slides along with the rotation of the pump casing 110 with the pump plunger 114 moving back and forth within the pump plunger hole 113 according to the swing of the tilt plate surface 111 a . The hydraulic fluid within the pump fluid chamber 113 a is dispensed and suctioned.
[0043] The pump eccentric ring member 118 is installed by a bolt 119 on the right edge of the pump casing 110 in the center of the drawing. The inner circumferential surface 118 a of the pump eccentric ring member 118 is formed in a tubular shape that is off-center versus the rotating shaft of pump casing 110 . Therefore, this inner circumferential surface 118 a is also a tubular shape offset in the same way versus the centerline of the transmission shaft 100 and the pump cylinder 112 .
[0044] The casing 130 of the hydraulic motor M is affixed and supported while clamped to the right crankcase 20 R. The motor casing 130 is formed from the spherical member 131 and the elongated member 132 , and is clamped by the bolt 133 . A support spherical surface 131 a is formed on the inner surface of the spherical member 131 . The hydraulic motor M includes a motor casing 130 , and a motor swing member 134 in sliding connect and supported on the support spherical surface 131 a . A motor tilt plate 135 is supported to allow rotation by the bearings B 7 , B 8 within the motor swing member 134 with a motor cylinder 136 facing the motor tilt plate 135 . A motor plunger 138 is installed to allow sliding within the multiple plunger holes 137 passing through in the axial direction and arrayed in a ring shape enclosed in the center axis of the motor cylinder 136 . The motor cylinder is supported for rotation along that external circumference in the elongated member 132 of motor casing 130 by way of the bearing B 9 . The motor swing member 134 is capable of swinging in a movement centering on the center O extending at a right angle (direction perpendicular to the paper surface) to the centerline of the transmission shaft 100 .
[0045] The outer side edge of the motor plunger 138 engages with the tilt plate surface 135 a of the motor tilt plate 135 projecting outwards, and the inner side edge of the motor plunger 138 forms a motor fluid chamber 137 a within the motor plunger hole 137 . A motor passage opening 139 functioning as an intake port and a dispensing (exhaust) port for the motor is formed in the edge of the motor plunger hole 137 . The edge of the motor swing member 134 is formed as an arm 134 a projecting to the outer side and projects outwards towards the radius to connect to the motor servo mechanism S. The arm 134 a is controlled by the motor servo mechanism S to move left and right, and is controlled to swing to center on the swing center O of the motor swing member 134 . When the motor swing member 134 swings, the motor tilt plate 135 supported internally inside it ( 134 ) also swings, and changes the angle of the tilt plate.
[0046] FIG. 6 is an enlarged cross-sectional view of the vicinity of the distributor valve 160 of the static hydraulic continuously variable transmission T. The distributor valve 160 is installed between the pump cylinder 112 and the motor cylinder 136 . The valve body 161 of the distributor valve 160 is supported between the pump cylinder 112 and the motor cylinder 136 , and is integrated with the cylinders by brazing. The motor cylinder 136 is coupled to the transmission shaft 100 by a spline 101 . The pump cylinder 112 , the distributor valve 160 , and the motor cylinder 136 rotate with the transmission shaft 100 as one unit. This integrated pump cylinder 112 , valve body 161 of the distributor valve 160 , and the motor cylinder 136 are called the output rotation piece R. The structure for attaching the output rotation piece R to the transmission shaft is described. A large diameter section 102 that is short along the axial length is formed on the outer circumferential side of the transmission shaft 100 corresponding to the left edge position of the pump cylinder. The left edge surface of the pump cylinder 112 contacts the edge surface of this large diameter section 102 , to perform positioning to the left.
[0047] The right side positioning of the output rotation piece R, is performed by the stop member 150 installed on the transmission shaft 100 facing the motor cylinder 136 . The stop member 150 includes a cotter pin 151 , a retainer ring 152 , and a C ring 153 . To install the stop member 150 , a ring-shaped first stop groove 103 , and second stop groove 104 are formed across the outer circumference of the spline 101 . A pair of cotter pins 151 is separately formed in a semicircular shape shown in FIG. 7 and is installed in the first stop groove 103 . A retainer ring 152 is installed above it as shown in FIG. 8 . The tip section 152 a of the retainer ring 152 covers the outer circumferential surface of the cotter pin 151 , and the inward facing flange 152 b of retainer ring 152 contacts the side surface of the cotter pin. Moreover, the C ring 153 is installed as shown in FIG. 9 in the second stop groove 104 , and prevents the retainer ring 152 from coming loose. As a result of the above, the right edge surface of the motor cylinder 136 directly contacts the stop piece 150 and is positioned towards the right.
[0048] The output rotation piece R is in this way positioned to the left by the large diameter piece 102 via the spline 101 and is positioned to the right versus the transmission shaft 100 by the stop piece 150 and rotates along with the transmission shaft 100 as one piece. A lubricating oil injection nozzle 152 e connecting the outer tilt plate 152 d and the inner circumferential ring groove 152 c of the retainer ring 152 is drilled as three sections along the entire circumference.
[0049] In FIG. 6 , the multiple pump side valve holes 162 and motor side valve holes 163 , extending towards the diameter and positioned at equal spaces along the periphery within the valve body 161 forming the distributor valve 160 , are formed in an array of two rows. A pump side switcher valve 164 is installed within the pump side valve hole 162 , and a motor side switcher valve 165 is installed within the motor side valve hole 163 and each ( 164 , 165 ) is capable of sliding movement.
[0050] The multiple pump side valve holes 162 are formed to correspond to the pump plunger holes 113 . Each of the pump side valve holes 162 , and pump flow passages 117 formed in the inner side edge of the pump plunger holes 113 , and the multiple pump side connecting passages 166 formed to respectively connect to them ( 162 , 117 ), are formed in the valve body 161 . The motor side valve holes 163 are formed to correspond to the motor plunger holes 137 . The motor connecting passages 139 formed on the inner edge side of the motor plunger holes 137 , and the motor connecting passages 167 connecting with the respective motor side valve holes 163 , are formed in the valve body 161 .
[0051] A pump side cam ring 168 is installed at a position enclosing the outer circumferential edge of the pump side switcher valve 164 on the distributor valve 160 . A motor side cam ring 169 is installed at a position enclosing the outer circumferential edge of the motor side switcher valve 165 on the distributor valve 160 . The pump side cam ring 168 is installed onto the inner circumferential surface 118 a of pump eccentric ring member 118 clamped by a bolt 119 to the tip of the pump casing 110 . See, FIG. 5 . The motor cam ring 169 is installed onto the inner circumferential surface 140 a of the motor eccentric ring member 140 positioned in contact with the tip of the elongated member 132 of motor casing 130 . See, FIG. 5 . The outer side edge of the pump side switcher valve 164 on the inner circumferential surface of the pump side cam ring 168 is engaged to allow sliding movement via the pump side restrictor ring 170 . The outer side edge of the motor side switcher valve 165 on the inner circumferential surface of the motor side cam ring 169 is engaged to allow sliding movement via the motor side restrictor ring 171 . The cam ring and the restrictor ring are both capable of relative rotation on either the pump side or the motor side.
[0052] A ring-shaped recess functioning as the inner side passage 172 is carved onto the outer circumferential surface of the transmission shaft 100 facing the inner circumferential surface of the valve body 161 . The inner edge of the motor side valve hole 163 and the pump side valve hole 162 are connected to this inner side passage 172 . An outer side passage 173 is formed near the external circumference of the valve body 161 to connect with the pump side valve hole 162 and motor side valve hole 163 .
[0053] The operation of the distributor valve 160 is described hereinafter. When the drive force of the internal combustion engine is conveyed to the transmission input gear 116 and the pump casing 110 rotates, the pump tilt plate 111 swings according to that rotation. The pump plunger 114 engaging with the tilt plate surface 111 a of the pump tilt plate 111 moves axially back and forth within the pump plunger hole 113 by way of the swinging of the pump tilt plate 111 . Hydraulic fluid is dispensed via the pump passage opening 117 from the pump fluid chamber 113 a during inward movement of the pump plunger 113 , and hydraulic fluid is suctioned into the pump fluid chamber 113 a via the pump passage opening 117 during outward movement.
[0054] At this time, the pump side cam ring 168 installed on the inner circumferential surface 118 of the pump eccentric ring member 118 coupled to the edge of the pump casing 110 , rotates along with the pump casing 110 . The pump side cam ring 168 is offset (eccentric) versus the rotation center of the pump casing 110 . In other words, it is installed offset (eccentric) to the valve body so that the pump side switcher valve 164 moves back and forth along the diameter within the pump side valve hole 112 ,according to the rotations of the pump side cam ring 168 .
[0055] The pump side switcher valve 164 moves back and forth in this way, and when moving inwards along the diameter within the valve body 161 , the pump side connecting passage 166 opens outwards along the diameter via a small diameter section 164 a of the pump side switcher valve 164 , and connects the pump passage opening 117 and the outer side passage 173 . When the pump side switcher valve 164 moves outward along the diameter within the valve body 161 , the pump side connecting passage 166 opens inwards along the diameter, and connects the pump passage opening 117 and the inner side passage 172 .
[0056] The pump tilt plate 111 swings along with the rotation of the pump casing 110 , the pump side cam ring 168 moves the pump side switcher valve 164 back and forth along the diameter, to match the position (lower dead point) where the pump plunger 114 is pressed farthest to the outside, to the position (upper dead point) that is furthermost to the inside during its back and forth movement. The pump plunger 114 consequently moves from the lower dead point to the upper dead point along with the rotation of the pump casing 110 , and the hydraulic fluid within the pump fluid chamber 113 a is dispensed from the pump passage opening 117 . The pump passage opening 117 at this time is connected to the outer side passage 173 so that the hydraulic fluid is sent to the outer side passage 173 . On the other hand, when the pump plunger 114 moves from the upper dead point to the lower dead point along with the rotation of the pump casing 110 , the hydraulic fluid within the inner side passage 172 is suctioned inside the pump fluid chamber 113 a via the pump passage opening 117 . In other words, when the pump casing 110 is driven, hydraulic fluid is dispensed from a pump fluid chamber 113 a on one side and supplied to the outer side passage 173 , and hydraulic fluid is suctioned from the inner side passage 172 into the pump fluid chamber 113 a on the other side of the transmission shaft 100 . 100571 However, the motor side cam ring 169 installed on the inner circumferential surface 140 a of the motor ring eccentric member 140 positioned in sliding contact on the edge of the motor casing 130 , is positioned eccentrically versus the rotation center of the transmission shaft 100 and the output rotation piece R, and motor cylinder 136 , when the motor ring eccentric member 140 is in the usual position. When the motor cylinder 136 rotates, the motor side switcher valve 165 moves back and forth along the diameter within the motor side valve hole 163 according to the motor cylinder 136 rotation.
[0057] When the motor side switching valve 165 moves inwards along the diameter within the valve body 161 , the small diameter section 165 a of the motor side switching valve 165 opens the motor side connection path 167 to the outside, connecting the motor passage opening 139 and the outer side passage 173 . When the motor side switching valve 165 moves outward along the diameter within the valve body 161 , the motor side connection path 167 opens inwards along the diameter, connecting the motor passage opening 139 and the inner side passage 172 .
[0058] The hydraulic fluid dispensed from the hydraulic pump P is sent to the outer side passage 173 , and this hydraulic fluid is supplied via the motor side connection path 167 , and the motor passage opening 139 to inside the motor fluid chamber 137 a . Thus, the motor plunger 138 is pressed axially outward. The outer edge of the motor plunger 138 is configured to be in slide-contact to the section where the motor tilt plate 135 moves from the upper dead point to the lower dead point. Due to this force pressing axially outwards, the motor plunger 138 moves along with the motor tilt plate 135 , along the tilted surface formed by the motor sliding member 134 and the bearing B 7 , B 8 . The motor cylinder 136 is consequently pressed by the plunger 138 and is driven. Along with the rotation of the motor cylinder 136 , the motor side cam ring 169 makes the motor side switching valve 165 move back and forth along the diameter in the valve body 161 , corresponding to the back and forth movement of the motor plunger 138 .
[0059] The motor cylinder 136 on the opposite side, moves the periphery of the transmission shaft 100 along with the rotation of the motor tilt plate 135 centering on the transmission shaft 100 , moving from the lower dead point to the upper dead point, and the hydraulic fluid within the motor fluid chamber 137 a is sent from the motor passage opening 139 to the inner side passage 172 , and is suctioned via the pump side connecting passages 166 and pump passage opening 117 .
[0060] A hydraulic shut off circuit joining the tilt plate hydraulic motor M and the tilt plate plunger-type hydraulic pump P is in this way formed by the distributor valve 160 . The hydraulic fluid dispensed according to the rotations of the hydraulic pump P is sent to the hydraulic motor M via the other hydraulic shut-off circuit (outer side passage 173 ), driving it. Moreover, the hydraulic fluid dispensed along with the rotation of the hydraulic motor M is returned to the hydraulic pump P via the other hydraulic shut-off circuit (inner side passage 172 ).
[0061] In the static hydraulic continuously variable transmission T described above, the hydraulic pump P is driven by the internal combustion engine 6 , the rotational drive power of the hydraulic motor M is converted by the distributor valve 160 and the hydraulic motor M, extracted from the transmission shaft 100 , and transmitted to the vehicle wheels. When the vehicle is being driven, the outer side passage 173 is the high pressure side fluid path, and the inner side passage 172 is the low pressure side. On the other hand, during times such as driving downhill, the drive force for the vehicle wheels is transmitted from the transmission shaft 100 to the hydraulic motor M, and the rotational drive force of the hydraulic motor P produces an effect of an engine brake conveyed to the internal combustion engine 6 . In this condition, the inner side passage 172 is the high pressure side fluid path, and the outer side passage 173 is the low pressure side fluid path.
[0062] The gear ratio of the static hydraulic continuously variable transmission T can be continuously changed by varying the tilt angle of the motor swing member 134 . The tilt angle of the motor swing member 134 is changed for a motor tilt plate angle of zero. In other words, when the motor tilt plate is perpendicular to the transmission shaft, the top gear ratio is reached, the amount of offset (eccentricity) of the eccentric (ring) member 140 reaches zero due to the effect of the lockup actuator A, see FIG. 5 , the center of the motor cylinder 136 matches the center of the eccentric member 140 , and the pump casing 110 , the pump cylinder 112 , the motor cylinder 136 , and the transmission shaft 100 rotates as one unit to efficiently transfer the drive power.
[0063] FIG. 10 is a vertical cross-sectional view of the vicinity of the centrifugal governor clutch C. When the inner side passage 172 and the outer side passage 173 are connected in the static hydraulic continuously variable transmission T, the high hydraulic pressure is no longer applied, and drive power is no longer transmitted between the hydraulic pump P and the hydraulic motor M. In other words, clutch control is implemented by controlling the degree of opening of the connection between the inner side passage 172 and the outer side passage 173 .
[0064] The centrifugal governor clutch C includes a spring sheet member 182 and a cam plate member 181 clamped by a bolt 180 to the edge of the pump casing 110 with a roller 183 held, respectively, within the multiple cam plate grooves 181 a formed and extending diagonally along the diameter on the inner surface of the cam plate member 181 . A pressure plate 184 includes an arm section 184 a facing the cam plate groove 181 a with a coil spring 185 with one end supported by the spring sheet member 182 and the other end acting on the pressure plate 184 for making the arm section 184 a of the pressure plate 184 apply a pressing force on the inside of the groove 181 a . A slide shaft 186 is provided for sliding along the axial line of the transmission shaft and is inserted into the center hole 181 b of the cam plate member 181 and also passing through the center section of the pressure plate 184 . A rod-shaped clutch valve 187 is engaged with the clutch valve engage section 186 a of the slide shaft 186 . One end of the coil spring 185 is supported by the spring sheet 182 a formed on the inner-facing flange of the spring sheet member 182 . The pressure plate 184 and the slide shaft 186 are both fabricated as separate pieces, and then coupled into a single piece to comprise the roller bearing member 188 . The pressure plate 184 is fabricated by forming the pressure plate 184 in a press, and the slide shaft 186 fabricated by cutting with machining tools and both parts are then welded together into one piece.
[0065] When the pump casing 110 is in a static state, or in other words a state where neither the cam plate member 181 or the spring sheet member 182 are rotating, the arm section 184 a presses the roller 183 into the cam plate groove 181 a by the pressing force applied to the pressure plate 184 by the coil spring 185 . The cam plate groove 181 a is in a tilted state so that the roller 183 is pressed along the diameter of the cam plate member 181 , and the pressure plate 184 , and the swing axis 186 is integrated therewith. The rod clutch valve 187 engaged in the swing shaft 186 are in a state shifted to the left.
[0066] When the pump casing 110 is driven by the rotation of the transmission input gear 116 , see FIG. 5 , and the cam plate 181 and the spring sheet member 182 rotate, the roller 183 is pressed back along the tilted surface of the cam plate member 181 outwards along the diameter by centrifugal force, and presses the arm section 184 a to the right and the pressure plate 184 moves to the right while opposing the force of the coil spring 185 . The amount of movement towards the right of the pressure plate 184 and the slide shaft 186 functioning as one piece with the pressure plate 184 are determined by the centrifugal force acting on the roller 183 . In other words, the amount of movement is determined according to the rotational speed of the pump casing 110 . When the rotational speed of the pump casing 110 increases, the rod clutch valve 187 engaged in the slide shaft 186 , extends along the inner section of the transmission shaft 100 , and shifts to the inner part of the clutch valve hole 105 . The centrifugal governor mechanism is in this way configured to apply a centrifugal force to the roller 183 by utilizing the centrifugal force from the rotation of the pump casing.
[0067] An inner side connecting fluid path 190 is formed in the transmission shaft 100 as shown in FIG. 10 that joins the clutch valve hole 105 and the inner side passage 172 . An outer side connecting fluid path 191 joins the clutch valve hole 105 and an outer side passage 173 with a ring-shaped groove 192 and a tilt fluid path 193 for a short connection are formed in the transmission shaft 100 and the pump cylinder 112 . When the pump casing 110 is in a static state, the inner side connecting fluid path 190 and the outer side connecting fluid path 191 are connected by way of the small diameter section 187 a of the rod-shaped clutch valve 187 , and consequently the inner side passage 172 and outer side passage 173 are connected so the clutch is disengaged.
[0068] When the pump casing rotation exceeds the specified speed, and the rod-shaped clutch valve 187 shifts to the innermost section of the clutch valve hole 105 due to the effect of centrifugal force from the governor mechanism, the small diameter section 187 a of the rod-shaped clutch valve 187 releases (away) from the opening on the clutch valve hole 105 side of the outer side connecting fluid path 191 , and the outer side connecting fluid path 191 opening is blocked by the large diameter side surface 187 b of rod-shaped clutch valve 187 . See position of rod-shaped clutch valve 187 in FIG. 6 . The connection between the inner side passage 172 and outer side passage 173 is therefore blocked and an oil circulation shut-off circuit is formed from the hydraulic pump P and outer side passage 173 and hydraulic motor M and inner side passage 172 , and the static hydraulic continuously variable transmission T functions. Switching from a clutch released state to a clutch engaged state is performed by the roller so that the clutch gradually becomes engaged (connected) according to this movement.
[0069] FIG. 11 is a vertical cross-sectional view of an essential section of the static hydraulic continuously variable transmission T showing the supply path for the lubricant fluid and the operating (hydraulic) fluid. The operating (hydraulic) fluid is supplied from the high-pressure oil pump of the oil pump cluster 90 driven by the internal combustion engine, via the fluid path within the crankcase, from the right end, to the transmission shaft center fluid path 200 formed along the axis and in the center of the transmission shaft 100 . The innermost section of the transmission shaft center fluid path 200 is joined to the fluid path 201 extending along the diameter to the outer circumference. The fluid path 201 is also joined with the output rotation piece inner fluid path 202 formed in parallel with the transmission shaft 100 within the output rotation piece R (motor cylinder 136 , valve body 161 , pump cylinder 112 ) that rotates as one piece with the transmission shaft 100 . The output rotation piece inner fluid path 202 is a fluid path including the fluid path 202 a within the motor cylinder 136 , the fluid path 202 b within the valve body 161 , and the fluid path 202 c within the pump cylinder 112 .
[0070] A check valve 210 for supplying replacement fluid within the outer side passage 173 is installed within the pump cylinder 112 . The output rotation piece inner fluid path 202 is joined to the check valve 210 via the fluid path 203 facing outwards along the diameter in the innermost section ( 202 ), and if necessary (according to leakage of operating fluid from the hydraulic shut-off circuit), operating fluid is supplied to the outer side passage 173 of the valve body 161 . A check valve and fluid path for supplying operational fluid to the inner side passage 172 are installed in the same way in another section of the pump cylinder 112 , and if necessary also supply operating fluid to the inner side passage 172 (omitted from drawing).
[0071] An outer ring groove 204 is formed on the outer circumference of the transmission shaft 100 corresponding to the innermost section of the output rotation piece inner fluid path 202 , and connects to the innermost section of the output rotation piece inner fluid path 202 . An inner ring groove 205 is formed on the inner circumference of the clutch valve hole 105 of the transmission shaft 100 , and connects to the outer ring groove 204 at one location via the connecting fluid path 206 . An orifice 206 a is formed in the connecting fluid path 206 . On the transmission shaft 100 , a lubricant oil injection nozzle 207 connecting to the inner ring groove 205 of the clutch valve hole and facing the external circumference of the transmission shaft 100 is drilled at three locations on the transmission shaft periphery. A portion of the oil supplied within the output rotation piece inner fluid path 202 is injected by way of the lubricant oil injection nozzle 207 , and the outer ring groove 204 , the connecting fluid path 206 , the inner ring groove 205 , and lubricates the pump tilt plate 111 , etc.
[0072] A fluid path 208 is formed at one location from the transmission shaft center fluid path 200 along the diameter, facing towards the stop member 150 on the right edge positioner section of the output rotation piece R on the transmission shaft 100 . An orifice 208 a is formed on its inner edge section. The outer edge section of the fluid path 208 connects along the diameter to the ring groove 152 c formed on the inner circumference of the retainer 152 . A portion of the oil supplied to the inside of the transmission shaft fluid path 200 is supplied via the fluid path 208 and the inner ring groove 152 c , to the lubricant oil injection nozzle 152 e formed at three locations on the periphery of the inner ring groove 152 c and the outer tilt plate 152 d of the retainer ring 152 and is dispensed from the lubricant oil injection nozzle 152 e and lubricates the motor tilt plate 135 , etc.
[0073] The distance L 1 between the inner edge surface 113 b of the pump plunger hole 113 and the pump side edge 161 a of the valve body 161 , is made large compared to the distance L 2 between the inner edge surface 137 b of the motor plunger hole 137 and the motor side surface 161 b of the valve body 161 . The larger distance is required because it is necessary to form a tilt fluid path 193 , see FIG. 10 , joining the clutch valve hole 105 and the outer side passage 173 between the inner edge surface 113 b of the pump plunger hole 113 of pump cylinder 112 and pump side edge 161 a of the valve body 161 on the pump side. Therefore, the pump plunger hole 113 are separated from the valve body 161 . There is no need to form a tilt fluid path on the (other) motor M side and therefore the distance between the inner edge surface 137 b of the motor plunger hole 137 and the motor side surface 161 b of the valve body 161 is small.
[0074] The above described embodiments render the following effects.
[0075] In the hydraulic pump cylinder 112 , a tilt fluid path 193 is formed on a passage opening 117 with a small diameter compared to the plunger hole 113 . In addition, the distance L 1 between the inner edge surface 113 b of the plunger hole 113 and the edge surface 161 a of the valve body is increased, and the axial length of the passage opening 117 is increased so that a tilt fluid path 193 with a large diameter can be formed without restrictions on the plunger hole 113 . Thus, the pressure on the high-pressure hydraulic path 173 can be sufficiently lowered when the clutch is disengaged.
[0076] The diameter of the plunger holes 113 of the hydraulic pump cylinder 112 is reduced so that a tilt fluid path 193 with an even large diameter can be formed.
[0077] FIG. 7 ( a ) is a frontal view of the cotter pin 151 with FIG. 7 ( b ) illustrating a cross-sectional view along I-I of FIG. 7 ( a ).
[0078] FIG. 8 ( a ) is a frontal view of the retainer ring with FIG. 8 ( b ) illustrating a cross-sectional view along I-I of FIG. 8 ( a ).
[0079] FIG. 9 ( a ) is a frontal view of the C clip with FIG. 9 ( b ) illustrating a cross-sectional view along I-I of FIG. 9 ( a ).
[0080] The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
[0081] The clutch mechanism for a hydrostatic continuously variable transmission of the preferred embodiment described above in detail is constructed such that a spring sheet 182 a is integrally formed at an inward flange of the cylindrical member separate from the cam plate member 181 to make the cylindrical spring sheet member 182 . The spring sheet member 182 is held between the cam plate member 181 and the transmission pump casing 110 and is integrally fixed with a bolt 180 used for fixing this cam plate member. Accordingly, the machining of the spring sheet member 182 is easy because it has no ring-like spring sheet of a small independent component of the prior art, and the number of component parts is decreased because a fixing clip is not required.
[0082] The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
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A clutch mechanism for a hydrostatic continuously variable transmission in which a high pressure oil path and a low pressure oil path are shortened to change-over a transmittance of power. A spring sheet is provided of which manufacturing and assembling are simple and the number of component parts is reduced. This clutch mechanism for a hydrostatic continuously variable transmission includes a cam plate member arranged at the end part of the transmission shaft, a roller engaged with the cam plate member and moved in a diametrical outward direction with a centrifugal force, a roller bearing member slid axially through an outward motion of the roller, a spring sheet member for biasing the roller bearing member toward the roller, and a spring sheet member for supporting the spring member. The spring sheet member is held by said cam plate member and said casing and is supported.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application depends from and claims priority to U.S. Provisional Application No. 61/830,887 filed Jun. 4, 2013, which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present disclosure relates to the field of food product containers. More particularly, the present disclosure is in the field of fitments for containers that are intended to hold food items such as baby food, yogurt, mashed fruits and vegetables, applesauce and other similar products that might necessitate the use of a spoon for easy consumption.
BACKGROUND OF THE INVENTION
[0003] Containers having a fitment with a tube spout have been used to store food product such as such as baby food, yogurt, mashed fruits and vegetables, applesauce, etc. for quite some time. Oftentimes the product contained within the container is easier for a user to consume if a utensil such as a spoon is used. For example, if the product can be removed from the container via the tube spout of the fitment and placed directly onto a spoon. Once on the spoon the product can neatly be consumed by the user. However, at times a spoon may not be available for the user. In such cases a new design which provides a spoon to the user is desired.
SUMMARY OF THE INVENTION
[0004] The present disclosure is directed towards an assembly for mounting to a container. The assembly includes a fitment with a passage. The fitment is for mounting to the container such that one end of the passage is in communication with the interior of the container. The passage also includes an opposite end. The assembly further includes a spoon. The spoon is at least partially disposed within the passage of the fitment.
[0005] The spoon may be attached to the fitment, and covered by a protective cover. The protective cover may include a first half and a second half. The protective cover may be secured with a safety seal, may be hinged at a top part of the cover, and may be hinged at a bottom part of the cover.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is an elevational front view of a container having an assembly of the present disclosure including a cover;
[0007] FIG. 2 is an elevational side view of the container having the assembly of FIG. 1 ;
[0008] FIG. 3 is a sectional side view of the container having the assembly of FIG. 1 ;
[0009] FIG. 4 is a perspective front view of the assembly of FIG. 1 with the cover in a closed position;
[0010] FIG. 5 is a perspective front view of the assembly of FIG. 1 with the cover in an open position;
[0011] FIG. 6 is an elevational front view of a portion of an assembly of the present disclosure with an alternate cover in a closed position; and
[0012] FIG. 7 is an elevational front view of the portion of the assembly of FIG. 4 with the alternate cover in an open position.
DETAILED DESCRIPTION OF THE INVENTION
[0013] An assembly for mounting to a container includes a fitment 15 with a passage 20 . When the fitment 15 is mounted to the container, one end 21 of the passage 20 is in communication with an interior of the container. The passage also includes an opposite end 22 . A spoon 25 is at least partially disposed within the passage 20 of the fitment 15 .
[0014] One embodiment of the container, as shown in FIGS. 1-3 , is a flexible pouch 30 . The flexible pouch 30 includes a front panel 31 and a back panel 32 . The fitment 15 is disposed between the front panel 31 and the back panel 32 at a top portion to the flexible pouch 30 . A gusset 33 is disposed between the front panel 31 and the back panel 32 and at a bottom portion of the flexible pouch 30 . The front panel 31 and back panel 32 are sealed to each other, the fitment 15 , and the gusset 33 , in a sealed area that runs along the perimeter of the flexible pouch 30 . The front panel 31 , back panel 32 , gusset 33 and fitment 15 define the interior of the flexible pouch 30 .
[0015] The flexible pouch 30 is made from a flexible material, preferably a laminate composed of sheets of plastic or aluminum or other suitable materials. The front panel 31 and back panel 32 can be separate sheets of the flexible material, or can be a single sheet folded over. An outer layer of the material may include preprinted information, such as a logo or the like, to provide the consumer with information regarding the contents of the pouch. The pouch 30 may be formed and/or filled using conventionally known manufacturing techniques, such as a horizontal form-fill-seal machine with a single or multiple lanes, a flat bed pre-made pouch machine, a vertical form-fill machine, or the like. An example of a method and apparatus for filling a flexible pouch with a product is disclosed in commonly assigned U.S. Pat. No. 6,199,601, which is incorporated herein by reference. The edges of the pouch are sealed, leaving an edge open for receiving a fitment. The spout fitment is inserted into the opened edge and the open edge is ultrasonically or heat-sealed, so as to seal the fitment to the walls of the pouch.
[0016] One embodiment of the fitment 15 includes a canoe portion 35 and a spout portion 36 . The canoe portion 35 of the fitment 30 is disposed between, and sealed to, the front panel 31 and back panel 32 of the flexible pouch 30 . The spout portion 36 extends from the canoe portion 35 . The passage 20 extends through both the canoe portion 35 and the spout portion 36 . The passage 20 includes one end 21 in communication with the interior of the flexible pouch, and the opposite end 22 . The passage 20 allows product to the added or removed from the interior of the flexible pouch 30 . Partially disposed within the passage 20 of the fitment 15 is the spoon 25 .
[0017] The spoon 25 includes a scoop portion 40 , and a handle portion 41 . The scoop portion 40 is disposed above the spout portion 36 , with the handle portion 41 of the spoon 25 extending into passage 20 of the fitment 15 . The spoon 25 and fitment 15 can be made of injection molded plastic, or any other material and/or method known to those skilled in the art.
[0018] In the shown embodiment, the spoon 25 is secured within the passage 20 by one or more frangible ribbons 45 . The frangible ribbons 45 extend axially from the spoon 25 and secure to an inside surface 46 of the spout portion 36 of the fitment 15 . The ribbons 45 are thin enough in manufacture such that a user can twist or pull the spoon 25 to break the ribbons 45 , thereby detaching the spoon 25 from the fitment 15 . The ribbons 45 extend from the spoon 20 in an area between an extendable potion 50 of the handle portion 41 and the scoop portion 40 of the spoon 25 .
[0019] The extendable portion 50 is generally located at a middle of the handle portion 41 . The extendable portion 50 has a concertina type design, enabling the handle portion 41 to be extended by a user pulling in opposite longitudinal directions from each end of the handle portion 41 , thereby allowing the handle portion 41 to have a more compact shape when attached to the fitment 15 , and a longer, more user friendly shape, when detached for use.
[0020] Also attached to the fitment 15 is a protective cover 55 . The protective cover 55 is disposed above the spout portion 36 of the fitment 15 , and encloses the scoop portion 40 of the spoon 25 not disposed within the passage 20 .
[0021] The first half 56 and second half 57 are generally hemispherical in shape, and are oriented in a clamshell style design. The clamshell design provides that the protective cover 55 can be transitioned from a closed position, as exampled in FIGS. 4 and 6 , to an open position, as exampled in FIGS. 5 and 7 . The hemispherical shape of the first half 56 and the second half 57 allows the protective cover 55 to be secured to the fitment 15 regardless of the rotational position, or orientation, of the spoon 25 within the passage 20 .
[0022] In one embodiment, as shown in FIGS. 4-5 , the cover 55 includes a first half 56 and a second half 57 . The first half 56 and second half 57 are secured to the spout portion 36 of the fitment 15 , and extend upwardly to envelope the spoon 25 . The first half 56 abuts the second half 57 along a cover seam 58 . The cover seam 58 can be a physical separation between the first and second halves 56 57 , or it can be a detachable type connection, such as an area of thin frangible material capable of being broken, torn, or otherwise removed or detached to enable separation of the halves 56 57 .
[0023] The first half 56 is attached to the second half 57 at the top of the first and second halves 56 57 by a top hinge 60 . The first half 56 is attached to the fitment 15 by way of a detachable portion, such as a tear away safety seal 61 . The safety seal 61 attaches to the fitment 15 and the first half 56 by way of an area of thin frangible material capable of being broken to enable separation. The second half 57 is securely attached to the fitment 15 . To access the spoon 25 , the safety seal 61 is removed, detaching the first half 26 from the fitment 15 . The first half 26 is pivoted about the top hinge 60 , separating the first half 56 from the second half 57 along the cover seam 58 , and providing access to the spoon 25 .
[0024] In another embodiment, as shown in FIGS. 6-7 , the first half 56 and second half 57 are each attached to the fitment 15 by way of a bottom hinge 65 . An alternate detachable portion, such as an alternate tear away safety seal 66 , attaches the first half 56 to the second half 57 . The alternate safety seal 66 runs along the cover seam 58 . To access the spoon 25 , the alternate safety seal 66 is removed, detaching the first half 56 from the second half 57 . Once detached from each other, the first half 56 and second half 57 are free to pivot about their respective bottom hinge 65 , thereby separating the first half 56 from the second half 57 , and providing access the spoon 25 .
[0025] The fitment 15 , spoon 25 , and protective cover 55 may be made of a food grade plastic using injection molding techniques, or with any other suitable material and manufacturing method known to those skilled in the art.
[0026] The present invention has been described in an illustrative manner. It is understood that the terminology which has been used is intended to be in the nature of words of description rather than limitation. As such, many modifications and variations of the present invention are possible in light of the above teachings.
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Containers having a fitment have been used to store food product. Oftentimes the product contained within the container is easier for a user to consume if a utensil such as a spoon is used. The present disclosure is directed towards an assembly for mounting to a container. The assembly includes a fitment with a passage. The spoon is at least partially disposed within the passage of the fitment. The spoon may be attached to the fitment, and covered by a protective cover. The protective cover may include a first half and a second half The protective cover can be secured with a safety seal.
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FIELD OF APPLICATION
The present invention relates to a fuel injection valve for use in an injection system for internal combustion engines. Such a fuel injection valve is particularly suitable for direct injection of the fuel into the combustion space of each cylinder of the internal combustion engine and can be used with advantage in diesel engines.
BACKGROUND OF THE INVENTION
Fuel injection valves of this type with indirect electromagnetic control of the nozzle needle of the fuel injection valve are revealed, for example, in the following publications:
U.S. Pat. No. 4,566,416, EP-A-0 228 578 and EP-A-0 262 539.
In the fuel injection valves revealed in the publications quoted above and in the fuel injection valve of the present invention, the nozzle needle is indirectly actuated electromagnetically by means of a hydraulic amplifier. The fuel pressure in a control space acts on a needle piston and holds the nozzle needle closed. The control space is connected to the high-pressure supply conduit of the fuel injection valve via a first throttle hole and the control space can be relieved via a second throttle hole. The outlet from this second throttle hole can be opened and closed by an electromagnetically actuated pilot valve. If the pilot valve is actuated, the second throttle hole is opened. Because of the first throttle hole, the pressure in the control space drops. In consequence, a force occurs on the nozzle needle in the opening direction of the nozzle needle and injection begins. If the pilot valve is closed again, the pressure in the control space builds up again, the nozzle needle is closed and the injection is, in consequence, ended. Fuel injection valves of this type are therefore suitable for generating intermittent injections such as are necessary, for example, in the case of diesel engines.
The maximum injection pressures of these injection valves can be more than 1000 bar. The minimum injection pressures vary between 100 and 300 bar. The engine is operated under load and up to full load by using the upper injection pressure range whereas the engine is operated at idle and at very low load in the lower pressure range.
In order to achieve good power and exhaust gas figures from the engine, the injection period must be short under load and at high rotational speed of the engine. This period is generally about one-thousandth of a second. The quantity injected at these operating points is substantially larger than that when the engine is idling. The fuel quantity required per working stroke at idle is, on the contrary, extremely small because it is only necessary to overcome the friction of the engine and there is no power output at the drive end of the crankshaft. In addition, the rotational speed of the engine is low. In order to avoid rough and noisy engine running at idle and at low load, it is desirable for the injection period to be relatively long, despite the small injection quantity. It should again, typically, be between one-thousandth and two-thousandths of a second.
Because the injection quantity is small, it is difficult to generate a long injection period with the fuel injection valves of known type and it is, in consequence, difficult to achieve quiet, smooth engine idling.
SUMMARY OF THE INVENTION
The object of the present invention is to propose a novel, improved fuel injection valve of simple design in which the opening motion of the injection valve element remains limited at low injection pressure (for example 200 bar) and medium injection pressure (for example between 300 and 500 bar) and a small injection quantity can therefore be injected during a long injection period whereas, at high injection pressure (for example 1000 bar or more), the opening motion of the injection valve is substantially more rapid and the opening path of the nozzle needle of the injection valve is substantially larger than at low to medium pressure and, therefore, a large injection quantity can be injected during a short injection period.
This makes it possible to achieve, in the first place, smooth running at idle and at low load and to satisfy, in the second place, the requirement for good power and exhaust gas figures under load and at high engine rotational speed.
The object is achieved by means of a novel fuel injection valve.
Because of the pressure drop in the control space, the nozzle needle of the fuel injection valve will only execute a first displacement or lift from the valve seat at low and medium injection pressures. This continues until a lift stop is reached which is preloaded by a strong spring and rests on a stop surface. The spring preloading force is sufficiently large for the lift stop not to be moved until a medium pressure level is reached. At high injection pressure, on the other hand, the pressure drop in the control space generates a force which is sufficiently large to move the lift stop and the nozzle needle so that there is a second lift range and, in consequence, a large injection quantity can be injected during a short injection period.
These and further advantages of the invention are explained by means of the following detailed description of different embodiment variants which are shown in the figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an axial sectional drawing of an electromagnetically controlled fuel injection valve according to the present invention;
FIG. 2 is an enlarged partial excerpt from FIG. 1 which shows, in detail, the specific features for realizing the desired lift curve;
FIG. 3 is an axial sectional drawing of a second embodiment variant of a fuel injection valve according to the present invention,
FIG. 3a is an enlarged view from above of a lift stop element of the fuel injection valve of FIG. 3,
FIG. 3b is a sectional drawing of the lift stop element along the line A--A of FIG. 3a and
FIG. 4 is a diagram which shows the shapes of the lift curves of the fuel injection valves of the present invention for relatively low to medium injection pressure and for high injection pressure.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, which shows a sectional drawing of a fuel injection valve 10 according to the present invention, the fuel under pressure reaches a longitudinal hole 14, which is introduced into the valve housing 16, via a supply connection 12. The hole 14 extends downwards as far as an intermediate plate 20 and opens into a hole 18 produced in the intermediate plate 20. The hole 18 opens into a hole 22 which is connected to an annular hole 22a which is located in the nozzle tip 24. The annular hole 22a extends in the nozzle tip 24 as far as the seat 24a of the atomizer nozzle 28, which is located between the nozzle tip 24 and the tip of the nozzle needle 26.
The atomizer nozzle 28 is embodied as a so-called seat-hole nozzle. In such an arrangement of the atomizer nozzle 28, the injection holes 30 open at the inside directly into the seat 24a, which is closed by the nozzle needle tip when no injection is to take place. This arrangement has the specific advantage that, assuming there is a sufficient fuel pressure in the annular hole 22a, the atomizer nozzle 28 generates good atomization in the combustion space of the associated internal combustion engine (not shown) even at a very small lift of the nozzle needle 26. As mentioned above, this has a favourable effect on the operating behaviour of the engine.
In FIG. 1, the seat-hole nozzle is shown as an example of an atomizer nozzle 28 which has good fuel atomization even at very small lift of the nozzle needle 26. Further arrangements of the atomizer nozzle 28 can be used in association with the present invention. In order to utilize the advantages of the present invention in an optimum manner, however, it is expedient to use atomizer nozzles which ensure good conversion of the pressure energy in order to generate small, finely distributed fuel droplets in the combustion space of the engine even at very small lift of the nozzle needle.
The hole 14 extends upwards as far as an annular groove 32 which is connected to the control space 40 by means of the throttle hole 34 and a longitudinal hole 36, both produced in the needle piston 38. A second throttle hole 42 opens at one end into the control space 40. At the other end, the throttle hole 42 is held closed by an electromagnetically actuated pilot needle 44. The pilot needle 44 can be moved away from the outlet end of the throttle hole 42 by means of the electromagnet 46.
The magnet 46 is screwed to the valve housing 16 by means of a nut 48. A control spring 50, a control spring screw 52 and a control spring sleeve 54 are also visible in FIG. 1. The stem 56 of the pilot needle 44 is guided within the magnet 46 on the longitudinal axis of the injection valve 10. The return force of the control spring 50 acts on the upper end of the stem 56 of the pilot needle 44. This force can be set to the desired value by selecting the thickness of the spring sleeve 54. The electromagnet 46 is supplied with electrical current pulses of a predetermined duration by means of the electrical connecting cable 58.
The nozzle tip 24 is screwed, together with the intermediate plate 20, in a sealed manner onto the valve housing 16 by means of a union nut 60. At its upper end, the nozzle needle 26 has a thin extension 26a and the lower extension 62a of the needle plunger 62 presses on the end of this thin extension 26a. The needle plunger 62 has, at its upper end, the needle piston 38, already mentioned, and is connected to this needle piston 38 as an integral part.
The needle piston 38, together with the valve housing 16, has a guide 38a with a closely toleranced sliding fit. The clearance of this sliding fit is typically 2-4 microns. The nozzle needle 26, together with the nozzle tip 24, likewise has a guide with a close sliding fit 26b. The clearance of this close guide is also typically 2-4 microns. Between these two guides 26b and 38a, there is a space 70 in which the pressure is substantially lower than that in the fuel passages previously mentioned. This space 70 is connected via a hole 72 in the valve housing 16 to a further space 74 in which the pilot needle 44 is located. Leakage fuel which reaches the space 70 from the control space 40 via the guide 38a and from the annular hole 22a via the guide 26b is evacuated into the space 74 through the hole 72. This fuel, together with the fuel which is relieved into the space 74 by the throttle hole 42 during each injection, flows from the space 74 back to the fuel tank (not shown) via a drain nipple 76.
A needle spring washer 64, a needle spring 66 and a lift stop element 68 can also be seen in the lower part of the valve housing 16. The preloading force of the needle spring 66 can be brought to a desired value by selecting the thickness of the needle spring washer 64.
The elements just described and further elements, which have been described earlier, of the fuel injection valve 10 are likewise shown in FIG. 2. FIG. 2 is an enlarged, partial excerpt from FIG. 1 which shows, in detail, the specific features for realizing the desired lift curve during the injection in accordance with the present invention.
If no injection occurs, i.e. in the closed condition of the nozzle needle 26 as shown in FIGS. 1 and 2, the lift stop element 68 is in contact with a stop surface 68a. Between this plane, lower stop surface 68a of the lift stop element 68 and the upper, plane surface 68b of the nozzle needle 26, there is a first free path H1 (see FIG. 2).
The extension 62a of the needle plunger 62 presses, because of the pressure in the control space 40, on the extension 26a of the nozzle needle 26 and therefore holds the latter reliably in its closed position on the valve seat 24a. The extension 62a could also extend as far as the upper, plane surface 68b of the nozzle needle 26. This would dispense with the extension 26a of the nozzle needle 26.
A second free path H2 is present between the upper, plane stop surface 68c of the lift stop element 68 and the associated surface 68d of the valve housing 16.
The mode of operation of the fuel injection valve 10 is now as follows in the case of low (for example 200 bar) and medium (for example 400 bar) pressure level. In this operating condition, which is the defining one for idling and low engine load, the nozzle needle 26 will traverse only a lift equal to the path H1 during the total injection procedure. For this purpose, the electromagnet 46 is excited, at a desired instant, by a current pulse of specified duration. The pilot needle 44 is moved away from the throttle hole 42 against the force of the control spring 50. In consequence, and because of the throttle 34, the pressure in the control space 40 drops rapidly. The pressure in the annular space 22a, which acts on the guide piston 26b of the nozzle needle 26, is now capable of opening the nozzle needle 26 so that injection begins.
The extensions 26a and 62a then move within the longitudinal hole 69, which is arranged on the longitudinal axis of the fuel injection valve 10, of the lift stop element 68. The lift stop element 68 is, on the other hand, in contact with the lower stop surface 68a.
After the nozzle needle 26 has traversed the first path or lift H1, the stop 68b comes into contact with the stop 68a. The force of the spring 66 is sufficiently large to ensure that the hydraulic pressure force, which tends to open the nozzle needle 26 further, is not sufficient to overcome this spring force. The nozzle needle 26 will therefore only execute the first lift H1.
In the case of this small first lift H1, the effective flow area of the injection holes 30 is restricted so that a small injection quantity is supplied to the engine combustion space (not shown) during a long injection period. If the current pulse to the electromagnet 46 is ended, the pilot needle 44 is pushed back by the control spring 50 onto the throttle hole 42 and closes the latter. The pressure builds up in the control space 40 and the hydraulic pressure force in the control space 40 will now close the nozzle needle 26 and end the injection.
The curve of the first lift H1 of the nozzle needle 26 is shown in FIG. 4 as the ordinate C as a function of time t (curve A).
At high injection pressure (for example 1000 bar), the fundamental mode of operation of the fuel injection valve 10 is similar to that at low and medium injection pressure. In this case, it must be noted that the hydraulic pressure force, which acts in the opening direction of the nozzle needle 26 because of pressure drop in the control space 40, also increases as the injection pressure increases.
If the electromagnet 46 is excited with a current pulse of specified duration at high injection pressure (for example 1000 bar), the pilot needle 44 again moves away from the throttle hole 42 so that the pressure in the control space 40 drops. The nozzle needle 26 is opened by the hydraulic pressure force and rapidly traverses the first lift H1. After the plane surfaces 68b and 68a come into contact, the larger hydraulic pressure force is now capable of moving the lift stop element 68 against the force of the spring 66 until the stop surface 68c touches the surface 68d of the valve housing 16 so that the second, larger lift H2 is traversed in addition to the first lift H1.
If the current pulse to the electromagnet 46 is ended and, in consequence, the pressure in the control space 40 builds up anew after the closing of the throttle hole 42 by the pilot needle 44, the pressure force in the control space 40, together with the spring force of the spring 66, will rapidly close the nozzle needle 26. By this means, the injection is rapidly interrupted and this, in turn, has favourable effects on the engine operational figures.
The curve thus described of the nozzle needle motion during the injection is represented by the curve B in FIG. 4.
The variation with time of the pilot needle lift P after excitation of the electromagnet 46 is shown in FIG. 4. The pilot needle 44 rapidly traverses its lift as far as the stop at the electromagnet end and then remains open until a time of approximately 1 ms has elapsed. At this instant, the current pulse (not shown) is interrupted and the pilot needle 44 will be rapidly pushed back by the control spring 50 onto its seat at the outlet from the throttle hole 42.
The curves A and B of the nozzle needle motion, as described further above, are shown in the lower diagram of FIG. 4. In the case of the curve A, the nozzle needle 26 traverses the first lift H1, which in this diagram corresponds to 10% of the maximum nozzle needle lift, which is given by the addition of the two lifts H1 and H2. This value of 10% is a guideline value. Depending on the specific engine application, the first lift H1 can be of different magnitude compared with the second lift H2.
After traversing the first lift H1, the curve B has a step S. This step results from the fact that the nozzle needle 26 is initially retarded when the stop surface 68b comes in contact with the stop surface 68a. The nozzle needle 26, together with the plunger 62, the stop piece 68 and the lower part of the spring 66, must subsequently be accelerated anew.
This step S is not a disadvantage with respect to the combustion in the engine. On the contrary, it can lead to an improvement in the combustion and the associated noise and exhaust gas emissions of the engine in certain applications. The step S just mentioned will be more or less marked depending on how large the masses of the nozzle needle 26, the needle plunger 62 and the lift stop element 68 are and on how rapidly the pressure drop in the control space 40 takes place and how large it is. In certain cases, this step S can be very short so that the transition from the first lift H1 to the second lift H2 is only noticeable as a kink in the opening motion of the nozzle needle 26. Depending on the operating pressure of the fuel injection valve 10, the slope or opening rate of the second lift H2 is equal to zero (curve A), equal to a curve between A and B or equal to a curve as at B (see FIG. 4).
After the step mentioned, the nozzle needle 26, together with the plunger 62, the stop piece 68 and the lower part of the spring 66, moves further and traverses the second lift H2 until the second, definitive lift stop 68d of the valve housing 16 is reached. The total lift therefore traversed by the nozzle needle 26 corresponds to the sum of the two partial lifts H1 and H2.
A further advantage of the present invention, in addition to achieving the curve A at low operating pressure and the curve B at high operating pressure of the fuel injection valve 10, is the fact that the curves of the nozzle needle opening motion of the second lift H2 between A and B for different operating pressures can be realized in a substantially more flexible and exact manner than in the case of the already known fuel injection valves of this type (such as those of EP-A-0 228 578 or EP-A-0 262 539 for example).
In the case of the present invention, the opening rate of the second lift H2 of the nozzle needle 26 can take on any given value between the curves A and B, depending on the operating pressure. This is the case because the nozzle needle 26 has executed the first lift H1 even at low operating pressure (for example 200 bar) and the fuel pressure acts on the seat surface 24a, and therefore the tip of the nozzle needle 26. In this condition, the hydraulic pressure forces which act from the nozzle tip 24 end on the nozzle needle 26 and from the control space 40 end on the plunger 62 are stable. It is therefore possible to achieve any given opening rate of the second lift H2 of the nozzle needle 26 in a stable and reproducible manner.
In the already known solutions where only one lift is traversed without an intermediate lift stop, the pressure in the control space must be greatly reduced at an already extremely high operating pressure of the fuel injection valve in order to balance the force of the closing spring and the missing pressure force of the valve, which is still closed. If the nozzle needle now opens and if the hydraulic seat force becomes effective under the nozzle tip, the nozzle needle traverses its lift very rapidly and it is not possible to control the opening rate.
It should also be noted that the fuel pressure at which the nozzle needle 26 is in a position to move the lift stop element 68 by the amount of the second lift H2 can be of different magnitude depending on the specific application (for example 200, 300, 400 or 500 bar). This is achieved by the specific matching of the control elements (for example, the force of the spring 66).
FIG. 3 shows an axial sectional drawing of a second embodiment of a fuel injection valve 100 according to the present invention. The elements of the fuel injection valves 10 and 100, which are the same, have been given the same numbers.
The fuel under pressure reaches the valve housing 102 via the supply connection 12 and a hole 104.
The hole 104 is connected to a hole 106 introduced on the longitudinal axis of the fuel injection valve 100. An intermediate piece of the needle plunger 108, a spring 110, a spring washer 112 and a lift stop element 114 are located in this hole 106.
An intermediate plate 116 is located between the lower end of the valve housing 102 and the nozzle tip 118. The nozzle tip 118 and the intermediate plate 116 are screwed onto the valve housing 102 in a sealed manner by means of a union nut 120. The nozzle needle 122 is guided in the nozzle tip 118 by means of a nozzle needle guide 124. The nozzle tip 118 and the nozzle needle 122 have an atomizer nozzle 126 with a common valve seat 122a and a single injection hole 128. Like the atomizer nozzle of the fuel injection valve 10, this arrangement of the atomizer nozzle 126 also permits optimum utilization of the properties of the present invention.
As shown in FIG. 3, the lower part 108b of the needle plunger 108 is connected to the extension 122b of the nozzle needle 122 by means of a press fit. In contrast to the fuel injection valve 10, a fixed mechanical connection between the needle plunger 108 and the nozzle needle 122 is necessary in this case because otherwise the nozzle needle 122 would not open. An alternative embodiment would be one in which both parts are welded or brazed together or in which both the nozzle needle 122 and the needle plunger 108 are manufactured from one workpiece.
In a further alternative variant, not shown in any more detail, the plate 116 could be omitted and the valve housing 122 could be embodied as far as the nozzle tip 118.
As compared with the fuel injection valve 10, as shown in FIGS. 1 and 2, the embodiment of the fuel injection valve 100 with the space 106 which is at high pressure has the advantage that the lower part of the fuel injection valve 100 can be made substantially thinner than is possible in the case of the fuel injection valve 10 because there is no need for a fuel supply hole 14 to the side of the fuel injection valve longitudinal axis.
In the case of the fuel injection valve 100, all the elements within the hole 106 and inside the nozzle tip 118 and the plate 116 are embodied in such a way that there is a connection without hydraulic resistance between the end of the hole 104 and the atomizer nozzle 126. This is realized by means of a passage 112a between the spring washer 112 and the needle plunger 108 and by means of a plurality (three in each case here) of flats which are applied to the periphery of the lift stop element 114 and the nozzle needle guide 124. The view from above of the lift stop element 114 is shown in FIG. 3a for better illustration of the embodiment of these flats. In addition, a section A--A of the lift stop element 114, in accordance with FIG. 3a (the same as in the fuel injection valve 100) is shown enlarged in FIG. 3b. The hydraulic through-flow area of the passage 112a and the flats is substantially larger than the through-flow area of the injection hole 128. Further alternative embodiments can also be realized.
The plunger 108 has at its upper end an integral plunger piston 130 having a close sliding fit 130b with the valve housing 102. It should also be noted that the nozzle needle 122, the plunger 108, the needle lift stop 114, the spring 110 and the spring washer 112 can be installed in the fuel injection valve 100 from underneath. This is a very simple arrangement.
A second needle piston 132 is guided inside the valve housing 102 with a close sliding fit 132b. The piston 132 now presses on the upper end of the plunger piston 130. The diameter of the second needle piston 132 can, as an option, be the same size as the diameter of the plunger piston 130 or, as is shown in FIG. 3, it can be slightly larger. This fact can also be taken into account in the fuel injection valve 10 by selecting the diameters of the pistons 26b and 38.
A space 134, which has a low pressure level, is formed between the piston 132 and the piston 130. A relief hole 136 connects this space 134 with the space 74. The significance of this space 134 and this hole 136 is the same as that of the space 70 and the hole 72 of the fuel injection valve 10.
The mode of operation of the fuel injection valve 100 is very similar to that of the fuel injection valve 10. It must be noted that the end of the nozzle needle guide 124 coincides exactly with the upper end of the nozzle tip 118 at the contact surface with the intermediate plate 116. The lower part 108b of the needle plunger 108 is now somewhat shorter than the intermediate plate 116 and, specifically, by precisely the amount of the first lift H1.
At low (for example 200 bar) and medium (for example 400 bar) pressure level, the nozzle needle 122 and the needle plunger 108, together with the piston 132, will therefore only move by the amount of the first lift H1 until the stop surface 114b comes into contact with the stop surface 114a of the stop piece 114. In consequence, only the first lift H1 is traversed in the case of low to medium injection pressure level because the hydraulic opening force or control force is not sufficient to overcome the force of the spring 110.
At high pressure level (for example 1000 bar) in the fuel injection valve 100, the nozzle needle 122, with plunger 108, will move the stop piece 114 further until the stop surface 114c of the contact piece 114 comes into contact with the associated surface 114d in the housing 102 so that the second lift H2 is traversed.
In the designs of the fuel injection valves 10 and 100, the motion of the first lift H1 of the nozzle needles 26 and 122 is controlled by hydraulic forces only. The hydraulic pressure force in the control space 40 ensures that the nozzle needle 26 or 122 closes the seat 24a or 122a in a sealed manner when no injection is to take place. This is always the case during operation of the engine. After the engine is stopped, the hydraulic pressure in the fuel injection valves drops after some time to ambient pressure (approximately 1 bar).
Before renewed starting of the engine, a small hydraulic pressure of approximately 50 bar must be generated in the injection valves because otherwise the compression pressure in the engine cylinder or cylinders could open the nozzle needle(s) 26 or 122 by the amount of the first lift H1. Because of the possibly dirty state of the seat 24a or 122a, the required sealing would be impaired under certain circumstances.
If, in the case of certain applications, the generation of this minimum pressure is not possible before the engine starts, it is advantageous to hold the nozzle needle 26 or 122 of the fuel injection valves 10 or 100 closed mechanically. This could, for example, take place by means of a weak spring acting on the nozzle needle 26 or 122, this spring generating a closing force corresponding to a pressure of approximately 50 bar on the surface of the seat 24a or 122a. Such a spring is approximately 3 to 10 times weaker than the lift stop spring 66 or 110 of each fuel injection valve 10 or 100 and does not therefore impair the function of the fuel injection valves 10 and 100 of the present invention.
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A fuel injection valve for intermittent fuel injection into a combustion space of a combustion engine comprises an injection valve indirectly actuated electromagnetically by a hydraulic amplifier. The opening motion of the injection valve element remains limited at low and medium injection pressure, while the opening motion of the injection valve element is substantially more rapid and the opening path of the injection valve element substantially larger at high injection pressure than it is at low to medium injection pressure. It is possible to operate the engine over the complete load and rotational speed range under optimum injection conditions.
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CROSS REFERENCE TO RELATED CASES
This application is a continuation-in-part of U.S. application Ser. No. 11/375,128, filed on Mar. 15, 2006 now abandoned, and published as U.S. Publication No. 2006/0275270, which is a continuation-in-part of U.S. application Ser. No. 11/116,234, filed Apr. 28, 2005 now U.S. Pat. No. 7,855,074, and published as U.S. Publication No. 2005/0282148, which claims the benefit of priority of U.S. Provisional Application Ser. No. 60/565,846, filed Apr. 28, 2004, and U.S. Provisional Application Ser. No. 60/643,175, filed Jan. 13, 2005. This application is also a continuation-in-part of U.S. application Ser. No. 11/375,033, filed on Mar. 15, 2006 now U.S. Pat. No. 7,785,883, and published as U.S. Publication No. 2006/0270029, which is a continuation-in-part of U.S. application Ser. No. 11/116,234, filed Apr. 28, 2005 now U.S. Pat. No. 7,855,074, which claims the benefit of priority of U.S. Provisional Application Ser. No. 60/565,846, filed Apr. 28, 2004, and U.S. Provisional Application Ser. No. 60/643,175, filed Jan. 13, 2005. This application also claims the benefit of priority of U.S. Provisional Application Ser. No. 60/752,034, filed Dec. 21, 2005. This application further claims the benefit of priority of International Application No. PCT/US2005/014444, filed Apr. 28, 2005. Each of these applications is hereby incorporated by reference in their entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
This invention was made with government support under contract number NBCHC060058, awarded by the Defense Advanced Research Projects Agency, issued by the U.S. Army Medical Research Acquisition Activity, and administered by the U.S. Department of the Interior-National Business Center. The government has certain rights in the invention.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is directed to a method for constructing an integrated artificial human tissue construct system and, in particular, construction of an integrated human immune system for in vitro testing of vaccines, adjuvants, immunotherapy candidates, cosmetics, drugs, biologics, and other chemicals. The artificial immune system of the present invention is useful for assessing the interaction of substances with the immune system, and thus can be used to accelerate and improve the accuracy and predictability of, for example, vaccine, drug, biologic, immunotherapy, cosmetic, and chemical development.
2. Background of the Technology
Despite the advent and promise of recent technologies, including combinatorial chemistry, high-throughput screening, genomics, and proteomics, the number of new drugs and vaccines reaching the market has not increased. In fact, the attrition rate within drug discovery programs exceeds 90%.
The introduction of these new (and expensive) technologies has not reduced the lost opportunity costs associated with immunotherapy development; rather, these costs have increased. It is now estimated that almost $1 billion is required to bring a new drug to the market.
The development and biological testing of human vaccines has traditionally relied on small animal models (e.g., mouse and rabbit models) and then non-human primate models. However, such small animal models are expensive and non-human primate models are both expensive and precious. Furthermore, there are many issues regarding the value of such animal studies in predicting outcomes in human studies.
A major problem remains the translation from test systems (animal or 2-dimensional (2D) cell culture) to human immunology. Successful transfer between traditional testing systems and human biology requires an intricate understanding of disease pathogenesis and immunological responses at all levels.
The body's distributed immune system can be roughly divided into four distinct compartments: tissues and blood, mucosal tissues, body cavities, and skin. Because of ease of study, most is known about the tissue and blood compartment and its lymphoid tissues, the spleen and lymph nodes.
The largest compartment is the MALT (mucosa-associated lymphoid tissue). Mucosal surfaces serve a wide range of functions, including exchange of gases (lungs), nutrient transport (digestive tract), sensory surfaces (nose, mouth, throat), and reproductive signals.
Mucosal immunity is important for several reasons. First, the vast majority of human pathogens, including many of the leading infectious disease killers, initiate infections at mucosal surfaces, the largest routes of entry into the body. Additionally, stimulation of a mucosal immune response can result in production of protective B and T cells in both mucosal and systemic environments, so that infections are stopped or significantly hindered before they enter the rest of body. Significantly, bioterrorism relies on entry of agents through mucosal surfaces, where pathogens or toxins are primarily encountered, not as injections.
Because of its large surface area and exposure to the outside world, the mucosal system is also more vulnerable to infection than other body components (Newberry & Lorenz (2005) Immunol Rev 206, 6-21). As an example, the digestive tract has roughly 10 14 commensal organisms and frequently encounters pathogens. Furthermore, an additional challenge for the gut-associated lymphoid system is that typical food antigens should be tolerated while pathogenic antigens should induce vigorous immune responses. A hallmark of the mucosal immune system is the production of secretory immunoglobulin A (IgA). MALT plasma cells secrete primarily dimeric IgA in an IgA 1 :IgA 2 ratio of 3:2, whereas IgA secreted in the tissue and blood compartment is primarily monomeric IgA in an IgA 1 :IgA 2 ratio of 4:1. IgA 2 is more resistant to proteolysis by pathogens than IgA 1 (see, e.g., http://microvetarizona.edu/Courses/MIC419/Tutorials/bigpicture.html).
The mammalian immune system uses two general adaptive mechanisms to protect the body against environmental pathogens. When a pathogen-derived molecule is encountered, the immune response becomes activated to ensure protection against that pathogenic organism.
The first immune system mechanism is the non-specific (or innate) inflammatory response. The innate immune system appears to recognize specific molecules that are present on pathogens but not on the body itself.
The second immune system mechanism is the specific or acquired (or adaptive) immune response. Innate responses are fundamentally the same for each injury or infection; in contrast, acquired responses are custom-tailored to the pathogen in question. The acquired immune system evolves a specific immunoglobulin (antibody) response to many different molecules present in the pathogen, called antigens. In addition, a large repertoire of T cell receptors (TCR) is sampled for their ability to bind processed forms of the antigens bound to major histocompatibility complex (MHC, also known as human leukocyte antigen, HLA) class I and II proteins on the surface of antigen-presenting cells (APCs), such as dendritic cells (DCs).
The immune system recognizes and responds to structural differences between self and non-self proteins. Proteins that the immune system recognizes as non-self are referred to as antigens. Pathogens typically express large numbers of complex antigens.
Acquired immunity is mediated by specialized immune cells called B and T lymphocytes (or simply B and T cells). Acquired immunity has specific memory for antigenic structures; repeated exposure to the same antigen increases the response, which increases the level of induced protection against that particular pathogen.
B cells produce and mediate their functions through the actions of antibodies. B cell-dependent immune responses are referred to as “humoral immunity,” because antibodies are found in body fluids.
T cell-dependent immune responses are referred to as “cell-mediated immunity,” because effector activities are mediated directly by the local actions of effector T cells. The local actions of effector T cells are amplified through synergistic interactions between T cells and secondary effector cells, such as activated macrophages. The result is that the pathogen is killed and prevented from causing diseases.
The functional element of a mammalian lymph node is the follicle, which develops a germinal center (GC) when stimulated by an antigen. The GC is an active area within a lymph node, where important interactions occur in the development of an effective humoral immune response. Upon antigen stimulation, follicles are replicated and an active human lymph node may have dozens of active follicles, with functioning GCs. Interactions between B cells, T cells, and FDCs take place in GCs.
Various studies of GCs in vivo indicate that the many important events occur there, including immunoglobulin (Ig) class switching, rapid B cell proliferation (GC dark zone), production of B memory cells, accumulation of select populations of antigen-specific T cells and B cells, hypermutation, selection of somatically mutated B cells with high affinity receptors, apoptosis of low affinity B cells, affinity maturation, induction of secondary antibody responses, and regulation of serum immunoglobulin G (IgG) with high affinity antibodies. Similarly, data from in vitro GC models indicate that FDCs are involved in stimulating B cell proliferation with mitogens and it can also be demonstrated with antigen (Ag), promoting production of antibodies including recall antibody responses, producing chemokines that attract B cells and certain populations of T cells, and blocking apoptosis of B cells.
Similar to pathogens, vaccines function by initiating an innate immune response at the vaccination site and activating antigen-specific T and B cells that can give rise to long term memory cells in secondary lymphoid tissues. The precise interactions of the vaccine with cells at the vaccination site and with T and B cells of the lymphoid tissues are important to the ultimate success of the vaccine.
Almost all vaccines to infectious organisms were and continue to be developed through the classical approach of generating an attenuated or inactivated pathogen as the vaccine itself. This approach, however, fails to take advantage of the recent explosion in our mechanistic understanding of immunity. Rather, it remains an empirical approach that consists of making variants of the pathogen and testing them for efficacy in non-human animal models.
Given worldwide health problems caused by known and emerging infectious agents and even potential biological warfare pathogens, it is time for a fresh approach to understanding disease pathogenesis, the development and rapid testing of vaccines, and insights gathered from such work. Advances in the design, creation and testing of more sophisticated vaccines have been stalled for several reasons. First, only a small number of vaccines can be tested in humans, because, understandably, there is little societal tolerance for harmful side effects in healthy people, especially children, exposed to experimental vaccines. With the exception of cancer vaccine trials, this greatly limits the innovation that can be allowed in the real world of human clinical trials. Second, it remains challenging to predict which epitopes are optimal for induction of immunodominant CD4 and CD8 T cell responses and neutralizing B cell responses. Third, small animal testing, followed by primate trials, has been the mainstay of vaccine development; such approaches are limited by intrinsic differences between human and non-human species, and ethical and cost considerations that restrict the use of non-human primates. Consequently, there has been a slow translation of basic knowledge to the clinic, but equally important, a slow advance in the understanding of human immunity in vivo.
The artificial immune system (AIS) of the present invention can be used to address the inability to test many novel vaccines in human trials by instead using human tissues and cells in vitro. The AIS enables rapid vaccine assessment in an in vitro model of human immunity. The AIS provides an additional model for testing vaccines in addition to the currently used animal models.
Attempts have been made in modulating the immune system. See, for example, U.S. Pat. No. 6,835,550 B1, U.S. Pat. No. 5,008,116, WO 2004/101773 A1, Suematsu et al. ( Nat Biotechnol, 22, 1539-1545, (2004)), and U.S. Patent Application No. 2003/0109042.
Nevertheless, none of these publications describe or suggest an artificial (ex-vivo) human cell-based, immune-responsive system comprising a vaccination site (VS) and a lymphoid tissue equivalent (LTE). The present invention comprises such a system and its use in assessing the interaction of substances with the immune system.
SUMMARY OF THE INVENTION
The present invention provides an artificial immune system for assessing potential vaccine agents without administration to animal subjects. The artificial immune system comprises a 3D matrix comprised of lymphoid tissue (a lymphoid tissue equivalent) and populations of B cells and/or T cells distributed within the 3D matrix. Also distributed within the 3D matrix are dendritic cells.
The present invention also provides a means by which the state of maturation of the dendritic cells within the artificial immune system can be controlled.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 . The state of the DCs can dictate naïve T cell migration behavior. DCs prepared using human serum (HS DCs) or fetal bovine serum (FBS DCs) were introduced into collagen gel containing autologous, negatively selected T cells. Initially, T cells were uniformly distributed throughout the gel. However, by day 12, the distribution patterns were distinct. HS DCs caused T cells to distribute preferentially towards the top of the collagen, while FBS DCs induced migration to a lesser degree.
FIG. 2 . DCs prepared using human serum (HS DCs) or fetal bovine serum (FBS DCs) that had more of an immature or mature phenotype, respectively, were introduced into collagen gel containing autologous, negatively selected T cells. When tetanus toxoid-pulsed HS DCs or FBS DCs were introduced to the T cells, T cell proliferation was greater with FBS DCs than with HS DCs. Thus, the range of DC maturity states affects T cell activation and proliferation.
FIG. 3 . OT-II reporter T cell responses were robustly detected at frequencies of about 1 antigen-specific cell per 100 T cells, and were still detectable at frequencies of about 1 antigen-specific cell per 10,000 T cells.
Wild-type (C57Bl/6) or OT-II ovalbumin (ova)-specific CD4 + T cells were mixed with mature ova-pulsed DCs (T:DC ratio ˜10:1) in 96-well co-cultures. Proliferation and cytokine production were assayed after 3.5 days. The ratio of ova-specific OT-II T cells to wild-type cells was varied as shown. (A) CFSE dilution flow cytometry analysis. Undivided T cells have a fluorescence of ˜103 units. Nearly all of the antigen-specific OT-II cells have divided multiple times in all cultures. (B) IL-2 production detected in co-cultures in 96-well round-bottom plates or round-bottom plates with collagen gels.
FIG. 4 . Use of chemokine CCL21 to enhance the expansion of rare T cells in vitro. CCL21 chemokine enhances the expansion/survival of antigen-specific T cells in co-cultures, modeling rare, specific T cell-DC encounters.
FIG. 5 . ECM production by BLS4 lymph node stromal cells. Antibody ER-TR7 was used to detect an ECM protein produced by lymph node stromal cells; it is known to colocalize with fibronectin in intact lymph nodes.
FIG. 6 . Lymphocyte survival in vitro is enhanced by co-culture with BLS4 lymph node stromal cells. The graph shows number of live cells in control cultures (splenocytes alone) or splenocytes cultured on BLS4 monolayers over 11 days. Adding BLS4 cells resulted in ˜4-fold more surviving splenocytes after 11 days.
FIG. 7 . The ratio of immature to mature dendritic cells present in T-DC co-cultures impacts T cell proliferation and T cell survival.
FIG. 8 . BLS4 stromal cells form reticular networks in protein-conjugated inverse opal scaffolds.
(A) and (B) Stromal cells observed immediately after injection into scaffolds (a few cells are highlighted by false-color overlays). Note the initially rounded morphology.
(C) and (D): After 24 hrs, BLS4 cells have attached to the scaffold and formed numerous intercellular connections stretching over and across pores of the scaffold. Shown are fluorescence micrographs taken through midplanes of two regions of scaffold layers (red=stromal cell f-actin, blue=cell nuclei, green=protein-conjugated scaffold surfaces).
FIGS. 9A-D . Immature population of reverse-transmigrated DCs from the vaccination site membrane (VSM) or the vaccination site cushion (VSC) is shown as CD83 + with few HLA-DR + and CCR7 + observed. CD14 is slightly decreased in VSM compared to VSC. These are for phenotypes before maturation signals are provided (e.g., TNFα).
FIGS. 10A-H . After maturation with Candida albicans /tetanus toxoid antigens/KLH and TNFα, there was an increase in the number of cells that are high in CD14 + and HLA-DR. Additionally, some of these cells are expressing more CD83 + /HLA-DR + /CCR7 + after antigen priming.
DETAILED DESCRIPTION OF THE INVENTION
The present invention concerns the development of accurate, predictive in vitro models to accelerate vaccine testing, allow collection of more informative data that will aid in redesigning and optimizing vaccine formulations before animal or clinical trials, and raise the probability that a vaccine candidate will be successful in human trials. More specifically, the present invention comprises controlling the maturation state of the dendritic cells (DCs) in the lymphoid tissue equivalent (LTE, artificial lymph node) of the artificial immune system (AIS), because the state of DC maturation appears to impact their behavior there.
Tissue engineering involves the development of synthetic or natural materials or devices that are capable of specific interactions with cells and tissues. The constructs combine these materials with living cells to yield functional tissue equivalents. Tissue engineering involves a number of different disciplines, such as biomaterial engineering, drug delivery, recombinant DNA techniques, biodegradable polymers, bioreactors, stem cell isolation, cell encapsulation and immobilization, and the production of 2D and 3D scaffolds for cells. Porous biodegradable biomaterial scaffolds are required for the 3D growth of cells to form the tissue engineering constructs. There are several techniques to obtain porosity for the scaffolds, including fiber bonding, solvent casting/particulate leaching, gas foaming/particulate leaching, and liquid-liquid phase separation. These produce large, interconnected pores to facilitate cell seeding and migration. As used herein, the terms “tissue-engineered construct” or “engineered tissue construct” (“ETC”) include any combination of naturally derived or synthetically grown tissue or cells, along with a natural or synthetic scaffold that provides structural integrity to the construct.
It is known that 3D biology is important to induce proper functionality of immunological ETCs (see, e.g., Edelman & Keefer, Exp. Neurol. 192, 1-6 (2005). A principal approach to studying cellular processes is to culture cells in vitro. Historically, this has involved plating cells on plastic or glass supports. Cells grown on solid or filter support are referred as two-dimensional (2D) cultures. Such 2D cultures on porous supports have been extremely useful for studying many aspects of biology. However, much more in vivo-like conditions can now be realized in 3D cultures. For example, many epithelial cells, both primary cultures and established lines, form complex epithelial structures when grown in 3D ECM.
Recently, in model in vitro lymph nodes, it has been shown that 3D interstitial tissue matrix facilitates not only T cell migration toward an APC, but also supports motility upon cell-cell interaction. A 3D collagen matrix environment, because of its spatial architecture, provides traction for lymphocyte crawling, mimicking some structural features of the lymph node cortex. This provides experimental justification for the importance of a 3D environment in the constructs that comprise the in vitro immune system.
The artificial immune system (AIS) of the present invention comprises a three-dimensional matrix comprised of lymphoid tissue. The matrix comprises a material selected from gelatin, collagen, synthetic ECM materials, PLGA, PGA, natural ECM materials, chitosan, protosan, and mixtures thereof. Distributed within the matrix comprising the lymphoid tissues are populations of at least one of B cells or T cells. Dendritic cells (mature and/or immature) are also distributed within the matrix.
Immature DCs (iDCs) and macrophages in the collagen cushion with naïve T cells tend to segregate the T cells into “zones” or clusters. An explanation may be that local chemokines and/or cytokines (such as CCL-21 and CXCL13) released from these APCs tend to act like “chemorepellants,” helping to organize the T/B cell zones in a 3D matrix similar to what is seen in lymph nodes in vivo.
Mature DCs in the collagen cushion release cytokines and/or chemokines (such as CCL-21 and CXCL13) and activate naïve T cells to proliferate and secrete cytokines. Thus, the state of APC differentiation in the model lymph node appears to affect the lymph node architecture and activation of lymphocytes.
The present invention comprises methods to modulate the state of antigen-presenting cells (APCs), including dendritic cells (DCs). More specifically, the present invention includes methods of modulating the state of APCs (e.g., DCs) in the artificial immune system (AIS). The AIS of the present invention supports in situ priming of both naïve T and B cells and subsequent interactions between activated antigen-specific helper T cells and B cells to promote B cell expansion, antibody class switching, and somatic hypermutation. Thus, the maturation state of the dendritic cells in the AIS of the present invention can be controlled, for example, by the choice of culture medium, by the choice of serum added to the culture media ( FIGS. 1 , 2 ), by the addition of cytokines and/or chemokines added to the culture media ( FIG. 4 ), or by the use of cells from a vaccination site.
The vaccination site (VS) is an in vitro skin and/or mucosal-equivalent scaffold that facilitates trafficking of blood monocytes and non-monocytic dendritic cell (DC) precursors and supports their natural conversion into mature antigen presenting dendritic cells within the artificial skin 3D tissue-engineered construct. Such a vaccination site will act as a skin-, gut-, or mucosal-equivalent tissue and comprises a skin construct (or a mucosal tissue, such as lung), together with vascular and lymphatic endothelium and blood-derived hematopoietic cells.
The skin construct can be derived from many sources, including complex sources, such as cadaveric human skin, less complex sources, such as commercially available skin-like products (EpiDerm, Episkin), or simple skin-like structures (using many different preparations of ECM and sources of skin fibroblasts and keratinocytes) optimized for integration into the in vitro system.
Blood cells (including monocytes) can be placed along the vascular endothelium. Such cells naturally migrate, convert to dendritic and other cells, and become resident in the skin.
If dendritic cells are present in the correct subtype and state of maturation for resting skin, the vaccination site is then ready to accept a vaccine candidate for testing. Upon vaccination, the vaccine will interact with skin-resident cells to induce further migration of monocytes and other cells into the skin, and their subsequent differentiation into more antigen-presenting cells (APCs), including macrophages and dendritic cells. Dendritic cells (DCs) and other antigen-presenting cells (APCs) pick up vaccine antigen and can be transferred to the lymphoid tissue equivalent (LTE). DCs in the LTE interact with T and B cells to initiate an adaptive immune response, and depending on the maturation state of the DCs, they will activate T and B cells to differing extents.
A step-wise approach to a VS is to build a 3D structure that comprises vascular and lymphatic endothelial cells that can support transendothelial trafficking of monocytes and other DC precursors in a manner that recapitulates in vivo differentiation, maturation and migratory functions.
It is known that a 3D tissue construct that permits heterologous cell-cell interactions impacts the differentiation of DC precursors, including monocytes, in a manner that more closely mimics an intact human system than is observed in 2D culture (see, e.g., Edelman & Keefer, Exp. Neurol. 192:1-6 (2005)). Specifically, co-culture of whole PBMCs with vascular endothelial monolayers, grown on either reconstituted type I collagen matrices (Randolph, et al., Blood 92: 4167-4177 (1998a); Randolph, et al., Science 282:480-483 (1998b); Randolph, et al., Proc. Natl. Acad. Sci. USA 95:6924-6929 (1998c); Randolph, et al., J. Exp. Med. 196:517-527 (2002)) or native amniotic connective tissue (Randolph & Furie, J. Exp. Med. 183:451-462 (1996)) promotes the passage particularly of monocytes across the endothelium, largely in response to endogenous production of the chemoattractant monocyte chemoattractant protein (MCP)-1 (CCL2) (Randolph & Furie, J. Immunol. 155:3610-3618 (1995)). This is consistent with the knowledge that many monocytes leave the blood each day, under normal steady state conditions. When the endothelium is activated, other inflammatory cell types, such as neutrophils, can traverse the endothelium, again with the same regulatory events that are understood to operate in vivo (Furie & McHugh, J. Immunol. 143:3309-3317 (1989)). If the fate of monocytes is followed with time in endothelial cell/collagen cultures, it becomes apparent that a substantial fraction of monocytes increase production of a range of molecules (including MHC II, CD40, CD83, CD86) known to be upregulated in DCs and these cells also acquire migratory properties such that they migrate out of the cultures, crossing the endothelium in the ablumenal to lumenal direction, away from the vascular endothelium and away from the macrophages that remain resident in the subendothelial matrix.
As shown in FIG. 10A of U.S. Appln. Publication No. 2005/0282148, vascular endothelial cells grown on 3D constructs of fibronectin-coated collagen form intercellular junctions that remain intact after passage of monocytes into subendothelial matrix to increasing depths (arrowheads, monocytes visualized by differential interference contrast microscopy). En face views and a cross-section of the cultures are shown, where emigrated leukocytes are distributed throughout the matrix under the characteristically flat endothelial monolayer. As described in design features 1 and 2, a lymphatic endothelial monolayer or an epidermal monolayer, respectively, on the currently bare lower surface of such a matrix. FIG. 10B is a schematic diagram showing the stages of monocyte behavior in such a 3D culture. The image on the left depicts the sequence of observations when the matrix does not contain a source of microbial antigen, whereas the images on the right depict the sequence of observations made when yeast particles (zymosan) are incorporated as a model microbial antigen in the matrix. In stage I, incubation of peripheral blood mononuclear cells (PBMCs) are incubated with endothelium for 1.5 hours results in the transmigration of most monocytes (3), some BDCA1+ blood dendritic cells (data not shown), natural killer cells (Berman et al., J. Immunol. 156:1515-1524, (1996)), but few lymphocytes, into the subendothelial collagen. Of the few lymphocytes that do migrate, these are likely of a memory phenotype (Gergel & Furie, Infect. Immun. 69:2190-2197, (2001)), consistent with our understanding that naive T cells traffic into lymph nodes directly and memory T cells can enter tissues. In stage II, the cell culture is washed, and monocytes accumulated in the subendothelial matrix are left with an intact endothelial monolayer, where the monocytes engulf phagocytic particles if such particles have been included in the collagen matrix. In stage III, some of the phagocytic monocyte-derived cells retraverse the same endothelium and accumulate in the apical compartment. These reverse-transmigrated monocytes previously or simultaneously differentiate into DC. Photographs (upper right, B) show their characteristic morphology. When no activation stimuli are included in the cultures (left), the reverse-transmigrated cells are immature DCs and promote T cells to produce IL-10 as observed by intracellular cytokine staining. Many of these cells are non-adherent, like DCs, but a few spreading cells are similar to less differentiated monocytes (left photo inset, B). When activation stimuli are included in the cultures, the reverse-transmigrated cells become mature DCs and promote development mainly of IFNy producing T cells.
As it is now possible to differentially isolate vascular and lymphatic endothelium (Podgrabinska, et al., Proc. Natl. Acad. Sci. USA, 99:16069-16074 (2002)), and given the knowledge and resources for preparing these cells, a functional VS comprising vascular and lymphatic endothelial cells can be constructed. The vascular and lymphatic endothelial cells support transendothelial trafficking of monocytes and other DC precursors in a manner that recapitulates in vivo differentiation and migratory functions. Several matrices can be used, including xenographic ECM sheets, natively polymerized human amniotic connective tissue (Randolph & Furie, J. Exp. Med. 183:451-462 (1996)), reconstituted collagen matrices, protasan/collagen membrane scaffolds, or preferably matrices that contain fibroblasts and/or mast cells. Several commercial preparations of dermal tissues containing fibroblasts are available and these are readily prepared in vitro, for example by seeding fibroblasts with matrix components and allowing the fibroblasts to modify and contract these components, as described earlier.
It is anticipated that the process of incorporating cells within the matrix could be adapted for the incorporation of a variety of cells such as fibroblasts or mast cells. In a preferred embodiment, vascular and endothelial monolayers are constructed that mimic the normal physiology of these vessels in coordinating recruitment and trafficking of immune cells during immunization. In another embodiment, the endothelium can be derived from human foreskin (Podgrabinska, et al., Proc. Natl. Acad. Sci. USA, 99:16069-16074 (2002)) or from adult skin.
The present invention comprises co-culture conditions to mimic the expansion of antigen-specific lymphocyte populations observed in vivo. It is a challenge to mimic the robust expansion of antigen specific T cells from their rare initial population to the significant numbers present during the peak of in vivo immune responses. Such expansion can be dramatic in vivo; for example, in experimental lymphocytic choriomeningitis virus infection in mice, 100-200 naïve T cells specific for one antigen transiently expand to ˜10 7 effector T cells, an expansion of about 50,000-fold (Blattman et al. (2002) J Exp Med 195, 657-664).
Furthermore, this is more rigorous than simply expanding T cells to a detectable population that could be correlated with a particular antigenic stimulation.
It requires that the cells, in fact, expand to a population size comparable to that observed in vivo to provide physiologic help for CTL and B cell priming.
The present invention comprises strategies comprising varying the cellular composition and presence of cytokines and/or chemokines in in vitro T cell cultures to better mimic the in vivo environment. These strategies enhance the expansion and survival of T cells primed under conditions of rare antigen-specific T cell-dendritic cell encounters.
In embodiments of the present invention, the cells are grown in dense co-cultures prepared in 96-well culture plates, to facilitate automation and rapid assessment of outcomes. Embodiments of the present invention include strategies to magnify the numbers of T cells expanded in single-step in vitro cultures. The strategies described can be implemented in a range of LTE formats, including inverse opal scaffolds, collagen matrices, and traditional well-format plate cultures.
The practice of the present invention will employ, unless otherwise indicated, conventional methods of immunology, histology, microbiology, cell and tissue culture, and molecular biology within the ordinary skill of the art. Such techniques are explained fully in the literature. All publications, patents, and patent applications cited herein are incorporated by reference in their entirety.
EXAMPLES
Example 1
Detection limits with antigen-specific reporter cells. We developed a system to track rare antigen-specific T cells mixed with dilute antigen-presenting dendritic cells (DCs), as a means to define culture conditions for T cell priming in vitro. We used a murine transgenic CD4 + T cell (OT-II, which recognizes peptides from ovalbumin (ova)) for this purpose, to identify general culture conditions that can be applied to both the mouse and human systems. In this example, to mimic the rare occurrence of antigen-specific T cells, these ‘reporter’ cells were mixed with varying ratios of wild-type C57BL/6 CD4 + T cells, and bone marrow-derived dendritic cells. Cultures were prepared with a fixed ratio of T cells to DCs of ˜10:1, approximately matching the ratio of these cells in lymph nodes in vivo. An advantage of this system is that it allows quantitative labeling, isolating, and identifying antigen-specific cells in these cultures at all times, which is simply not possible in vivo.
We tested whether we could detect antigen-specific T cell priming at T cell dilutions approaching the in vivo frequency of mouse and human naïve T cells.
OT-II ova-specific T cells were labeled with the fluorescent dye CFSE (used to track cell proliferation; each time a cell divides, its fluorescence is halved). OT-II T cells, wild-type T cells, and ova-pulsed mature DCs were mixed and cultured for 3.5 days.
As shown in FIG. 3A , when OT-II T cells make up 10% of the T cells in the co-culture (red curve), numerous rounds of cell division were detected, as indicated by the multi-peaked histogram. Undivided cells in this experiment had a fluorescence of ˜103 units; thus nearly all the antigen-specific cells have divided several times.
As shown in the other curves, significant numbers of OT-II T cells that had proliferated were still detected when they made up only about 1% of the T cell population, and further, detectable OT-II cells were found even when their frequency was only ˜1 in 10,000 among the T cells initially added to the culture. Measurement of IL-2 production ( FIG. 3B ) and interferon-γ (IFN-γ) production (data not shown) showed a dose-dependent response that decayed as the number of OT-II cells present declined.
Thus, this system allows the mimicking of rare antigen-specific T cell encounters, even with precursor T cell frequencies similar to the rarity of natural naïve T cells in vivo.
Example 2
When we compared T cell priming in dense 96-well cultures (2×10 5 to ˜5×10 5 cells per well) to priming in collagen gels also prepared in 96-well plates, IL-2 production was about 50% of the level seen in the no-matrix case. This result is consistent with published data on T cell priming in collagen (Gunzer et al. (2000) Immunity 13, 323-332) and may reflect slower migration of T cells through the matrix in their search for antigen-bearing DCs, relative to the cells-only aggregates formed in no-matrix cultures.
Example 3
In another embodiment of the present invention, the strategy to enhance expansion of rare T cells in vitro comprises T cell-dendritic cell co-cultures, comprising a mixture of immature and mature DCs, to enhance the proliferation and survival of antigen-specific T cells. Immature DCs also aid in zone formation typical of in vivo lymph nodes (see FIG. 1 ). The collagen matrix model has enabled us to show basic results that suggest the maturation state of the DC may impact its behavior in the lymph node. Immature DCs/macrophages in the collagen cushion with naïve T cells tend to segregate the T cells into “zones” or clusters. One possible explanation is the local chemokines released from these APCs tend to act like “chemorepellants” helping to organize the T/B cell zones in a 3D matrix similar to that found in the lymph node. Mature DCs in the collagen cushion with naïve T cells activate these T cells to proliferate and secrete cytokines. Thus, the state of APC differentiation in the lymph node appears to assist in the formation of the lymph node architecture, or activation of lymphocytes.
Example 4
Phenotypic and Functional Characterization of RT-DCs
To examine the determination of functional capacity and phenotypic characteristics of the vaccination site, experiments were conducted to examine markers of DC differentiation and maturation. The phenotypic markers used to characterize cells related to the VS were the macrophage profile (CD68, CD206, CD36, CD205, CD209), DC profile (CD83, CD1a, CD205, CD207, CD208, CD209), maturation status profile (HLA-DR, CD40, CD80, CD86 CD16, CD32, CD64), chemokine receptor profile (CCR7, CCR2, CXCR4, CXCR5, CCR6), lineage profile (CD56, CD3, CD19, CD14, CD31, CD144) and survival markers such as annexin V or 7AAD. Reverse transmigrated DCs (RT-DCs) were generated from the vaccination site collagen membrane and collagen cushion modules, presented with antigens (Candida albicans, tetanus toxoid combination, KLH), and driven to maturity with TNFα ( FIGS. 9 , 10 )
Example 5
Creation of lymph node-like stromal cell networks in the LTE and their impact on lymphocyte function. ECM production by BLS4 cells: Creation of 3D reticular structures by lymph node stromal cells cultured in 3D inverse opal LTE scaffolds
In addition to secreting factors that support lymphocyte survival and/or priming, lymph node stromal cells likely assist in providing the physical network in 3D cultures to support T cell and DC motility and subsequent interactions ( FIG. 6 ).
When BLS4 (murine) stromal cells are placed in standard 2D culture plates, they spread to form confluent layers typical of fibroblasts ( FIG. 8 ) However, when BLS4 cells were injected into fibronectin/laminin-conjugated inverse opal LTE hydrogel scaffolds, their behavior and morphology were entirely different. Immediately after injection, the cells were rounded and situated within the void spaces of the scaffold ( FIG. 8 ). Within 1 hr, we observed the cells attaching, spreading, and forming numerous intercellular connections spanning multiple pores of the scaffold in all three dimensions. After 24 hrs, cells in scaffolds were fixed and stained with fluorescent markers for f-actin and cell nuclei to visualize the cells in 3D.
As can be seen in FIGS. 5 and 8 , extensive cell-cell 3D interconnections similar to the 3D web-like nature of the natural stromal network in lymph nodes were evident.
In an experiment where stromal cells, lymphocytes, and dendritic cells were ‘re-aggregated’ in culture without scaffolds to guide the stromal cell assembly, we observed lymphocytes with highly extended lamellipodia in fixed samples, suggesting that co-culture with stromal cells strongly influences lymphocyte attachment and polarization.
Example 6
OT-II and wild-type T cells (at a ˜1:10 ratio) were mixed with DCs (total T:DC ratio ˜10:1) in 96-well plate co-cultures and the ratio of immature to mature ova protein-pulsed DCs was varied. OT-II T cell proliferation was tracked by CFSE dilution. Surprisingly, significantly greater T cell proliferation/survival was found when the ratio of immature to mature DCs was ˜1:1, with fewer DCs initially bearing antigen than in the ˜1:10 iDC:mDC case ( FIG. 7 ).
The above description and examples are for the purpose of teaching the person of ordinary skill in the art how to practice the present invention, and it is not intended to detail all those obvious modifications and variations of it that will become apparent to the skilled worker upon reading the description. It is intended, however, that all such obvious modifications and variations be included within the scope of the present invention, which is defined by the following claims. The claims are intended to cover the claimed components and steps in any sequence which is effective to meet the objectives there intended, unless the context specifically indicates the contrary.
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The present invention relates to methods of constructing an integrated artificial immune system that comprises appropriate in vitro cellular and tissue constructs or their equivalents to mimic the normal tissues that interact with vaccines in mammals. The artificial immune system can be used to test the efficacy of vaccine candidates in vitro and thus, is useful to accelerate vaccine development and testing drug and chemical interactions with the immune system.
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BACKGROUND AND SUMMARY OF INVENTION
The present invention relates to an automatically operating apparatus for feeding one or more elongate workpieces, such as strip-metal, tubular sections or profiled sections, to one or more working machines, for example shearing machines, punching machines, stamping machines, drilling machines and/or welding machines. The feeding apparatus is constructed for intermittently feeding stepwise an elongate workpiece along a given path and comprises, inter alia, a fixed and a movable clamping element. The workpiece is clamped in the movable clamping element and moved thereby to the working machine, with the fixed clamping element out of engagement with said workpiece. When the grip of the movable clamping element is released and said element is withdrawn, the workpiece is released therefrom and the fixed clamping element is moved into engagement with said workpiece. The length of the path of movement of said elongate workpiece is determined by limit switches arranged at respective ends thereof.
Known feed mechanisms of the aforedescribed kind are encumbered with a number of disadvantages. For example, the clamping force exerted by the movable clamping element is not always satisfactory. Further, since the aforementioned limit switches are not normally provided with the feeding apparatus when purchasing the same, they must be bought separately and installed by the customer, thereby complicating the process of setting those feeding apparatus available on the market at present to the correct length of feed stroke.
One object of the present invention is to provide a novel feeding apparatus of the aforedescribed kind which is reliable in operation and with which the length of feed stroke can be readily adjusted, and with which said length of feed stroke can be finely adjusted while the apparatus is in operation. A further object of the invention is to provide a feeding apparatus which, while operating at a high speed, requires the minimum of energy, and which can be readily adapted to work with different working machines.
Accordingly the present invention comprises an apparatus for intermittently feeding elongate workpieces stepwise in the direction of their longitudinal axis along a given path, said apparatus including a frame structure having a drive unit and a fixed clamping element; a further clamping element arranged for movement along said path, said further clamping element being so arranged that it will advance the workpiece when moving in one direction but will not move said workpiece when moving in the opposite direction, characterized in that the movable clamping element is connected, through a piston rod, to a piston which, in the direction of said movement path, cooperates with a pressure cylinder having a rear end plate which is displaceably arranged in said cylinder so as to alter the volume thereof and therewith the length of stroke of the movable clamping element; and in that a clamping ring which is displaceable on said cylinder is arranged to be clamped around the cylinder in a manner such as to compress the same around said end plate for fixing said plate in the desired position along the length of the cylinder.
BRIEF DESCRIPTION OF THE DRAWINGS
An exemplary embodiment of the invention will now be described with reference to the accompanying drawings, in which
FIG. 1 is a side view of the feeding apparatus,
FIG. 2 is a plan view of said feeding apparatus,
FIG. 3 is an axial sectional view through said end plate taken along line III--III,
FIG. 4 is a horizontal sectional view taken along line IV--IV through the fixed clamping element and through an adjustable abutment by means of which fine adjustment of the length of stroke of said feeding apparatus is effected, and
FIGS. 5, 6 and 7 illustrate alternatives for roughly setting the length of stroke of the movable clamping element.
DETAILED DESCRIPTION OF THE INVENTION
Mounted on a frame structure 1, which is located adjacent a working machine (not shown), is an attachment means 2 for a drive unit 3, and a fixed stationary clamping element 4. The attachment means 2 and the clamping element 4 are connected together by means of two mutually parallel guides 6 which extend in the direction of feed 5, on which guides 6 a clamping element 7 is sideably mounted for reciprocatory movement.
A cylinder 8 is mounted on one end in the attachment means 2 in a manner such that said attachment means serves as the front end wall of the cylinder. Arranged for movement in the cylinder 8 is a piston 9 which is connected to the movable clamping element 7 through a piston rod 10. The active volume of the cylinder is determined by a rear end plate 11 which is arranged for movement in said cylinder and which is held in a selected position therealong by means of a clamping ring 12 extending around said cylinder, said clamping ring being arranged to be moved along the cylinder to a position in register with the selected position of the end plate 11, whereafter the clamping ring 12 is tightened around the cylinder by means of a clamping device, such as a knot-and-bolt arrangement 13. The cylinder is compressed in this way around the end plate 11, to secure the same in the position to which it has been moved. The clearance between the peripheral surface of the end plate and the inner wall of the cylinder is minimal, and hence the wall of the cylinder need not be compressed to any great extent in order to securely hold the end plate 11. In order to prevent the end plate 11 from being unintentionally removed from the cylinder, the rear end of the cylinder 8 is provided with a screw-threaded hole into which a screw 14 is screwed so as to project into the rearward path of the end plate 11. Alternatively, a circlip can be arranged internally of the cylinder.
An elongate workpiece A is progressively advanced intermittently in its longitudinal direction by causing the movable clamping element 7 when located in a withdrawn position, i.e. the rearward limit position of said element, to grip the workpiece and to move said workpiece during forward movement of said clamping element in the direction of feed 5, to a forward limit position. During this feeding stroke, the workpiece passes freely through the fixed clamping element 4, although said fixed clamping element also grips the workpiece when said forward limit position is reached, whereafter the movable clamping element releases its grip on the workpiece and is returned to its rear limit position. The movable clamping element then re-grips the workpiece, whereupon the grip of the fixed clamping element is relinguished and the feeding movement repeated. The feeding movement of the movable clamping element 7 is effected by supplying air under pressure to the cylinder 8 through a passage 16 arranged in the end plate 11, the piston 9 being moved in the feed direction 5 and the movement of said piston being transmitted to the movable clamping element via the piston 10. Return movement of the movable clamping element is effected in a similar manner, by supplying air under pressure to the cylinder 8 through a passage 15 in the attachment means 2.
As will best be seen from FIG. 3, in addition to including the passage 16 for supplying air to the cylinder 8 and for venting said cylinder, the displaceable end plate 11 is also provided with a sealing ring 17, a regulateable damping means 18 and a reversing valve 19 having a compression spring 20. The said end plate 11 also includes a connection 21 for connecting said plate to a source of air under pressure, a signal-air connection 22 and a venting passage 23 for said signal-air to effect a given function thereof. By signal air is meant an air signal to the control means. As will be understood, the end plate 11 constitutes a means for stopping the movement of the piston 9 in its return stroke, and hence the position at which the end plate is fixed in the cylinder defines the rearward turning or limit position of the movable clamping element 7. The damping means 18 dampens the movement of the piston at the end of its rearward stroke, in order to soften the contact of the piston with said end plate.
The reversing valve 19, which is arranged for axial displacement in the end plate 11, is spring-biassed and compressed-air biassed in a direction towards the piston 9. The pressure spring 20 is arranged to compensate the compressed air in the cylinder, so that the valve can not be opened when compressed air is supplied to the cylinder through the passage 16.
At the end of its return stroke, and immediately before contacting the end plate 11, the piston 9 strikes the reversing valve 19, which is then displaced to the left in FIG. 3 to an open position. Air under pressure then passes the left part of the valve and out through the signal-air connection 22, to a control unit 24 for reversing the direction of movement of the piston. Compressed air is then passed through the passage 16 to the cylinder 8, while air is ventilated through the passage 15 in the attachment means 2. The signal-air line is evacuated through a passage 23.
Because the displaceable end plate 11 includes air-supply means, damping means and said reversing valve, and, at the same time, serves as stop means for rearward movement of the piston, it is a simple matter to alter the length of stroke of the feeding apparatus. All that is required in order to set the apparatus ready for use is to loosen the nut-and-bolt arrangement 13 and to move the end plate 11 (and the clamping ring 12) to the desired position along the cylinder 8, and then tighten said screw and nut arrangement. At the same time an optimal volume of the cylinder is obtained, since the top-dead-centre of the piston is at the end plate 11.
The fixed clamping element 4 forms a stop for the feed stroke of the movable clamping element 7 and thus also for the movement of piston 9 to the right cylinder 8 as seen in FIG. 1.
Arranged in the fixed clamping element 4 is a damper means 25 whose damping effect can be adjusted by means of a device 26, and an axially movable abutment 27. The fixed clamping element 4 is also provided with a horizontal, rectangular recess 28 which accommodates two mutually co-operating wedges 29 and 30. One of said wedges 29 is connected to the abutment 27. The other of said wedges, 30, is provided with a screwthreaded bore 31, in which a meshing peg 32 is screwed. The peg is also pivotally mounted on the clamping element 4 and is provided with a flange 33 which, together with a plate 34 mounted on said fixed clamping element, prevents axial movement of the peg. A setting wheel or knob 35 is mounted on the free end of the peg 32, and the fixed clamping element 4 exhibits a scale 36 which shows the setting of the knob or wheel 35. The wedge 30 can be displaced in the longitudinal direction of the peg by rotating the knob or wheel 35. The wedge 29 transmits movement of the wedge 30 to the abutment 28, thereby adjusting the setting of said abutment.
Referring to FIG. 2 the movable clamping element 7 includes a shoulder 37, and a further shoulder 38 having arranged therein a bore (not shown). Arranged in the bore within the movable clamping element is an axially displaceable reversing valve 39. The reversing valve 39 is of similar construction to the reversing valve 19 in the displaceable end plate 11. Since the valve 39 is not subjected to any counter pressure, it has not been provided with the pressure spring 20. A signal-air line 40 connects the reversing valve 39 to the control unit 24.
At the end of a feeding stroke, the shoulder 37 of the movable clamping element 7 comes into contact with the damper 25, thereby damping the movement of said clamping element. The reversing valve 39 contacts the abutment 27, causing the reversing valve to be moved to the left in FIG. 2 to an open position. Air under pressure then passes out through the signal-air line 40 to the control unit 24, for reversing the direction of movement of the piston. Air under pressure is then supplied to the cylinder 8 through the passage 15 in the attachment means 2, while air is permitted to escape through the passage 16 in the end plate 11.
The length of stroke of the apparatus can be finely adjusted by adjusting the forward limit position of the movable clamping element 7, this being effected by displacing the abutment 27 in its longitudinal direction, by turning the setting knob 35. As indicator on the knob 35 moves along a scale 36 to show the setting of the abutment 37. The design of the fine-adjustment means enables the length of stroke of the feeding apparatus to be finely adjusted while the apparatus is in operation.
To enable the length of stroke of the apparatus to be roughly set a measurement scale 41 is arranged on the frame structure parallel to the guides 6, said rough setting being effected by adjusting the rear limit position of the movable clamping element 7. The adjustment can be effected by providing the movable clamping element with an indicating means, for example a needle 42, which is moved along the scale as the clamping element is moved. The position of the clamping element is read-off on the scale by means of the needle. A corresponding scale 43 is provided on the cylinder 8. When the clamping element is set to the desired position, the end plate 11 is displaced so that it contacts the piston 8. The clamping ring 21 is then positioned with the aid of the scale 43 on the cylinder 8, so that it adopts a position in which it is located around the cylinder and the end plate 11, whereafter the nut-and-bolt arrangement 13 is tightened.
Alternatively, as illustrated in FIG. 5, a structure 44 of substantially U-shaped configuration when seen in cross-section can be used for setting the clamping ring 12, instead of the scale 43. The structure 44 is pivotally arranged for displacement along the scale 41 in a plurality of spaced-apart sleeves 45 welded on the frame structure 1, and having a length between the forward leg 46 and the rearward leg 47 of said U-shaped structure which corresponds approximately to the sum of the thickness of the movable clamping element, the length of the piston rod 10, the thickness of the piston 9 and the thickness of the end plate 11. The positional setting of the clamping ring 12 on the cylinder 8, for roughly setting the length of stroke of the apparatus in accordance with the above, is effected by displacing the leg 46 of the substantially U-shaped structure 44 along the scale 41 to a desired rearward limit position for the clamping element 7. The clamping element is then moved from a rearward position to a position in which its leading surface is in contact with the uppraised leg 46 of the structure 44. The rearward leg 47 of said structure then rests against the cylinder 8, and when displacing the clamping ring 12 rearwardly into contact with the leg 47, a correct position of the clamping ring is obtained. The use of a substantially U-shaped structure 44 instead of duplicating the provision of scales for setting the clamping ring to the desired position eliminates any risk of error in the setting of said ring.
A further embodiment of a device for roughly setting the length of stroke of the apparatus is illustrated in FIG. 6. This device comprises a stirrup-like structure generally shown at 57 having legs 58 and 59 of approximately equal length and displaceably arranged in the attachment means 2. One leg, 58, is provided with a measurement scale 60 and is attached to the ring 12. The other leg, 59, extends through a bore in the attachment means 2. One leg, 58, is provided with a measurement scale 60 and is attached to the ring 12. The other leg, 59, extends through a bore in the attachment means 2 and in the piston 9 and is connected to the end plate 11, said bore being provided with a seal (not referenced). In order to set the apparatus to a desired working stroke, the clamping ring is moved to a desired position along the cylinder 8, while using the scale on the leg 58, thereby moving at the same time the end plate 11, which as a result of the construction of the stirrup-like structure is always located in register with the clamping ring 12. As will be understood, the scale 41 arranged on the frame-structure is unnecessary.
It is also possible to modify the apparatus described above in a manner such that only one leg 58 provided with a scale is necessary, in which case said structure has a length which corresponds approximately to the length of the stroke of piston rod 10, the thickness of the piston 9 plus half the thickness of the end plate. The length of stroke of the apparatus is set by means of the scale 60, whereafter the leg 58 is locked in the attachment means 2 and the movable clamping element 7 is moved into contact with the free end of said leg. The end plate 11 is then brought into contact with the piston 9, and the nut-and-bolt arrangement 13 of the clamping ring tightened.
In accordance with a best mode, FIG. 7, however, rough setting of the length of stroke of the movable clamping element 7, is effected by a sleeve-like element generally shown at 70, said element including an outer sleeve 71 and an end piece 72. The inner extremity of the sleve 71 is fixed in the clamping ring 12, so that axial movement of the sleeve 71 results in similar movements of said ring. Extending between the end piece 72 and the end plate 11 is a distance element 73, said element being fixed to said plate and said end piece, so that axial movement of said distance causes the end plate to be moved through a corresponding distance. The clamping ring 12 has mounted thereon in a manner similar to the FIG. 6 embodiment, a scale 74, from which the rough setting of the ring 12 and the end plate 11 can be read. It will be evident that with this embodiment, the ring 12 and plate 11 are always in register with one another.
Arranged in the clamping element beneath the workpiece A is one or more vertically oriented cavities 48, in which pistons 49 having a connecting part are movable transversely of said workpiece. By supplying compressed air at 55 through the control unit 24 to the lower part of the piston housing, the piston 49 is urged against the workpiece, which in turn is urged against the upper part 50 of the clamping elements. The workpiece is therewith in friction engagement with said clamping element. For the purpose of quickly releasing the engagement of the clamping elements with the said workpiece, pressure springs 56 are arranged between the upper part of the piston housing and said piston. When the workpiece to be fed to the working machine is a profiled workpiece, the illustrated upper part of respective clamping elements can be replaces with a grooved upper part.
For the purpose of guiding the workpiece A through the feeding apparatus, two pairs of mutually co-operating guide wheels 51 are rotatably mounted on horizontal bracket structures 52 adjacent the attachment means 2 and the fixed clamping element 4 respectively. As will be seen from FIG. 2, the bracket structures 52 are provided with slots or grooves 53 extending transversely of the path of travel of the workpiece A, so that the pairs of wheels 51 can be adjusted to guide said workpiece. The guide wheels can be locked in place in the grooves or slots 53 by, for example, a nut and bolt arrangement 54 extending through the wheel journals and the bracket structure. As will be understood, the guide wheels can be exchanged for guide jaws. The number of guide wheels arranged in the bracket structures will, of course, increase with the number of workpieces to be fed simultaneously to the working machine.
The upper surfaces of the clamping elements on which the workpieces are slidable, and also the upper surface of the attachment means 2, can be coated with a friction reducing substance, such as polytetrafluoroethylene (Teflon®), to facilitate feeding of the workpiece to the working machine.
Suitably the control unit 24 can be coupled to the working machine in a manner such that the working tool of said maching is brought into contact with the workpiece when the movable clamping element is in its forward limit position. When a longer feed distance is required, the control unit can be set so that the movable clamping element executes two or more feed strokes before the said machining tool is activated.
The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
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There is provided a measuring apparatus for successively and intermittently feeding one or more elongate workpieces (A) to a working machine. Between an attachment means (2) and a fixed clamping element (4) there is arranged a further clamping element (7) which is reciprocatingly movable along a pair of guides (6). As the movable clamping element (7) makes a working stroke, the workpiece (A) is able to pass freely through the fixed clamping element (4). Upon return movement of the movable clamping element (7), however, the workpiece is held by the fixed clamping element, with the movable clamping element (7) returning to its rearward limit position out of engagement with the workpiece. The movable clamping element (7) is connected, via a piston rod (10), to the piston (9) of a pneumatic cylinder (8) of variable volume, said cylinder having an end plate (11) which is displaceable therein. The end plate (11) is held in selected positions along the cylinder (8) by means of a displaceable clamping ring (12) arranged to co-operate with a screw and nut arrangement (13). The end plate (11) has arranged therein a compressed-air connection (16), a damper (18), and a reversing valve (19), and defines the rear limit position of the movable clamping element (7). The forward limit position of said clamping element is determined by a reversing valve (39) arranged in said movable clamping element and adapted to co-act with a movable abutment (27) in the fixed clamping element (4). The length of stroke of the apparatus can be roughly set by positioning the end plate (11) in the cylinder (8) and then finely adjusting the setting of the working stroke (27).
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TECHNICAL FIELD
[0001] The present invention relates to computer data storage, and more particularly to cache memory subsystems.
BACKGROUND OF RELATED ART
[0002] In order to take advantage of the ever-increasing speed of microprocessors, data storage must either use expensive memory or provide for appropriate cache memory subsystems at appropriate points in the computer network system processing the data. The cache memory is conventionally smaller, faster than the computer system memory and operates at a higher speed than the system memory. The purpose of the cache is to position the information, both instructions and data, that the computer processor is to use next. The information may then be made available to the processor more quickly due to the speed of the cache memory. In most cache systems, when the system processor requests information, the request is first sent to the cache memory. If the cache contains the information, a “hit” signal is issued, and the requested information is sent to the appropriate function under the processor control. If the requested information is not in the cache, a signal indicative of a “miss” is returned to the processor, and the information is then retrieved from the slower system memory.
[0003] In the discussion that follows, when the term data is used with respect to caches, it is meant to cover both instructions and data for storage.
[0004] A cache is a collection of cache lines: each line includes a tag identifying the line and each line also includes the data content of the line. A successful identification of a tag is a hit. Otherwise, there is a miss. The cache lines are arranged in sets. The address of the data requested includes an index that is used to access the correct set in the cache; the address also includes an address tag that is compared to the cache line tag. If the tags match, there is a hit, and the cache line data is returned to the user. If none of the tags in the set match, the requested line has to be sought from a lower level storage that might be another cache or memory. This is considered a miss. If there is only one cache line in the set, the cache is called direct-mapped. If there is more than one cache line in the set, the cache is called n-way set associative (where n is the number of cache lines in each set). The n locations in each set in an n-way set associative cache are called ways. If the whole cache is a single set and the number of cache lines in the set is equal to the number of ways in the cache, the cache is called fully-associative. When a new cache line is brought in from a lower level storage, it makes space for itself by evicting an already existing line. The candidate for eviction is chosen based upon a selected replacement policy or protocol. Standard eviction protocols are usually variations of a LRU (least recently used) policy, i.e. the cache line that has not been used for the longest time has the highest probability of being evicted.
[0005] Direct-mapped or low-associativity caches are subject to interference misses or conflict misses problems. This occurs when accesses to a relatively small number of lines, the number of accesses being larger than the associativity, map to the same set. The access tags differ but there is not enough space in the set to simultaneously keep all of the accesses. If such accesses to these lines are repetitive and in a round-robin fashion, there could be a situation where the accesses always result in a miss. This behavior pattern is known as thrashing. While there may be space in the whole cache to store all of these lines, there is not enough space in any one set to do so.
[0006] The problem is further aggravated when multiple hardware threads share a cache. A problem arises when the different threads are running and sharing the same workload, and the associativity in the cache is just enough for one thread, but falls short when multiple threads share the cache. In another situation, the different threads could be running workloads that have very different cache access patterns. One thread might not reuse any of the data it brings into the cache, thus polluting or overloading the cache, while another thread, potentially needing more space in the cache, is not being afforded that space because the first thread's data, although never reused, is occupying valuable space.
[0007] Increasing the associativity of the cache has been considered but does not necessarily solve this problem. In fact, increased associativity could increase the problem, particularly in the case of multiple threads sharing a cache. This can be the case because there is no expedient to identify or to weight the value of a line before allocating it space in a cache set. If a thread is streaming through data, it could potentially use up most of the associativity of a set, even if the data is not used. Another drawback of higher associativity leads to a super-linearly higher power requirement in the cache because multiple simultaneous tag comparisons are required to identify a hit or a miss. Such comparisons, if done serially, would significantly increase the access latency of the cache.
[0008] Many solutions to improving the utilizing of cache associativity or providing extra associativity, as required, have been tried. However, most of these solution schemes evaluate the worthiness or weight of a cache line before affording it space in the cache. One solution to increase associativity while keeping the power requirement low, the average latency low and the associativity flexible, is to have a small fully-associative buffer in addition to the usual low-associativity cache. This buffer is searched upon the occurrence of a miss in the main cache. It is called a victim buffer or a victim cache. The limitation of this approach is that the victim buffer can handle associativity extension up to a relatively small total amount of extra associativity. Also, there might continue to be associativity lying unused in other parts of the cache.
[0009] An idea similar to the victim cache is a micro-cache that provides one or more extra sets in the cache that adaptively associate themselves with and, thus, extend one or more of the existing sets in the cache. The main drawback of such a scheme is that the size of the micro-cache must be limited so as not to increase the overall cache area drastically. Control logic complexity and latency increases are other concerns with the micro-cache scheme. Schemes to reduce the chances of thrashing due to repetitive uniformly spaced addresses have included index-hashing, Column-Associative caches and Skewed-Associative caches. In simple address-hashing schemes, the bits of the address that select the index are hashed and are then used to index into the cache sets. The disadvantage with this technique is that the hashing is static and can still suffer from the same problems described above. Hash-Rehash caches and Column-Associative caches use two hash functions to hash the index-bits in the address to evaluate the index. The first hash function is applied first, and upon a miss, the second hash function is applied. The existing storage in the cache is used to place a conflicting address. Column-Associative caches extend Hash-Rehash caches with a few relatively minor optimizations. The drawback of these schemes is that they have been described for direct-mapped caches only. The Skewed-Associative cache reduces the chance of set interference by using different hashes for indexing into different ways of a cache. These hashes are applied simultaneously rather than serially as in the earlier schemes. Thus, lines that would originally all map to the same set typically get mapped to different sets. The disadvantage of this scheme is that extra mapping hardware is required.
[0010] There has also been proposed a (Most Recently Used) MRU bit array that eliminates the need for data swapping between the primary and secondary locations for a line in a multiple-access cache. The MRU bit array is accessed beforehand to determine which location should be probed first. LRU-Based Column-Associative Caches extend the Column-Associative Cache to more than two (2) locations for a line, but require even longer sequential searches through the caches. If the primary location results in a miss, the secondary location is searched. If the secondary location results in a miss, a tertiary location is searched, etc. The disadvantage of this scheme is the long latency to access the cache and the overall performance gain this scheme can give, given the additional hardware overhead required to implement this scheme.
[0011] The problem of sharing the storage in a cache is optimally even more important when there are multiple threads that share the cache. This problem has only recently come into prominence with the design of semiconductor chips with multiple processing units. Such multi-core (multi-CPU) chips typically let caches be shared by more than one thread. Often, for Level 2 caches, the number of threads sharing the cache is sixteen (16) or more. Under such circumstances, it is highly likely that a few “bad” threads could hijack the space on the cache by being aggressive in accessing the cache, while not being very efficient in using the data fetched. An example of such a thread might be one that is running a streaming benchmark. The workload accesses a lot of data; regularly spaced, randomly spaced or a mixture of the two, and brings accessed data into the cache, but only rarely reuses the data in the cache. In such a scenario, all the other threads that bring in less data, but which would have actually reused the data, might suffer at the expense of the few “bad” threads.
[0012] The v-way cache addresses a problem similar to the problem that will hereinafter be addressed in the present invention by using a tag-array independent from the data-array. The tag-array is organized as a set-associative array, whereas the data array is organized as a direct-mapped array. The tag-array has forward pointers to the entry in the data-array containing the data corresponding to the tag. The data can be anywhere in the data-array, and not necessarily tied one-to-one to the tag-array entry. Also, the tag-array trades utilization for flexibility. It is typically only half or less-than-half full. However, a given set can grow in associativity, if necessary, at the expense of another set or sets in the cache, shrinking in associativity. The benefits of this scheme are reduction in conflict misses due to higher associativity and global replacement of data due to keeping the data-array separate. The disadvantages are that every access to data requires an initial access to the tag-array, followed by another sequential access to the data-array depending on the forward pointer. This detached tag-array and data-array design, therefore, leads to a longer best-case latency. Similarly, on a replacement, after a data line eviction in the data-array, the reverse pointer is followed to the tag-array entry to invalidate it.
[0013] Several other solutions to the problem of efficiently and fairly allocating storage in a cache shared by multiple threads (fair partitioning) have been proposed. Many of these schemes use way-partitioning that reallocate the existing ways in a set among threads sharing the cache. The drawback of these schemes is that the ideas are not scalable, as the number of threads sharing a cache grows because the set-associativity of the cache could be smaller than the number of threads. Partitioning the ways among the threads works well when there are fewer threads than ways, thereby allowing at least one way in a set to be allocated to each thread.
[0014] In addition, the Utility-based Cache Partitioning relies on hardware structures called UMONs (Utility Monitors) that count the “utility” characteristics of each thread for each cache set (or, over all cache sets) over a large number of clocks (5 million) and adjusts the partition every so often. This might be too large of a granularity for the system to be reactive enough.
[0015] Accordingly, there is a need for an efficient way to share cache associativity in a processor system without relying on extraneous storage (like a victim-cache or a micro-cache), without being limited to direct-mapped caches (like the hash-rehash or column-associative caches), without relying on way-partitioning (that works when there are fewer threads than associativity) and without reacting slowly to the dynamics of cache utilization, especially when a large number of threads share the cache (like in Utility Based Computing),
SUMMARY OF THE INVENTION
[0016] In its broadest aspects, the present invention provides for the improved utilization of cache storage by determining which lines of data are worthy of the cache space, i.e. have sufficient value to be provided cache space and then judiciously utilizing space in a cache set different from the set that the cache line indexes into.
[0017] More particularly, the present invention relates to a cache memory including a plurality of sets of cache lines, and provides an implementation for increasing the associativity of selected sets of cache lines including the combination of providing a group of parameters for determining the worthiness of a cache line stored in a basic set of cache lines, providing partner sets of cache lines, in the cache memory, associated with the basic set, applying the group of parameters to determine the worthiness level of a cache line in the basic set and responsive to a determination of a worthiness in excess of a predetermined level, for a cache line, storing said worthiness level cache line in said partner set.
[0018] In accordance with one operative aspect of the invention, the cache memory is an n-way set associative cache and the access input to the cache is greater than n input threads. In providing for the partnering, there is provided an implementation enabling said basic set to borrow ways from said partner set, wherein the number of ways in the set of cache lines is increased. A function is provided associated with said basic cache for indicating the cache lines stored in said partner cache.
[0019] For best results, the means for determining the worthiness level and the means for storing cache lines in the partner set are dynamically operative while data lines are being input into the cache memory.
[0020] In accordance with another aspect of the invention, an implementation is provided for evicting selected cache lines from said basic set in order to prevent exceeding the capacity of said basic set, wherein the means for determining said worthiness level determine the worthiness of an evicted cache line. The worthiness of a cache line may be determined by the reuse potential of the cache line, and the reuse of an evicted cache line may have already been so tracked prior to eviction.
[0021] Apparatus for applying the cache line set partnering of the present invention in cache memory system may be embodied in the combination of a data array for storing said basic and partner sets of cache lines, a tag array for storing tags to said respective cache lines and a ghost tag array for storing tags for respectively indicating the cache lines stored in said partner cache.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] The present invention will be better understood and its numerous objects and advantages will become more apparent to those skilled in the art by reference to the following drawings, in conjunction with the accompanying specification, in which:
[0023] FIG. 1 is a diagrammatic illustration of a conventional 4-way set associative cache in a cache memory;
[0024] FIG. 2 is a simplified diagrammatic 4-way set associative cache of FIG. 1 illustrating how the cache may be accessed by many cores, i.e. multi-CPUs that provide a number of access threads exceeding the number of ways (4);
[0025] FIG. 3 is the conventional 4-way set associative cache shown in FIG. 1 modified to include a ghost tag array used in implementing the present invention;
[0026] FIG. 4 is a diagrammatic illustration in accordance with FIG. 3 showing how the ghost tag array functions in implementing the present invention;
[0027] FIG. 5 is a flowchart illustrating how the steps embodying a primary aspect of the present invention is carried out;
[0028] FIG. 6 is a flowchart illustrating how a determination is made as to whether to retain a candidate cache line for eviction in a cache partnership association according to the present invention; and
[0029] FIG. 7 is a flowchart of an algorithm to determine the replacement of cache lines in the partner cache set when the latest cache line achieves the worthiness level required for storage in the partner cache.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0030] Conventionally, processors supporting memory caches have two main storage arrays (FIG. 1 )—a Tag Array 11 and a Data Array 10 . The structure of a 4-way set associative cache is shown in FIG. 1 . The Data Array 10 of the cache holds cache lines 12 that are, in a typical desktop or server processor, 16 bytes to 128 bytes in size and are accessed by an address. The Tag Array holds the “tags” 14 that are a part of the address 13 used to identify the cache line. The bits in the cache lines address 13 are broken into bit-fields and used to locate a cache line. The bits used to find the appropriate set in the cache are called the “index” bits 15 . The set may have more than one cache-line in it.
[0031] In the illustration shown in FIG. 1 , the cache memory is a 4-way cache, i.e. there are four (4) cache lines in a set and each line has a corresponding tag 14 . The cache line address 13 has a tag 16 that is compared to a corresponding tag 14 in the tag array 11 , and if a match is found, then the appropriate cache line 12 in the data array 10 is retrieved. This is a cache “hit”. If none of the tags in the indexed set in the Tag Array match the tag for the cache line being searched, it is considered a cache “miss” and appropriate action is taken to fetch the line from a lower level storage. Once a cache line is identified, it is returned to the requester, which could be a processor or another cache. If necessary, part 17 of the cache line address, typically the least significant bits, could be used to identify the exact byte 18 in a cache line 19 that was requested.
[0032] When a cache is shared by many cores, e.g. multi-CPU semiconductor chips that will have many more threads (simultaneously running execution sequences that may each access the cache), the cache appears as a uniform resource to all of the threads. However, the thread that uses the space in the cache most aggressively tends to use up more space in the cache. Aggressively making requests to the cache and thereby using more of the cache does not necessarily imply that the thread is using the cache efficiently. The overall throughput, performance or both may suffer because the other threads could be starved for cache space. FIG. 2 shows an overall 4-way set associative memory cache 21 , like that of FIG. 1 , shared by four (4) cores 22 - 25 (CPUs) running two (2) threads 26 (paths) each.
[0033] To more efficiently use the cache space, whether a single thread or multiple threads use it, it is important to recognize that cache lines are making effective use of the cache space and which lines are not. A cache line that is used one or more times after the first access brings it in might be considered one that uses the cache space more effectively than a cache line that, after the initial access, is never used again before it is evicted. Several schemes to measure reuse effectiveness use counters that count how often a line was accessed after being brought into the cache.
[0034] It should be noted that reuse potential is not the only attribute that could determine worthiness. For example, the threads providing cache lines could be given weights or priorities that could be used to determine the worthiness of cache lines from such threads.
[0035] The present invention prefers an embodiment, to be hereinafter described in detail, that uses an extra Tag Array that may be referred to as a “Ghost Tag Array” or “Shadow Tag Array”. A purpose of this Ghost Tag Array is to retain information about cache lines that are no longer in the main (basic) data array.
[0036] This implementation is shown in FIG. 3 , which is the memory array of FIG. 1 with the supplementary Ghost Tag Array 30 that does not have any data array corresponding to it. It is relatively small in hardware overhead because it only keeps part of the information the primary Tag Array would keep per cache line. It only needs to store the actual tag portion of a cache line and a few more bits to keep track of “worthiness”, which will be hereinafter described. The purpose of the Ghost Tag Array is to hold the tag information for cache lines evicted from the main Tag Array. Such stored tags for lines evicted from any set in the relatively recent past could indicate a line that could have used extra associativity if the cache set could have provided it. Counter-based schemes, typically, measure the reuse of cache lines that are in the Tag and Data Arrays. With the Ghost Tag Array we can also measure the reuse potential of a cache line that is no longer in the main Tag and Data Arrays. The partner set implementation of the present invention may use any appropriate scheme to determine the “worthiness” of a cache line, i.e. to determine whether a line could use extra associativity if it were provided to it as a means of staying in the cache.
[0037] FIG. 4 shows the operation of the various components of the memory cache in accordance with the present invention. The process involves: 1 . Identifying a cache line that is “worthy” of being given preference, both when evaluating offering extra associativity and during replacement or eviction; and 2 , extending a cache line set's associativity by “borrowing ways from another set or sets in the cache. FIG. 4 shows a “Main Set”, i.e. the basic sets extending across the Tag Array 11 (tag set 32 ), the Ghost Tag Array 30 (tag set 33 ) and the Data Array 10 (line set 31 ). These are “main” or basic only in the sense that the line set 31 represents a set that is looking to extend its associativity at a given point in time. Otherwise, basic line set 31 is not different from any other set. FIG. 4 also shows a Partner Set 34 of a corresponding four (4) cache lines extending across the Data Array 10 , the Ghost Tag Array 30 (tag line 35 ) and the Tag Array 11 (tag line 36 ). The partner set implementation involves selecting a set of cache lines from all the sets in the memory cache that can be used by the basic or Main Set for the purpose of borrowing associativity. In the preferred embodiment, this partner set 34 is identified by a simple rehash of the index bits that index into the Main (basic) Set 31 . We will refer to the index bits that index into the Main Set, the primary index, and refer to the index that identifies the Partner Set, the secondary index. A simple example of a rehash is one that flips the most significant bit of the primary index to generate the secondary index. For example, assume a cache with 1024 cache line sets. Then, sets 0 and 512 could be partners; and sets 1 and 513 would be partners; etc. Another scheme could use a simple bit flip of all the bits that identify the basic set so as to identify the partner set to the basic set. In this case, in a cache with 1024 sets, sets 0 and 1023 , 1 and 1022 , etc. will be partners.
[0038] Now, with respect to FIG. 5 , a generalized overall description of the flow of the present invention will be described in the form of the flowchart. Upon receiving a data access request step 50 , the memory cache controller calculates the primary index from the request's address, as previously described with respect to FIG. 1 . Using the primary index, the Tag Array is looked up and after tag comparison a hit or miss is identified, decision step 51 . If Yes, a hit, the request is handled as a regular hit, step 52 , so that the data is returned to the requester in case of a load and/or data is accepted into the Data Array in case of a store. If the decision is No, a miss, all the other sets that could be holding data corresponding to the main (basic) set would conventionally be looked up. However, in our illustrative implementation, there is only a single partner set per main (basic) set. There is maintained, per set, a bit in the tag array that indicates if the partner set corresponding to this basic set should be looked at. For example, if no space in the partner set is currently borrowed, there is no need to look up the partner set. Since this access to the partner set is in the critical access path, it is desirable to avoid the extra lookup. If the bit in the main (basic) set that identifies if any space in the Partner Set is in use (“using partner set” bit), step 52 , is OFF (No), or, if the bit is ON (Yes) and a lookup of the Partner Set, step 53 , results in No (a miss), the miss is conventionally handled by requesting the lower level storage (not shown). Simultaneously, the Ghost Tag Array corresponding to the Main Set is looked up, step 54 . A determination is made, step 55 , as to whether the tag hits in the Ghost Tag Array, indicates that the requested line was in the cache in the past and could have resulted in a hit had there been sufficient space in the cache to retain the line in the cache. This will result in step 55 Yes, and the line is recognized as “worthy” of extra associativity and the tag is marked as “high-associativity eligible”, or simply, “worthy”, step 56 . At that point, and also in case the lookup in the Ghost Tag Array set corresponding to the Main Set results in a miss, step 55 , No, the cache waits for miss data to come back from the lower level storage, steps 57 and 58 , at which point the Handle Replacement In Main-Set (HRIM) flowchart is executed, as will be subsequently described with respect to FIG. 6 , followed by installing the newly brought in line in the Main Set's Tag Array and Data Array. In case there was a hit in the Ghost Tag Array, step 55 , Yes, then step 59 , the tag is removed from the Ghost Tag Array since it has found a place in the main array, and the HRIM flowchart is executed. In case there was a miss in the Ghost Tag Array, step 55 , No, then step 62 , the tag is created in the Ghost Tag Array and corresponding data placed in the main (basic) array.
[0039] As ancillary considerations, in case of a store-back cache (also known as write-back cache), the miss handling described above applies to both load and store misses (in most cases). In case of a store-through cache (also known as a write-through cache), the miss handling described above applies only to load misses since store-misses do not bring any data into the cache.
[0040] Continuing with respect to FIG. 5 , if the bit in the Main Set that identifies “using partner set” is ON, step 52 , Yes, and lookup of the Partner Set results in a hit, step 53 , Yes, the data is returned to the requester in case of a load and data is accepted into the Data Array in case of a store, step 60 . Then, step 61 , the HRIM flowchart is executed (as will be hereinafter described with respect to FIG. 6 ) and the tag and data from the Partner Set's Tag Array and Data Array are moved into the Main Set in the cache. The rationale for this data movement is that the next time this data is accessed it is a hit in the Main Set itself rather than requiring a second lookup into the Partner Set. This data and tag movement can be handled in the background and does not affect the critical path of returning data to the requester. If this is the last line belonging to the Main Set that was in the Partner Set, then the bit in the Main Set identifying “using partner set” can be cleared to avoid unnecessary lookups into the Partner Set in the future. It is easy to imagine a scheme to keep track of whether the line is the last line belonging to the Main Set in a Partner Set. The “using partner set” bit could be extended to “number of lines in partner set”. A count of 0 indicates that the Partner Set is not in use by the Main Set. A count of 1 indicates, in the situation described above, that the cache line in the Partner Set that belongs to the Main Set is the last such cache line, and if it is ever moved back to the Main Set, the “number of lines in partner set” should, upon decrementing, become 0, and, thus, indicate that the Partner Set is no longer being used by the cache lines in the Main Set.
[0041] As has been previously mentioned, the means for determining the worthiness level and the means for storing cache lines in the partner set are, preferably, dynamically operative while data lines are being input into the cache memory. In such a dynamic environment, an implementation is provided for evicting selected cache lines from said basic set in order to prevent exceeding the capacity of said basic set, wherein the means for determining said worthiness level determine the worthiness of an evicted cache line. The worthiness of a cache line may be determined by the reuse potential of the cache line and the reuse of an evicted cache line may have already been so tracked prior to eviction. An embodiment of this will be described with respect to the Handle Replacement In Main-Set (HRIM) flowchart of FIG. 6 . A replacement candidate, i.e. candidate for eviction is identified in the Main (basic) Set, step 62 . The replacement policy could be any of the usual replacement policies used in caches (LRU, pseudoLRU, FIFO, Random, etc.) or, as a proposed optimization, could utilize the “worthy” bit information to reduce the probability of replacing cache-lines that have proven to be reused. Developers of eviction routines should provide routines to ensuring that lines that have been recently brought in and have not had a chance to prove their “worth” should not be overly penalized, and similarly, lines that proven their worth in the past but have not been used in a long time are not retained in the cache at the expense of other lines.
[0042] If the replacement candidate in the Main Set is marked “worthy” or high associativity eligible, step 63 , Yes, then additional associativity must be borrowed in the cache so as not to lose the data from the Data Array. The tag and data corresponding to this replacement candidate are attempted to be moved to the Partner Set, step 64 . An example of such a move to partner procedure will be described with respect to the Move To Partner Set (MTPS) flowchart of FIG. 7 . If the attempt to save the line in the Partner Set succeeds, then, step 66 , we have made space in the Main Set's Tag and Data Array. The “using partner set” bit in the Main Set is marked and this step is complete. If the attempt to save the line in the Partner Set fails, a No from “Fail?” decision, step 65 , or, if the replacement candidate in the Main Set is not marked “worthy”, step 63 , No, its tag is then moved to the corresponding Ghost Set, step 67 . To make space for this tag in the Ghost Set, an algorithm, similar to the replacement algorithm, herein identifies a candidate to be evicted from the Ghost Set. The Data corresponding to the line evicted from the Main Set is removed from (marked invalid in) the Data Array. The Tag and Data Array locations, thus freed up in the Main Set, are populated with the miss data when it returns from lower level storage.
[0043] When a cache data line is found to be sufficiently worthy to be moved to the partner set, an additional determination must be made as to space available in the partner set.
[0044] A flowchart, MTPS flowchart ( FIG. 7 ) will now be described. The cache line that is identified to be moved to the Partner Set needs space in the Partner Set. To make space in the Partner Set, a replacement algorithm is used to identify a replacement candidate in the Partner Set, step 70 . It is suggested that the replacement algorithm be optimized to take into consideration the “worthy” attribute of a line and be further optimized to distinguish lines that originally belong to the Partner Set and lines that originally belong to the Main Set but are borrowing space in the Partner Set. If the, thus, recognized candidate is marked as “worthy”, Step 71 , Yes, the attempt to make space in the Partner Set is deemed a failure, step 72 , and that is returned, i.e. communicated to, the Cache Controller. How the cache controller handles such a reported failure by the MTPS algorithm has been described in FIG. 6 . If the replacement candidate identified in the Partner Set is not marked “worthy”, step 71 , No, it is moved to the Partner Set's Ghost Set, step 73 . A replacement algorithm similar to the one described earlier in the description of the Main flowchart makes space in the Ghost Set. The tag and data corresponding to the line that is attempting to move into the Partner Set are appropriately installed.
[0045] Since the steps laid out in the HRIM flowchart, FIG. 6 , and the MTPS flowchart, FIG. 7 , occur in parallel with the fetching of the miss data, there is no latency overhead introduced by this process. It may be argued that the hit latency is compared longer to a typical cache when there is a miss to the Main Set and a hit to the Partner Set, since that constitutes a second lookup. It is believed that a hit on the second lookup is a better option as compared to the miss on the first lookup with no opportunity for a second lookup. Special care must be taken to make sure that the Main Set always has the most “worthy” lines that access that set, and the Partner Set acts to catch a few that spill over from the Main Set on a best-effort basis.
[0046] Although certain preferred embodiments have been shown and described, it will be understood that many changes and modifications may be made therein without departing from the scope and intent of the appended claims.
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A cache memory including a plurality of sets of cache lines, and providing an implementation for increasing the associativity of selected sets of cache lines including the combination of providing a group of parameters for determining the worthiness of a cache line stored in a basic set of cache lines, providing a partner set of cache lines, in the cache memory, associated with the basic set, applying the group of parameters to determine the worthiness level of a cache line in the basic set and responsive to a determination of a worthiness in excess of a predetermined level, for a cache line, storing said worthiness level cache line in said partner set.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a divisional of application Ser. No. 10/313,635, filed Dec. 5, 2002, which is a continuation of application Ser. No. 08/716,324, filed Oct. 4, 1996, which is a U.S. National Stage of International Application No. PCT/EP95/01263, filed Apr. 6, 1995, which claims priority of German Application No. P 44 11 862.7, filed Apr. 6, 1994. The disclosures of application Ser. No. 10/313,635, application Ser. No. 08/716,324 and International Application No. PCT/EP95/01263 are expressly incorporated by reference herein in their entireties.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a process for producing homogeneous multicomponent dispersions and products derived therefrom, in particular a process for producing homogeneous multicomponent dispersions in which particles having a mean particle size of preferably not more than 100 μm are dispersed in an aqueous and/or organic medium
[0004] 2. Description of the Related Art
[0005] In the production of ceramic materials, glasses and composite materials, the finely divided starting materials needed, for example the oxides, nitrides, borides, carbides and carbonitrides of Al, Si, Zr and Ti and the silicides, sulphides, arsenides, antimonides, selenides, phosphides and tellurides of alkali metals, alkaline earth metals, Sc, Y, Ti, Zr, Nb, Ta, Cr, Mo, W, Fe, Co, Ni and the lanthanides, are generally first processed to give a suspension (slip) of the starting materials in an aqueous or organic dispersion medium. After appropriate conditioning (adjustment of the rheology, solids content, dispersion state, etc.), the slip is either processed directly to give a green body using appropriate shaping methods or is first converted into a powder which is either pressed directly to form a green body or is redispersed and then shaped into a green body by appropriate shaping methods. Suitable shaping methods are tape casting, slip casting, pressure casting, electrophoresis, injection molding, freeze casting, centrifugation, gel casting, sedimentation, hot casting and freeze injection molding. The desired material or sintered body is finally obtained from the green body by sintering.
[0006] Sintering the usually ceramic starting materials to high density requires sintering aids, e.g. finely divided carbon (carbon black) and/or metals such as finely divided Al and B or materials selected from among the abovementioned starting materials. If these sintering aids are dispersed in aqueous or organic systems during preparation of the slip, different surface-chemical properties and/or very different particle sizes of the individual components result in difficulties such as an undesired formation of agglomerates and inhomogeneities in the multicomponent slip obtained. Naturally, such an inhomogeneity or agglomerate formation in the slip also has an unfavorable effect on the materials finally obtained therefrom.
SUMMARY OF THE INVENTION
[0007] It is therefore an object of the present invention to provide a process for producing multicomponent dispersions of finely divided particles, in particular particles having a mean particle size of not more than 100 μm, preferably not more than 50 μm and in particular not more than 10 μm, which dispersions have the particles very homogeneously distributed and are therefore suitable for producing solid products, e.g. sintered bodies, having excellent homogeneity and advantageous properties resulting therefrom.
[0008] The present invention provides a process for producing homogeneous multicomponent dispersions in which the finely divided particles are dispersed in an aqueous and/or organic medium, wherein:
(a) if kinds of particles (having comparable or significantly different (mean) particle sizes) are present in which the groups X present on the surface of the kinds of particles are of poorly compatible or incompatible nature, at least one kind of particles is brought into contact with one or more species A which have at least one group B and at least one group Y, where under the conditions used the groups B form covalent, ionic or coordinate bonds with groups X present on the surface of this at least one kind of particles and the groups Y are groups which are compatible in terms of their nature with the surface groups of the other kind(s) of particles present in the dispersion; or (b) if kinds of particles (having comparable or significantly different (mean) particle sizes) are present of which at least one kind of particles has groups X on the surface and at least one other kind of particles has groups W on the surface, these particles are brought into contact with one or more species D which have at least one group B and at least one group E, where under the conditions used the groups X and the groups B on the one hand and the groups E and the groups W on the other hand form covalent, ionic or coordinate bonds; or (c) if kinds of particles having significantly different (mean) particle sizes are present, the particles are, separately as such or in dispersion, provided with opposite surface charges and the particles thus treated are then mixed.
DETAILED DESCRIPTION OF THE INVENTION
[0012] The particles to be dispersed are preferably particles of materials which can be used in the production of ceramic materials, glasses and composites (e.g. ceramic/ceramic, glass/ceramic, glass/metal and ceramic/metal). Thus, they are, in particular, solid particles of inorganic or metallic origin such as carbon particles. The particles are particularly preferably particles of Si, B, Al, Ti, Zr, W, Mo, Cr and Zn and the (mixed) oxides, hydrated oxides, nitrides, carbides, silicides, borides and carbonitrides derived therefrom. Concrete examples are (anhydrous or hydrated) Al 2 O 3 , ZrO 2 , Si 3 N 4 , mullite, cordierite, perovskites, e.g. BaTiO 3 , PZT and PLZT, SiC, TiC, Ti(C,N), B 4 C, BN, AlN, TiB 2 , ZrB 2 , ZrC, WC, MoSi 2 , chromium carbide, aluminum carbide, ZnO, and carbon black. Of course, particles of other materials, for example these mentioned in the introduction, can also be used according to the invention. In general, the dispersions to be produced according to the invention contain particles of at least two different materials.
[0013] Furthermore, according to the invention, preference is given to using those materials comprising “nanosize” or “nanodisperse” or “submicron” particles or powders. In the present context, “nanosize” means an average particle size of not more than 100 nm, in particular not more than 50 nm and particularly preferably not more than 30 nm, with there being no specific lower particle size limit, but this being preferably 0.1 nm and in particular 1 nm. “Submicron” means, in the present context, a mean particle size of from greater than 100 nm to 1 μm.
[0014] Of course, it is also possible to use larger (kinds of) particles in the process of the invention, but the (mean) particle size should preferably not exceed 100 μm, in particular 50 μm and particularly preferably 10 μm.
[0015] The variants (a) to (c) of the process of the invention all serve to modify at least two kinds of particles (in general of different materials) which, for example owing to their different particle sizes and/or different surface properties, can be processed as such only with difficulty or not at all to give reasonably homogeneous dispersions, in such a way that their surfaces or surface properties are the same or at least very similar (variant (a)), that their surfaces attract electrostatically (variant (c)) or that they are, by means of their surface groups, chemically bound to one another (variant (b)).
[0016] In the following, the three variants of the process of the invention are discussed in more detail. In the interest of simplicity, the discussion will assume two-component systems, i.e. in each case there should be present only two kinds of particles which, either owing to their significantly different particle sizes and/or owing to their different surface properties, can be processed to give a reasonably homogeneous dispersion only subject to particular precautions, if at all. However, the present invention is not restricted to such two-component systems but it is also possible for there to be simultaneously present three, four, five, etc., kinds of particles which can also be similar or the same in terms of their particle size and/or surface properties, as long as there is present at least one kind of particles which cannot readily form homogeneous dispersions with the others for the abovementioned or other reasons. It is also possible, if more than two kinds of particles are present, to combine two or all of the variants (a) to (c) of the invention with one another.
[0017] The variant (a) of the process of the invention is, for example, an advantageous way of producing homogeneous dispersions when the two kinds of particles, which can be of comparable size, differ (significantly) in respect of the nature of the surface groups. This is the case, for example, when the surface groups X are polar or hydrophilic groups such as —OH, —COOH, etc., while the second kind of particles has surface groups which are nonpolar or hydrophobic, for example hydrocarbon radicals (e.g. —CH 3 ). Naturally, such a combination normally leads to dispersions in which the particles having polar surface groups X are preferentially situated adjacent to particles having similar surface properties, i.e. likewise having surface groups X, and the particles having nonpolar surface groups are preferably situated adjacent to particles having likewise nonpolar surface groups, i.e. not to a random distribution of the particles and thus to inhomogeneities.
[0018] According to the variant (a) of the invention, this situation can be altered in various ways such that the particles become very similar or even identical in respect of their surface properties and a random distribution of these in the dispersion is thereby made possible. All these possibilities have in common that one or both kinds of particles are modified on their surface in such a way that the surface groups of the particles are then very similar or even identical (e.g. all hydrophobic or all hydrophilic). This can be achieved by reacting the particles having the surface groups X with species (compounds) A which have, on the one hand, a group B which reacts with the said groups X to form a covalent, ionic or coordinate bond and, on the other hand, a group Y which is very similar or even identical in nature to the groups located on the surface of the other kind of particles. The end effect of this procedure is that the surface groups X are in practical terms replaced by surface groups Y which are (more) suitable for producing a homogeneous dispersion. However, it has to be realized that the groups X are not simply removed but are still always present in altered form (namely as part of a covalent, ionic or coordinate bond) and now merely serve as the anchoring point for the “new” surface groups Y. In the ideal case, the groups on the surface of the other kind of particles are likewise groups Y, although in many cases it is also sufficient if these surface groups are ones which, in terms of their nature, belong to the same class as the groups Y. For example, it is generally sufficient, when the surface groups of the other kind of particles are acid groups, for the group Y to likewise be an acid group (e.g. a carboxylic acid or sulfonic acid group). Of course, an analogous situation also applies in the case of, for example, basic, nonpolar or polar groups. Furthermore, the surface groups of the other kind of particles can be ones which have been fixed to the surface of this other kind of particles in a similar manner to the groups Y. In other words, it is of course also possible to modify the other kind of particles having, for example, surface groups X′ with species A′ having at least one group B′ and at least one group Y′ in such a way that in the end there are present surface groups Y′ which are the same as or at least have a comparable nature to the surface groups Y. However, for reasons of economy of effort, it is generally preferred to modify only one kind of particles in such a way that their surface groups are then compatible with the surface groups of the other kind of particles. However, it can also be the case that, for example, species A having a suitable group B and a suitable group Y are obtainable only with difficulty, if at all and it is therefore more advantageous to use (more readily obtainable) species A having at least one group B and at least one group V and to accordingly also modify the surface groups (e.g. Y) of the other kind of particles in such a way that they are compatible (or even identical) with the groups V.
[0019] The reaction of the kind of particles having the surface groups X with the species A can be carried out either in the presence of the other (possibly already surface-modified) kind of particles (e.g. in the dispersion medium) or separately therefrom (before production of the final dispersion). The latter variant has the advantage that it can also be used when it cannot be ruled out that, under the reaction conditions used, the surface groups of the other kind of particles will also react with the groups B or even the groups Y or the other kind of particles can lead to some form of interference with the reaction between the groups X and B.
[0020] The procedure in the above reaction or surface modification is comprehensively described for the example of nanosize particles in DE-A4212633, the full scope of the disclosure of which is hereby incorporated by reference. If the surface modification of the one kind of particles is carried out in the absence of the other kind of particles, the dispersion medium used can subsequently be removed in a customary manner (e.g. by filtration), which can be followed by washing and drying of the particles. This procedure also has the advantage that no residual (i.e. unreacted) species A are present in the homogeneous dispersion to be produced later. The particles thus modified can then be dispersed together with the unmodified, or likewise previously modified in an appropriate manner, other kind of particles in the actual dispersion medium so as to produce a homogeneous dispersion.
[0021] Concrete examples of species A and suitable dispersion media, etc., are indicated further below.
[0022] The variant (b) of the process of the invention is particularly advantageous when kinds of particles having significantly different particle sizes are to be dispersed together, but can also be advantageously employed for the dispersion of kinds of particles having comparable sizes. Nevertheless, this variant (b) will be explained in more detail for the case of the joint dispersion of (significantly) larger particles having surface groups X (e.g. particles in the submicron or micron range) and (significantly) smaller particles having surface groups W (e.g. nanosize powders). The variant (b) differs from the variant (a) essentially only in that the group Y of the species A, which in the case of the variant (a) has to be compatible only with the surface groups of the other kind of particles, is replaced by the group E which can react with the surface groups W of the other kind of particles to form a covalent, ionic or coordinate bond (similar to the case of the groups X and B). Although in the case of the variant (b) too, the reaction between the groups X and B with the groups E and W can be carried out simultaneously (in the final dispersion medium), preference is given to carrying out these reactions in succession. Particular preference is given to first reacting the larger particles having the surface groups X with the species D (as in the case of the variant (a) with the species A), then removing the dispersion medium used and washing and, if desired, drying the particles obtained. Subsequently, the particles thus surface-modified can be combined and reacted with the smaller particles having surface groups W, which is advantageously carried out in the dispersion medium to be used for the final dispersion, so as to avoid again having to remove the reaction medium.
[0023] Both in the variant (a) and in the variant (b), the species A or D do not necessarily have to have only one group B and one group Y or E, but, on the contrary, in some cases it can be advantageous if these species are anchored, for example, via two or even three groups B or E to the particles having the surface groups X or W, at least as long as it is ensured that such multiple anchoring is sterically possible.
[0024] The process according to alternative (b) just indicated for the case of larger particles having surface groups X and smaller particles having surface groups W can be regarded essentially as a chemical coating of the larger particles with the smaller particles, with the species D serving as coupling agent. In comparison, the process according to variant (c) of the process of the invention can be described as electrostatic coating of larger particles with smaller particles. In this variant, it has to be ensured, first and foremost, that the signs of the surface charges of the two kinds of particles to be dispersed (having significantly different particle sizes) are different, so that, owing to their opposite surface charges, the larger particles attract the smaller particles and vice versa. Naturally, this process increases in efficiency with increasing surface charges of the participating particles. In the present context, the expression “significantly different particle size” means, in particular, particles whose (mean) particle sizes differ by at least a factor of 3, preferably at least a factor of 5 and more preferably at least a factor of 10.
[0025] The charging of the surfaces of the participating particles can be carried out in various ways. For example, one or both kinds of particles can be (separately) electrostatically charged and then added together or in succession to the dispersion medium.
[0026] According to a particularly preferred embodiment of the variant (c), the larger and the smaller particles are first dispersed separately and the dispersions thus prepared are combined and mixed, with the pH values of the separate dispersions being selected such that, both in these dispersions and also in the resulting dispersion (after combining), the zeta potentials of the kinds of particles have a different sign and, in particular, have as high as possible a positive value or as high as possible a negative value.
[0027] The zeta potential is a measure of the number of surface charges generated. It is pH-dependent and is either positive or negative in relation to the isoelectric point of the respective material. In other words, the higher the zeta potential the higher the charging of the particles and the higher the force of attraction for particles of opposite charge.
[0028] The formation of negative or positive surface charges is preferably effected or aided by addition of an acid or base. Acids suitable for this purpose are, for example, inorganic acids such as HCl, HNO 3 , H 3 PO 4 and H 2 SO 4 and also organic carboxylic acids such as acetic acid, propionic acid, citric acid, succinic acid, oxalic acid and benzoic acid. Suitable bases are, for example, NH 3 , NaOH, KOH, Ca(OH) 2 and also primary, secondary and tertiary aliphatic and aromatic amines and tetraalkylammonium hydroxides. However, it is a prerequisite for this embodiment of the variant (c) of the process of the invention that the particles originally used have surface groups which are (sufficiently) negatively or positively charged depending on the pH selected. This requirement is not always met by particles which have not been surface-modified. In particular, it has to be taken into account that two kinds of particles to be combined not only have to each have suitable surface groups which bear positive or negative charges depending on the pH, but that these surface groups also have to have opposite (and preferably large) surface charges at the desired pH of the final dispersion so as to ensure the presence of strong forces of attraction. Thus, in the case of the variant (c) it can also be necessary to modify at least one of the two kinds of particles on the surface in such a way as to result in particles having surface groups which together with the other kind of particles fulfill the above-mentioned conditions. Hence, for example in the case of larger particles having surface groups X which in combination with the other kind of particles would not be suitable for the pH-dependent electrostatic coating process (e.g. because the zeta potentials of the two kinds of particles would have the same sign at the desired or any pH), the procedure can be to react these particles first with species A (as described above in variant (a)), where the group Y of the species A is one which has a suitable zeta potential at the desired pH.
[0029] If the other kind of particles has a zeta potential having the “correct” sign but a relatively low value, the second kind of particles can also be appropriately modified so as then to have surface groups which result in a zeta potential having still the same sign but a higher value at the desired pH.
[0030] If, in the case of the variant (c), one of the kinds of particles is already present in a suitable (charged) form, it is of course only necessary for the other kind of particles to be appropriately charged, possibly after prior surface modification (as described above).
[0031] The species which can be used for the purposes of surface modification in the above variants (a) to (c) of the process of the invention are described in more detail below.
[0032] In the case of the species A and D, the groups B and Y or B and E are, for example, joined to one another by means of a single (covalent) bond or (preferably) by means of a hydrocarbon radical. This hydrocarbon radical can include one or more hetero atoms such as halogen, O, S and N, either as part of the basic structure and/or merely bound thereto (particularly in the case of halogen). The hydrocarbon radical can be a saturated or unsaturated, aliphatic, cycloaliphatic or aromatic hydrocarbon radical or a combination thereof and this radical preferably has a molecular weight not exceeding 500, in particular 300 and particularly preferably 200. Particular preference is given to using connecting groups whose basic structure comprises not more than 30, in particular not more than 20 and particularly preferably not more than 10, atoms (carbon atoms plus hetero atoms). Concrete examples of connecting groups are C 2-20 -(cyclo)alk(en)ylene groups such as ethylene, propylene, butylene, (cyclo)pentylene and (cyclo)hexylene, C 5-12 -(hetero)arylene such as phenylene, naphthylene and pyridylene, and also combinations of one or more of these groups.
[0033] The nature of the groups B, E and Y in the species A and D of course depends on the nature of the groups present on the surfaces of the particles to be dispersed. However, preferred groups B, E and Y are those of the formulae —COT, —SO 2 T, —POT 2 , —OPOT 2 , —OH, —NHR 1 and —CO—CHR 1 —CO—, where T are halogen (F, Cl, Br or I), —OCO—, —OR 1 and —NR 1 2 (and can be identical or different) and R 1 are identical or different and are H or C 1-8 -alkyl (preferably C 1-4 -alkyl), where Y can also be a group of the formula —CR 2 3 in which R 2 are identical or different and are hydrogen, halogen Cm particular F and Cl) and C 1-8 -alkyl (preferably C 1-4 -alkyl) and one group R 2 can also be OR 3 or SR 3 (R 3 =C 1-8 -alkyl or C 6-12 -aryl). The additional meanings for Y are explained by the fact that Y is a group which does not have to react with any other group to form a covalent, ionic or coordinate bond but only has to be similar to or the same as the groups present on the surfaces of the other kind of particles to be dispersed, where these groups can also be hydrophobic (nonpolar) groups.
[0034] Concrete examples of preferred species A and D are the following, which must, however, not be regarded as restricting the present invention:
monocarboxylic and polycarboxylic acids having from 2 to 12 carbon atoms, for example acetic acid, propionic acid, butyric acid, pentanoic acid, hexanoic acid, acrylic acid, methacrylic acid, crotonic acid, citric acid, adipic acid, succinic acid, glutaric acid, oxalic acid, maleic acid, fumaric acid, itaconic acid, toluenesulfonic acid, trifluoroacetic acid, stearic acid, trioxadecanoic acid and the corresponding anhydrides (such as acetic anhydride, propionic anhydride, succinic anhydride and maleic anhydride), halides (such as acetyl chloride, propanoyl chloride, butanoyl chloride and valeryl chloride), esters (e.g. ethyl acetate) and amides (e.g. acetamide); monoamines and polyamines such as those of the general formula R 3-n NH n , where n=0, 1 or 2 and the radicals R are, independently of one another, alkyl groups having from 1 to 12, in particular from 1 to 6 and particularly preferably from 1 to 4, carbon atoms (e.g. methyl, ethyl, n- and i-propyl and butyl) and alkylene (in particular ethylene and propylene) mines, for example ethylenediamine, propylenediamine and diethylenetriamine; β-dicarbonyl compounds having from 4 to 12, in particular from 5 to 8, carbon atoms, for example acetylacetone, 2,4-hexanedione, 3,5-heptanedione, acetoacetic acid and C 1-4 -alkyl acetoacetates; and compounds having at least two different functional groups, for example alanine, arginine, asparagine, aspartic acid and other amino acids, and also betaine, EDTA, guanidineacetic acid, guanidinepropionic acid, guanidinebutyric acid, azodicarbonamide, 8-hydroxyquinoline, 2,6-pyridine-dicarboxylic acid, methacrylonitrile, diaminomaleonitrile, acetimide, guanine and guanosine and also guanidine carbonate, guanidine nitrate and guanidinobenzimidazole.
[0039] Other preferred species A and D for use in the present invention are those in which at least one of the groups B and Y or B and E have the formula -MZ n R 3-n or —AlZ m R 2-m , where M is Si, Ti or Zr, Z is a group which is reactive with a surface group X or W, R are groups which are nonreactive with a surface group X or W and are identical or different groups if (3-n) is equal to 2, n is 1, 2 or 3, preferably 1 or 2, and m is 1 or 2. Of course, it is also possible to use corresponding groups in which M or Al is replaced by Sc, Y, La, Ce, Nd, Nb, Ta, Mo, W, B, etc.
[0040] Among the above groups, particular preference is given to those containing Si. Concrete examples of corresponding species are the following: mercaptopropyltrimethoxysilane, 3-(trimethoxysilyl)propyl methacrylate, 3-(triethoxysilyl)propylsuccinic anhydride, cyanoethyltrimethoxysilane, 3-thiocyanatopropyltriethoxysilane, 3-(2-aminoethylamino)-propyltrimethoxysilane, 3-aminopropyltriethoxysilane, 7-oct-1-enyltrimethoxysilane, phenyltrinethoxy-silane, n-butyltrimethoxysilane, n-octyltrimethoxysilane, n-decyltrimethoxysilane, n-dodecyltriethoxysilane, n-hexadecyltrimnethoxysilane, n-octadecyltrimethoxysilane, n-octadecyltrichlorosilane, dichloromethyl-vinylsilane, diethoxymethylvinylsilane, dimethyloctadecylmethoxysilane, tert-butyldimethylchlorosilane-methyldisilazane, diethoxydimethylsilane, diethyl trimethylsilyl phosphite, 2-(diphenylmethylsilyl)ethanol, diphenylsilanediol, ethyl(diphenylmethylsilyl) acetate, ethyl-2,2,5,5-tetramethyl-1,2,5-azadisilolidine 1-acetate, ethyltriethoxysilane, hydroxytriphenylsilane, trimethylethoxysilane, trimethylsilyl acetate, allyldimethylchlorosilane, (3-cyanopropyl)dimethylchlorosilane and vinyltriethoxysilane.
[0041] For the (separate) surface modification, the particles concerned are usually dispersed in a suitable solvent (dispersion medium) which is inert under the reaction conditions, for example water, an aliphatic or aromatic hydrocarbon such as hexane or toluene or an ether such as diethyl ether, tetrahydropyran or THF or a polar, protic or aprotic solvent (for example an alcohol such as methanol ethanol n- and i-propanol and butanol a ketone such as acetone and butanone, an ester such as ethyl acetate, an amide such as dimethyl-acetamide and dimethylformamide, a sulfoxide or sulfone such as sulfolane and dimethyl sulfoxide) and reacted with the surface-modifier (for example species A or species D) in an appropriate manner (possibly at elevated temperature and/or in the presence of a catalyst).
[0042] Subsequently, the dispersion medium can be removed and the surface-modified material can be, if desired, washed and dried and redispersed in the final dispersion medium (aqueous and/or organic). Examples of suitable dispersion media are the solvents already mentioned above as examples of suitable media for the surface modification.
[0043] The dispersion medium used preferably has a boiling point which makes it possible to remove the same without difficulty by distillation (possibly under reduced pressure). Preference is given to solvents having a boiling point below 200° C., in particular below 150° C., although the use of higher-boiling liquids (e.g. having boiling points >350° C.) is of course also possible.
[0044] In the case of the production of ceramic materials, glasses and composites, the content of (final) dispersion medium is generally from 10 to 90% by volume, preferably from 15 to 85% by volume and in particular from 20 to 80% by volume. The remainder of the dispersion is composed of (modified) starting powders, inorganic and/or organic processing aids and possibly free modifiers (e.g. species A or species D) still present.
[0045] The homogeneous dispersion obtained according to the invention can either be further processed as such (see below) or the dispersion medium is completely or partially removed (e.g. to a desired solids concentration). A particularly preferred method of removing the dispersion medium (in particular when this comprises water) is freeze drying in its various embodiments (e.g. freeze spray drying).
[0046] The homogeneous dispersion or the dry homogeneous multicomponent mixture of ceramic powders obtained by the process of the invention can then be further processed to produce green bodies or sintered bodies. The homogeneous ceramic slip obtainable according to the invention can, for example, be shaped directly to give a green body by means of the shaping methods mentioned in the introduction, e.g. by tape casting, slip casting, pressure casting, injection molding, electrophoresis, gel casting, freeze casting, freeze injection molding or centrifugation.
[0047] Alternatively, as mentioned above, a sinterable powder can be obtained from the slip, for example by filtration, evaporation of the dispersion medium, spray drying or freeze drying. This is then either pressed as such to form a green body or else the sinterable powder is redispersed, preferably using a surfactant as dispersing aid, and this suspension is then processed by one of the abovementioned shaping processes to form a green body. In this embodiment, suitable dispersing aids are, for example, inorganic acids such as HCl, HNO 3 and H 3 PO 4 ; organic acids such as acetic acid, propionic acid, citric acid and succinic acid; inorganic bases such as NaOH, KOH and Ca(OH) 2 ; and organic bases such as primary, secondary and tertiary amines and also tetraalkylammonium hydroxides; organic polyelectrolytes such as polyacrylic acid, polymethacrylic acid, polysulfonic acids, polycarboxylic acids, salts (e.g. Na or NH 4 ) of these compounds, N,N-dialkylimidazolines and N-alkylpyridinium salts; or nonionic surfactants such as polyethylene oxides, fatty acid alkylolamides, sucrose-fatty acid esters, trialkylamine oxides and fatty acid esters of polyhydroxy compounds.
[0048] The green body can finally be sintered at customary temperatures, which in most cases are in the range from 1000 to 2500° C., to give a sintered body. However, in certain cases the usable sintering temperatures can also be significantly lower, e.g. 250° C. or less.
[0049] The following examples serve to illustrate the present invention, but without limiting it.
EXAMPLE 1
Production of Al 2 O 3 /SiC Dispersions According to Variant (a)
[0000] (a) Surface Modification of SiC Powders in Toluene
[0050] A 500 ml three-neck round-bottom flask fitted with precision glass stirrer, reflux condenser and drying tube was charged with 70 ml of toluene whose water content had been determined by means of Karl Fischer titration. To ensure reproducible results, it was made a condition that the water content of the toluene used had to be within a range of 0.10±0.04% by weight
[0051] 1.27 g of aminoethylaminopropyltrimethoxysilane or 1.74 g of 3-(triethoxysilylpropyl)succinic anhydride were dissolved in a further 30 ml of toluene and added while stirring to the three-neck round-bottom flask. After addition of 50 g of SiC powder (UF 45, Lonza), the suspension was held at 130° C. for 5 hours. The modified SiC powder was then filtered off and washed three times with 100 ml each time of toluene. After drying for 16 hours at 120° C. in a drying oven, the powder was milled for production of the slip.
[0052] An analogous experimental procedure was also used for the modification of Si and B 4 C. For 50 g of each of the powders, use was made of 2.46 g (B 4 C) or 0.68 g (Si) of 3-(triethoxysilylpropyl)succinic anhydride or 1.80 g (B 4 C) or 0.49 g (Si) of aminoethylaminopropyltrimethoxysilane.
[0053] (b) Combining Al 2 O 3 and SiC
[0054] 2 g of a double-comb polymer having acid functional groups (Dapral EN 1469, ICI) were dissolved in 100 ml of distilled water and then 5.6 g of the SiC powder surface-modified with aminoethylaminopropyltrimethoxysilane as described in (a) were added and dispersed by means of ultrasound. This was followed by the addition of 128 g of Al 2 O 3 powder (CS 400 M, Martinswerk). The resulting suspension was predispersed by means of ultrasound, while the final homogenization of the suspension was carried out by milling for 2 hours in a stirred ball mill (1000 rpm).
[0055] Since the surface-chemical properties of SiC were, as a result of the previous modification of this, essentially the same as those of Al 2 O 3 , a homogeneous, stable two-component suspension having a solids content of 35% by volume and an SiC content of 5% by volume could be produced. The viscosity of the suspension was 12 mPa.s at a shear rate of 200 s −1 . Shaped bodies having relative green densities of 59-62% were produced from this slip by slip casting in plaster moulds, and these shaped bodies were sintered at 1800° C. in a flowing nitrogen atmosphere to give sintered bodies having a relative density of above 98%. The sintered bodies had a homogeneous distribution of the SiC particles. The mean grain size of the sintered bodies was between 2 and 2.5 μm, while strengths between 650 and 700 mPa were measured.
[0056] Surprisingly, the pressureless densification at 1800° C. thus leads to very high densities while maintaining an extremely fine microstructure. This can only be attributed to a significantly improved homogeneity of the slip.
EXAMPLE 2
Chemical Coating of SiC with Nanosize Carbon Black According to Variant (b)
[0057] 3.75 g of carbon black having surface carboxyl groups (EW 200) were placed in one liter of toluene. While stirring, 150 g of the SiC powder modified with aminoethylaminopropyltrimethoxysilane as described in Example 1 (a) were added. After addition was complete, the suspension was reacted for 5 hours at 130° C. using a water separator. After this reaction time, the modified powder was filtered off, washed three times with 100 ml each time of toluene and dried at 110° C. for 16 hours in a drying oven. This gave a visually homogeneous, deep black powder.
EXAMPLE 3
Production of Al 2 O 3 /TiN Slips Containing Nanosize TiN by Electrostatic Coating According to Variant (c)
[0058] Al 2 O 3 slips containing between 1 and 5% by volume of TiN were produced by a procedure similar to Example 1. The production of homogeneous Al 2 O 3 /TiN slips by electrostatic coating is based on the zeta potentials of Al 2 O 3 and TiN which have opposite signs in the pH range between 3 and 8. The composite slip was produced in the following manner:
[0000] (a) Production of an Aqueous Al 2 O 3 Suspension
[0059] To produce an aqueous Al 2 O 3 suspension (Al 2 O 3 powder AKP 50 from Sumitomo), the corresponding amount of water was initially charged and a weighed amount of Al 2 O 3 powder was slowly added while stirring continuously. The pH was maintained at values between 3 and 4 by addition of HCL. The suspension was meanwhile treated with ultrasound in order to achieve effective dispersion.
[0000] (b) Production of a Nanodisperse TiN Suspension
[0060] The procedure was similar to (a), with the TiN used being a nanosize powder surface-modified by a method similar to Example 1(a). The pH of the suspension was kept between 3 and 9 by means of tetrabutylammonium hydroxide.
[0000] (c) Production of the Final Dispersion
[0061] The Al 2 O 3 and TiN suspensions produced in (a) and (b) above were mixed together while stirring continuously and treated with ultrasound. After mixing the two suspensions, the pH of the composite slip was between 4 and 5.
[0000] (d) Further Processing
[0062] The composite slip was stabilized by addition of a nonionic protective colloid in a concentration of 2% by weight (based on Al 2 O 3 and TiN) (Tween® 80, ICI).
[0063] The amounts of dispersion medium (water), Al 2 O 3 and TiN and also the ratio Al 2 O 3 /TiN were such that slips containing from 1 to 5% by volume of nanosize TiN and from 20 to 30% by volume of solids were obtained (see Table 1).
[0064] The resulting slips can be used directly for shaping processes such as slip casting or pressure slip casting or, after being concentrated, can be processed to give extrusion compositions. Green bodies produced by slip casting had an extremely homogeneous distribution of the nanodisperse TiN particles in the Al 2 O 3 matrix.
TABLE 1 Numerical example for the production of 20 or 30% strength by volume Al 2 O 3 /TiN composite slips having TiN contents of from 1 to 5% by volume (for 100 ml of slip) Solids content [% by volume] TiN content 20 30 [% by volume] Al 2 O 3 suspension TiN suspension Al 2 O 3 suspension TiN suspension 1.0 78 g Al 2 O 3 in 1 g TiN in 118 g Al 2 O 3 in 1.56 g TiN in 50 ml H 2 O, 30 ml H 2 O, 60 ml H 2 O, 10 ml H 2 O, pH = 3-4 pH = 8-9 pH = 3-4 pH = 8-9 Protective colloid 1.58 g 2.40 g 2.5 77 g Al 2 O 3 in 2.6 g TiN in 116 g Al 2 O 3 in 3.90 g TiN in 50 ml H 2 O, 30 ml H 2 O, 60 ml H 2 O, 10 ml H 2 O, pH = 3-4 pH = 8-9 pH = 3-4 pH = 8-9 Protective colloid 1.59 g 2.41 g 5.0 75 g Al 2 O 3 in 5.21 g TiN in 113 g Al 2 O 3 in 7.8 g TiN in 50 ml H 2 O, 30 ml H 2 O, 60 ml H 2 O, 10 ml H 2 O, pH = 3-4 pH = 8-9 pH = 3-4 pH = 8-9 Protective colloid 1.60 g 2.42 g
EXAMPLE 4
Production of Homogeneous Al 2 O 3 /SiC Composite Slips by Electrostatic Coating According to Variant (c)
[0065] Owing to different surface-chemical properties, the Al 2 O 3 and SiC particles in aqueous suspensions have surface charges with opposite signs in the pH range between 3 and 8. Thus, the prerequisites for electrostatic coating of Al 2 O 3 with SiC (or vice versa) are met in this pH range.
[0066] Based on this principle, aqueous Al 2 O 3 slips having SiC contents between 5 and 15% by volume were produced in the following manner:
[0000] (a) Production of an Aqueous Al 2 O 3 Suspension
[0067] To produce an aqueous Al 2 O 3 suspension (Al 2 O 3 powder CS 400 m, Martinswerk, d 50 ˜400 nm), the appropriate amount of deionized water was initially charged and a weighed amount of Al 2 O 3 powder was added while stirring continuously. The pH was maintained at values between 3 and 4 by addition of HCl. The suspension was meanwhile treated with ultrasound so as to achieve effective dispersion.
[0000] (b) Production of the Aqueous SiC Suspension
[0068] The procedure was similar to (a), with the SiC powder used being the powder surface-modified according to Example 1(a) (TF 45, Lonza; mean particle size 90 nm). The pH of the suspension was maintained between 6 and 7 by addition of dilute ammonia.
[0000] (c) Production of the Final Dispersion
[0069] The suspensions produced as described in (a) and (b) above were mixed while stirring continuously. After the reaction, the pH of the resulting slip was between 4 and 5.
[0000] (d) Further Processing
[0070] The composite slip was stabilized by addition of a nonionic protective colloid (Tween® 80, ICI) in a concentration of 2% by weight based on total solids.
[0071] The slips produced are summarized in Table 2.
[0072] On the slips containing 5% by volume of SiC and having solids contents of 30% by volume, viscosities of 16 mPa.s were measured at shear rates of 200 s − . Slip casting of this slip in plaster moulds gave green bodies having green densities between 0.56 and 0.58 which had a very homogeneous SiC distribution in the Al 2 O 3 matrix. These green bodies were subjected to pressureless sintering at 1800° C. in a flowing nitrogen atmosphere to form sintered bodies having relative densities of over 98% on which flexural strengths of over 700 MPa were measured. The homogeneous SiC distribution in the green bodies led, after sintering, to a microstructure having mean grain sizes between 2 and 3 μm, which was very fine for an Al 2 O 3 powder having mean starting particle sizes of 400 nm and for a sintering temperature of 1800° C.
TABLE 2 Numerical example for the production of 20 or 30% strength by volume Al 2 O 3 /SiC composite slips having SiC contents between 5 and 15% by volume (for 100 ml of slip) Solids content [% by volume] SiC content 20 30 [% by volume] Al 2 O 3 suspension SiC suspension Al 2 O 3 suspension SiC suspension 5.0 75.6 g Al 2 O 3 in 3.2 g SiC in 113 g Al 2 O 3 in 4.8 g SiC in 70 ml H 2 O, 10 ml H 2 O, 60 ml H 2 O, 10 ml H 2 O, pH = 3-4 pH = 6-7 pH = 3-4 pH = 6-7 Protective colloid 1.57 g 2.35 g 10 71.4 g Al 2 O 3 in 6.4 g SiC in 107 g Al 2 O 3 in 9.6 g SiC in 70 ml H 2 O, 10 ml H 2 O, 60 ml H 2 O, 10 ml H 2 O, pH = 3-4 pH = 6-7 pH = 3-4 pH = 6-7 Protective colloid 1.55 g 2.33 g 15 67.5 g Al 2 O 3 in 9.69 g SiC in 101.2 g Al 2 O 3 in 14.4 g SiC in 60 ml H 2 O, 20 ml H 2 O, 55 ml H 2 O, 15 ml H 2 O, pH = 3-4 pH = 6-7 pH = 3-4 pH = 6-7 Protective colloid 1.54 g 2.31 g
[0073] The following examples further illustrate the surface modification of particles suitable for producing ceramic materials.
EXAMPLE 5
Surface Modification of Carbon Black
[0074] 50 g of carbon black were placed in a 2 l three-neck round-bottom flask fitted with precision glass stirrer, reflux condenser and drying tube. To this carbon black were added 1.3 l of toluene whose water content had been determined prior to the modification reaction by means of Karl-Fischer titration. To ensure reproducible results, it was made a condition that the water content of the toluene used had to be within a range of 0.10±0.04% by weight
[0075] 45.4 g of aminoethylaminopropylsuccinic anhydride were dissolved in a further 0.2 l of toluene and added while stirring to the three-neck round-bottom flask. The resulting suspension was held at 130° C. for 5 hours, whereupon the surface-modified carbon black was filtered off and washed three times with 100 ml each time of toluene. After drying for 16 hours at 120° C. in a drying oven, the powder was milled.
EXAMPLE 6
Surface Modification of B 4 C
[0076] A 500 ml three-neck round-bottom flask fitted with precision glass stirrer, reflux condenser and drying tube was charged with 70 ml of toluene whose water content had been determined prior to the modification reaction by means of Karl-Fischer titration. To ensure reproducible results, it was made a condition that the water content of the toluene used had to be within a range of 0.10±0.04% by weight
[0077] 1.80 g of aminoethylaminopropyltrimethoxysilane or 2.46 g of 3-(triethoxysilylpropyl)succinic anhydride were dissolved in a further 30 ml of toluene and added while stirring to the three-neck round-bottom flask. After addition of 50 g of B 4 C, the suspension was reacted for 5 hours at 130° C., whereupon the modified powder was filtered off and washed three times with 100 ml each time of toluene. After drying for 16 hours at 120° C. in a drying oven, the powder was milled for the production of the slip.
EXAMPLE 7
Surface Modification of n-TiN Powder
[0078] For the modification of n-TiN powder, 200 ml of H 2 O/methanol mixtures (1:1) were placed in a three-neck flask fitted with reflux condenser and drying tube and 0.7 g of guanidinepropionic acid was added thereto. After the guanidinepropionic acid had dissolved while heating and stirring, 10 g of n-TiN powder were added in portions while stirring, whereupon the mixture was heated under reflux (90° C.) for 4 hours. The hot suspension was then filtered through a suction filter (pore width: 3-6 μm) and the residue was washed thoroughly with the H 2 O/ethanol mixture, whereupon the filter cake was dried for 10 hours at 90° C. The dried powder could be redispersed to a mean particle size of down to 40 nm.
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A process for producing a dispersion of at least two types of finely divided particles. The process comprises providing at least a first type and a second type of finely divided particles with opposite surface charges and particle sizes which differ by a factor of at least three, and combining the particles and a dispersion medium and forming a substantially homogeneous dispersion of the at least two types of finely divided particles.
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FIELD OF THE INVENTION
[0001] The present invention relates to electronic packaging and, more particularly, to chip packaging.
BACKGROUND
[0002] It has long been desirable to be able to pack as many chips into as small a space as possible. More recently, this has led to the development of various integration techniques.
[0003] One such integration method, shown in FIG. 1 , involves directly attaching one die 102 onto a second die 104 . This allows the top die 102 and bottom die 104 to communicate directly with each other. In addition, the two chips 102 , 104 are externally connected using wirebonds 106 connected to the chip(s) via a routing trace 108 . While this approach results in a smaller package, it also results in a problem if the two chips are the same size or of nearly the same size, because, in some cases, there might not be enough room for wirebond pads 110 to exist on one of the dies. Moreover, using this approach with multiple chips (e.g. by stacking several of these two chip units on top of one another in a multi-chip on multi-chip arrangement is both difficult and expensive if wirebonds 106 must be used.
[0004] Another integration option, shown in FIG. 2 , is to use solder ball 202 , flip-chip attachment methods to allow the two die stack to be externally connected. This approach is cheaper than the wirebond approach and, thus, can allow some of the multi-chip on multi-chip arrangements ( FIG. 3 ) to be more easily or cheaply achieved. However, this integration option suffers from the same problem as noted above if the two chips are the same or nearly the same size, because there might not be enough room for solder ball pads to exist on one of the dies.
[0005] Still further, the process of stacking the multi-chips ( FIG. 3 ) would require each of the dies to be very, very thin so that the height of the chip 102 that would attach to the chip 104 containing the solder bump pads will be less than the height of a solder ball bump 202 itself. Compounding the problem is the fact that the multi-chip on multi-chip stack's overall height will likely also have to be small so that it can fit within standard packages. This requires handling many wafers or dies that are very thin and then performing dual side processing on these thin wafers. As a result, there is a significant risk of yield loss and damage to dies, especially if solder balls 202 must be mounted on those very thin pieces.
[0006] Yet another integration option, shown in FIG. 4 , is to use a passive device known as an “interposer” 402 that can act as a routing element to connect the two dies together and externally. This approach has the advantage that it eliminates the issue of whether the two dies 404 , 406 are identical or close in size because it can always be made big enough to accommodate a wirebond or solder bump connection. However, interposers typically also have has significant drawbacks. For example, they usually require fabrication of an entirely new part (the interposer with its attendant routing 408 ) which could be complicated and expensive. Moreover, the typical interposer option does not eliminate the issue of handling very thin wafers or doing dual-side processing of those very thin wafers, so the above-mentioned decreased yield and increased damage risks remain. Still further, interposers are typically very thick, so, even if the interposer has through-connections 408 , the length of the connections between the two dies are now larger, so the electrical performance of the chip to chip connection can be degraded.
[0007] The interposer option also does not dispense with the problems noted above with creating a multi-chip to multi-chip stack ( FIG. 5 ).
[0008] In addition, with such an approach it may be necessary to use vias in chips containing active devices which, in some applications, might not be desirable because they take up potential circuit area, increase the risk of yield loss, or both.
[0009] Yet further, to add a third ‘chip’ to the stack, each of the individual chips must be even thinner than the option that only had two chips, thereby further adding to the risks of decreased yield and damage.
[0010] Thus, there is a need for a packaging option that does not suffer from the problems and/or risks presented by the foregoing options presently available.
SUMMARY OF THE INVENTION
[0011] We have developed a process for integrating chips together that reduces or eliminates the problems present with the above processes.
[0012] Depending upon the particular variant, our approaches can provide one or more of the following benefits: they can be used with two chips of any arbitrary size, they can allow the final stack height to be very thin so that multi-chip on multi-chip configurations can be created, they can eliminate the need to make vias in an active chip, they can eliminate the need to make through-die vias entirely (i.e. whether or not the die contains devices), they can eliminate the need for a specially created interposer chip, they involve a thick and stable platform, they eliminate the need to perform dual-side processing of the individual die, and they still allow for the use of small, dense connections without the electrical performance ‘hit’ imposed by an interposer through-via structure.
[0013] One example variant involves a packaging method. The method involves attaching a first chip to a stable base, forming contact pads at locations on the stable base, applying a medium onto the stable base such that it electrically insulates sides of the first chip, forming electrical paths on the medium, attaching a second chip to the first chip to form an assembly, and removing the stable base.
[0014] Another example variant involves a package having at least two chips electrically connected to each other, at least one contact pad, an electrically conductive path extending from the contact pad to a contact point on at least one of the chips, a planarizing medium, and a coating material on top of the planarizing medium.
[0015] Through use of one or more of the variants described herein, one or more of various advantages described herein can be achieved. The advantages and features described herein are a few of the many advantages and features available from representative embodiments and are presented only to assist in understanding the invention. It should be understood that they are not to be considered limitations on the invention as defined by the claims, or limitations on equivalents to the claims. For instance, some of these advantages are mutually contradictory, in that they cannot be simultaneously present in a single embodiment. Similarly, some advantages are applicable to one aspect of the invention, and inapplicable to others. Thus, this summary of features and advantages should not be considered dispositive in determining equivalence. Additional features and advantages of the invention will become apparent in the following description, from the drawings, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 illustrates, in overly simplified form, a chip stack having a wirebond external connection;
[0017] FIG. 2 illustrates, in overly simplified form, a chip stack having a solder ball external connection;
[0018] FIG. 3 illustrates, in overly simplified form a chip on chip stack;
[0019] FIG. 4 illustrates, in overly simplified form an interposer-based approach to chip stacking;
[0020] FIG. 5 illustrates, in overly simplified form an interposer-based multi-chip to multi-chip stack;
[0021] FIG. 6 illustrates, in overly simplified form, an example stable base suitable for use as the starting point;
[0022] FIG. 7 illustrates, in overly simplified form, the example stable base after the support coating has been applied;
[0023] FIG. 8 illustrates, in overly simplified form, an enlarged portion of the example stable base after the openings have been formed in the support coating;
[0024] FIG. 9 illustrates, in overly simplified form, an enlarged portion of the example stable base after pads have been formed within what was the openings in the support coating;
[0025] FIG. 10 illustrates, in overly simplified form, the enlarged portion of the example stable base after all of the first chips for the enlarged portion have been attached to the stable base;
[0026] FIG. 11 illustrates, in overly simplified form, the enlarged portion of the example stable base after planarization down to the surface of the first chip;
[0027] FIG. 12 illustrates, in overly simplified form, the enlarged portion of the example stable base after removal of the planarizing medium in some areas to expose at least the pad body;
[0028] FIG. 13 illustrates, in overly simplified form, the enlarged portion of the example stable base after formation of the contacts;
[0029] FIG. 14 illustrates, in overly simplified form, the enlarged portion of the assembly after the second chips have been attached to it;
[0030] FIG. 15 illustrates, in overly simplified form, the complex assembly of FIG. 14 after addition of the coating material;
[0031] FIG. 16 illustrates, in overly simplified form, the complex assembly of FIG. 15 after removal of the stable base;
[0032] FIG. 17 illustrates, in overly simplified form, the complex assembly of FIG. 16 after addition of the conductive bonding material;
[0033] FIG. 18 illustrates, in overly simplified form, two individual packaged units following dicing from the complex assembly of FIG. 15 ;
[0034] FIG. 19 illustrates, in overly simplified form, an enlarged portion of the example stable base after formation of the contacts;
[0035] FIG. 20 illustrates, in overly simplified form, the enlarged portion of the assembly after the second chips have been attached to it to form a more complex assembly;
[0036] FIG. 21 illustrates, in overly simplified form, the complex assembly of FIG. 20 after addition of the coating material as described above;
[0037] FIG. 22 illustrates, in overly simplified form, the complex assembly of FIG. 21 after removal of the stable base as described above;
[0038] FIG. 23 illustrates, in overly simplified form, the complex assembly of FIG. 22 after addition of the conductive bonding material as described above,
[0039] FIG. 24 illustrates, in overly simplified form, two individual packaged units following dicing from the complex assembly of FIG. 22 as described above;
[0040] FIG. 25 illustrates, in overly simplified form, a variant in which an individual packaged unit from the first family approach is externally connected to a pad of an interposer via a solder ball bump;
[0041] FIG. 26 illustrates, in overly simplified form, a variant in which an individual packaged unit from the first family approach is externally connected to some other element by wirebond connections;
[0042] FIG. 27 illustrates, in overly simplified form, a variant in which an individual packaged unit from the second family approach is externally connected to a pad of an interposer via a solder ball bump; and
[0043] FIG. 28 illustrates, in overly simplified form, a variant in which an individual packaged unit from the second family approach is externally connected to some other element by wirebond connections.
DETAILED DESCRIPTION
[0044] The approach will now be described with reference to two simplified example major implementation variants. The first simplified example implementation family, shown in FIGS. 6 through 18 , involves creation of a chip package that contains a stack of two chips of differing size in which the initial chip in the stack is smaller in extent than the chip that will be stacked on top of it. The second simplified example implementation family involves creation of a chip package that contains a stack of two chips of differing size in which the initial chip in the stack is larger in extent than the chip that will be stacked on top of it. These two major examples are used because they illustrate the two extremes, with all other examples, including equally sized chips, falling between the two.
[0045] Notably, in the interest of brevity, only the steps pertinent to understanding the approach are described. Thus, there may be additional straightforward intermediate steps that may need to be performed to go from one described step to another. However, those intermediate steps will be self evident to the pertinent audience. For example, as described a step may involve depositing a metal in a particular area. From that description, it is to be understood that, absent express mention of a process and that it is the required or only way to accomplish the transition, any suitable known intermediate process can be used. For example, one variant may involve, applying a photoresist, patterning, metal deposition, stripping of the photoresist and, if appropriate, removal of overburden. Another variant might involve electroless or electroplating and thus patterning, seed deposition, etc. Thus, unless expressly stated otherwise, it should be presumed that any known way to get from one point in the process to another point in the process can be used and will be acceptable.
[0046] The process begins with a piece of material that will act as a stable base for most of the process, but will later be removed. Depending upon the particular implementation, this base can be any of a number of different things, for example, a silicon wafer that can later be removed through an etching process, or a material such as glass, sapphire, quartz, a polymer, etc. the relevant aspects being i) that the material that will be used as the base has sufficient rigidity and stability to withstand the processing steps described below, and ii) that the material can be removed when necessary in the process using a technique that will not damage the package created up to that point, irrespective of whether the process involves removal by chemical, physical or heat action (or some combination thereof) or some other process.
[0047] The purpose of the material is to primarily provide mechanical support during the processing steps and thereby avoids the thin wafer handling problems noted above because, to the extent “thin” components are involved, they are handled at the chip level, while still allowing the major steps to be performed at the wafer level.
[0048] Advantageously, through this approach, the contact formation and use techniques as described in U.S. patent application Ser. Nos. 11/329,481, 11/329,506, 11/329,539, 11/329,540, 11/329,556, 11/329,557, 11/329,558, 11/329,574, 11/329,575, 11/329,576, 11/329,873, 11/329,874, 11/329,875, 11/329,883, 11/329,885, 11/329,886, 11/329,887, 11/329,952, 11/329,953, 11/329,955, 11/330,011 and 11/422,551, all incorporated herein by reference, can be employed, even though through-chip vias need not be part of the techniques described herein, although they are not incompatible, and thus can be used, with some implementations.
[0049] The process will now be described with reference to the figures, bearing in mind that dimensions are not to scale and are grossly distorted for ease of presentation even though specific dimensions may be provided for purposes of explanation.
[0050] FIG. 6 illustrates, in overly simplified form, an example stable base 600 suitable for use as the starting point. The stable base 600 of this example is a wafer of silicon that is about 300 mm in diameter and 800 μm thick.
[0051] Initially, a thin layer of support coating 702 , for example about 0.5 μm, is applied to a surface 704 of the stable base 600 . Depending upon the method to later be used to remove the stable base 600 , as described below, the support coating 702 can be selected to be a material that can act as an etch stop for later processing, a release layer to ultimately allow the clean removal of the stable base 600 material without damaging the chips and connections that will be added in later steps, or both.
[0052] Depending upon the particular implementation, the support coating 702 can be an oxide or other dielectric, a polymer, a metal, a deposited semiconductor material, or some combination thereof.
[0053] In one example variant, the support coating 702 is simply used as an etch stop that will be left in place when processing is finished.
[0054] In another example variant, the support coating 702 is used as an etch stop that will be removed in a later processing step.
[0055] In yet another example variant, the support coating 702 is used as a release layer that, by etching, causes separation of the stable base 600 from the subsequently deposited parts (which will be discussed in greater detail below).
[0056] In still another example, the support coating 702 is a combination. In the combination case, for example, a metal could be added as an etch stop and then, subsequently, a dielectric could be deposited to prevent the connection pads that, will be created in a later step described below, from being shorted after the final work was done. In this specific example case, the dielectric would therefore remain while the metal that would be used as an etch stop will ultimately be removed.
[0057] FIG. 7 illustrates, in overly simplified form, the example stable base 600 after the support coating 702 has been applied. For purposes of this example explanation, the support coating 702 is a dielectric.
[0058] Next, openings 802 are formed in the support coating 702 in the areas where the ultimate connection pads will be. The openings 802 extend down to the support material so that the final contacts that will be created in those openings 802 will be accessible after the stable base 600 is removed.
[0059] Depending upon the particular implementation, the openings can be created using any approach suitable for the particular support coating 702 used.
[0060] FIG. 8 illustrates, in overly simplified form, an enlarged portion 800 of the example stable, base 600 after the openings 802 have been formed in the support coating 702 . For purposes of this example explanation, the openings have been formed by patterning and etching.
[0061] Next, the pads 902 for the ultimate contacts are formed. Depending upon the particular implementation variant, the pads 902 can be sized and of materials that are suitable for conventional solder connections or wirebond connection pad or can be made up of materials suitable for other types of connection contacts, for example, those suitable for use with a post and penetration connection or the other types of connections described in the above-incorporated applications, as well as gold stud bumps, copper pillars, or combinations of suitable metals like solder tipped copper pillars, gold covered copper, etc or alloys. In addition, the layers could incorporate, as described below in connection with FIG. 17 , conductive bonding material so that they do not have to be separately placed later in the process.
[0062] FIG. 9 illustrates, in overly simplified form, the enlarged portion of the example stable base 600 after pads 902 have been formed within what had been the openings 802 in the support coating 702 . As shown, the pad 902 is made up of a layer 904 of deposited gold underlying a pad body 906 of copper. In some variants, the pad 902 could be or contain a conventional under-bump-metal (UBM) set of materials, for example, nickel/gold. In other variants, it could be a conventional aluminum or copper pad with nickel or gold as a barrier or oxidation barrier. Note additionally, the layer 904 could additionally have something underneath it, for example, a solid material, or one of a “malleable” or “rigid” material as described in the above-incorporated applications, to allow for different types of stacking options. In some variants, these materials could be attached to or partially embedded in the stable base 600 at appropriate locations prior to starting the process. Finally, although the specific materials described are all electrically conducting, in some variants, some of the locations for the pad 902 can be filled by materials that are nonconducting (for example, if they are to be used for alignment or spacing purposes).
[0063] Next, the first chip 1002 is placed and attached to the stable base 600 , in this case so that it is “face-up” (i.e. the circuitry on the chip faces away from the stable base 600 ). In the case of a chip that does not have through-vias, the chip is attached in any way suitable for forming a physical connection between the first chip 1002 and the stable base 600 . Depending upon the particular implementation, the attachment can involve using, for example, epoxy, solder, covalent bonding, a tack and/or fuse connection, thermo compression, wafer fusion, copper fusion, adhesive or thermal release bonding tapes or films, etc.
[0064] Alternatively, and advantageously, in some implementation variants, the pad 902 can even be configured to later serve as a wirebond or flip chip pad, as the flip chip bump itself or as a combination of a pad and bump.
[0065] Optionally, if the first chip 1002 has conventional through-chip vias, or throughchip connections or vias such as described in the above-incorporated applications, the first chip 1002 can be attached “face-down” so it makes contact from the bottom.
[0066] Depending upon the particular implementation, the first chip 1002 may have undergone additional processing pre- or post-dicing from its original wafer. However, the last processing step for the first chip 1002 prior to use in this process should ideally be either that the wafer is thinned and then the individual chips diced from it, or the chips are diced from the wafer and then thinned so that only the individual chips are handled in thin form.
[0067] FIG. 10 illustrates, in overly simplified form, the enlarged portion 800 of the example stable base 600 after all of the first chips 1002 for the enlarged portion have been attached to the stable base 600 .
[0068] Once the first chip 1002 has been attached to the stable base 600 , the surface of the stable base 600 is planarized using a planarizing medium 1102 .
[0069] Depending upon the particular implementation variant, the planarizing medium 1102 can be a spin-on glass, polymer, epoxy, dielectric, oxide, nitride or other appropriate material, the important aspects being that the planarizing medium 1102 be non-electrically conducting and will form or can be treated to form a substantially planar surface.
[0070] In some variants, the planarizing medium 1102 is applied so that it is coincident or nearly coincident with the top of the first chip 1002 . In such a case, if the material will naturally form a planar surface, no further processing may be needed within this step. Alternatively, in other variants, the planarizing medium 1102 is applied so that it covers the first chip 1002 and may or may not naturally form a flat surface. In such a case, the planarizing medium 1102 can be planarized by further processing, for example, polishing, lapping, etching, liftoff, developing out material, etc. In another, variant similar to the second case, only the surface 1004 of the first chip 1002 (or some portion thereof) can be re-exposed by, for example, one or more of the foregoing processes. Alternatively, if the first chip is the same size or larger than the contact area of the chip that will be stacked on top of it, simple use of a conformal insulating coating to at least cover the sides of the first chip 1002 can be used if the height of the first chip 1002 is short enough. In general, the pertinent aspect for this step is that a surface is formed such that metal routing layers can later be added without creating open circuits or shorting to the sides of the first chip 1002 .
[0071] FIG. 11 illustrates, in overly simplified form, the enlarged portion 800 of the example stable base 600 after planarization down to the surface 1004 of the first chip 1002 .
[0072] Next, the planarizing medium 1102 is removed in specific areas 1202 to expose the pad body 906 and any other areas which may need to be exposed for purposes of forming connections.
[0073] Advantageously, if the planarizing medium 1102 is a photo-sensitive material, such as a photo-sensitive polyimide, then a simple pattern and expose can be used to make the planarizing medium 1102 ready for this step. Note that as part of this step, etching can be performed wherever it is needed or desired, for example, on top of the first chip 1002 , on top of the pad body 906 (such as shown in FIG. 12 ), on top of some other area, etc., as long as the sides of the first chip 1002 are protected so that undesirable shorting cannot occur to those areas in subsequent steps.
[0074] FIG. 12 illustrates, in overly simplified form, the enlarged portion 800 of the example stable base 600 after removal of the planarizing medium 1102 in some areas to expose at least the pad bodies 902 . Note that, in the example of FIG. 12 , additional etching has been performed on the first chip 1002 to allow for creation of contact posts.
[0075] At this point, metal connections 1302 , 1304 are formed so that, for example, the pad bodies 902 are connected to the first chip 1002 , the pad bodies 902 , other connection points are rerouted to positions which can ultimately align with corresponding connections of another chip or some other element, or (optionally, if needed) elevated contacts 1306 are formed. Of course, in many variants, some combination of both of these will occur and, in some cases, a pad body 902 , can be intentionally connected to another pad body (not shown).
[0076] Because the height of the first chip 1002 can be small, since it is only handled as a die, the opening formed by removal of the planarizing medium 1102 can have a low aspect ratio. This allows the use of a low cost deposition technique or even a simple plating process for making connections. In other words, specialized or advanced via filling techniques are not required and, in fact can be used, and the process can be less costly.
[0077] FIG. 13 illustrates, in overly simplified form, the enlarged portion 800 of the example stable base 600 after formation of the contacts 1302 , 1304 , 1306 .
[0078] At this point, a package assembly 1308 has been created that is suitable for addition of a second chip 1402 onto the first chip 1002 . Thus, in the next step, the second chip 1402 is attached to the assembly 1308 . Note that, because the entire process up to this point has involved a thick substrate (i.e. the stable base 600 ) this process is more robust than with processes where two chips are joined by hybridizing to a very thin substrate. Also note that, although the second chip 1402 can be thin at this point, all the contacts 1404 of the second chip 1402 will ideally have been put on the second chip 1402 while it is still in wafer form and thick; then the wafer containing the second chip 1402 can be thinned, diced and the second chip 1402 chip can be attached to the assembly 1308 .
[0079] Advantageously, it should now be understood that, through use of a variant described herein, dual side processing and thin wafer-scale handling for processing are reduced or, ideally, eliminated.
[0080] Returning to the process, at this point the second chip 1402 is aligned with and attached to the respective connection points of the assembly 1308 . Depending upon the particular implementation variant, this may involve a conventional solder attachment, a tack & fuse approach, a post and penetration connection, covalent bonding, etc.
[0081] Advantageously, where tight-pitch connections (e.g. <50 μm pitch and preferably <30 μm) are used a tack & fuse approach is desirable, although not necessary. Moreover, using low height (<25 μm high) contacts, such as can be formed using approaches from the above-incorporated patent applications, alone or in conjunction with tight pitch connections, are particularly advantageous in keeping the overall height of the final package small.
[0082] It should also now be appreciated that variants of the approaches described herein can have the advantages provided by small contact size and short connection lengths without via parasitics while also having the advantages provided by an the interposer (i.e. overcomes chip size restrictions). Moreover, these advantages can be obtained while allowing thick wafer handling and avoiding or eliminating dual-side processing.
[0083] FIG. 14 illustrates, in overly simplified form, the enlarged portion of the assembly 1308 after the second chips 1402 have been attached to it to form a more complex assembly 1406 .
[0084] At this point, the main processing is complete. However, if additional chips are to be joined to the complex assembly 1406 , the approach of the preceding steps can advantageously and straightforwardly be repeated as necessary.
[0085] Optionally, however, the process can be continued, for example, by adding an additional coating material 1502 to, for example, protect the chips, act as a thermal conductor, or allow the complex assembly 1406 to be planar, etc. Depending upon the particular implementation variant, the coating material 1502 can optionally be a material that is resistant to the etchants that might be used in some cases in the next step. In most implementation variants, the coating material 1502 will be a non-electrically-conductive type of material and, more particularly, one of the materials that were suitable for use as the planarizing medium 1102 . Advantageously, in some cases, the coating material 1502 can also, or alternatively, provide structural support so that the wafer-like assembly created by the process described herein, can be handled in a wafer-like way after the stable base 600 has been removed.
[0086] FIG. 15 illustrates, in overly simplified form, the complex assembly of FIG. 14 after addition of the coating material 1502 .
[0087] Next, the stable base 600 is removed from the complex assembly 1406 . Depending upon the particular material used as the stable base 600 , removal can occur through any of a number of processes, the only constraint being that the process be suitable to achieve the desired removal and expose the stable base 600 side of the pads 902 . Depending upon the particular implementation, the removal can be effected by grinding, lapping and/or etching down to the coating 702 if it is an etch stop layer. If the coating 702 is a sacrificial layer, that layer can be sacrificed by the appropriate process (e.g. heating, etching, chemically reacting, exposing to specific wavelength(s) of light, for example ultra-violet or infra-red, etc.) thereby allowing the complex assembly 1406 to “float away” from the stable base 600 , thereby eliminating the need to remove the stable base 600 in a destructive manner. Thus, for some variants where the sacrificial layer approach is used, the stable base 600 can become reusable, further reducing costs.
[0088] Advantageously, if an etch is used and the support coating 702 , planarizing medium 1102 and coating material 1502 are resistant to that etch process, then the chips in the complex assembly 1406 would be completely protected from the etch, so an aggressive process like a wet etch could be used in a batch process to remove the stable base 600 without concern.
[0089] Following removal of the stable base 600 , the remaining complex assembly 1406 is, if the support coating 702 , planarizing medium 1102 and coating material 1502 are polymer(s), compliant and resistant to cracking.
[0090] FIG. 16 illustrates, in overly simplified form, the complex assembly 1406 of FIG. 15 after removal of the stable base 600 .
[0091] At this point, if, as described in conjunction with FIG. 9 , the pad 902 for the contact was formed such that the bonding material, for example, gold or a solder, was added at the time of pad 902 formation, the complex assembly 1406 will be fully formed and the only thing that need be done after this point to complete the package formation process is to dice the entire wafer into individual packaged units.
[0092] Alternatively, if the now-exposed side of the pad 902 will be used with a conductive bonding material 1702 , like a solder bump or gold ball, for example, the conductive bonding material 1702 can be added at this point. Advantageously, it should be noted that, because the conductive bonding material 1702 is not attached to one of the fragile pieces of silicon there is no stress created on the chips or as would be on an interposer if one were used.
[0093] FIG. 17 illustrates, in overly simplified form, the complex assembly 1406 of FIG. 15 after addition of the conductive bonding material 1702 .
[0094] Finally, the complex assembly 1406 is diced into individual packaged units 1802 . Here too, it should be noted that, even if the individual chips within the complex assembly 1406 were very thin, the risk of damaging them is minimal.
[0095] FIG. 18 illustrates, in overly simplified form, two individual packaged units 1802 following dicing from the complex assembly 1406 of FIG. 15 .
[0096] The second simplified example implementation family will now be described. Due to the fact that the initial steps are the same as described in connection with FIG. 6 through FIG. 12 , those steps will not be reiterated here. Moreover, since this example varies from the first simplified example implementation family only with respect to the relative sizes of the chips in the stack, only those aspects particularly different for such a difference will be discussed.
[0097] Picking up following completion of the steps resulting in FIG. 12 , at this point, metal connections 1902 , 1904 are formed so that, for example, the pad bodies 902 are connected to the first chip 1002 , the pad bodies 902 , other connection points are rerouted to positions which can ultimately align with corresponding connections of another chip or some other element, or (optionally, if needed) elevated contacts 1906 are formed. Of course, as with the example of FIG. 13 , in many variants, some combination of both of these will occur and, in some cases, a pad body 902 , can be intentionally connected to another pad body (not shown).
[0098] FIG. 19 illustrates, in overly simplified form, an enlarged portion 1900 of the example stable base 600 after formation of the contacts 1902 , 1904 , 1906 .
[0099] At this point, as with FIG. 13 , a package assembly 1908 has been created that is suitable for addition of a second chip 2002 onto the first chip 1002 . Thus, in the next step, the second chip 2002 is attached to the assembly 1908 . As with the first example family, note that, although the second chip 2002 can be thin at this point, all the contacts 2004 of the second chip 2002 will ideally have been put on the second chip 2002 while it is still in wafer form and thick; then the wafer containing the second chip 2002 can be thinned, diced and the second chip 2002 chip can be attached to the assembly 1908 .
[0100] At this point the second chip 2002 is aligned with and attached to the respective connection points of the assembly 1908 . As noted above, depending upon the particular implementation variant, this may involve a conventional solder attachment, a tack & fuse approach, a post and penetration connection, covalent bonding, etc.
[0101] FIG. 20 illustrates, in overly simplified form, the enlarged portion of the assembly 1908 after the second chips 2002 have been attached to it to form a more complex assembly 2006 .
[0102] Note that, because the second chip 2002 is smaller in extent than the second chip 1402 , the second chip 2002 does not connect to the peripheral contacts 1902 , 1904 , but rather only connects to the contacts 1906 within the extent of the second chip 2002 . However, through use of routing layers, contacts at the periphery can be routed to be within the extent of the second chip 2002 so that, in effect, the routing can move a contact at the periphery to a different and more centralized location.
[0103] Thereafter the processing proceeds as described in connection with FIG. 15 through FIG. 18 . Thus, FIG. 21 illustrates, in overly simplified form, the complex assembly 2006 of FIG. 20 after addition of the coating material 1502 as described above.
[0104] FIG. 22 illustrates, in overly simplified form, the complex assembly 2006 of FIG. 21 after removal of the stable base 600 as described above.
[0105] FIG. 23 illustrates, in overly simplified form, the complex assembly 2006 of FIG. 22 after addition of the conductive bonding material 1702 as described above.
[0106] FIG. 24 illustrates, in overly simplified form, two individual packaged units 2402 following dicing from the complex assembly 2006 of FIG. 22 as described above.
[0107] From the above it should now be apparent that some of the above steps can be iteratively employed in the same approach to add a third or additional chips.
[0108] Finally for these two families, it should be evident that variants involving two chips of the same size can be processed in the same manner as described above in connection with either the first or second family of implementations.
[0109] Based upon the above, it should advantageously further be appreciated that the above approach is not incompatible with aspects of the wirebond or interposer approaches, should there be a need or desire to employ those as well.
[0110] FIG. 25 illustrates, in overly simplified form, a variant in which an individual packaged unit 1802 from the first family approach is externally connected to a pad 2502 of an interposer 2504 via a solder ball bump 1702 .
[0111] FIG. 26 illustrates, in overly simplified form, a variant in which an individual packaged unit 1802 from the first family approach is externally connected to some other element (not shown) by wirebond connections 2602 .
[0112] FIG. 27 illustrates, in overly simplified form, a variant in which an individual packaged unit 2402 from the second family approach is externally connected to a pad 2502 of an interposer 2504 via a solder ball bump 1702 .
[0113] FIG. 28 illustrates, in overly simplified form, a variant in which an individual packaged unit 2402 from the second family approach is externally connected to some other element (not shown) by wirebond connections 2602 .
[0114] It should thus be understood that this description (including the figures) is only representative of some illustrative embodiments. For the convenience of the reader, the above description has focused on a representative sample of all possible embodiments, a sample that teaches the principles of the invention. The description has not attempted to exhaustively enumerate all possible variations. That alternate embodiments may not have been presented for a specific portion of the invention, or that further undescribed alternate embodiments may be available for a portion, is not to be considered a disclaimer of those alternate embodiments. One of ordinary skill will appreciate that many of those undescribed embodiments incorporate the same principles of the invention and others are equivalent.
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A packaging method involves attaching a first chip to a stable base, forming contact pads at locations on the stable base, applying a medium onto the stable base such that it electrically insulates sides of the first chip, forming electrical paths on the medium, attaching a second chip to the first chip to form an assembly, and removing the stable base. A package has at least two chips electrically connected to each other, at least one contact pad, an electrically conductive path extending from the contact pad to a contact point on at least one of the chips, a planarizing medium, and a coating material on top of the planarizing medium.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an arrangement for making secure from sliding a spigot-and-socket joint for the connection of a pipe end with the socket end of a connecting pipe, which joint utilizes a securing ring axially held on the socket end and with a seal in the base of the socket.
2. The Prior Art
Non-sliding arrangements for spigot-and-socket joints are known in various forms of construction. As regards these, two groups may essentially be distinguished. In a first group of non-sliding arrangements the spigot-and-socket joint is held together by means of a clamp divided into two parts along the direction of the tube axis, this clamp surrounding the spigot-and-socket joint on the external side and being supported on the external periphery of the so-called spigot end of the one pipe and on the external periphery of the socket of the other pipe.
In the second group of spigot-and-socket joints a securing ring is used, this ring, and/or the sealing parts lying at the base of the socket, being so constructed that they can absorb pushing forces acting on the spigot-and-socket joint.
The main task of a non-sliding arrangement without doubt consists of ensuring as reliable as possible an absorption of pushing forces, but the properties afforded by spigot-and-socket joints, i.e. the deflectability and the electric connection of the pipe ends, should at the same time be preserved. In addition, a simple and easy laying of the pipes should be afforded.
The known non-sliding arrangements of both the first and second groups are not in a position to fulfil all the requirements mentioned above. With the non-sliding arrangements of the first group, the deflectability of the tubes is not ensured in the case of the majority of forms of construction. Additionally, since the pipe clamps used are relatively thick-walled, they can be fitted to the external diameter only with difficulty, as they must have an internal diameter which corresponds at least to the largest possible pipe diameter. For this reason provision is made externally for abutments which, e.g., are constructed at the so-called spigot end as a weld bead, at the socket end as an external collar.
With the non-sliding arrangements of the second group, the securing ring may be used to absorb the pushing forces when it is held in axial direction at the socket end. This is the case in particular with the securing ring constructed nowadays mostly as a screw-on ring. The screw-on ring has an external coarse thread which can be screwed in a counterthread arranged on the internal side of the socket. If the securing ring is designed as a press-on ring, it is held in axial direction by means of screws disposed in the socket end. With the securing ring thus constructed, pushing forces can indeed be absorbed, but considerable difficulties are caused when endeavoring to connect those parts which are used for the non-sliding arrangement with the pipe having the so-called spigot end in such a way that this pipe is held non-slidably in the socket. In a known method of construction a clamping ring, which has been slit and is then disposed in the base of the socket is used, which is supported by means of a slanting or arched surface on a slanting surface of the screw-on ring. By means of the slanting surface, a radial force is to be exerted on the clamp ring which thereby is pressed with its internal periphery which has a roughening or grooving onto the external periphery of the pipe with the spigot end. Although the clamp ring is constructed to be flexible by means of additional recesses extending along the direction of the pipe axis, a clamping of the pipe secure from sliding is not achieved, because on the one hand the clamping surface of the clamp ring restricted in its constructional height cannot be kept sufficiently great, and on the other hand the radial force exerted by the screw-on ring is considerably reduced by friction. The other conditions which are to be laid upon a good spigot-and-socket joint are fulfilled by this known construction, i.e., retaining the normal socket pipe dimensions and deflectability of the pipes. However, the non-sliding arrangement itself, as already mentioned, is not completely reliable.
Accordingly, the object of the invention is to construct a non-sliding arrangement of the type first defined above in such a manner that the retaining of the normal socket dimensions, the deflectability of the pipes and also the electric connection between the pipes are ensured, while in addition a satisfactory non-sliding arrangement is achieved.
SUMMARY OF THE INVENTION
This object is achieved according to the invention in that, between the external periphery of the pipe end of the pipe and the internal periphery of the securing ring, a securing part in the form of a sleeve is arranged whose end facing the seal forms an abutment for the securing ring and whose section protruding out of the securing ring at the opposite end can be clamped securely onto the tube by means of a clamping device.
DESCRIPTION OF THE DRAWINGS
The invention will now be understood by reference to the attached drawings and to the following description.
In the Drawings:
FIG. 1 shows a longitudinal section through a spigot-and-socket joint according to a first embodiment of a non-sliding arrangement according to the present invention;
FIG. 2 shows a section through the spigot-and-socket joint along line II--II in FIG. 1;
FIG. 3 shows a longitudinal section through a spigot-and-socket joint according to a further form of embodiment of a non-sliding arrangement according to the present invention;
FIG. 4 shows a section through the spigot-and-socket joint along line IV--IV in FIG. 3;
FIG. 5 shows a longitudinal section through a spigot-and-socket joint according to a further embodiment of a non-sliding arrangement according to the present invention;
FIG. 6 shows a section through the spigot-and-socket joint along line V--V in FIG. 5;
FIG. 7 shows a longitudinal section through a spigot-and-socket joint according to a further embodiment of a non-sliding arrangement according to the present invention; and
FIG. 8 shows a longitudinal section through an embodiment of a non-sliding arrangement for a plug-in socket connection.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the Figures, two pipes 1, 2 are partly represented; of these, pipe 1 has a so-called spigot end 3 and the other pipe 2 has a socket end 4. At the base 5 of the socket end 4 a soft sealing ring 6 is inserted which seals the gap 7 formed between the spigot end 3 and the socket end 4. On the side opposite to the gap side of the sealing ring 6 a supporting ring 8 is disposed, which acts to compress the soft sealing ring 6. In FIG. 3 the supporting ring 8 is missing, but it could be used in this embodiment also.
The external periphery of the spigot end 3 of the pipe 1 is surrounded by a securing element 10 in the form of a sleeve which consists of two half cups 11, 12. The half cups 11, 12 have a collar 14 at their ends facing the seal, including slanting or arched shoulders 15 onto which a securing ring 16, which is designed as a screw-on ring, is supported. The securing ring 16 is provided with an external coarse thread 17 which is screwed into a corresponding internal thread 18 of the socket end 4. The end of the securing element 10 protruding out of the screw-on ring 16 is constructed as a clamp, whose portions 19, 20 form in each instance with the half cups 11, 12 one-piece constructional elements. The clamp portions 19, 20 have tensioning lugs 21, 22, each with a perforation 23, 24, through each of which a screw bolt 23 with a nut 26 passes, by means of which screws the clamp portions 19, 20 are pressed against the external periphery of the pipe 1. So that the half cups 11, 12 effect as good as possible a friction closure with the external surface of the pipe, the internal surfaces of the half-cups 11, 12 are provided with a roughening or friction grooving 27.
In FIGS. 3 and 4, the parts which correspond to those of FIGS. 1 and 2 are similarly denoted and will not be further explained. The securing element 10a is distinguished from the securing element 10 according to FIGS. 1 and 2 only in that the clamp portions 19, 20 and the half-cups 11, 12 are not formed as one piece, but instead are separate from each other. The remainder of the construction of the securing element 10a is the same as in the embodiment according to FIGS. 1 and 2.
So that the clamping effect of the clamp portions 19, 20 is influenced as little as possible by the external diameter tolerances of pipe 1, it is possible to provide the clamp portions with elements extending axially parallel, permitting greater flexibility. These are according to FIG. 2 flat areas 30 or recesses 31 which have been represented only in dotted lines. Such elements of greater flexibility may be disposed in any desired number on the outer and/or inner surface.
Furthermore, the half-cups 11, 12 may be partly split in axial direction. In FIGS. 1 and 2 a slit 32 is provided in each instance on the longitudinal sides situated opposite each other of the securing element, although several such slits 32 may also be provided. In appropriate manner the slits 32 extend to the end facing the seal of the half-cups 11, 12. The divided collar 14 arising as a result can then be pressed better through the screw-on ring 14 against the outer surface of the pipe 1.
As only traction is exerted on the clamp portions 19, 20, these may be made relatively thin-walled, in such a manner that if required the arrangement of areas 30, 31 of greater flexibility or of slits 32 in the sleeve portions may be dispensed with.
If need be, the clamp portions 19, 20 could be disposed close to each other for the arrangement of two or more tensioning bolts 25, as a result of which the clamping surface is increased and thereby the power closure is improved.
With the embodiment according to FIGS. 3 and 4 it would also be possible to provide slits in the portion of the half-cups 11, 12 which protrude over the screw-on ring 16, these slits being staggered in relation to the slits 32 of the portion of the half-cups 11, 12 which faces the seal. In addition, it would be possible to arrange on the clamp portions 19, 20 separated from the half-cups 11, 12, portions of greater flexibility, inside also.
The securing element 10 may, for example, be produced as a casting. In this case it would be simple to provide slits 32 or parts of greater flexibility 30, 31 on the casting pattern, in such a manner that no further processing would be necessary.
The securing element 10a may, however, be made also from relatively thin metal plate, which is quite adequate for the absorption of the pushing forces. The clamp portions 19, 20 would be separate portions appropriately in this case. The collar 14 on the metal plate sleeve 10a may, for example, be secured by means of brazing.
It is essential for the described securing element 10, 10a that the transmission of the pushing forces from the screw-on ring 16 onto the collar 14 on the one hand, and from the half-cups 11, 12 onto the outer surface of the tube 1 should take place at different points. Indeed, the screw-on ring 16, because of the slanting shoulders 15 of the collar 14, also exerts a holding force, but this is limited in view of the narrow area conditions. This drawback is eliminated with the securing element 10 described, in that outside the screw-on ring 16 a clamping force can be produced that is so great that a reliable non-sliding arrangement is presented. Indeed, in this connection, it is necessary to make the perforation of the screw-on ring 16 so great that the half-cups 11, 12 find room between the external circumference of the pipe 1 and the internal periphery of the screw-on ring 16. The weakening of the screw-on ring 16 associated with this may be tolerated because of the small wall thickness that is necessary for the half-cups 11, 12, in particular when the screw-on ring 16 is made of a cast iron of greater toughness, e.g., spheroidal graphite iron. If need be, the wall thickness of the securing portion can be reduced further, if it consists only in one portion which has only one slit extending along the direction of the pipe axis, i.e. the two half-cups are joined together in one piece along one edge.
With the described securing element 10, 10a all the objects that are to be achieved by a good non-sliding arrangement for a spigot-and-socket joint are met: Greater security against pushing forces, bendability of the pipes, and good electrical connection. In addition, any supplementary processing is done away with, so that the tubes 1 can be shortened without drawbacks.
The assembly of the described securing element 10 is very simple. It is first of all inserted into the screw-on ring 16, and pushed together with this onto the spigot end 3 of the pipe 1. After the screw-on ring 16 has been screwed into the socket end 4, the clamp 19, 20 is securely clamped, and thus the non-sliding arrangement is fitted. Because of the reliable non-sliding arrangement it is possible, especially when the pipe dimensions are small, to screw together two or more pipes before laying, and to lower them down together into a pipe ducting trench, in such a manner that the width of the trench can be smaller and it is possible to dispense with corresponding troughs for the screwed sockets in the trench.
It has now been found that with the non-sliding arrangement according to FIGS. 1 to 4 it is possible without difficulty to hold together securely axially spigot-and-socket joints at operational pressures of 16 atmospheres nominal pressure. With greater pipe diameters, e.g. at a nominal diameter 300, however, the non-sliding arrangement is no longer perfectly ensured. This defective security occurs also when the securing element is provided internally with a roughening or grooving. This is not sufficient to improve considerably the friction closure that can be achieved by means of the contraction of the clamp.
Therefore, in order to produce a spigot-and-socket joint in such a manner that a movement of the pipe end in the securing element can be safely avoided in the case of still higher pressures and/or also greater pipe diameters, in a further embodiment of the invention the securing element is appropriately constructed in the upper section, at least partly, as a clamping grid, which is covered by the clamp. By this means it is achieved that in practical terms a positive locking is obtained between the securing element and the spigot end of the one pipe.
In the spigot-and-socket joint according to FIGS. 5 to 8, on the external periphery of the spigot end 3 of the pipe 1, a securing element 10b is mounted, onto which end facing the seal an abutment 14 has been fixed, e.g. welded on. The abutment 14 is appropriately constructed as a ring with a circular cross-section, and extends over the sleeve portion(s). The securing ring 16 constructed as a screw-on ring rests against the abutment 14. The portion of the securing element 10b protruding out of the screw-on ring 16 has a portion constructed as a clamping grid 13. Laid around this clamping (friction) grid portion 13 is a clamp 19, 20, whose tensioning lugs 21, 22 each have a perforation 23, 24 through which a screw bolt 25 with a nut 26 extends. By means of the clamp 19, 20, the said portion 13 of the securing element 10 is pressed against the external periphery of the spigot end 3 of the pipe 1.
By the term clamping grid 13 there is understood a netting-like portion of the upper section of the securing element 10b consisting of cross-bars and openings, whose cross-bars come forward at least partly on one side. Suitable, for example, as a clamping grid is a material described as a stretching grid, which may be produced direct from a metal sheet. By this means it is possible to construct the upper section at least partly as a clamping grid, which thus forms an integral section of the securing element 10b. As may be seen from FIG. 5, the exial expansion of the clamping grid 13 is rather smaller than that of the clamp 19, 20, i.e. the transition from the clamping grid 13 onto the smooth-walled portion of the securing element is covered by the clamp 19, 20. By this means it is achieved that not only on the clamping grid 13, but also on the transition portion, a pressure is applied, for the crosswires of the clamping grid 13 are pressed into the surface of the pipe 1. As a result there arises at the clamping area of the securing element 10b practically a positive locking which permits the transmission of very great axial forces without shifting the spigot end 3 of the pipe in the securing element 10b.
The clamp 19, 20 may be constructed in various ways, e.g. according to FIG. 5, with two portions and and two tension rods 25, 26. The clamp may, however, be constructed also in one or more parts. Then as many tension rods 25, 26 are required as there are parts of the clamp. In the case of large diameters it is also possible to make the clamp so wide that on the tensioning lugs in axial direction two and more tension rods 25, 26 are arranged side by side. The securing sleeve 10b is divided axially and is in one piece according to FIG. 5, as is also the abutment 14. However, it is also possible to subdivide the securing sleeve 10b axially twice or several times, in which event the abutment ring 14 may be subdivided in the same way or also be left in one piece.
In FIG. 7 a representation is given of a non-sliding arrangement whose construction in the area of the clamping grid 13 deviates from the construction according to FIG. 5. The securing sleeve 10b has here in its upper portion openings 29 into which stop cams 28 connected with the clamp 19 engage. The clamping grid 13 forms as in FIG. 5 an integral portion of the securing element 10b. By means of the stop cams 28 it is achieved that the transition zone of the clamping grid 13 is partly balanced in the smooth-walled portion of the securing element 10b, in that a part of the axial forces is led via the clamp 19, 20 and the stop cams 28 directly into the smooth-walled section of the securing element 10b.
The other reference figures in FIG. 7 agree with those of FIGS. 5 and 6 and accordingly will no longer be dealt with.
In FIG. 8 a further form of embodiment of the non-sliding arrangement is represented. The securing element 10b consists here in a smooth-walled lower portion and in a clamping grid 13 separated from it, which lie front face one against the other. So that here a satisfactory non-sliding arrangement may be achieved, the upper portion of the securing element is provided with the openings 29 as in FIG. 7, into which the stop cams 28 of the clamp 19, 20 engage. On the edge of the clamp 19, 20 which lies opposite the stop cams 28, a supporting edge 33 is provided onto which the clamping grid 13 rests. The supporting edge 33 may extend as a continuous or as a divided edge around the internal circumference of the clamp sleeve 19, 20. Appropriately, the stop cams 28 and the supporting edge 33 have in the radial direction a height smaller than the wall thickness of the smooth-walled portion of the securing element 10b.
By means of the clamping grid 13 it is achieved that by means of the cross-wires of the clamping grid drepressions are made into the surface of the pipe 1, by means of which a positive locking between the securing element 10b and the pipe 1 is practically achieved.
In FIG. 8, a plug-in socket connection is represented which deviates from the screwed socket connection represented in FIGS. 5 and 7. In this, the socket end 4 has a holding flange 40 onto which screw hooks 41 with nuts 42 engage. The screw hooks 41 pass through perforations 43 of the securing ring 16 and hold it firmly in axial direction. The securing ring 16 is supported by the abutment and has a number of interruptions 44.
The socket end 4 has an internal flange 45 which defines an annular space designed to receive the soft seal 6. As a result of the place-saving manner of construction, the described non-sliding arrangements may be used practically with all spigot-and-socket joints.
The securing element 10b is appropriately made of metal plate, e.g. about 2.0 to 2.5 mm thick, of which a part is formed as a clamping grid 13. It is also possible to make the clamping grid 13 separately and to join it with the smooth-walled portion of the securing element 10b, e.g. by welding or brazing. The thin-walled securing element 10b adapts itself without difficulty to the unevennesses of the external outline of the pipe.
The securing element can, instead of being made of metal plate, be made as a casting e.g. of ductile cast iron, such as spheroidal graphite iron or the like. When using a casting the securing element may be preferably constructed according to the form of embodiment of FIG. 8, i.e. with separate clamping grid 13.
Furthermore, the securing element 10b has the same advantages as the securing elements 10 and 10a described earlier, i.e., when using them the bendability of the the spigot-and-socket joint, a satisfactory electric connection or transition, and easy laying of the pipe ducting are ensured.
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A spigot and socket connection of the type which comprises a pipe end held within a socket by means of a retaining ring includes a device for securing the connection against sliding of the components. This device comprises a sleeve-like securing element lying between the pipe end and the retaining ring. The securing element carries an abutment which is engaged by the retaining ring, and the element is securely clamped to the external surface of the pipe end.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a reference voltage generating circuit, and more particularly, to a reference voltage generating circuit with high accuracy.
[0003] 2. Description of the Prior Art
[0004] In the fields of digital-to-analog converters (DAC) and analog-to-digital converters (ADC), the allowance range of amplitudes of an input signal is determined according to the relative voltage levels of the positive and negative reference voltages. The noise standard of each circuit in an ADC or DAC is also determined by the allowance range of amplitudes of an input signal. In other words, the larger the relative level of the reference voltage is, the less the design complexity of the noise demands is.
[0005] The relative reference voltage levels generated inside the IC, however, are lower than those generated outside the IC. Therefore, in general, the external voltage source V DD and the ground voltage GND are often utilized to generate needed reference voltages.
[0006] Please refer to FIG. 1 , which is a diagram of a conventional reference voltage generating circuit 100 . As shown in FIG. 1 , the reference voltage generating circuit 100 includes a capacitor C REF , an external capacitor C OFF , and two switches SW 1 and SW 2 . The connections between these components are shown in FIG. 1 and a detailed description is thus omitted here. However, in the following disclosure, the operation of the reference voltage generating circuit 100 is illustrated.
[0007] In a first stage, the switch SW 1 is turned on and the switch SW 2 is turned off. The capacitor C REF samples the external voltage source in the first stage. In a second stage, the switch SW 2 is turned on and the switch SW 1 is turned off. The capacitor C REF redistributes charges with the external capacitor C OFF . The first stage and the second stage are alternatively performed such that the capacitor C REF acts as a resistor. Therefore, the reference voltage generating circuit 100 can be regarded as an RC filtering circuit utilized to filter out noises of the external voltage source. This also means a clean reference voltage V REF (i.e. the noise in the reference voltage V REF is substantially eliminated) can be generated.
[0008] If the aforementioned reference voltage generating circuit 100 is utilized in the sigma-delta DAC or sigma-delta ADC, for the reference voltage generating circuit 100 has to utilize the same capacitor C REF to perform the sampling operation in the first stage and generate the reference voltage V REF in the second stage, as well as the first stage and the second stage correspond to only half of the sampling period of the input signal of the sigma delta modulator, the operational clock which is originally utilized in the sigma-delta ADC (DAC) does not correspond to the first and second stages. Therefore, two additional operational clocks, which can point out the first stage and the second stage, have to be generated for the reference voltage generating circuit 100 . In this way, the complexity of the entire circuit can raise, and a high sampling frequency cannot be utilized.
SUMMARY OF THE INVENTION
[0009] It is therefore one of the primary objectives of the claimed invention to provide a reference voltage generating circuit utilizing a capacitor to sample an external voltage source in a first stage and utilizing another capacitor to generate a reference voltage, to solve the above-mentioned problem.
[0010] According to an exemplary embodiment of the claimed invention, a reference voltage generating circuit for generating a reference voltage according to a predetermined voltage is disclosed. The reference voltage generating circuit comprises: a first capacitor; a second capacitor; a reference voltage sampling capacitor; a first switch, for alternatively coupling the second capacitor to the predetermined voltage, wherein the first switch couples the second capacitor to the predetermined voltage in a first stage such that the second capacitor samples the predetermined voltage; a second switch, for alternatively coupling the second capacitor to the first capacitor, wherein the second switch couples the second capacitor to the first capacitor in a second stage in order to generate the reference voltage; and a third switch, for alternatively coupling the first capacitor to the reference voltage sampling capacitor, wherein the third switch couples the first capacitor to the reference voltage sampling capacitor in the first stage such that the reference voltage sampling capacitor redistributes charges with the first capacitor to generate the reference voltage.
[0011] According to another exemplary embodiment of the claimed invention, a sigma-delta analog-to-digital converter (ADC) is disclosed. The sigma-delta analog-to-digital converter (ADC) comprises: a reference voltage generating circuit, for generating a reference voltage according to a predetermined voltage and a sigma delta modulator, for receiving the reference voltage from the reference voltage sampling capacitor in the first stage and receiving an analog signal in the second stage in order to generate a corresponding digital signal according to the analog signal and the reference voltage. The reference voltage generating comprises: a first capacitor; a second capacitor; a reference voltage sampling capacitor; a first switch, for alternatively coupling the second capacitor to the predetermined voltage, wherein the first switch couples the second capacitor to the predetermined voltage in a first stage such that the second capacitor samples the predetermined voltage; a second switch, for alternatively coupling the second capacitor to the first capacitor, wherein the second switch couples the second capacitor to the first capacitor in the second stage such that the second capacitor redistributes charges with the first capacitor in order to generate the reference voltage; and a third switch, for alternatively coupling the first capacitor to the reference voltage sampling capacitor, wherein the third switch couples the first capacitor to the reference voltage sampling capacitor in the first stage such that the reference voltage sampling capacitor redistributes charges with the first capacitor to generate the reference voltage.
[0012] According to another exemplary embodiment of the claimed invention, a sigma delta digital-to-analog converter (DAC) is disclosed. The sigma delta digital-to-analog converter (DAC) comprises: a reference voltage generating circuit, for receiving a predetermined voltage and filtering the predetermined voltage to generate a reference voltage, and a sigma delta modulator, for receiving the predetermined voltage from the reference voltage sampling capacitor according to a digital signal in the first stage to generate an analog signal. The reference voltage generating circuit comprises: a first capacitor; a second capacitor; a reference voltage sampling capacitor; a first switch, for alternatively coupling the second capacitor to the predetermined voltage, wherein the first switch couples the second capacitor to the predetermined voltage in a first stage such that the second capacitor samples the predetermined voltage and breaks the electrical connection between the second capacitor and the predetermined voltage in a second stage; a second switch, for alternatively coupling the second capacitor to the first capacitor, wherein the second switch couples the second capacitor to the first capacitor in the second stage such that the second capacitor redistributes charges with the first capacitor in order to generate the reference voltage and breaks the electrical connection between the first capacitor and the second capacitor in the first stage; a third switch, for alternatively coupling the first capacitor to the reference voltage sampling capacitor, wherein the third switch couples the first capacitor to the reference voltage sampling capacitor in the first stage such that the reference voltage sampling capacitor redistributes charges with the first capacitor to generate the reference voltage and breaks the electrical connection between the first capacitor and the reference voltage sampling capacitor in the second stage.
[0013] According to another exemplary embodiment of the claimed invention, a reference voltage generating method for receiving a predetermined voltage and filtering the predetermined voltage to generate a reference voltage is disclosed. The reference voltage generating method comprises: utilizing a first capacitor to sample the predetermined voltage in a first stage; coupling the first capacitor to a second capacitor in a second stage such that the first capacitor redistributes charges stored in the first capacitor with the second capacitor to generate the reference voltage; and coupling a reference voltage sampling capacitor to the second capacitor in the first stage to obtain the reference voltage from the second capacitor.
[0014] These and other objectives of the present invention will no doubt become obvious to those of ordinary skill in the art after reading the following detailed description of the preferred embodiment that is illustrated in the various figures and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a diagram of a conventional reference voltage generating circuit.
[0016] FIG. 2 is a diagram of a reference voltage generating circuit according to the present invention.
[0017] FIG. 3 is a diagram of operational clocks utilized in the reference voltage generating circuit shown in FIG. 2 according to the present invention.
[0018] FIG. 4 is a diagram illustrating the reference voltage generating circuit shown in FIG. 2 being utilized in a sigma-delta ADC.
[0019] FIG. 5 is a diagram illustrating that the circuit shown in FIG. 4 is in a first stage.
[0020] FIG. 6 is a diagram illustrating that the circuit shown in FIG. 4 is in a second stage.
[0021] FIG. 7 is a diagram illustrating the reference voltage generating circuit utilized in a sigma-delta DAC according to the present invention.
[0022] FIG. 8 is a diagram illustrating that the circuit shown in FIG. 7 is in a first stage.
[0023] FIG. 9 is a diagram illustrating that the circuit shown in FIG. 7 is in a second stage.
DETAILED DESCRIPTION
[0024] Please refer to FIG. 2 , which is a diagram of a reference voltage generating circuit 200 according to the present invention. As shown in FIG. 2 , the reference voltage generating circuit 200 includes two capacitors C EX and C REF , an external (off-chip) capacitor C OFF , and three switches SW 1 , SW 2 , and SW 3 . The connections between these components are shown in FIG. 2 and a detailed description is thus omitted here. Please note, each switch SW 1 , SW 2 , and SW 3 is marked by a corresponding operational clock.
[0025] Please refer to FIG. 3 , which is a diagram of operational clocks utilized in the reference voltage generating circuit 200 shown in FIG. 2 according to the present invention. When the reference voltage generating circuit 200 lies in a first stage, meaning that the first clock φ 1 is at a high voltage level, the switch SW 3 is turned on, and the switches SW 1 and SW 2 are turned off. The capacitor C EX redistributes charges with the external capacitor C OFF such that a needed reference voltage V REF is generated. When the reference voltage generating circuit 200 lies in a second stage, meaning that the second clock φ 2 is at a high voltage level, the switches SW 1 and SW 2 are turned on, and the switch SW 3 is turned off. The capacitor C EX samples the external voltage source V DD , and store charges in the capacitor C EX . In addition, in the second stage, the reference voltage V REF generated in the previous stage is outputted because the switch SW 2 is turned on.
[0026] The theorems of the reference voltage generating circuit 200 shown in FIG. 2 and the conventional voltage generating circuit 100 are quite similar. The capacitor is frequently switched such that the capacitor acts as a resistor. Therefore, an RC filtering circuit is formed and can be utilized to filter the external voltage source V DD such that the clean reference voltage V REF is generated.
[0027] Please refer to FIG. 4 , which is a diagram illustrating the reference voltage generating circuit 200 shown in FIG. 2 being utilized in a sigma-delta ADC. Please note, because the sigma-delta ADC is well known, those skilled in the art can easily understand the circuit structure of other components. Only the reference voltage generating circuit 200 and an integrator 400 are shown in FIG. 4 , and other components (such as an equalizer, feedback circuit) are omitted here. As is shown in this embodiment, the reference voltage generating circuit 200 utilizes the sampling capacitor Cs, which is originally inside the sigma-delta modulator, as the above-mentioned capacitor C REF to obtain the reference voltage V REF .
[0028] Please note that each switch shown in FIG. 4 is also labeled by a corresponding operational clock. To illustrate simply, the corresponding clock of each switch is the same as the operational clocks shown in FIG. 3 .
[0029] FIG. 5 is a diagram illustrating when the circuit shown in FIG. 4 is in the first stage, meaning that the first clock φ 1 shown in FIG. 3 is at a high voltage level. As shown in FIG. 5 , the sampling capacitor Cs starts to sample an input analog signal A in . In the reference voltage generating circuit 200 , the capacitor C EX redistributes charges of the previous stage with the external capacitor C OFF such that the reference voltage V REF is generated.
[0030] FIG. 6 is a diagram illustrating when the circuit shown in FIG. 4 is in the second stage, meaning that the first clock φ 2 shown in FIG. 3 is at a high voltage level. The polarization of the reference voltage V REF is determined according to the feedback digital signal D (D′) outputted by the sigma-delta ADC. Furthermore, the input analog signal A in sampled in the first stage and the feedback reference voltage are inputted into the integrator 400 through the sampling capacitor Cs. In the reference voltage generating circuit 200 , the sampling capacitor Cs obtains the reference voltage V REF , which is originally stored inside the external capacitor C OFF , and the capacitor C EX simultaneously samples the external voltage source V DD or the ground voltage G ND for the next first stage. Therefore, the entire sigma-delta ADC can be operated correctly to generate needed digital signals.
[0031] Please refer to FIG. 7 , which is a diagram illustrating the reference voltage generating circuit 200 utilized in a sigma-delta DAC according to the present invention. Please note, as the sigma-delta DAC is well known, those skilled in the art can easily understand the circuit structure of other components. Only the reference voltage generating circuit 200 and an integrator 700 are shown in FIG. 7 , and other components, such as an equalizer or a feedback circuit, are omitted here. Furthermore, as is shown in this embodiment, the reference voltage generating circuit 200 also utilizes the sampling capacitor Cs which is originally inside the sigma-delta modulator as the above-mentioned capacitor C REF to obtain the reference voltage V REF .
[0032] Please note that each switch shown in FIG. 7 is labeled by a corresponding operational clock. To illustrate simply, the corresponding clock of each switch is the same as the operational clocks shown in FIG. 3 .
[0033] FIG. 8 is a diagram illustrating when the circuit shown in FIG. 7 is in a first stage, meaning that the first clock φ 1 shown in FIG. 3 is at a high voltage level. As shown in FIG. 8 , the sampling capacitor Cs samples the reference voltage V REF , which is generated by the external capacitor C OFF in the previously stage, according to an input digital signal D (D′). In the reference voltage generating circuit 200 , the capacitor C EX starts to sample the external voltage source V DD or the ground voltage G ND for the next stage.
[0034] FIG. 9 is a diagram illustrating when the circuit shown in FIG. 7 is in the second stage, meaning that the second clock φ 2 is at a high voltage level. At this time, the sampling capacitor Cs inputs the sampled reference voltage into the integrator 700 . In the reference voltage generating circuit 200 , the capacitor C EX redistributes charges with the external capacitor C OFF such that the reference voltage V REF is generated across the two ends of the external capacitor C OFF . Therefore, when the entire circuit is back to the first stage, the sampling capacitor Cs can sample the reference voltage V REF again. The entire sigma-delta DAC can thus operate correctly to generate needed analog signals.
[0035] Please note that the circuits shown in FIG. 4 and FIG. 7 are differential circuits. However, the present invention is not limited to be utilized in the differential circuits. In addition, the present invention can be also utilized in single-ended circuits, which also obeys the spirit of the present invention.
[0036] With a capacitor C EX , the reference voltage generating circuit of the present invention does not need to utilize a same capacitor to generate the reference voltage and sample the external voltage source. The reference voltage generating circuit of the present invention can utilize the original operational clock to work. The conventional two additional operational clocks are eliminated. Therefore, the present invention can reduce the circuit complexity and can be utilized in a high frequency circuit.
[0037] Those skilled in the art will readily observe that numerous modifications and alterations of the device and method may be made while retaining the teachings of the invention. Accordingly, the above disclosure should be construed as limited only by the metes and bounds of the appended claims.
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A reference voltage generating circuit includes: a first capacitor; a second capacitor; a reference voltage sampling capacitor; a first switch for alternatively coupling the second capacitor to a predetermined voltage to allow the second capacitor to sample the predetermined voltage; a second switch for alternatively coupling the second capacitor to the first capacitor to allow the second capacitor to redistribute charges with the first capacitor in order to generate the reference voltage; and a third switch for alternatively coupling the first capacitor to the reference voltage sampling capacitor to allow the reference voltage sampling capacitor to redistribute charges with the first capacitor in order to output the reference voltage.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable
REFERENCE TO A “MICROFICHE APPENDIX”
Not applicable
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to lifting apparatus and accessories, and more particularly to an improved spreader bar lifting apparatus for use with cranes and other lifting devices that use slings. Even more particularly the present invention relates to an improved spreader bar arrangement that includes a main beam or bar that supports a flexible member preferably comprised of a plurality of links or sections, and wherein the links or sections have connectors that enable connections to be made between the links and a load to be lifted or load lines (eg. slings).
2. General Background of the Invention
Spreader bars are commonly used in industry for lifting large objects with a single hook that is attached to the crown block and lift cables of a crane. A lifting hook is commonly provided with a pair of slings that depend from the crane hook at angles in a bridle fashion, each of the slings connecting to an end portion of the spreader bar. Parallel, depending lift lines are then suspended from the end portions of the spreader bar downwardly to the load that is to be lifted.
One of the problems with spreader bars is that of sizing the spreader bar to meet a particular load. Loads typically differ in size and in configuration. Some devices have been patented that enable the overall length of the bar to be changed by changing the center section to which a pair of end caps attach. An example of such as a spreader bar that has been patented can be seen in my prior U.S. Pat. No. 4,397,493, and entitled “Spreader Bar Assembly”. Other spreader bar patents include U.S. Pat. Nos. 4,538,849 and 5,863,085, each incorporated herein by reference.
In some situations, a user has a pair of cranes or like lifting devices such as for example a ship having two cranes positioned at opposite ends of an opening in the hull above a hold or other cargo area. This presents a problem to the ship operator when very heavy loads of differing configurations are to be lifted out of the cargo area. Sometimes the position of the load in the cargo area requires that a crane be positioned at such an angle of inclination that the lifting capacity of the boom is at its lowest portion of its range.
BRIEF SUMMARY OF THE INVENTION
The present invention provides an improved spreader bar apparatus that includes a pair of bar sections. The present invention provides an improved spreader bar apparatus that includes a bar or beam member having first and second end portions. Each of the end portions provides a lifting portion that can be attached to a lifting device such as a crane. A flexible member is supported by each of the bar members at the lifting portions, the flexible member preferably extending in a curved fashion below the bar and in between the two bar ends.
The flexible member provides attachments at spaced apart intervals along the flexible member, each of the attachments being a location that can support a lifting line, sling or the like.
The flexible member is preferably comprised of a plurality of links connected together end to end.
The flexible member can be comprised of a plurality of links that are pinned together.
The flexible member can be comprised of a plurality of plate members, each plate member being an elongated structure having end portions, wherein one end portion of one plate member is connected to an end portion of another plate member, preferably using a pinned connection. At that pinned connection, a third plate member can be positioned to extend downwardly from the pinned connection and assume a generally vertical position. This third plate member functions as a load carrying member to which a depending lift line, sling or the like can be attached (for example, using shackles).
The plurality of plate members thus includes a first plurality of laterally extending plate members and a second plurality of vertically extending plate members. In one embodiment, the apparatus includes two separate lifting cranes positioned at spaced apart locations, each of the lifting cranes supporting a separate end of the bar.
BRIEF DESCRIPTION OF THE DRAWINGS
For a further understanding of the nature, objects, and advantages of the present invention, reference should be had to the following detailed description, read in conjunction with the following drawings, wherein like reference numerals denote like elements and wherein:
FIG. 1 is a front, elevational view of the preferred embodiment of the apparatus of the present invention;
FIG. 2 is a top, plan view of the preferred embodiment of the preferred embodiment of the apparatus of the present invention taken along lines 2 — 2 of FIG. 1;
FIG. 3 is a sectional view of the preferred embodiment of the apparatus of the present invention taken along lines 3 — 3 of FIG. 1;
FIG. 4 is a partial, perspective view of the preferred embodiment of the apparatus of the present invention;
FIG. 5 is a front elevational view of the preferred embodiment of the apparatus of the present invention shown during use;
FIG. 6 is another front, elevational view of the preferred embodiment of the apparatus of the present invention shown during use;
FIG. 7 is a partial, exploded perspective view of the preferred embodiment of the apparatus of the present invention; and
FIG. 8 is a partial perspective view of the preferred embodiment of the apparatus of the present invention illustrating a connection be ween the spreader bar and a load using lifting slings and shackles.
DETAILED DESCRIPTION OF THE INVENTION
FIGS. 1, 2 , 5 and 6 show the preferred embodiment of the apparatus of the present invention, designated generally by the numeral 10 . Spreader bar apparatus 10 is comprised generally of an elongated bar 11 having end portions 12 , 13 and center portion 14 .
Ends 15 , 16 are fitted to the bar 11 for example, using welding.
The bar 11 can be an elongated, cylindrically shaped member, such as a section of pipe. The bar 11 can be hollow or solid. The ends 15 , 16 are connected, preferably by welding, to the end portions 12 , 13 of bar 11 . End 15 is welded to bar 11 at end portion 12 . End 16 is welded to bar 11 at end portion 13 . If removable connections between bar 11 and end 15 , 16 are desired, the ends 15 , 16 can be constructed to be removable and not welded such as those shown in the Jon Khachaturian patent 4,397,493, incorporated herein by reference.
The combination of bar 11 and its ends 15 , 16 , support an elongated flexible member 17 that can be comprised of a plurality of links 18 , 19 , 20 , 22 , 23 , 25 . In FIGS. 1, 3 , 4 , and 7 , the flexible member 17 is shown comprised of a plurality of links connected together and preferably using a pinned connection at adjacent links such as the pinned connection 33 shown in the drawings. Each pinned connection 33 can be comprised of pin 26 having threaded portion 27 , washer 28 and nut 29 as shown in FIG. 4 .
In FIG. 4, outside links 18 form attachments to inside links 19 and lifting link 20 . The outside plate line 18 and inside plate link 19 are laterally extending as shown in FIGS. 1 and 4. The lifting link 20 is generally vertically extended (or nearly vertically extended) as shown by FIGS. 1 and 4. Each of the links 18 , 19 , 22 , 23 and 25 have a pair of openings 21 . These openings 21 are at the end portions of each of the links 18 , 19 , 22 , 23 , 25 as shown in FIGS. 4 and 7. Link 20 has an upper 35 opening 21 and a lower opening 24 . Large, horizontally extended links 22 define center links for the flexible member 17 as shown in Figure 1 . At this center position, there are preferably two large horizontal links 22 as shown in FIG. 3 .
Each bar end 15 , 16 has a pinned connection 33 as shown in FIG. 7 that forms an attachment between an end 15 or 16 and diagonally extending links 23 . In FIG. 7, each end 15 or 16 is comprised preferably of a pair of spaced apart plates 30 , 31 each being welded to end portion 12 or 13 of bar 11 . Alternatively, the plates 30 , 31 can be welded to the cylindrically shaped socket portion of a removable end cap that fits each end portion 12 , 13 of bar 11 . Stiffener plates 32 can be provided as shown in FIGS. 2 and 7 for forming an attachment between each of the plates 30 and 31 and bar 11 .
The stiffeners 32 can be welded to the respective plates 30 or 31 and also are welded to the end portion 12 or 13 of bar 11 . An additional link 34 forms a part of the connection that is pinned using pin connection 33 at each end 15 or 16 . As shown in FIG. 7, this additional link is a vertically extending lifting link 34 having an opening 35 that aligns with the openings 36 in diagonally positioned links 23 or 25 and the openings 37 , 38 in plates 30 , 31 respectively of end 15 . The lifting link 34 also has an opening 39 that enables a connection to be formed with a lifting member or connecting member such as shackle 40 , shackle pin 41 and lifting sling (vertical or inclined) 42 .
Shackles 40 can also be used to form an attachment between one of the lifting links 20 that depends from links 18 , 19 of flexible member 17 as shown in FIG. 8 . Slings 42 can then be connected between the shackle 40 that is attached to a link 20 and shackles 43 attached to load 44 .
FIGS. 5 and 6 illustrate a completed rigging wherein spreader bar 10 forms an interface between the load 44 to be lifted and a lifting device (or devices) such as cranes 45 , 46 . Each of the cranes 45 , 46 provides a lifting line 47 and a hook 48 for engaging and supporting slings 42 .
In FIG. 5, the load 44 has been “centered”, being connected to flexible member 17 with slings 42 that are at equal distances from large, horizontal center link 22 . In FIG. 6, an offset loading arrangement is illustrated. In FIG. 6, the slings 42 are connected to links 20 that are to the right of the center, large horizontal link 22 . Such a situation might occur depending upon the load 44 to be lifted, the initial position of the load 44 (such as its location in the hold of a ship) or the position of equipment that is near or surrounding the load 44 to be lifted.
PARTS LIST
Part Number
Description
10
spreader bar apparatus
11
bar
12
end portion
13
end portion
14
center portion
15
end
16
end
17
flexible member
18
outside plate link
19
inside plate link
20
lifting link
21
opening
22
large horizontal link
23
diagonally positioned link
24
opening
25
diagonally positioned link
26
pin
27
threaded portion
28
washer
29
nut
30
plate
31
plate
32
stiffener plate
33
pinned connection
34
lifting link
35
opening
36
opening
37
opening
38
opening
39
opening
40
shackle
41
shackle pin
42
sling
43
shackle
44
load
45
crane
46
crane
47
lifting line
48
crane hook
The foregoing embodiments are presented by way of example only; the scope of the present invention is to be limited only by the following claims.
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A spreader bar includes an elongated bar member having end portions that support a flexible lifting member that is supported below the bar. The flexible lifting member is preferably comprised of a plurality of link sections that are pinned together, load carrying links depending from the flexible member, preferably at pinned connections that join the additional links.
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BACKGROUND OF THE INVENTION
1. Field of Invention
The present invention relates to equipment utilized during measurement while drilling (MWD) data retrieval in subterranean wells. In particular, the invention relates to filtering apparatus and related methods for preventing debris from entering sensitive areas in a drilling system such as a turbine power source used to operate directional sensors, while maintaining desired flow rates for optimal drilling.
2. Description of the Related Art
Horizontal (directional) drilling continues to prove to be an extremely efficient method for retrieving oil. Conventional vertical wells are limited by surface land formations limiting possible rig set up, and subterranean oil formations that are extremely difficult to extrapolate through conventional methods for maximum oil production. Horizontal drilling offers a solution to many complications currently faced through conventional vertical wells. Some of the most important pieces of equipment required in horizontal drilling are directional sensors located at the distal end of a drill string that transmit vital survey, formation, and performance data to the surface without requiring costly down time. The directional sensors require local power which is commonly provided by turbine alternators which are located near the directional sensors in the drill string. The turbine alternators are operated by circulating drilling mud through the drill string and into a turbine causing the turbine to spin thereby generating electricity to power the directional sensors. Turbine alternators are preferred over alternative battery power sources because they generally offer a more effective power source with a longer operating life.
It is well known that the turbines within such alternators are highly sensitive. If a turbine is damaged, a power failure may occur resulting in loss of electricity to the directional sensors. This can bring horizontal drilling operations to a halt until the turbines are repaired or replaced, which can be a very expensive and time consuming process since it requires removal of the entire drill string from the well, repair/replacement of the turbine alternators, and reinsertion of the drill string into the well. It is therefore important to avoid such extended down time.
In order to protect the turbines and limit potential power failures to the directional sensors, a MWD drill pipe screen or mud screen is ordinarily placed at the top of the drill string to control debris from entering the drill string and finding its way to the vital turbine alternators. It is to be appreciated that when such a screen or filter becomes clogged, there is usually an associated spike in the pressure of the drilling mud used to operate the turbines. When such a spike is noticed, it is a signal to the drilling operators to change the screen, or risk damage to the drill string from buildup of excessive pressure. Replacing the drill pipe screen is a cumbersome process, requiring drilling operations to be shut down while the filter is removed, cleaned and/or replaced, but this preferable to a blowout from excessive pressure, or causing damage to the turbines at the other end of the drill string.
Existing drill pipe screens include spiral drill pipe screens, bar/rod drill pipe screens, slotted tube drill pipe screens, and perforated drill pipe screens. However, each of these types of drill pipe screen suffers from one or more disadvantages. For example and without limitation, existing drill pipe screens (particularly spiral and slotted tube screens) tend to clog readily, and may cause a spike in drilling mud pressure after a relatively short period of time (e.g., 2-3 runs). In addition, existing drill pipe screens may cause small pressure spikes even though the screen may not be completely clogged, forcing the drilling operators to stop operations to check the status of the screen only to find that it is not significantly clogged and operations could have continued. This results in unnecessary downtime to check and thereafter clean or replace a drill pipe screen that did not actually need to be serviced. Current screens also suffer extensive failures due to damage sustained to the base metal of the screen (particularly bar-rod and perforated screens) allowing debris to pass through the screen and reach the sensitive turbine, potentially causing serious damage and drilling down time, and loss of drilling mud circulation which affects all drilling processes.
The oil and gas industry continues to streamline drilling processes with a keen eye on safety and cost management. However, as vital as drill pipe screens are to horizontal drilling, screen designs have not changed in the industry for an extended length of time. As horizontal drilling proves to be an effective method of drilling, a need has arisen for improved MWD drill pipe screens and related methods that maximize necessary drilling mud circulation, that are strong and reliable in order to provide substantial debris filtration, and that perform for extended periods of time without removal, repair or replacement in order to maximize efficiency and reduce costs.
SUMMARY OF THE INVENTION
The present invention addresses these needs by providing drill pipe screens and related methods that provide reliable long-term filtering of drilling mud in MWD systems without allowing debris to pass through the screens and without causing intermittent pressure spikes at times when the screens are not completely clogged, while maintaining desired circulation rates of drilling fluids. Embodiments of the present invention accomplish such functionality through the use of unitary hollow cylindrical bodies having an alternating pattern of elongated parallel peripheral slots and small peripheral relief ports along the length of such bodies in which the primary filtering is provided through the elongated peripheral slots, and intermittent pressure spikes are avoided because of the peripheral relief ports.
In embodiments of the invention, a single cylindrical piece of hollow metal is provided, preferably in the form of a tube of iron, stainless steel or the like, although other durable metals may also be used. For example and without limitation, 1018 mild steel, 4140 steel, 4142 steel, 4145 steel or a stainless steel alloy may be used. An alternating pattern comprising a set of elongated parallel peripheral slots followed by a set of small peripheral relief ports are provided along the length of such tubes. Each set of parallel peripheral slots are provided in the wall of the tube aligned in parallel with the axial center of the tube, through which drilling mud will be passed from inside the tube to outside the tube. The lengths and widths of such slots are preferably the same for each slot in the set, and may be varied according to the strength of the metal material of the tube. The slots are preferably evenly spaced apart and radially positioned around the perimeter of the tube, and are sized in order to provide sufficient strength to avoid breakage of the portions of the tube between the slots from debris in the drilling mud caught inside the tube as mud flows outward from the inside of the tube through the slots, while at the same time providing sufficiently large openings for good flow of drilling mud through the slots themselves.
In embodiments of the invention, a separate set of smaller peripheral relief ports is provided adjacent to each set of peripheral slots. The relief ports are also preferably evenly spaced apart, and are also radially positioned around the perimeter of the tube. The relief ports are preferably provided in the form of small circular openings, although different symmetrically shaped openings may also be used (hexagonal, octagonal, oval, square, rectangular, etc.). It is to be appreciated that a portion of the tube is present between each set of relief ports and the adjacent set of slots, forming cylindrical bands between slots and ports. Such bands provide peripheral strength to the tube, and the slots and ports are positioned in order that such bands are sufficiently large and strong enough to avoid breakage in the material of the tube adjacent to the slots from debris in the drilling mud caught inside the tube as mud flows through the slots and relief ports.
By way of example and without limitation, a typical embodiment of a screening tube of the present invention may include a first set of peripheral ports at one end (e.g., the bottom) of a hollow metallic tube, followed by a first set of elongated slots along the length of the tube, followed by a second set of peripheral ports, followed by a second set of elongated slots along the length of the tube, followed by a third set of peripheral ports, followed by a third and final set of elongated slots along the length of the tube reaching the opposite end (e.g., the top) of the tube, it being understood that the positioning of the slots and ports also define sets of circumferential bands of tube material between each set of slots and each set of ports. In most embodiments, the same number of slots and ports are provided in each set (e.g. 16 slots and 16 ports), although different numbers of each may also be provided (e.g. 15 slots and 17 ports); and, in most embodiments the slots and ports are ordinarily in axial alignment with each other along the length of the tube, although they may be provided in different patterns as well, such as offset, helical, etc. In most embodiments, a first set of relief ports is provided at the lowermost end of the tube, although in other embodiments a first set of slots may be the lowest item provided on the tube.
A lower cap is designed to be welded or otherwise permanently attached to the bottom end of a tube of the present invention, the lower cap having a plurality of holes therein. An upper cap is also designed to be welded or otherwise attached to the opposite upper end of such a tube for engagement within the drill string
A key to the design of embodiments of the present invention is that wide peripheral integrity bands must be provided in the tube between sets of slots, and these bands must have sufficient length in order to provide sufficient strength to avoid breakage of the tube, but that the relief ports are also necessary in the integrity bands because without the relief ports, the presence of long peripheral bands could cause undesired pressure spikes as the tube fills with debris during screening operations. In particular, as mud is filtered through an embodiment of the present invention, the lowermost set of slots will be the first to slowly become clogged with debris. At the point in time when such a lowermost set of slots becomes completely clogged, it is to be appreciated that escaping mud must now flow through the remaining unclogged upper slots and relief ports. At this same point in time, the mud flowing through the tube encounters the lowermost peripheral band of the tube, where flow is interrupted and debris begins to readily accumulate. The encounter of this interruption in flow could cause a spike in fluid pressure if the integrity band were too long, but the presence of the relief ports in the integrity band allows the flow of mud to continue, thereby stabilizing the pressure of the flowing mud so that no significant spike is encountered.
In preferred embodiments, the openings for the slots and/or ports are the same size on the inside of the tube and on the outside of the tube. Of course, as shown in FIG. 3 , since the tube is generally cylindrical in shape, the material of the tube wall itself between the openings in these embodiments will be smaller in size (e.g., surface width) on the inside of the tube than on the outside of the tube. Thus, in preferred embodiments, the material of the tube wall between adjacent slots and/or ports exhibits a taper, so that the width of the inside surface of the tube wall between particular adjacent slots or ports of the tube is smaller than the width of the outside surface of the tube wall between the same adjacent slots or ports of the tube.
However, in other embodiments the openings for the slots and/or ports may be tapered so that the opening for a particular slot or port on the outside of the tube may be wider than the opening for that same slot or port on the inside of the tube. In further embodiments, the slots and/or ports may be oppositely tapered so that the openings for a particular slot or port on the inside of the tube may be wider than the opening for that same slot or port on the outside of the tube.
In different exemplary embodiments, and without limitation, the preferred lengths of the cylindrical tubing may range from about 16 inches to about 48 inches, preferred outside diameters of the tubing may range from about 1 and ⅜ inches to about 3 and ⅛ inches, and preferred inside diameters of the tubing may range from about ⅞ inches to about 2 and ⅞ inches. In different exemplary embodiments, and without limitation, the preferred number of slots in each set may range from 10 to 20 , and the preferred number of peripheral ports in each set may range from 10 to 20 with a potential total of as few as 20 to as many as 120 slots or holes in an entire exemplary screen unit. In different exemplary embodiments, and without limitation, preferred widths of the slots and holes may range from about ⅛ inch to about ½ inch, preferably about ¼ inch, and preferred lengths of the slots may range from about 4 inches to about 8 inches, preferably about 6 and ¾ inches. In different exemplary embodiments, and without limitation, preferred lengths of the integrity bands between adjacent sets of slots along the tube may range from about ¾ inch to about 2 and ¼ inches, preferably about 1 and ¼ inches, it being understood that the relief ports are provided in the middle of the integrity bands. It is to be appreciated that the above ranges are exemplary, and that measurements outside of these ranges are also within the scope of the present invention. It is also to be appreciated that embodiments of the present invention may include a wide variety of different combinations of different tubing sizes, lengths, widths and diameters, as well as a wide variety of different combinations of slot numbers, sizes, lengths and widths and different relief port numbers, sizes, lengths and widths.
In an exemplary preferred embodiment (illustrated in the drawings), three sets of sixteen (16) slots and three sets of sixteen (16) relief ports are provided; the walls of the exemplary tube have a sectional width of ¼ inch, an inside diameter of 2 and ⅜ inch and an outside diameter of 2 and ⅞ inch. (See, e.g., FIG. 3 .)
It is therefore an important object of the present invention to provide mud screens for use in MWD drilling systems that operate for long periods of time without causing intermittent pressure spikes at times when the screens are not completely clogged.
It is also an important object of the present invention to provide reliable mud screens for use in MWD drilling systems that are durable, resist breakage and prevent debris from passing through the screens.
It is also an important object of the present invention to provide mud screens for use in MWD drilling systems that maintain desired circulation rates of drilling fluids.
Additional objects of the invention will be apparent from the detailed description and the claims herein.
BRIEF DESCRIPTIONS OF THE DRAWINGS
FIG. 1 is a schematic view of a typical drill string having a directional sensor powered by a turbine alternator that is operated using mud flowing through a drill screen.
FIG. 1A is an enlarged cut away view of a section of the drill string of FIG. 1 showing the placement of an embodiment of a filter of the present invention.
FIG. 2 is a side elevational view of an embodiment of the present invention.
FIG. 3 is sectional view along line A-A of FIG. 2 .
FIG. 4 is a partially cut away perspective view of an embodiment of the present invention.
FIG. 5 is an exploded perspective view of an embodiment of the present invention.
FIG. 6 shows top, side, and isometric views of embodiments of top and bottom end caps of the present invention.
FIG. 7 is a side elevational view of an alternative embodiment of the present invention.
FIG. 8 is a perspective view of the embodiment of FIG. 7
DETAILED DESCRIPTION
Referring to the drawings wherein like reference characters designate like or corresponding parts throughout the several views, and referring particularly to FIG. 5 , it is seen that this illustrated embodiment of the present invention includes an elongated cylindrical body 9 to which a lower end cap 11 and an upper end cap 12 are to be attached. Referring to FIG. 2 , it is seen that the illustrated cylindrical body 9 includes at least one set of elongated slots 7 separated longitudinally along the length of cylindrical body 9 by at least one set of relief ports 4 . The slots 7 of each set are provided in parallel to each other, and parallel to the central axis of the cylindrical body 9 . The relief ports 4 of each set are provided longitudinally between each set of slots 7 . In the illustrated embodiment, a set of relief ports is also provided at the bottom end of cylindrical body 9 . Although the illustrated embodiments show three sets of slots 7 and three sets of ports 4 , it is to be appreciated that more or fewer sets of slots and ports may be provided so long as a set of ports is provided between each set of slots. Similarly, although the illustrated embodiment depicts a set of relief ports at the bottom end of cylindrical body 9 , another set of relief ports may also be provided at the upper opposite end of cylindrical body 9 . Further, although the illustrated embodiment depicts sixteen slots in each set, and sixteen ports in each set, it is to be appreciated that different numbers of slots and/or ports may be provided in each set, and that the number of slots or ports in one set may not be the same as in another set.
It is to be appreciated that the size and number of slots 7 provided is usually in direct correlation to the length of the cylindrical body 9 , depending upon the flow rates desired and the durability of the material of which body 9 is made. The slots 7 should generally be narrow in width to allow for effective filtering, but should also be long enough to adequately allow for fluids to continue moving down the drill string.
It is to be appreciated that the positioning of slots 7 defines a set of circumferential integrity bands 8 between each set of slots 7 . Integrity bands 8 are bisected by ports 4 , defining smaller bands 5 , 6 on either side of ports 4 which provide strength to cylindrical body 9 along its length to prevent breakage, fatigue or other failure.
FIG. 3 is a sectional view along line A-A of FIG. 2 , but also depicts an exemplary view along line B-B of FIG. 2 as well. In some embodiments of the invention, the openings of slots 7 and ports 4 are the same size on the inside and on the outside of body 9 , with no tapering. However, in other embodiments, these openings may be tapered such that they are wider on the outside of cylindrical body 9 than on the inside of cylindrical body 9 , and in other embodiments these openings may be tapered in an opposite direction such that they are wider on the inside of the cylindrical body 9 than on the outside of cylindrical body 9 . It is to be appreciated that some or all of the slots and/or ports may be tapered from outside to inside, or from inside to outside, or not at all; and that each individual slot and/or port may have its own inside-out taper, or outside-in taper, or no taper at all. In some embodiments, the slots 7 and ports 4 may be cut or machined into an existing hollow tubular body 9 ; in other embodiments, the tubular body 9 may be cast in a mold with the slots 7 and ports 4 defined in the mold.
FIG. 1 depicts a typical MWD mud screen of the present invention in operation on a horizontal well. Connection ( 1 ) depicts one possible location for placement of a mud screen of the present invention, between a Kelly bar and the drill pipe for easy accessibility. Connection ( 2 ) depicts another possible location for placement of a mud screen of the present invention, between the drill collar and a non-magnetic pipe section for optimal filtering.
FIG. 2 illustrates an embodiment of a mud screen of the present invention after all manufacturing has been completed, and the end caps 11 , 12 have been attached by welding or the like. Connection ( 3 ) depicts where the end caps are welded to the cylindrical body 9 , which may be through Metal Inert Gas (MIG) or Tungsten Inert gas (TIG) welding applications, or other similar processes. Exemplary circular relief ports 4 are provided at the base of the illustrated cylindrical body 9 to allow high velocity drilling mud to drain while protecting vital weld points. Along the length of cylindrical body 9 , between slots 7 and ports 4 , circumferential integrity bands 8 , bisected into bands 5 and 6 by ports 4 are provided to optimize strength and durability of the unit.
Without relief ports 4 , circumferential bands 5 and 6 would form a single integrity band 8 in cylindrical body 9 having a sufficient length to withstand the increased pressure of the mud which can build up in these areas without breakage to body 9 . Such an integrity band 8 may have a length of, for example and without limitation, approximately 1 and ¼ inch. However, as noted elsewhere herein, without the relief ports, once a lower section of slots becomes clogged with debris, a pressure spike would often be detected in the integrity band 8 . Thus, a set of relief ports 4 are provided in embodiments of the present invention which divide such an integrity band 8 into two parts 5 and 6 in order to provide relief for flowing mud which avoids pressure spikes without loss of strength to body 9 .
FIG. 4 depicts a partially cut-away view of an embodiment of a mud screen of the present invention in which a lower end cap 11 has been attached using an exemplary weld bevel of 30 degrees 15 to allow for a full penetration weld. Such a weld bevel may be used to secure each end cap 11 , 12 to the cylindrical body 9 in order to minimize internal erosion.
FIG. 5 depicts an embodiment of the present invention before end caps 11 , 12 are adhered to body 9 , which may be through MIG or TIG welding applications. Top, side and isometric views of exemplary upper 12 and lower 11 end caps are shown in FIG. 6 .
It is to be understood that variations and modifications of the present invention may be made without departing from the scope thereof. It is to be appreciated that the features disclosed herein may be used different combinations and permutations with each other, all falling within the scope of the present invention. It is also to be understood that the present invention is not to be limited by the specific embodiments disclosed herein, but only in accordance with the appended claims when read in light of the foregoing specification.
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The present invention includes drill pipe screens and related methods that provide reliable long-term filtering of drilling fluids used to operate alternator turbines that are used to provide power in measurement while drilling (MWD) systems without allowing debris to pass through the screens to the turbines, and without causing intermittent pressure spikes at times when the screens are not completely clogged while maintaining desired circulation rates of drilling fluids. Embodiments of the invention include cylindrical bodies having alternating sets of elongated slots and peripheral ports located thereon to provide filtering of and relief to drilling fluids under pressure.
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CROSS-REFERENCE TO RELATED APPLICATION
The present application claims priority to pending Chinese Patent Application No. CN201110446162.4, filed Dec. 28, 2011, the contents of which are incorporated by reference its entirety.
FIELD OF THE INVENTION
The present invention generally relates to application of nuclear technologies, and particularly to neutron scattering and security detection technologies. More particularly, the present invention relates to a fast-neutron detector.
BACKGROUND OF THE INVENTION
In traditional safety detection technologies for nuclear materials, it is a common technology to use 3 He proportional counters and polyethylene moderators for fast-neutron detection. However, this technology at least has the following two drawbacks:
1. The supply of 3 He gas is insufficient. Since 3 He is an important nuclide for detecting neutron, the insufficient supply problem of 3 He which has been occurring commonly throughout the world has already imposed a serious challenge to application of nuclear material security detection technologies so that manufacturing costs of security apparatuses rise abruptly.
2. In this technology, the moderated volume and the measured volume of neutrons are independent on each other, i.e., the moderated volume is constituted by polyethylene whereas the measured volume is constituted by 3 He proportional counter. The moderated volume is in a competitive relation to the measured volume in space, and a final detection efficiency depends on a product of a fast-neutron moderating efficiency and a thermal neutron absorbing efficiency to which the moderated volume and the measured volume correspond respectively, whereby the moderated volume cannot be made too large, nor the measured volume can be made too large, which limits the maximum fast-neutron detection efficiency achieved by this technology.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a novel technical solution for fast-neutron detection without using the nuclide 3 He in short supply, so as to reduce manufacturing costs and better meet the increasing market demand for security check apparatuses.
A further object of the present invention is to enable the implementation of the fast-neutron maximum detecting efficiency in the technical solution of the present invention to be free of inter-restraint factors, so as to obviate the competitive relationship between the moderated volume and the measured volume in the prior art, and obtain a greater fast-neutron detecting efficiency.
Generally speaking, the present invention inventively employs the following basic ideas to achieve the above objects of the present invention, so as to obtain a high fast-neutron detecting efficiency while advantageously reducing the manufacturing costs of the fast-neutron detector:
1. Using plastic scintillators to achieve neutron moderating and signal forming function required by the fast-neutron detector;
2. Carrying out neutron-sensitive coating film treatment on the surface of the plastic scintillators to achieve the neutron absorbing function required by the fast-neutron detector.
In particular, the present invention provides a fast-neutron detector, comprising: a plastic scintillator array which includes at least one plastic scintillator unit, wherein sidewall surfaces of each plastic scintillator unit are covered or coated with a neutron-sensitive coating film.
Preferably, the plastic scintillator array has a first end for receiving incident fast-neutrons and a second end opposite to the first end. And preferably, the fast-neutron detector further comprises: a light guide device disposed at the second end of the plastic scintillator array and configured to collect and guide light formed in the plastic scintillator unit and being emergent to the second end; and a photoelectrical converting device disposed at an emergent end of the light guide device and configured to convert the light collected and guided by the light guide device thereon into electrical signals.
Preferably, the at least one plastic scintillator unit comprises a plurality of plastic scintillator units.
Preferably, the neutron-sensitive coating film is formed by directly coating a film on the sidewall surfaces of each plastic scintillator unit.
Preferably, the neutron-sensitive coating film is first formed by film coating on a substrate, then the sidewall surfaces of the plastic scintillator unit are covered (or wrapped) with the substrate after film coating in a way that the neutron-sensitive coating film is in contact with the sidewall surfaces of the plastic scintillator unit.
Preferably, a material for forming the neutron-sensitive coating film contains boron or gadolinium.
Preferably, the thickness of the neutron-sensitive coating film is in a range of 0.1 μm-4 μm.
Preferably, the height of each plastic scintillator unit is 10 cm-50 cm, and the length and the width thereof are 0.1 cm-5 cm.
Preferably, a cross section of each plastic scintillator unit is a regular polygon, preferably a square or a regular hexagon.
Preferably, the fast-neutron detector according to the present invention may further comprise: an amplifying shaping circuit configured to receive the electrical signal outputted from the photoelectrical converting device and amplify and shape it; a signal picking circuit configured to receive the electrical signal outputted by the amplifying shaping circuit and extract a time signal therefrom; a delay circuit configured to receive the time signal outputted by the signal picking circuit and delay it; a coincidence circuit at least having a first input channel and a second input channel, wherein the first input channel receives a non-delay time signal outputted by the signal picking circuit, and the second input channel receives a delay time signal outputted by the delay circuit, and the coincidence circuit generates a coincidence pulse signal according to the non-delay time signal and the delay time signal; and a counter configured to receive the coincidence pulse signals outputted by the coincidence circuit and count them to finally obtain a coincidence count.
In the novel fast-neutron detector based on such film-coated plastic scintillators according to the present invention, it can be approximately believed that the moderated volume is identical with the measured volume. Therefore, the present invention advantageously addresses the mutual competition and counterbalance problem of the two types of volumes in the prior art and can obtain a higher fast-neutron detecting efficiency.
From the following detailed description of preferred embodiments of the present invention with reference to the drawings, those skilled in the art can better understand the above and other objects, advantages and features of the present invention.
BRIEF DESCRIPTION OF DRAWINGS
Preferred embodiments of the present invention will be described in detail hereafter with reference to the drawings by way of example, but not limitation. Like reference numbers throughout the drawings refer to the like or similar parts or portions. Those skilled in the art should appreciate that these drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is a schematic perspective view of a plastic scintillator array used in a fast-neutron detector according to a preferred embodiment of the present invention;
FIG. 2 is a schematic enlarged perspective view of a plastic scintillator unit used in the plastic scintillator array shown in FIG. 1 ;
FIG. 3 is a schematic cross-sectional view of the plastic scintillator unit shown in FIG. 2 ;
FIG. 4 is a schematic view of wrapping the sides of the plastic scintillator unit in a film-coated substrate according to another preferred embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of the film-coated substrate shown in FIG. 4 ;
FIG. 6 is a schematic structural view of the fast-neutron detector according to a preferred embodiment of the present invention, showing a moderation procedure and an absorbing procedure as well as ionizing and light-emitting procedure which happen after the fast-neutrons are incident into the plastic scintillator array;
FIG. 7 is a schematic block diagram of a processing circuit for processing electrical signals outputted by a photoelectrical converting device to improve n/γ ratio based on a time coincidence method.
FIG. 8 is an exemplary curve graph showing time distribution relationship between a neutron recoil proton signal and a neutron capture signal.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
A fast-neutron detector according to the present invention employs a plastic scintillator array 10 shown in FIG. 1 to achieve neutron moderating and optical signal forming functions. The plastic scintillator array 10 has a first end for receiving incident fast-neutrons and a second end opposite to the first end. When the fast-neutrons are incident into the scintillator array 10 from the first end, moderating, absorbing, ionizing and light-emitting procedures will happen therein so as to achieve measurement of fast-neutrons.
The plastic scintillator array 10 may be comprised of at least one (preferably a plurality of) identical plastic scintillator unit(s) 12 , and its overall configuration (defined by an outer envelope line of the array) may be in any suitable shape such as a squire, rectangle, circle or hexagon. In the preferred embodiment shown in FIG. 1 , the plastic scintillator array 10 is constructed as a m×m square array, wherein in represents the number of plastic scintillator units included by a side length of the array. Therefore, in is generally a positive integer greater than or equal to 2, preferably equal to 6 or 10 or more, more preferably equal to 12, 15, 20, 25, 30 or more. Nevertheless, in an extreme case, in may be equal to 1, that is, in the extreme case, the plastic scintillator array stated in the present application may be comprised of only one plastic scintillator unit 12 .
A cross section of each plastic scintillator unit 12 may preferably be one of various regular polygons, preferably a square or a regular hexagon. FIG. 2 is a schematic enlarged perspective view of the plastic scintillator unit 12 used in the plastic scintillator array 10 shown in FIG. 1 , and FIG. 3 is a schematic cross-sectional view of the plastic scintillator unit shown in FIG. 2 , wherein the plastic scintillator unit 12 has a height H, a length L and a width W. IN some embodiments of the present invention, the height H of the plastic scintillator unit may be about 10 cm-50 cm, and the length L and width W may be about 0.1 cm-5 cm respectively. Particularly, in the preferred embodiment shown in FIGS. 2-3 , the height H of the plastic scintillator unit is preferably about 20 cm; the length L and the width W are preferably equal to each other, equal to about 1 cm. Of course, the height H, the length L and the width W may be optimally adjusted as particularly desired.
The sidewall surfaces of each plastic scintillator unit 12 are covered or coated with a layer of neutron-sensitive coating film 14 with a thickness T. The material for forming the neutron-sensitive coating film preferably contains boron or gadolinium. In some embodiments of the present invention, the thickness T may be in a range of about 0.1 μm-about 4 μm, preferably about 1 μm. Of course, a specific magnitude of the thickness T here may be appropriately adjusted as desired.
In some preferred embodiment of the present invention, the neutron sensitive coating film 14 may be directly formed on the sidewall surfaces of each plastic scintillator unit 12 , as shown in FIG. 2 . Those skilled in the art may appreciate that the method requires that a temperature for the film coating process is lower than a softening temperature of the plastic scintillator unit 12 .
In some other preferred embodiments of the present invention, as shown in FIGS. 4-5 , the neutron-sensitive coating film 14 can be first formed on the substrate 13 by film coating, then the sidewall surfaces of the plastic scintillator unit 12 are covered by the substrate 13 with the neutron-sensitive coating film 14 in a way that the neutron-sensitive coating film 14 is in contact with the sidewall surfaces of the plastic scintillator unit 12 , so that the plastic scintillator unit has a neutron-sensitive property. In such an embodiment, the substrate 13 is preferably made of aluminum foil or other suitable materials.
No matter whether the plastic scintillator unit 12 is directly film-coated or the substrate 13 is film-coated, the film-coating process may be one of various suitable manners such as magnetron sputtering, electron beam evaporation, electrophoresis or atomic layer deposition.
The moderating procedure and the absorbing procedure shown in FIG. 6 will occur after the neutrons are incident into the plastic scintillator array 10 . Both the moderating procedure and the absorbing procedure produce high-energy charged particles, wherein what are obtained in the moderating procedure are recoil protons which energy is approximately equal to that of the incident neutrons. What are obtained in the absorbing procedure are charged particles after nuclear reaction. If 10 B is selected as the neutron reaction nuclide, the reaction formula is as follows:
n
+
10
B
→
{
7
Li
+
α
+
2.79
MeV
(
6.1
%
)
Li
*
7
+
α
+
2.31
MeV
(
93.9
%
)
The charged particles obtained from the above reaction formula are a particles and 7 Li nucleus. These charged particles (protons p, a, 7 Li) occurs ionizing light emission in the scintillators, and the emitted light spreads along each plastic scintillator unit. It should be noted here that, before entering each plastic scintillator unit 12 , α and 7 Li first penetrate a neutron absorbing material with unequal thicknesses (depending on reaction position). Since energy loses during the penetration, an magnitude of the signal formed in each plastic scintillator unit 12 is reduced. Therefore, the thickness of the neutron absorbing material is preferably not too large, and 1 μm or so may be usually a desirable value.
Preferably, the second end of the plastic scintillator array 10 is provided with a light guide device 20 configured to collect and guide light formed in the respective plastic scintillator units 12 and being emergent to the second end of the plastic scintillator array 10 . At an emergent end of the light guide device 20 is provided a photoelectrical converting device 30 configured to convert the light collected and guided by the light guide device 20 thereon as electrical signals.
The photoelectrical converting device 30 is preferably a photoelectrical multiplier tube. However, in some embodiments, other photoelectrical converting devices such as a photodiode are also possible.
In addition, in some other embodiments of the present invention, at the first end of the plastic scintillator array 10 may also be provided identical or similar light guide device and/or photoelectrical converting device to collect and detect light which might be emergent from the first end of the plastic scintillator array 10 to further improve the detecting efficiency.
As shown in FIG. 6 , when the light guide device 20 and the photoelectrical converting device 30 are provided only at the second end of the plastic scintillator array 10 , a layer of reflection material (e.g., aluminum foil, or polytetrafluoroethylene) may be preferably added to the first end of the plastic scintillator array 10 so as to increase the number of photons collected by the light guide device 20 and the photoelectrical converting device 30 at the second end.
In order not to obscure the technical solution of the present application, some common circuits usually needed after the photoelectric converting device 30 (e.g., an analog/digital converting circuit that may be needed in the subsequent processing) will not be described in detail or will be omitted hereafter, because these ordinary processing circuits are well-known and readily implemented for those skilled in the art.
Table 1 exemplarily lists intrinsic detecting efficiencies of 1 MeV neutrons obtained by analog computation where changing the dimensions of the plastic scintillators and the thickness of the neutron-sensitive coating film coated with boron, so that those skilled in the art can better implement the present invention with reference to these data in various specific applications.
TABLE 1
1 MeV neutron detecting
Height
Width/Length
Boron thickness
efficiency
H (cm)
W/L (cm)
(μm)
(%)
10
0.5
0.5
14.4
10
0.5
1
17.3
10
0.5
2
15.9
10
1
0.5
10.2
10
1
1
13.6
10
1
2
13.7
20
0.5
0.5
40.0
20
0.5
1
41.6
20
0.5
2
34.1
20
1
0.5
31.6
20
1
1
36.6
20
1
2
32.0
50
0.5
0.5
47.4
50
0.5
1
47.3
50
0.5
2
37.8
50
1
0.5
38.9
50
1
1
42.9
50
1
2
36.0
Since the detector of the present invention is implemented based on the plastic scintillators which are per se sensitive to the X/γ, the detector of the present invention cannot prevent from sensitivity to X/γ measurement, which is disadvantageous for improvement of the n/γ ratio. In order to eliminate the above disadvantageous effect and increase the n/γ ratio, in some further preferred embodiments of the present invention, a time coincidence method is particularly employed to select neutron events on the basis principle that each captured neutron necessarily experiences complete loss of incident kinetic energy (the main objects for the loss are recoil protons); after a period of time after production of the recoil protons, the neutrons will be captured and form charged particles; the time distribution of the two groups of charged particles is in a certain relationship, and the relationship may be extracted by a coincidence circuit so that the n/γ ratio may be increased.
FIG. 7 is a schematic block diagram of a processing circuit for processing electrical signals outputted by a photoelectrical converting device to increase the n/γ ratio based on a time coincidence method. As shown in this figure, the photoelectrical converting device 30 converts the light collected and guided thereon into an electrical signal, then an amplifying shaping circuit 31 receives the electrical signal outputted from the photoelectrical converting device 30 and amplifies and shapes it; a signal picking circuit 32 receives the electrical signal outputted by the amplifying shaping circuit 31 and extracts a time signal therefrom (for example, by means of threshold judgment and selection or other time extracting methods known in the art); a delay circuit 33 receives the time signal outputted by the signal picking circuit 32 and delays it; a coincidence circuit 34 receives a non-delay time signal outputted by the signal picking circuit 32 at its first input channel, receives the delay time signal outputted by the delay circuit 33 at its second input channel, and generates a coincidence pulse signal according to the non-delay time signal and the delay time signal; a counter 35 receives the coincidence pulse signals outputted by the coincidence circuit 34 and counts them to finally obtains a coincidence count.
FIG. 8 exemplarily illustrates a time distribution relationship between a neutron recoil proton signal and a neutron capture signal. It can be seen from this figure that an average time delay is about 60 microseconds. As can be seen, when a time window of the coincidence circuit shown in FIG. 7 is set to be about 200 microseconds, a higher true coincidence count rate can be ensured. Of course, the coincidence time of 200 microseconds might also increase the count rate of accidental counting. A user can select a suitable time window in specific applications according to actual situations.
So far, those skilled in the art can appreciate that although exemplary preferred embodiments have been illustrated and described in detail, many other variations or modifications conforming to the principles of the present invention can be directly determined or derived from the disclosure of the present application without departing from the spirit and scope of the present invention. Therefore, the scope of the present invention shall be understood and recognized as covering all of these other variations or modifications.
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The present invention provides a fast-neutron detector, comprising: a plastic scintillator array which includes at least one plastic scintillator unit, wherein sidewall surfaces of each plastic scintillator unit are covered or coated with a neutron-sensitive coating film. The fast-neutron detector based on such film-coated plastic scintillators according to the present invention advantageously addresses the mutual competition problem between a moderated volume and a measured volume in the prior art and can obtain a higher fast-neutron detecting efficiency.
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This is a divisional application of Ser. No. 07/735,615, filed Jul. 25, 1991 by Anthony Edward WALSBY and Keith Brian CLARKE for TREATMENT OF WATER TO REMOVE GAS VACUOLATE CYANOBACTERIA, now U.S. Pat. No. 5,422,002, which in turn is a continuation of Ser. No. 07/435,706 filed Nov. 13, 1989, abandoned, which in turn is a continuation of Ser. No. 07/101,658 filed Sep. 28, 1987.
FIELD OF THE INVENTION
The present invention relates to a method of and apparatus for the treatment of water to remove gas vacuolate cyanobacteria.
In some water treatment processes at present in operation, the water to be treated before being supplied to the customer is first allowed to stand in settlement tanks where the sediment and foreign bodies in the water taken from the reservoir or lake is allowed to settle to form a sludge at the bottom.
However, in certain areas and at certain times of the year gas-vacuolate cyanobacteria otherwise known as blue-green algae can form in a lake or reservoir. These cyanobacteria cannot be removed in settlement tanks because they float upwards and on the surface of the water.
BACKGROUND THEORY
It is well known that these cyanobacteria float because they contain gas vesicles that is they embody microscopic gas filled structures which ensure that they float rather than sink.
The gas vesicles of cyanobacteria are hollow, cylindrical structures with cone shaped ends. When a gas vesicle is subjected to a moderate pressure (up to 1 bar) it shows only a small volume change (shown to be about 1 part in 650 per bar for gas vesicles of cyanobacterium Anabaena flos-aquae in a report by A. E. Walsby in the Proceedings of the Royal Society of London, Volume 216, pages 355-368) but at a certain critical pressure the structure collapses flat. A. E. Walsby, in a paper in the Proceedings of the Royal Society of London, Volume 178, pages 301-326, showed that the average critical collapse pressure of gas vesicles in Anabaena flos-aquae varies from 4 bar to 8 bar with a mean value of about 6 bar. When the gas vesicle collapses the conical ends flatten to sectors of circles and pull away from the central cylinder, which flattens to a rectangular envelope. The contained gas diffuses out of the structure and dissolves in the surrounding water as the gas vesicle collapses.
When the gas vesicles inside cells of cyanobacteria are collapsed the cyanobacteria lose their means of buoyancy and sink. This is illustrated in FIG. 1 of a paper by A. E. Walsby in Bacteriological Reviews, Volume 36 pages 1-32, an article which contains much other information on gas vesicles and their properties. It has been established from research carried out by P. K. Hayes and A. E. Walsby in a paper in the British Phycological Journal, Volume 21, pages 191-197 that the median critical pressure of gas vesicles from different species of cyanobacteria varied from about 5-9 bar and were inversely correlated with the mean diameters.
PRIOR ART
Various methods of treating cyanobacteria or dispersing them have not been found to be successful and the most practical method of removal would be to cause them to sink, by collapsing their gas vesicles, whereby they could be removed along with the rest of the sediment in the water.
There have been two previous attempts to do this. The first involved an attempt to collapse gas vesicles in cyanobacteria by subjecting them to ultra sound as described in the discussion section of a paper by A. J. Brook in water treatment and examination, Volume 8 pages 133-137.
The second involved attempts to collapse gas vesicles by explosions detonated under water, described by A. E. Walsby in the New Scientist of 21 Nov. 1968 pages 436-437, and by D. Menday in Water Research Volume 6, pages 279-284.
Neither of these methods have proved to be practicable in a method of removing cyanobacteria from water. We describe here a new method of collapsing gas vesicles of cyanobacteria with a hydrostatic head of water, and the subsequent removal of these pressure-treated organisms from water by sedimentation.
Although not directly relevant to the treatment of water to remove gas vacuolate cyanobacteria, a method for the disposal of solid wastes has been disclosed in British Patent Specification No. 1,163,494. The method for disposing of solid biologically activated waste materials disclosed in this Specification, includes the steps of:
(a) providing the waste materials in an aqueous slurry;
(b) pumping the slurry to a well;
(c) transporting the slurry in the well to a porous and permeable underground formation; and
(d) pressure injecting the slurry under positive well head pressure directly into the porous and permeable underground formation at a pressure which the formation readily accepts the slurry without fracturing it.
Such a method would be totally unsuitable for the treatment of water to remove gas vacuolate cyanobacteria, in view of the following:
(a) the earlier Specification teaches the disposal of waste solids and not purification of water; and
(b) the various steps proposed in the earlier Specification are costly and time consuming and could in no way be technologically adapted to the treatment of water.
Other methods not directly relevant to the treatment of water to remove gas vacuolate cyanobacteria have been disclosed in British Patent specifications 1,521,258; 1,527,731: 1,540,065; and 1,573,907. All of these relate to the treatment of waste water and sewage by injection of gas containing free oxygen under pressure. The method employed in each of these specifications is such that it would prevent the collapse of the gas vesicles in gas vacuolate cyanobacteria as described by A. E. Walsby in the paper in the Proceedings of the Royal Society Volume 178 pages 301-326 and further, as is made clear in the last of these specifications No. 1,573,907, the addition of oxygen under pressure would cause the material to float rather than to sediment out.
SUMMARY OF THE INVENTION
It is an object of the present invention to overcome the above problems by providing a method of and apparatus for the removal of gas vacuolate cyanobacteria from water.
According to one aspect of the present invention there is provided a method of treatment of water to remove gas vacuolate cyanobacteria which includes the steps of: hydrostatically subjecting the water removed from a body of water to a predetermined pressure in order to collapse the gas vesicles inside the cells of the cyanobacteria, and separating the thus treated cyanobacteria by allowing them to sink to the bottom of settlement means along with any other sediment in the water.
Preferably the said predetermined pressure is approximately six bar, but may be as much as ten bar. A pressure exceeding 10 bar may be used but it is normally more than is needed to collapse the gas vesicles inside the cells of cyanobacteria that live in fresh water.
According to another aspect of the present invention there is provided apparatus for treatment of water to remove gas vacuolate cyanobacteria, including: means for hydrostatically subjecting the water removed from a body of water to a predetermined pressure in order to collapse the gas vesicles inside the cells of the cyanobacteria; and settlement means for separating the thus treated cyanobacteria that sink to the bottom of said settlement means along with any other sediment in the water.
The means for applying a hydrostatic pressure to the water may comprise firstly a lined bore-hole sunk in the ground, or secondly a tower case located above the ground, or thirdly a pump delivery pipe having at its remote end a diffuser or pressure relief valve necessary to ensure that the pump produces the required additional hydrostatic pressure in the pipe, or fourthly any combination of the bore-hole, the tower case and the pump delivery pipe with diffuser or relief value. In the case of the bore-hole and tower, the water is preferably applied through a centrally located pipe extending down the lined bore-hole or tower case to the bottom thereof. The minimum depth of the bore-hole or height of the tower case lies in the range of 31 m to 102 m, the preferred depth or height being 60 m.
Preferably the bore-hole is steel lined, but other designs of bore-hole, such as a down pipe linked to an up pipe in the form of a U-tube, may be used instead.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described in greater detail by way of example with reference to the accompanying drawings, wherein;
FIG. 1 is a diagrammatic representation of one preferred form of apparatus for the treatment of water to remove cyanobacteria;
FIG. 2 is an elevation view of one preferred apparatus for hydrostatically subjecting the water to a predetermined pressure in order to collapse the gas vesicles in the cyanobacteria;
FIG. 3 is a diagrammatic representation of a first alternative form of the apparatus shown in FIG. 1; and
FIG. 4 is a diagrammatic representation of a second alternative form of the apparatus shown in FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring first to FIG. 1, the apparatus for the treatment of water to remove cyanobacteria comprises: a pump 10, a steel-lined bore hole 12 and a settling tank 14. Water from a lake or reservoir 16 is pumped by the pump 10 through a pipe 18 having an appropriate filter in its nozzle inlet section 20. The pumped water is passed to the bore-hole 12 via a pipe 22. As mentioned above the bore-hole 12 is lined with a steel lining to contain the water under pressure. A pipe 24 extends centrally down the bore-hole 12 to within a short distance from the bottom. Any other suitable lining material may be used instead of steel.
The preferred depth of the bore-hole 12 is about 60 m. However, the actual depth for any particular set of conditions is quite critical and has to be determined by experiment. Sufficient pressure must be generated, by the hydrostatic head at the bottom of pipe 24, to collapse enough gas vesicles to cause loss of the cyanobacteria's buoyancy. The minimum pressure required depends on the species of cyanobacterium present and may be from 3 bar to 10 bar. Since a pressure of 1 bar is generated by a vertical water column of 10.2 m the required depth of pipe 24 below the surface is, correspondingly, about 31 m to 102 m. According to the nature of the cyanobacteria and the location, the preferred depth may therefore lie in the range of from 31 m to 102 m.
The water from the reservoir 16 is thus pumped by the pump 10 down to the bottom of the pipe 24, where for a depth of 60 m the hydrostatic pressure of the water at the bottom of the bore-hole 12 is approximately 6 bar. The water which flows out of the top of the bore-hole 12 is passed to the settling tank 14 by means of a pipe 26.
The construction of the bore-hole 12 is shown in greater detail in FIG. 2. After the bore-hole 12 has been dug in the ground it is sealed against penetration of liquid from the ground by being steel lined with a series of plates 13 or annular rings which are welded together. A circular steel plate 15 is provided at the bottom of the bore-hole 12. As shown, the pipe 22 from the pump 10 is connected to the centrally located vertical pipe 24 by means of an elbow joint 28 and flanges 30 and 32. The pipe 24 is centrally located within the steel-lined bore-hole by means of locating spiders 34 which are provided at equi-spaced intervals from top to bottom of the bore-hole 12.
In operation, water from the lake or reservoir 16, containing cyanobacteria is pumped to the bottom of the bore-hole 12 by means of the pipe 24, where the hydrostatic pessure builds up to about 6 bar. This pressure is sufficient to collapse the gas vesicles in the cyanobacteria, so that when they are carried out of the bore-hole 12 and into the settling tank 14 via the pipe 26, their specific gravity is now greater than unity so that they sink with the other sludge and foreign bodies to the bottom of the settling tank leaving clean treated water at the top of the settling tank from which it can be drawn for further treatment before being supplied to the customer.
A first alternative construction is shown in FIG. 3, wherein the height of the level of the lake or reservoir is above the location of the treatment apparatus and part of the hydrostatic head can be supplied by the difference in vertical level between the reservoir surface and the top of the bore-hole or between the top of a tower 44 and the top of a bore-hole 40. The required depth of the bore-hole 40 is reduced accordingly. As shown in FIG. 3, water from a reservoir 16 is pumped up to the top of a tower 44 by means of the pump 10 through a pipe 46. The bottom of the tower 44 is connected to the pipe 24 of the bore-hole 40 by a pipe 42.
Water is pumped into the top of the tower through the pipe 46 at a rate so as to maintain the level of water near the top of the tower 44. In this case the desired pressure of 6 bar can be produced by ensuring that the total head between the too of the tower 44 and the bottom of the pipe 24 is 60 m.
A second alternative construction is shown in FIG. 4 in which necessary to collapse the gas vesicles inside the cells of the cyanobacteria can be generated in a water container or pipe. As shown a pump 50 takes water from the reservoir 16 via the pipe 18 and supplies it to a horizontal cylindrical container or pipe 52 which is provided with a diffuser or pressure relief valve 54 at the other end. Water passing through the valve 54 is collected in the settling tank 14. The pressure which builds up in the container or pipe 52 is sufficient to collapse the gas vesicles inside the cells of the cyanobacteria which then sink to the bottom of the settling tank 14. Lastly a combination of the constructions shown in FIGS. 3 and 4 is possible.
Whilst the above constructions have been described in connection with water treatment processes for public water supply customers, it will be appreciated that the same method and apparatus could be used to decrease the amount of cyanobacteria that contain gas vesicles in natural lakes or other water impoundments, and thereby to improve the water quality. In this case the pressure-treated water is returned to the lake either directly from the bore-hole, in which case the cyanobacteria will settle out on the lake bottom, or after removing the cyanobacteria by sedimentation in a settling tank. The preferred method would be to withdraw water from a particular depth at one end of the lake and to return it after treatment to the lake at another depth at a point remote from the withdrawal site, so as to minimize mixing of the treated and untreated water. Regard would be paid to the patterns of water circulation in the lake so that withdrawal occurred at a site, such as at lee shores, where the cyanobacteria tended to accumulate.
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The treatment of water to remove gas vacuolate cyanobacteria is effected by subjecting the water to a predetermined pressure by being pumped down a centrally located pipe in a bore-hole, which is steel lined. This causes the gas vesicles in the cyanobacteria to collapse. The treated water is then stored in a settling tank where the cyanobacteria sink to the bottom and can be removed along with any other sediment in the water. The method can be applied to decrease the amount of cyanobacteria with gas vesicles in a lake or other water impoundment. (FIG. 1 )
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BACKGROUND OF THE INVENTION
This invention relates to the preparation of 1,3-propanediol. In one aspect, the invention relates to a cobalt-catalyzed process for manufacturing 1,3-propanediol in high yields without the use of a phosphine ligand for the cobalt catalyst.
1,3-propanediol (PDO) is an intermediate in the production of polyesters for fibers and films. It is known to prepare PDO in a two-step process involving (1) the cobalt-catalyzed hydroformylation (reaction with synthesis gas, H 2 /CO) of ethylene oxide to intermediate 3-hydroxypropanal (HPA) and (2) subsequent hydrogenation of the HPA to PDO. The initial hydroformylation process can be carried out at temperatures greater than 100° C. and at high syngas pressures to achieve practical reaction rates. The resulting product mixture is, however, rather unselective for HPA.
In an alternate synthesis method, the cobalt catalyst is used in combination with a phosphine ligand to prepare HPA with greater selectivity and at lower temperature and pressure. However, the use of a phosphine ligand adds to the cost of the catalyst and increases the complexity of catalyst recycle.
It would be desirable to prepare HPA in a low temperature, selective process which did not require the use of a phosphine ligand with the cobalt catalyst.
It is therefore an object of the invention to provide an economical process for the preparation of 1,3-propanediol which does not require the use of a phosphine-ligated catalyst for preparation of the HPA intermediate. It is a further object of one embodiment of the invention to provide a process for the preparation of 1,3-propanediol in which essentially all the cobalt hydroformylation catalyst can be conveniently recycled.
SUMMARY OF THE INVENTION
According to the invention, 1,3-propanediol is prepared in a process comprising the steps of:
(a) contacting ethylene oxide with carbon monoxide and hydrogen in an essentially non-water-miscible solvent in the presence of an effective amount of a non-phosphine-ligated cobalt catalyst and an effective amount of a lipophilic phosphine oxide promoter at a temperature within the range of about 50° to about 100° C. and a pressure within the range of about 500 to about 5000 psig, under reaction conditions effective to produce an intermediate product mixture comprising less than 15 wt % 3-hydroxypropanal;
(b) adding an aqueous liquid to said intermediate product mixture and extracting into said aqueous liquid at a temperature less than about 100° C. a major portion of the 3-hydroxypropanal so as to provide an aqueous phase comprising 3-hydroxypropanal in greater concentration than the concentration of 3-hydroxypropanal in said intermediate product mixture, and an organic phase comprising at least a portion of the cobalt catalyst or a cobalt-containing derivative thereof and at least a portion of the lipophilic phosphine oxide;
(c) separating the aqueous phase from the organic phase;
(d) contacting the aqueous phase comprising 3-hydroxypropanal with hydrogen in the presence of a hydrogenation catalyst at a pressure of at least about 100 psig and a temperature during at least a portion of the hydrogenation step of at least 40° C. to provide a hydrogenation product mixture comprising 1,3-propanediol;
(e) recovering 1,3-propanediol from said hydrogenation product mixture; and
(f) returning at least a portion of the organic phase comprising cobalt catalyst and lipophilic phosphine oxide to the process of step (a).
The process enables the production of 1,3-propanediol in high yields and selectivity without the use of a phosphine ligated cobalt catalyst in the hydroformylation step. The process also enables the recovery and recycle of essentially all the cobalt catalyst.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic flow diagram of one embodiment of the invention 1,3-propanediol preparation process.
DETAILED DESCRIPTION OF THE INVENTION
The invention 1,3-propanediol preparation process can be conveniently described by reference to FIG. 1. Separate or combined streams of ethylene oxide 1, carbon monoxide and hydrogen 2 are charged to hydroformylation vessel 3, which can be a pressure reaction vessel such as a bubble column or agitated tank, operated batchwise or in a continuous manner. The feed streams are contacted in the presence of a non-phosphine-ligated cobalt catalyst, i.e., a cobalt carbonyl composition which has not been prereacted with a phosphine ligand. The hydrogen and carbon monoxide will generally be introduced into the reaction vessel in a molar ratio within the range of about 1:2 to about 8:1, preferably about 1.5:1 to about 5:1.
The reaction is carried out under conditions effective to produce a hydroformylation reaction product mixture containing a major portion of 3-hydroxypropanal (HPA) and a minor portion of acetaldehyde, while maintaining the level of 3-hydroxypropanal in the reaction mixture at less than 15 wt %, preferably within the range of about 5 to about 10 wt %. (To provide for solvents having different densities, the desired concentration of HPA in the reaction mixture can be expressed in molarity, i.e., less than 1.5M, preferably within the range of about 0.5 to about 1M.) Generally, the hydroformylation reaction is carried out at elevated temperature less than 100° C., preferably about 60° to about 90° C., most preferably about 75° to about 85° C., and at a pressure within the range of about 500 to about 5000 psig, preferably (for process economics) about 1000 to about 3500 psig, with higher pressures generally imparting greater selectivity. The concentration of 3-hydroxypropanal in the intermediate product mixture can be controlled by regulation of process conditions such as ethylene oxide concentration, catalyst concentration, reaction temperature and residence time. In general, relatively low reaction temperatures (below about 90° C.) and relatively short residence times (about 20 minutes to about 1 hour) are preferred. In the practice of the invention it is possible to achieve HPA yields (based on ethylene oxide conversion) of greater than 80%, with formation of more than 7 wt % HPA in the dilute hydroformylation product mixture, at rates greater than 30 -1 . (Catalytic rates are referred to herein in terms of "turnover frequency" or "TOF" and are expressed in units of moles per mole of cobalt per hour, or h -1 .) Reported rates are based on the observation that, before a majority of the ethylene oxide is converted, the reaction is essentially zero-order in ethylene oxide concentration and proportional to cobalt concentration.
The hydroformylation reaction is carried out in a liquid solvent inert to the reactants. By "inert" is meant that the solvent is not consumed during the course of the reaction. In general, ideal solvents for the phosphine ligand-free process will solubilize carbon monoxide, will be essentially non-water-miscible and will exhibit low to moderate polarity such that the 3-hydroxypropanal intermediate will be solubilized to the desired concentration of at least about 5 wt % under hydroformylation conditions, while significant solvent will remain as a separate phase upon water extraction. By "essentially non-water-miscible" is meant that the solvent has a solubility in water at 25° C. of less than 25 wt % so as to form a separate hydrocarbon-rich phase upon water extraction of HPA from the hydroformylation reaction mixture. Preferably this solubility is less than about 10%, most preferably less than about 5 wt %. The solubilization of carbon monoxide in the selected solvent will generally be greater than 0.15 v/v (1 atm, 25° C.), preferably greater than 0.25 v/v, expressed in terms of Ostwald coefficients.
The preferred class of solvents are alcohols and ethers which can be described according to the formula
R.sub.2 --O--R.sub.1 (1)
in which R 1 is hydrogen C 1-20 linear, branched, cyclic or aromatic hydrocarbyl or mono- or polyaklene oxide and R 2 is a C 1-20 linear, branched, cyclic or aromatic C 1-20 hydrocarbyl or mono- or polyalkylene oxide. The most preferred hydroformulation solvents can be described by the formula ##STR1## in which R 1 is hydrogen or C 1-8 hydrocarbyl or alkenylene oxide and R 3 , R 4 and R 5 independently selected from C 1-8 hydrocarbyl and alkylene oxide. Such ester include, for example, methyl-t-butyl ether, ethyl-t-butyl ether, ethoxyethyl ether, phenylisobutyl ether, diphehenyl ether, diethyl ether, and diisopropyl ether. Blends of solvents such as tetrahydrofuran/toluene, tetrahydrofuran/heptane and t-butylalcohol/hexane can also be used to achieve the desired solvent properties. The currently preferred solvent, because of the high yields of HPA which can be achieved under moderate reaction conditions, is methyl-t-butyl ether.
The catalyst is a non-phosphine-ligated cobalt carbonyl compound. Although phosphine-ligated catalysts are active for hydroformylation reactions, the invention process is designed to achieve good yield and selectivity without the additional expense of the ligand. The cobalt catalyst can be supplied to the hydroformylation reactor in essentially any form including metal, supported metal, Raney-cobalt, hydroxide, oxide, carbonate, sulfate, acetylacetonate, salt of a carboxylic acid, or as an aqueous cobalt salt solution, for example. It may be supplied directly as a cobalt carbonyl such as dicobaltoctacarbonyl or cobalt hydridocarbonyl. If not supplied in the latter forms, operating conditions can be adjusted such as that cobalt carbonyls are formed in situ via reaction with H 2 and CO, as described in J. Falbe, "Carbon Monoxide in Organic Synthesis," Springer-Verlag, N.Y. (1970). In general, catalyst formation conditions will include a temperature of at least 50° C. and a carbon monoxide partial pressure of at least about 100 psig. For more rapid reaction, temperatures of about 120° to 200° C. should be employed, at CO pressures of at least 500 psig. Addition of high surface area activated carbons or zeolites, especially those containing or supporting platinum or palladium metal, can accelerate cobalt carbonyl formation from noncarbonyl precursors. The resulting catalyst is maintained under a stabilizing atmosphere of carbon monoxide, which also provides protection against exposure to oxygen. The most economical and preferred catalyst activation and reactivation (of recycled catalyst) method involves preforming the cobalt salt (or derivative) under H 2 /CO in the presence of the catalyst promoter employed for hydroformylation. The conversion of Co +2 to the desired cobalt carbonyl is carried out at a temperature within the range of about 75° to about 200° C., preferably about 100° to about 140° C. and a pressure within the range of about 1000 to about 5000 psig for a time preferably less than about 3 hours. The preforming step can be carried out in a pressurized preforming reactor or in situ in the hydroformylation reactor.
The amount of cobalt present in the reaction mixture will vary depending upon the other reaction conditions, but will generally fall within the range of about 0.01 to about 1 wt %, preferably about 0.05 to about 0.3 wt %, based on the weight of the reaction mixture.
The hydroformylation reaction mixture will include a lipophilic phosphine oxide to accelerate the reaction rate without imparting hydrophilicity (water solubility) to the active catalyst. By "lipophilic" is meant that the promoter tends to remain in the organic phase after extraction of HPA with water. The phosphine oxide will be present in an amount effective to promote the hydroformylation reaction to HPA, generally an amount within the range of about 0.01 to about 0.6 moles per mole of cobalt.
Suitable phosphine oxides include those represented by formula (1): ##STR2## in which each R group is independently selected from unsubstituted and inertly-substituted C 1-25 linear, branched, cyclic and aromatic hydrocarbyl and mono- and polyalkylene oxide. Such phosphine oxides include triphenylphosphine oxide, tributylphosphine oxide, dimethylphenylphosphine oxide and triethylphosphine oxide. The currently preferred phosphine oxide, because of its availability and demonstrated promotion of ethylene oxide hydroformylation, is triphenylphosphine oxide.
It is generally preferred to regulate the concentration of water in the hydroformylation reaction mixture, as excessive amounts of water reduce (HPA+PDO) selectivity below acceptable levels and may induce formation of a second liquid phase. At low concentrations, water can assist in promoting the formation of the desired cobalt carbonyl catalyst species. Acceptable water levels will depend upon the solvent used, with more polar solvents generally being more tolerant of higher water concentrations. For example, optimum water levels for hydroformylation in methyl-t-butyl ether solvent are believed to be within the range of about 1 to about 2.5 wt %.
Following the hydroformylation reaction, hydroformylation reaction product mixture 4 containing 3-hydroxypropanal, the reaction solvent, 1,3-propanediol, the cobalt catalyst and a minor amount of reaction by-products, is cooled and passed to extraction vessel 5, wherein an aqueous liquid, generally water and optional miscibilizing solvent, are added via 6 for extraction and concentration of the HPA for the subsequent hydrogenation step. Liquid extraction can be effected by any suitable means, such as mixer-settlers, packed or trayed extraction columns, or rotating disk contactors. Extraction can if desired be carried out in multiple stages. The water-containing hydroformylation reaction product mixture can optionally be passed to a settling tank (not shown) for resolution of the mixture into aqueous and organic phases. The amount of water added to the hydroformylation reaction product mixture will generally be such as to provide a water:mixture ratio within the range of about 1:1 to about 1:20, preferably about 1:5 to about 1:15. The addition of water at this stage of the reaction may have the additional advantage of suppressing formation of undesirable heavy ends. Extraction with a relatively small amount of water provides an aqueous phase which is greater than 20 wt % HPA, preferably greater than 35 wt % HPA, permitting economical hydrogenation of the HPA to PDO. The water extraction is preferably carried out at a temperature within the range of about 25° to about 55° C. with higher temperatures avoided to minimize condensation products (heavy ends) and catalyst disproportionation to inactive, water-soluble cobalt species. In order to maximize catalyst recovery, it is optional but preferred to perform the water extraction under 50 to 200 psig carbon monoxide at 25° to 55° C.
The organic phase containing the reaction solvent and the major portion of the cobalt catalyst can be recycled from the extraction vessel to the hydroformylation reaction via 7. Aqueous extract 8 is optionally passed through one or more acid ion exchange resin beds 9 for removal of any cobalt catalyst present, and the decobaited aqueous product mixture 10 is passed to hydrogenation vessel 11 and reacted with hydrogen 12 in the presence of a hydrogenation catalyst to produce a hydrogenation product mixture 13 containing 1,3-propanediol. The hydrogenation step may also revert some heavy ends to PDO. The solvent and extractant water 15 can be recovered by distillation in column 14 and recycled to the water extraction process, via a further distillation (not shown) for separation and purge of light ends. PDO-containing stream 16 can be passed to distillation column 17 for recovery of PDO 18 from heavy ends 19.
Hydrogenation of the HPA to PDO can be carried out in aqueous solution at an elevated temperature during at least a portion of the hydrogenation step of about 40° C., generally within the range of about 50° to about 175° C., under a hydrogen pressure of at least about 100 psig, generally within the range of about 200 to about 2000 psig. The reaction is carried out in the presence of a hydrogenation catalyst such as any of those based upon Group VIII metals, including nickel, cobalt, ruthenium, platinum and palladium, as well as copper, zinc and chromium. Nickel catalysts, including bulk, supported and fixed-bed forms, provide acceptable activities and selectivities at moderate cost. Highest yields are achieved under slightly acidic reaction conditions.
Commercial operation will require efficient cobalt catalyst recovery with essentially complete recycle of cobalt to the hydroformylation reaction. The preferred catalyst recovery process involves two steps, beginning with the above-described water extraction of HPA from the hydroformylation product mixture. A majority of the cobalt catalyst will remain in the organic phase, with the remaining cobalt catalyst passing into the water phase. The organic phase can be recycled to the hydroformylation reactor, with optional purge of heavy ends. Optionally, further decobalting of catalyst in the water layer can be effected by suitable method, such as complete or partial oxidation of cobalt followed by precipitation and filtration, distillation, deposition on a solid support, or extraction using a suitable extractant, preferably prior to final cobalt removal by ion exchange (9).
The invention process permits the selective and economic synthesis of PDO-at moderate temperatures and pressures without the use of a phosphine ligand for the hydroformylation catalyst. The process involves preparation of a reaction product mixture dilute in intermediate HPA, then concentration this HPA by water extraction followed by hydrogenation of the aqueous HPA to PDO.
EXAMPLE 1
A 300-ml stirred batch reactor was charged under nitrogen with 0.87 g dicobaltoctacarbonyl, 1.5 g toluene (marker), 2 g deionized water and 146 g methyl-t-butyl ether (MTBE). The nitrogen atmosphere was flushed with H 2 , and the reactor was filled to 600 psig H 2 and then to 1200 psig with 1:1 CO/H 2 . Reactor contents were heated to 80° C. for one hour, and 10 g of ethylene oxide were then injected, with simultaneous increase in reactor pressure to 1500 psig via addition of 1:1 CO/H 2 . Reactor contents were samples and analyzed via capillary g.c. (with flame ionization detector) at approximately 40% and nearly 100% conversion of EO, which occurred within two hours. At approximately 40% conversion, 3.3 wt % HPA had been formed at a rate of 18 h -1 .
EXAMPLE 2
Example 1 was repeated in the absence of added water and with addition of 0.14 g of sodium acetate trihydrate as promoter, added at a ratio Na/Co of 0.2. HPA was formed at a rate of 41 h -4 . After cooling and addition of 30 g deionized water for extraction, only 77% of the cobalt catalyst remained with the upper solvent layer. 23% of the cobalt was extracted with the aqueous product. This fraction corresponds approximately to the amount of sodium acetate added to promote the reaction.
EXAMPLE 3
These experiments illustrate the effectiveness of triphenylphosphine oxide both to accelerate the hydroformylation reaction and to permit the recycle of essentially all the cobalt catalyst in the organic phase following water extraction of product HPA. Example 1 was repeated with addition of 0.4 g of triphenylphosphine oxide as promoter, for a ratio of 0.26 moles promoter per mole of cobalt. At approximately 50% conversion, 4.3 wt % HPA had been formed at a rate of 39h -1 , or more than a two-fold rate increase over that observed in the absence of promoter in Example 1. The reaction was terminated at 95% conversion of ethylene oxide with formation of 8.6 wt % HPA.
Following the reaction, the mixture was cooled to room temperature. 32.7 g of deionized water were added for extraction of product under 200 psig synthesis gas. After 30 minutes, mixing was terminated and 37.5 g of an aqueous product layer containing 22.0 wt % HPA was isolated. The aqueous layer contained 165 ppm cobalt, or only 3% of the total charged. The upper organic layer (107.34 g) was analyzed to contain 0.2 wt % cobalt. Recycle of 97% of the cobalt catalyst with the organic layer represents reduction in cobalt loss by a factor of 7, relative to that observed with sodium acetate promotion in Example 2.
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1,3-Propanediol is prepared in a process which involves reacting ethylene oxide with carbon monoxide and hydrogen in an essentially non-water-miscible solvent in the presence of a non-phosphine-ligated cobalt catalyst and a lipophilic phosphine oxide promoter to produce an intermediate product mixture containing 3-hydroxypropanal in an amount less than 15 wt %; extracting the 3-hydroxypropanal from the intermediate product mixture into an aqueous liquid at a temperature less than about 100° C. and separating the aqueous phase containing 3-hydroxpropanal from the organic phase containing cobalt catalyst; hydrogenating the 3-hydroxypropanal in the aqueous phase to 1,3-propanediol; and recovering the 1,3-propanediol.
The process enables the production of 1,3-propanediol in high yields and selectively without the use of a phosphine ligand-modified cobalt catalyst.
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CROSS REFERENCE RELATED TO APPLICATION
This application is a division of 09/783,649, filed Feb. 14, 2001, now U.S. Pat. No. 6,410,787, which claims the benefit of the following provisional application: U.S. Ser. No. 60/184,020, filed Feb. 22, 2000, under 35 USC 119(e)(i).
FIELD OF THE INVENTION
The present invention relates to (2S)-enantiomers of 2-aminoindan derivatives and a novel process for the preparation of them.
BACKGROUND OF THE INVENTION
Schizophrenia is a common and devastating mental disorder which is currently an unmet medical need. It is characterized by so-called positive (hallucinations, delusions) and negative (blunted affect, poverty of speech, social & emotional withdrawal) symptoms, as well as cognitive deficits (working memory impairment). About 1% of the world population is affected, men and women equally, with typical onset between ages 15 and 25. Antagonists of the neurotransmitter dopamine are known to block psychosis. The present invention provides compounds of formula I (wherein each R is independently C 1-8 alkyl), a highly selective D 3 receptor antagonist, for the treatment of Schizophrenia and other CNS diseases.
Racemic forms of formula I and their preparations have been disclosed in PCT publication WO 97/45403. The present invention has discovered that the (2S)-enantiomer of formula I is the form that possesses the superior desirable bioactivity. The present invention also provides a process for the synthesis, in a large scale, of said (2S)-enantiomer in a highly enantiomerically enriched form, which solved an extremely challenging problem of a long period of time.
Information Disclosure
PCT International Publication No. WO097/45403 discloses aryl substituted cyclic amines as selective dopamine D3 ligands.
U.S. Pat. No. 5,708,018 discloses 2-aminoindans as selective dopamine D3 ligands.
SUMMARY OF THE INVENTION
The present invention provides compounds of formula I:
or a pharmaceutically acceptable salt thereof wherein each R is independently C 1-8 alkyl.
More preferably, a compound of formula I of the present invention is (2S)-(+)-2-(dipropylamino)-6-ethoxy-2,3-dihydro-1H-indene-5-carboxamide or a pharmaceutically acceptable salt thereof.
In another aspect, the present invention also provides:
a process for the preparation of (2S)-enantiomers of formulas I in a highly enantiomerically enriched form; novel intermediates in a highly enantiomerically enriched form useful for preparing compounds of formula I; a pharmaceutical composition comprising a compound of formula I, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier (the composition preferably comprises a therapeutically effective amount of the compound or salt), a method for treating a disease or condition in a mammal wherein a D 3 receptor is implicated and modulation of a D 3 receptor function is desired comprising administering a therapeutically effective amount of a compound of formula I, or a pharmaceutically acceptable salt thereof to the mammal; a method for treating or preventing anxiety, obesity, depression, schizophrenia, a stress related disease (e.g. general anxiety disorder), panic disorder, sleep disorders, a phobia, mania, obsessive compulsive disorder, post-traumatic-stress syndrome, immune system depression, a stress induced problem with the gastrointestinal or cardiovascular system, or sexual dysfunction in a mammal comprising administering a therapeutically effective amount of a compound of formula I, or a pharmaceutically acceptable salt thereof to the mammal; a method for treating or preventing ADHD (attention deficit hyperactivity disorder), migraine, substance abuse (including smoking cessation), cognitive deficits, memory impairment alzheimer's disease, movement disorders including choreatic movements in huntington's disease or motor complications such as dystonias and dyskinesias in Parkinson's disease, extrapyramidal side effects related to the use of neuroleptics, and “Tics” including Tourette's syndrome in a mammal comprising administering a therapeutically effective amount of a compound of formula I, or a pharmaceutically acceptable salt thereof to the mammal.
DETAILED DESCRIPTION OF THE INVENTION
The following definitions are used, unless otherwise described.
The term alkyl refer to both straight and branched groups, but reference to an individual radical such as “propyl” embraces only the straight chain radical, a branched chain isomer such as “isopropyl” being specifically referred to.
The carbon atom content of various hydrocarbon-containing moieties is indicated by a prefix designating the minimum and maximum number of carbon atoms in the moiety, i.e., the prefix C i-j indicates a moiety of the integer “i” to the integer “j” carbon atoms, inclusive. Thus, for example, C 1-8 alkyl refers to alkyl of one to eight carbon atoms, inclusive.
Mammal refers to human or animals.
Pharmaceutically acceptable salts refer to organic acid addition salts such as tosylate, methanesulfonate, acetate, citrate, malonate, tartarate, succinate, benzoate, ascorbate, α-ketoglutarate, α-glycerophosphate, or suitable inorganic salts including hydrochloride, hydrobromide, sulfate, nitrate, bicarbonate, and carbonate salts, etc.
The term “chiral salt” refers to a salt containing a chiral acid. The term “chiral acids” refers to the acids having one or more chiral centers. Examples of chiral acids are tartaric acid, di-benzoyltartaric acid, di-para-toluoyltartaric acid, camphorsulfonic acid, and mandelic acid. The preferred chiral acid is mandelic acid.
All temperatures are in degrees Centigrade.
[α] D 25 refers to the angle of rotation of plane polarized light (specific optical rotation) at 25° C. with the sodium D line (589 A).
The compounds of formula I are active orally or parenterally. Orally the formula I compounds can be given in solid dosage forms such as tablets or capsules, or can be given in liquid dosage forms such as elixirs, syrups or suspensions as is known to those skilled in the art. It is preferred that the formula I compounds be given in solid dosage form and that it be a tablet.
Typically, the compounds of formula I can be given in the amount of about 0.5 mg to about 250 mg/person, one to three times a day. Preferably, about 5 to about 50 mg/day in divided doses.
The exact dosage and frequency of administration depends on the particular compound of formula I used, the particular condition being treated, the severity of the condition being treated, the age, weight, general physical condition of the particular patient, other medication the individual may be taking as is well known to those skilled in the art and can be more accurately determined by measuring the blood level or concentration of the active compound in the patient's blood and/or the patient's response to the particular condition being treated.
Thus, the subject compounds, along with a pharmaceutically-acceptable carrier, diluent or buffer, can be administrated in a therapeutic or pharmacological amount effective to alleviate the central nervous system disorder with respect to the physiological condition diagnosed. The compounds can be administered intravenously, intramuscularly, topically, transdermally such as by skin patches, buccally or orally to man or other vertebrates.
The compositions of the present invention can be presented for administration to humans and other vertebrates in unit dosage forms, such as tablets, capsules, pills, powders, granules, sterile parenteral solutions or suspensions, oral solutions or suspensions, oil in water and water in oil emulsions containing suitable quantities of the compound, suppositories and in fluid suspensions or solutions.
For oral administration, either solid or fluid unit dosage forms can be prepared. For preparing solid compositions such as tablets, the compound can be mixed with conventional ingredients such as talc, magnesium stearate, dicalcium phosphate, magnesium aluminum silicate, calcium sulfate, starch, lactose, acacia, methylcellulose, and functionally similar pharmaceutical diluent or carrier materials. Capsules are prepared by mixing the compound with an inert pharmaceutical diluent and filling the mixture into a hard gelatin capsule of appropriate size. Soft gelatin capsules are prepared by machine encapsulation of a slurry of the compound with an acceptable vegetable oil, light liquid petrolatum or other inert oil.
Fluid unit dosage forms for oral administration such as syrups, elixirs, and suspensions can be prepared. The forms can be dissolved in an aqueous vehicle together with sugar, aromatic flavoring agents and preservatives to form a syrup. Suspensions can be prepared with an aqueous vehicle with the aid of a suspending agent such as acacia, tragacanth, methylcellulose and the like.
For parenteral administration, fluid unit dosage forms can be prepared utilizing the compound and a sterile vehicle. In preparing solutions, the compound can be dissolved in water for injection and filter sterilized before filling into a suitable vial or ampoule and sealing. Adjuvants such as a local anesthetic, preservative and buffering agents can be dissolved in the vehicle. The composition can be frozen after filling into a vial and the water removed under vacuum. The lyophilized powder can then be sealed in the vial and reconstituted prior to use.
The present invention provides a process for preparing compounds of formula I in a highly enantiomerically enriched form as depicted in Scheme I. The starting material I-1 in Scheme I can be prepared according to the procedures described in Chart A of U.S. Pat. No. 5,708,018.
In step 1, compound I-1 is converted to compound I-2 as a racemic mixture via catalytic hydrogenation in the presence of an appropriate catalyst, such as palladium on carbon, W-2 Raney nickel or platinum on sulfide carbon, in an appropriate solvent, such as ethanol, THF, ethyl acetate or combinations thereof. The desired enantiomer I-2b can be obtained by treating structure I-2 with an appropriate chiral acid in an appropriate solvent to form the corresponding chiral salt complex, which subsequently crystallizes from the solvent. Resolutions to separate an individual enantiomer I-2a or I-2b from a racemic mixture often pose a significant challenge in the quest to obtain enantiomerically pure compound. In general, a wide variety of enantiomerically pure acids can provide some measure of enantiomer enrichment. However, the choice of the particular chiral acid and solvent system proves very important to the efficiency of the resolution (enantiomeric purity and chemical yield). The preferred chiral acids in the present invention for the resolution include tartaric acid, di-benzoyltartaric acid, di-para-toluoyltartaric acid, camphorsulfonic acid, and mandelic acid. The most preferred chiral acid is mandelic acid. An examination of resolving acids and solvent systems indicate that (R)-(−)-mandelic acid and (1R)-(−)-10-camphorsulfonic acid perform very well for the resolution of racemic I-2 to induce the crystallization of almost enantiomerically pure I-2b, with (R)-(−)mandelic acid being preferred. Note that it is not necessary to obtain enantiomer I-2b as 100% pure enantiomeric material at this stage of the synthesis since subsequent crystallization procedures in the following procedures will serve to provide a slight upgrade to the final enantiomeric purity. It will be apparent to those skilled in the art that other chiral acids commonly used to perform resolution of amines may also be useful for this resolution. Solvent systems in the present invention, which are found to be useful to optimize the recovery of compound I-2b, include alcohol solvents such as methanol, ethanol, isopropanol, etc. as well as co-solvents of alcohol(s), acetonitrile (ACN), or water in various proportions such as tetrahydrofuran (THF), ether, , methyl tertiary butyl ether (MTBE), dimethoxyethane (DME), etc. The preferred solvent system in combination with (R)-(−)-mandelic acid is a mixture of methanol and tetrahydrofuran.
Next, alkylation of I-2b, in a form of free base or chiral salt complex, with an alkylation agent in the presence of an appropriate base and an appropriate polar solvent system at a temperature in a range of about 20° C. to 90° C. provides compound I-3. The appropriate base includes K 2 CO 3 , Na 3 PO 4 , Na 2 B 4 O 7 , etc. The preferred base is Na 3 PO 4 The appropriate solvent includes ACN, dimethylformamide (DMF), or THF. The preferred solvent is ACN. The preferred temperature is in a range of from about 60° C. to about 75° C. Compound I-3 is then converted to compound I-4 by acetylation followed by hydrogenolysis in the presence of an appropriate catalyst, such as palladium on carbon or platinum on sulfide carbon, and an appropriate acetylation reagent such as acetic anhydride, or acetyl chloride with catalytic dimethylaminopyridine, in an appropriate solvent, such as acetic acid, an alcohol, water or combinations thereof, at a temperature in a range of from about 20° C. to reflux. The preferred condition for this reaction is in acetic anhydride/acetic acid at a temperature in a range of from about 55° C. to about 70° C. Bromination of compound I-4 with a brominating reagent in the presence of an acid and a polar solvent system at a temperature in a range of from about −78° C. to about room temperature provides compound I-5. The instant bromination provides an unexpected improvement in regioselectivity for bromination at the desired position by using an appropriate brominating reagent. A suitable brominating reagent may be Br 2 , dibromantin, N-bromosuccinimide (NBS), pyridinium tribromide (pyrHBr 3 ). The preferred brominating reagent is pyridinium tribromide. The acid in the reaction is preferably a strong acid such as HBr, H 2 SO 4 , TiCl 4 , TFA, MeSO 3 H, Cl 3 CCO 2 H, Cl 2 CCO 2 H, or citric acid. The more preferred acid is TFA. The suitable polar solvent may be ACN, DMF, EtOAc, an alcohol such as methanol, CH 2 Cl 2 , MTBE, THF, etc. The preferred solvent is CH 2 Cl 2 The preferred temperature is in a range from about −15° C. to room temperature. Finally, carboxamidation I-5 in the presence of transition metal such as palladium, palladium on carbon or palladium acetate and associated ligands such as mono or bidentate phosphines in an appropriate solvent with an appropriate base at a temperature in a range from about 70° C. to about 140° C. provides the desired compound I-6. Preferred ligands include triphenylphosphine, tri-orthotolulyphosphine, or 1,3-bis(diphenylphosphino)propane. Preferred temperature is in a range from about 95° C. to about 105° C. The appropriate solvents include dimethylformamide, dioxane, toluene, dimethoxyethane, dimetylacetamide, etc. The preferred solvent is dimethylformamide. The appropriate base include potassium carbonate, tertiary amine bases, Na 3 PO 4 , LiHMDS, Li-amides, alkoxides, etc. The preferred base is potassium carbonate.
Without further elaboration, it is believe that one skilled in the art can, using the preceding description, practice the present invention to its fullest extent. The following detailed example describe how to prepare the various compounds and/or perform the various processes of the invention and are to be construed as merely illustrative, and not limitations of the preceding disclosure in any way whatsoever. Those skilled in the art will promptly recognize appropriate variations from the procedures both as to reactants and as to reaction conditions and techniques.
EXAMPLE
Preparation of (2S)-(+)-2-(Dipropylamino)-6-ethoxy-2,3-dihydro-1H-indene-5-carboxamide
Step 1: Preparation of 4-ethoxycinamic acid
4-Ethoxybenzaldehyde (1) is condensed with malonic acid in the presence of base (Knovenagel reaction) to obtain the cinnamic acid derivative 2. This is accomplished by dissolving 1 in pyridine with 0.15 eq. of piperidine and heating the resulting solution to 50-135° C. (preferably 105-125° C.) after which a solution of malonic acid (2 eq.) dissolved in pyridine is added in a slow stream. Approximately 40% of the pyridine is slowly distilled off and the heating continued at 125° C. until TLC indicated that all of 1 has been consumed. Cool to 40° C. and add excess concentrated hydrochloric acid, keeping the temperature at around 40° C. Cool to below room temperature and filter the solid product (2), washing with water and then drying.
1 H NMR (300 MHz, CDCl 3 ) δ 1.43 (t, J=7.0 Hz, 3H), 4.07 (q, J=7.0 Hz, 2H), 6.31 (d, J=16.0 Hz, 1H), 6.90 (d, J=8.8 Hz, 2H), 7.49 (d, J=8.7 Hz, 2H), 7.74 (d, J=15.9 Hz, 1H).
Step 2: Preparation of 4-ethoxycinnamic Acid
4-Ethoxycinnamic acid (2) is hydrogenated at 40 p.s.i. with catalytic 5% palladium on carbon in tetrahydrofuran solvent to obtain 3-(4-ethoxyphenyl)propionic acid (3). A sample is recrystallized from ethyl acetate/hexane to obtain an analytically pure sample (m.p. 101-103° C.).
1 H NMR (300 MHz, CDCl 3 ) δ 1.40 (t, J=7.0 Hz, 3H), 2.65 (t, J=7.7 Hz, 2H), 2.90 (t, J=7.7 Hz, 2H), 4.01 (q, J=7.0 Hz, 2H), 6.83 (d, J=8.6Hz, 2H), 7.12 (d, J=8.6 Hz, 2H).
Step 3: Preparation of 6-ethoxy-1-indanone
To carboxylic acid 3 is added thionyl chloride (2 eq.) and catalytic dimethylformamide. The solution is stirred until analysis indicated that all of the carboxylic acid had been converted to the acid chloride. Remove volatile reagents under vacuum. The acid chloride is dissolved in dichloromethane and added to a slurry of aluminum chloride (1.1 eq.) in dichloromethane over 15-60 minutes. The resulting mixture is heated to reflux for 30 minutes (until analysis indicated that all of the starting material had been consumed) and then cooled to 0-15° C. Water is added slowly to quench the reaction and then the mixture is extracted. The organic layer is washed with saturated aqueous sodium bicarbonate and the organic solution is stripped of dichloromethane solvent under vacuum to afford a residue that is redissolved in methyl t-butyl ether and then dried with magnesium sulfate. The solution is filtered and the solvent removed under vacuum to afford solid 4. The solid could be recrystallized from octane to afford an analytical sample (m.p. 57-58° C.).
1 H NMR (300 MHz, CDCl 3 ) δ 1.41 (t, J=7.0 Hz, 3H), 2.66-2.71 (m, 2H), 3.04 J=5.7 Hz, 2H), 4.04 (q, J=7.0 Hz, 2H), 7.13-7.18 (m, 2H), 7.32-7.35 (m, 1 H).
Step 4: Preparation of 6-ethoxy-1H-indene-1,2(3H)-dione-2-oxime
A solution of 6-ethoxy-1-indanone and isoamylnitrite (1.5 eq.) in ethyl acetate are cooled to approximately 0° C. and concentrated hydrochloric acid (1.1 acid equivalents) is added at a rate to keep the temperature below 40° C. After the addition is completed the slurry is stirred at 5-10° C. until analysis indicated that all of the starting material is consumed. The product is filtered and rinsed with cold ethyl acetate. The oxime product (5) can be easily purified by refluxing as a slurry in anhydrous ethanol, cooling filtering, and then washing the solid with more ethanol and then drying (m.p. 220° C. decomp.).
1 H NMR (300 MHz, DMSO-d 6 ) δ 1.32 (t, J=7.0 Hz, 3H), 3.65 (s, 2H), 4.06 (q, J=7.0 Hz, 2H), 7.14 (d, J=2.5 Hz, 1H), 7.27 (dd, J=2.6, 8.4 Hz, 1H), 7.49 (d, J=8.4 Hz, 1H), 12.57 (s, 1H).
Step 5: Preparation of (±)-trans-2-amino-6-ethoxy-2,3-dihydro-1H-inden-1-ol
6-Ethoxy-1H-indene-1,2(3H)-dione 2-oxime is slurried in absolute ethanol, and approximately 0.5 eq. 2N sodium hydroxide is added. Palladium on carbon is added, and the mixture is hydrogenated in a Parr shaker with an initial hydrogen pressure of 40 psi for several hours (depending upon the scale of the reaction and the catalyst loading). After analysis indicated that all of the starting material is consumed, the catalyst is filtered from the solution and then the solvent is removed under vacuum, and the residue is diluted with water and extracted with ethyl acetate several times. The ethyl acetate extracts are combined and concentrated under vacuum. Hexane is added and the resulting slurry is cooled to 0-15° C. and the solid product (6) is rinsed with cold ethyl acetate/hexane (1:1). The product is dried under vacuum.
An analytical sample is obtained by combined an aliquot of the product (6) with p-toluene sulfonic acid, and the resulting salt is crystallized from methanol/diethylether to afford a material of m.p. 172-173° C.
1 H NMR (300 MHz, CDCl 3 ) δ 1.394 (t, J=7.0 Hz, 3H), 2.51 (dd, J=8.3, 14.9 Hz, 1H), 3.13 (dd, J=7.3, 15.1 Hz, 1H), 3.43 (q, J=7.2 Hz, 1H), 4.02 (q, J=7.0 Hz, 2 H), 4.73 (d, J=6.7 Hz, 1H), 6.78 (dd, J=2.2, 8.2 Hz, 1H), 6.90 (d, J=2.2 Hz, 1H), 7.06 (d, J=8.2 Hz, 1H).
Step 6: Preparation of (1S, 2S)-trans-(−)-2-amino-6-ethoxy-2,3-dihydro-1H-inden-1-ol (R)-(−)-mandelate
(±)-trans-2-Amino-6-ethoxy-2,3-dihydro-1H-inden-1-ol in a mixture of methanol and tetrahydrofuran is added to a warm solution of a slight molar excess of (R)-(−)-mandelic acid in tetrahydrofuran, so that the result is a solution at about 60° C. in about 3-4 ml/g methanol and about 40-50 ml/g tetrahydrofuran. The desired mandelate salt (7) crystallizes from solution and is isolated by filtration and drying. (m.p. 170-195° C.). When treated with (R)-(−)-10-camphorsulfonic acid in methanol, the desired enantiomer (7) crystallizes from solution as the sulfonic acid salt complex (m.p. 238-239° C.). [α] 25 D =−8° (c=0.94, methanol).
Step 7: Preparation of (1S, 2S)-trans-2-(dipropylamino)-6-ethoxy-2,3-dihydro-1H-inden-1-ol
Aminoalcohol mandelate salt (7) is added to acetonitrile solvent with excess tribasic sodium phosphate and n-bromopropane and stirred until analysis indicates that starting material is completely converted to the dipropyl-substituted material (8). The preferred procedure is to heat the slurry at 60-70° C. for two-three days. The reaction is cooled, filtered, and the solids rinsed with methyl t-butyl ether. The solution is concentrated under vacuum and then more methyl t-butyl ether is added and the solution extracted with aqueous sodium hydroxide. The organic layer is washed with excess dilute aqueous hydrochloric acid and the aqueous hydrochloric acid extracts are combined and back-washed with methyl t-butyl ether and then made basic with concentrated aqueous sodium hydroxide. This aqueous solution is then washed with methyl t-butyl ether. The ether is removed under vacuum to obtain the dipropyl compound (8) as a solid. It is apparent to those skilled in the art that other similar alkylating reagents can be utilized in place of n-bromopropane, such as n-propyliodide, etc. Also, other bases can be utilized in place of the phosphate base, such as sodium carbonate, organic tertiary amine bases such as diisopropylethylamine, etc. The preferred procedure is to use n-bromopropane and tribasic sodium phosphate. Additionally, it is apparent to those skilled in the art that reductive amination procedures can also be used to perform this chemical transformation, including using propanal in the presence of a hydride transfer reducing reagent such as sodium triacetoxyborohydride, sodium cyanoborohydride, etc. Alternatively, the amine can be repetitively acylated to form the propionamide of the amine and then reduced to the amine with lithium aluminum hydride, diisobutylhydride, a borane reagent, etc. two times to introduce the required propyl groups. The preferred method to obtain 8 is to heat 7 with n-bromopropane in the presence of tribasic sodium phosphate. An analytical sample can be crystallized from ethyl acetate/hexane (m.p. 74-75° C.).
1 H NMR (300 MHz, CDCl 3 ) δ 0.90 (t, J=7.4 Hz, 6H), 1.40 (t, J=7.0 Hz, 3H), 1.52 (sextet, J=7.3 Hz, 4H), 2.38 (br.s, 1H), 2.47-2.64 (m, 4H), 2.72 (dd, J=9.1, 15.1 Hz, 1H), 2.89 (dd, J=7.8, 15.1 Hz, 1H), 3.41 (dd, J=7.7, 16.6 Hz, 1H), 4.02 (q, J=7.0 Hz, 2H), 5.07 (d, J=7.4 Hz, 1H), 6.78 (dd. J=2.4, 8.2 Hz, 1H), 6.92 (d, J=2.2 Hz, 1 H), 7.06 (d, J=8.2 Hz, 1H); [α] 25 D =34° (c=1.01, methanol).
Step 8: Preparation of (S)-5-ethoxy-2,3-dihydro-N,N-dipropyl-1H-inden-2-amine
(1S)-Trans-2-(dipropylamino)-6-ethoxy-2,3-dihydro-1H-inden-1-ol 8 is placed into a hydrogenation reactor with a catalytic amount of 5% palladium on carbon and acetic acid added as solvent. Acetic anhydride (excess over one equivalent—sufficient to completely convert all of 8 to the unisolated acetate intermediate) is also added and the mixture is hydrogenated at 40 p.s.i. while heating to 25°-80° C. (preferred temperature is 60°-70° C. When analysis indicated that 8 had been completely converted into 9 the mixture is cooled and filtered. The solvent is removed by heating under vacuum and the residue is extracted with methyl t-butyl ether and aqueous sodium hydroxide (added until the solution indicated a pH greater than 12). The aqueous layer is back extracted with more methyl t-butyl ether and the combined organic layers are washed with dilute aqueous sodium hydroxide solution. The methyl t-butyl ether solution is then extracted twice with 1 N aqueous hydrochloric acid, adding sufficient acid to wash all of the amine product into the aqueous layer). The aqueous acid layers are combined and washed with methyl t-butyl ether after which the aqueous layer is adjusted to a pH greater than 12 and then extracted with two portions of dichloromethane. The dichloromethane is washed with water and the solvent removed by heating under vacuum to afford 9. An analytical sample can be prepared as the p-toluenesulfonic acid salt from methanol/diethylether to afford crystals (m.p. 136-138° C.).
1 H NMR (free base, 300 MHz, CDCl 3 ) δ 0.88 (t, J=7.3 Hz, 6H), 1.39 (t, J=7.0 Hz, 2H), 1.49 (sextet, J=7.5 Hz, 4H), 2.46-2.51 (m, 4H), 2.75-3.01 (m, 4H), 3.64 (quintet, J=8.2 Hz, 1H), 3.99 (q, J=7.0 Hz, 2H), 6.68 (d, J=8.2 Hz, 1H), 6.73 (s, 1 H), 7.05 (d, J=8.1 Hz, 1H); [α] 25 D =11° (c=0.82, methanol).
Step 9: Preparation of (R)-5-bromo-6-ethoxy-2,3-dihydro-N,N-dipropyl-1H-inden-2-amine
Pyridinium perbromide 1-1.5 equivalents (preferably 1.3-1.4 equivalents) is added to dichloromethane solvent and cooled between −60° C. and 25° C. (−15° C. to 25° C. is the preferred temperature range). A −15° C. solution of (S)-6-ethoxy-2,3-dihydro-N,N-dipropyl-1H-inden -2 -amine (9) and trifluoroacetic acid (1-5 equivalents with 3 equivalents being preferred) dissolved in dichloromethane is added. After stirring for several hours the reaction is warmed to 0° C. When analysis indicated that all of 9 had been consumed, the reaction is quenched with a reducing agent such as aqueous sodium bisulfite. Aqueous sodium hydroxide is then added to make the pH greater than 12 and most of the dichloromethane and pyridine are removed by heating under vacuum. The residue is extracted several times with methyl t-butyl ether, the organic layers are combined, stirred with magnesium sulfate to dry, filtered, and the solvent removed by heating under vacuum to afford 10 in crude form. If necessary, this is crystallized from methanol/methyl t-butyl ether as the hydrochloride salt to afford purified 10 as its hydrochloride salt (m.p. of an analytical sample 202-204° C.).
It will be apparent to one skilled in the art that other methods of brominating 9 exist, such as direct treatment with bromine, N-bromosuccinimide, dibromohydantoin, etc. Other acid catalysts can also be utilized, such as acetic acid and other low molecular weight carboxylic acids, mineral acids, organic sulfonic acids, etc. Trifluoroacetic acid is the preferred acid catalyst.
1 H NMR (free base, 300 MHz, CDCl 3 ) δ 0.86 (t, J=7.4 Hz, 6H), 1.41-1.55 (m, 7 H), 2.43-2.49 (m, 4H), 2.76-2.99 (m, 4H), 3.57 (quintet, J=8.2 Hz, 1H), 4.05 Hz, 2H), 6.73 (s, 1H), 7.31 (s, 1H); [α] 25 D =5° (c=1.01, methanol).
Step 10: Preparation of (S)-(+)-(dipropylamino)-6-ethoxy-2,3-dihydro-1H-indene-5-carboxamide
Compound 10 (as its hydrochloride salt) is combined with dimethylformamide with a catalytic amount of palladium acetate (0.008-0.08 equiv., with 0.01-0.04 equiv. being preferred) and 1,3-bis(diphenylphosphino)propane (approximately twice the number of molar equivalents as the palladium catalyst), potassium carbonate, and hexamethyldisilylazane. The reaction is heated to 70°-120° C. (100° C. being preferred) under an atmosphere of carbon monoxide until analysis indicated that all of 10 had been consumed. The reaction is cooled, diluted with methyl t-butyl ether (MTBE) and water, and filtered to remove solids. The two-phase mixture is made basic and product is extracted into MTBE. The extracts are washed with dilute base, then water. The solution is placed under vacuum and heated to remove volatile reagents and solvents. The residue is slurried with aqueous hydrochloric acid and filtered. The filtrate is extracted with MTBE. The aqueous phase is made basic with aqueous sodium hydroxide, and the product is extracted into methyl t-butyl ether. The extracts are washed again with water and then dried by distillation. The resulting MTBE solution is treated with magnesium silicate adsorbent, which is removed by filtration. The methyl t-butyl ether filtrate is concentrated and heptane added at approximately 50° C. followed by gradual cooling to induce the crystallization of 11 which is filtered and dried. It is readily apparent to one skilled in the art that a variety of palladium catalysts (PdCl 2 , Pd n (dba) m , etc.) and associated ligands (triphenylphosphine, tri-ortho-tolulyphosphine, etc) can be utilized in varying catalytic quantities.
Additionally, 10 in its free base form can be dissolved in an etheral solvent such as tetrahydrofuran and cooled to −20° to −78° C. (preferably −25° to −50° C.) and a solution of an alkyllithium such as t-butyllithium added. Trimethylsilylisocyanate (see Parker, K. A.; Gibbons, E. G. “A Direct Synthesis of Primary Amides from Grignard Reagents”, Tetrahed. Lett 1975, 981-984) is then added and the solution is allowed to slowly warm to 10° C. and then quenched by the addition of water. Methyl t-butyl ether is added and the mixture is extracted. The organic layer is dried with magnesium sulfate and the solvent removed to afford 11 which is purified as the hydrochloride salt by treating with a methanol solution of hydrochloric acid, concentrating under vacuum, and recrystallizing the solid from ethyl acetate. The crystals are converted to the freebase by treatment with aqueous sodium hydroxide, extraction into ethyl acetate, drying with magnesium sulfate, and removal of the solvent under vacuum (m.p. 100-101° C.).
1 H NMR (CDCl 3 ) δ 7.99 (s, 1H), 7.87 (bs, 1H), 6.78 (s, 1H), 6.12 (bs, 1H), 4.17-4.11 (q, J=7.0 Hz, 2H), 3.72-3.61 (m, 1H), 3.06-2.78 (m, 4H), 2.48-2.43 (m, 4H), 1.54-1.41 (m, 7H), 0.87 (t, J=7.3 Hz, 6H; [α] 25 D =+4.94° (c=0.842, MeOH).
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The present invention relates to (2S)-enantiomers of 2-aminoindan derivatives of formula I:
and a novel process for the preparation of them.
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FIELD
[0001] The embodiments of the inventions are directed to a vanity table, and, more particularly, a vanity table that organizes items such a jewelry and/or cosmetics.
BACKGROUND
[0002] Vanity table are known and typically have a pivotal top that can be rotated to an open position to expose a storage compartment. Typically the storage compartment is used to hold cosmetic items and the interior surface of the top has a mirror disposed thereon. This allows a user to comfortably sit at the vanity table, rotate the top to its open position to expose the mirror and provide easy access to the compartment. The user can then have access to and apply her cosmetic items comfortably while simultaneously being able to view herself in the mirror.
[0003] U.S. Design Pat. No. Des. 303,593 discloses a vanity table with a storage top that has a left and right section, each of which is hingedly attached to the side of the table along one of its long edge so that each section can be rotated away from the center of the table to an open position to expose a storage compartment underneath.
[0004] U.S. Design Pat. No. Des. 303,594 discloses a vanity table having a mirror centrally disposed on a top of the table and a cabinet disposed on top of the table on each side of the mirror. It appears that a plurality of hooks are disposed on a side wall of the left cabinet.
[0005] U.S. Design Pat. No. Des. 311,832 disclose a vanity table that combines certain features of Design Pat. Nos. 303,593 and 303,594 discussed above. In particular, a vanity table is disclosed with a storage top that has a left and right section, each of which is hingedly attached to the side of the table along one of its long edges so that each section can be rotated away from the center of the table to an open position to expose a storage compartment underneath. A mirror is centrally disposed on top of the table and a cabinet disposed on top of the table on each side of the mirror.
[0006] U.S. Pat. No. 4,192,329 discloses a portable dressing table or vanity that has a centrally disposed mirror that can be rotated to an upright position when the table is being used and can be folded down flat so that it forms part of the top surface of the table. On each side of the mirror is a lid hingedly coupled along an inner long edge so that the lid can be rotated from a closed position where it forms part of the top of the table to an open position where the lid is rotated towards the center of the table to expose a storage compartment underneath.
SUMMARY
[0007] According to one aspect of the invention, there is provided a vanity having a body including a front, a back, a left side, a right side, a top extending from the back to the front and from the left side to the right side, and a bottom generally parallel with the top, the bottom extending from the back to the front and from the left side and to the right side. The top includes three sections: a left section, a middle section and a right section. The left section is pivotally coupled to the body's back adjacent to the body's left side and extends to the body's front, the right section is pivotally coupled to the body's back adjacent to the body's right side and extends to the body's front, and the middle section is locate between the left and right sections, the middle section having a fixed portion attached to the body's back and extends towards the body's front and a movable portion pivotally coupled to the fixed portion and extends to the body's front.
[0008] According to a second aspect of the invention, there is provided a vanity having a body including a front, a back, a left side, a right side, a top extending from the back to the front and from the left side to the right side, and a bottom generally parallel with the top, the bottom extending from the back to the front and from the left side and to the right side. The top includes three sections: a left section, a middle section and a right section. The left section is pivotally coupled to the body's back adjacent to the body's left side and extends to the body's front, the right section is pivotally coupled to the body's back adjacent to the body's right side and extends to the body's front, and the middle section is locate between the left and right sections.
[0009] According to a third aspect of the invention, there is provided a vanity having a body including a front, a back, a left side, a right side, a top extending from the back to the front and from the left side to the right side, and a bottom generally parallel with the top, the bottom extending from the back to the front and from the left side and to the right side. The top includes three sections: a left section, a middle section and a right section wherein the left section is pivotally coupled to the body's back adjacent to the body's left side and extends to the body's front, the right section is pivotally coupled to the body's back adjacent to the body's right side and extends to the body's front, and the middle section is locate between the left and right sections, the middle section having a fixed portion attached to the body's back and extends towards the body's front and a movable portion pivotally coupled to the fixed portion and extends to the body's front. The vanity further includes a cabinet located on the fixed portion of the middle section of the top, the cabinet extending generally parallel with the front and back of the body.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a perspective view of an embodiment of the vanity table.
[0011] FIG. 2 is a front elevation view of the vanity table shown in FIG. 1 .
[0012] FIG. 3 is a rear elevation view of the vanity table shown in FIG. 1 .
[0013] FIG. 4 is a perspective view of an embodiment of the vanity table showing its top left, right and middle sections rotated to their partially open position and left and right top drawers pulled out.
[0014] FIG. 5 is a perspective view of an embodiment of the vanity table showing its top sections rotated to their closed position, the left and right bottom drawers pulled out and the cabinet door swung open.
[0015] FIG. 6 is a top elevation view of the interior of the upper left drawer according to an embodiment of the invention.
[0016] FIG. 7 is a top elevation view of the interior of the upper right drawer according to another embodiment of the invention.
[0017] FIG. 8 is a top elevation view of the interior of the bottom left according to another embodiment of the invention.
[0018] FIG. 9 is a top elevation view of the interior of the bottom right drawer according to another embodiment of the invention.
DETAILED DESCRIPTION
[0019] FIG. 1 is a perspective view of an embodiment of the vanity table 10 . The vanity table 10 has a front 12 , a back 14 , a left side 16 , a right side 18 , a top 20 extending from the back 14 to the front 12 and from the left side 16 to the right side 18 and a bottom 22 , generally parallel with the top 20 , the bottom 22 extending from the back 14 to the front 12 and from the left side 16 and to the right side 18 . Four legs 24 extend from generally the bottom 22 of the table.
[0020] The top 20 of the table has three sections: a left section 26 , a middle section 28 and a right section 30 . The left section 26 is pivotally coupled to the body's back 14 adjacent to the body's left side 16 and extends to the body's front 12 . The right section 30 is pivotally coupled to the body's back 14 adjacent to the body's right side 18 and extends to the body's front 12 . The middle section 28 is locate between the left and right sections, 26 and 28 . In one embodiment, the middle section 28 has a fixed portion 32 attached to the body's back 14 and extends towards the body's front 12 and a movable portion 34 pivotally coupled to the fixed portion 32 and extends to the body's front 12 . In another embodiment, the middle section 28 is pivotally coupled to the body's back 14 and extends to the body's front 12 . In another embodiment, the middle section 28 is fixedly coupled to the body's back 14 and front 12 .
[0021] In the embodiments where the middle section 28 includes a fixed portion 32 and a movable portion 34 or where the middle section 28 is fixedly coupled to the body's back 14 and front 12 , a cabinet 36 can be disposed on an exterior surface of the fixed portion 32 . The cabinet 36 extends generally parallel with the front 12 and back 14 of the body. The cabinet 36 will be described in further detail hereinafter, but it can be seen that it has a door 38 with an exterior surface on which is disposed a mirror 40 .
[0022] A plurality of drawers 42 , 44 , 46 and 48 (see FIG. 2 ) are located underneath the top 20 of the body. In an embodiment, there are two drawers 42 , 46 located under the left section 26 of the top 20 , two drawers 44 , 48 located under the right section 30 of the top 20 and one drawer 49 located under the middle section 28 of the top 20 . Of course the number of drawers may be varied. In addition, instead of having legs 24 supporting the body, a series of drawers or a cabinet may be located under both the left and right sections of the top 20 that extend to the floor. Room is left under the middle section 28 to allow a user to place comfortably her legs when she is using the vanity table 10 .
[0023] FIG. 2 is a front elevation view of the vanity table 10 shown in FIG. 1 . It can be seen the located an interior surface of the left, right and middle sections 26 , 30 and 28 of the top 20 are cutouts 50 that allow a user to rotate the sections of the top 20 to their open position as will be explained in detail hereinafter. FIG. 3 is a rear elevation view of the vanity table 10 shown in FIG. 1 .
[0024] FIG. 4 is a perspective view of an embodiment of the vanity table 10 showing its top left, right and middle sections 26 , 30 and 28 rotated to their partially open position and left and right top drawers pulled out. The left section 26 of the top 20 has an interior surface on which is disposed a plurality of elastic loops 52 that can be used to secure items such as brushes, mascara or lipstick tubes or such to the interior of the left section 26 as shown. The middle section 28 has an interior surface on which is disposed a mirror 54 , as shown. The right section 30 has an interior surface that does not have anything disposed thereon although it could also have a plurality of elastic loops 52 or a mirror 54 , for example. The location of the various items on the interior surfaces of the sections may be arranged differently from that shown in FIG. 4 but still define features of the embodiments of the invention. Located underneath the left and right top sections 26 and 30 is an upper left and right drawer 42 and 44 respectively which are show partially pulled out. Each of the drawers has various dividers 56 used to form compartments within the drawer. The dividers 56 may be fixed or they may be removable so that a user can configure the storage space located within the drawer according to her desired use. Located underneath the middle section 28 is a compartment that also has dividers 56 which may or may not be removable. Located directly underneath the upper left and right drawers 42 and 44 is a lower left and right drawer as seen in FIG. 5 .
[0025] FIG. 5 is a perspective view of an embodiment of the vanity table 10 showing its top 20 sections rotated to their closed position, the left and right bottom drawers 46 and 48 pulled out and the cabinet door 38 swung open. The lower left 46 drawer has a plurality of dividers 56 used to create lipstick tube holders 58 . A sole divider 56 divides the remaining portion of the compartment of the lower left drawer 46 . Alternatively instead of a sole divider, multiple dividers may be located in the drawer. The bottom right drawer 48 also has a plurality of dividers 56 as well as it may or may not have a ring holder 51 . The ring holder 51 may be formed of a plurality of slits formed in an spongy material as is well know or plurality of rolls adjacent one another where the ring is secured between adjacent rolls.
[0026] The cabinet 36 is located on the fixed portion 32 of the middle section 28 of the top 20 and extends generally parallel with the front 12 and back 14 of the body. The cabinet 36 has a back wall 60 , a top 62 , a bottom 64 , a first side wall 66 , a second side wall 68 that define a cavity 70 and a door 38 hingedly couple to the first side wall 66 of the cabinet 36 , the door 38 having an interior surface and an exterior surface. Located inside the cabinet 36 are a plurality of hooks 72 disposed on an interior surface of the back wall 60 . The door 38 has an exterior surface on which is disposed a mirror 40 (see FIG. 1 ).
[0027] A plurality of receptacles 74 are located along the bottom of the cabinet's cavity 70 . In one embodiment, the cavity 70 and interior surface of the door 38 may be lined with antitarnish cloth. In addition, an earring stand 76 is disposed on the interior surface of the door 38 . The earring stand 76 has a plurality of vertical bars 78 attached to the interior surface of the door 38 . A plurality of crossbars 80 extend between the vertical bars 78 , as shown. The crossbars 80 can be fixedly attached or they may be removably attached to the vertical bars 78 .
[0028] The vanity table 10 allows a user to sit comfortably at the table and locate her jewelry and cosmetics in an organized fashion. The mirrors 40 and 54 provided on the exterior surface of the cabinet 36 door 38 and on the interior surface of the middle section 28 of the top allow the user to properly apply her makeup, as well as see how an article of jewelry will look on her.
[0029] FIG. 6 is a top elevation view of the interior of the upper left drawer according to an embodiment of the invention. FIG. 7 is a top elevation view of the interior of the upper right drawer according to another embodiment of the invention. A ring holder 51 may be provided in the back of the drawer and may be formed of a plurality of slits formed in an spongy material as is well know or plurality of rolls adjacent one another where the ring is secured between adjacent rolls. FIG. 8 is a top elevation view of the interior of the bottom left drawer according to another embodiment of the invention. FIG. 9 is a top elevation view of the interior of the bottom right drawer according to another embodiment of the invention. While each drawer is shown having a particular configuration, the embodiments of the invention are not limited to what is shown and various arrangements are contemplated. As previously mentioned, the dividers may be removable so that a user can configure the interior of the drawers to suit her particular needs. If the drawer is meant to hold jewelry, it may be lined with an antitarnish cloth. Alternatively, if it is meant to hold cosmetic items it made be made of a material that is easily cleaned. For example, the interior of the drawer may be lined with plastic or vinyl or an insert of plastic that holds the dividers may be provided separately so that it can be placed in the drawer.
[0030] In other embodiments, the pivotable sections of the top may have other configurations. Fir example, a particular pivotable top section, whether it be the left, right or middle section, may not extend the entire distance from the back of the body to its front. Instead, it may only extend halfway so that it extends from the front of the body to a point midway between the front and the back of the body. The remaining portion would be fixed, i.e. not movable. In another embodiment, a particular top section may be slidable so that it folds like an accordion or closet door as it is slid towards the back of the body. It will be understood by those of ordinary skill in the art that various configurations of the described embodiments are possible. Thus, as an example, the left top section may be of the pivotable lid-type while the right top section may be of the slidable-type or vice versa.
[0031] In other embodiments, the loops for holding brushes may be located on other positions of the vanity organizer. For example, they may be located in one of the drawers. As an example, the drawer underneath the middle top section may be provided with loops in its interior. Or the loops may be provided on the interior surface of the middle top section adjacent one or both side of the mirror. In addition, a panel could be added to the bottom of the vanity organizer that can be pivoted away from the bottom of the organizer towards the user. The lops may be provided on an exterior surface of such a panel so that as the panel is pivoted towards the user, the loops face the user and are accessible to the user.
[0032] While the top left, right and middle drawers have been shown as pullout-type drawers, in other embodiments, the may be fixed since access to the interior of these drawers is provided through the left, right and middle top sections.
[0033] In other embodiments, the left and right top sections are not pivotably coupled to the back of the body, but rather are coupled along one of their sides. For example, the top left section may be pivotally coupled along its right side to a center section of the top so that as it is rotated open, it rotates towards the middle top section. The top right section may be pivotally coupled along its left side to a center section of the top so that as it is rotated open it rotates towards the top middle section. The exterior surfaces of such left and right top sections may be provided with mirror so that when they are rotated open, and the middle section is rotated open, they present a three-way or tri-fold type mirror to the user. The top left and right sections may be adjustable when in their rotated open position so that the user can adjust the angle of the mirror located on the exterior surface of the sections.
[0034] In addition, in some embodiments, the middle top section may have coupled on its interior surface a left and right panel that each fold inward underneath the interior surface of the top middle section so that the middle section can be rotated to its closed position. When the middle section is rotated to its open or partially open position, the left and right panels may be rotated away from the interior surface of the middle section and each panel may be provided with a mirror to provide a three-way or tri-fold mirror to the user. The angle of the left and right panels may be adjusted by the user.
[0035] The cabinet 36 located on top of the organizer may in one embodiment, be removable. In other embodiments, the cabinet 36 may be rotatably coupled to the vanity organizer so that it can be rotated preferably 360 degrees, for example. In addition, the cabinet 36 located on top of the organizer may be of the swivel type with multiple compartments such as described in the following applications: U.S. Ser. No. 11/368,019 entitled “Swivel Organizer” filed Mar. 3, 2006; U.S. Ser. No. 29/263,540 entitled “Swivel Organizer” filed Jul. 25, 2006; U.S. Ser. No. 29/277,341 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/277,342 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/277,343 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/277,344 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/277,345 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/277,346 entitled “Swivel Organizer” filed Feb. 22, 2007; U.S. Ser. No. 29/281,878 entitled “Swivel Organizer” filed Jul. 5, 2007; U.S. Ser. No. 29/281,880 entitled “Swivel Organizer” filed Jul. 5, 2007; U.S. Ser. No. 29/295,087 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,095 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,097 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,098 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,101 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,104 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,106 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,110 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,113 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,115 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,118 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,119 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,121 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,123 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,124 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,128 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,134 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,136 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,139 entitled “Swivel Organizer” filed Sep. 21, 2007; U.S. Ser. No. 29/295,141 entitled “Swivel Organizer” filed Sep. 21, 2007 all of which are hereby incorporated herein by reference in their entirety.
[0036] In addition, the cabinet 36 , whether it is rotatable or not may include a tri-fold mirror arrangement as described in U.S. Ser. No. 11/610,170 entitled “Tri-Fold Mirror Swivel Organizer” filed Dec. 13, 2006 and U.S. Ser. No. 11/768,979 entitled “Tri-Fold Mirror Organizer” filed Jun. 27, 2007 all of which are hereby incorporated herein by reference in their entirety.
[0037] The hinges used to couple the top left and right sections preferably have a stop so that those top sections can be rotated about 110 degrees. The top middle section uses hinges that allow a user to adjust the tilt of the middle section by using adjustable hinges.
[0038] The vanity organizer has been described in various embodiments as hold jewelry items and cosmetic items. Alternatively, the vanity organizer may house all jewelry items or all cosmetic items depending on the needs of the user.
[0039] The embodiments of the invention are subject to many variations and modifications while remaining within the scope of the embodiments of the invention.
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A vanity table organizer that includes multiple compartments for storing jewelry, cosmetic and/or both items in a user friendly and efficient, manner.
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This application is a continuation-in-part of Ser. No. 08/185,562 filed Jan. 24, 1994, now U.S. Pat. No. 5,436,467.
This invention relates to thermoelectric devices and in particular to materials for such devices.
BACKGROUND OF THE INVENTION
Thermoelectric devices for cooling and heating and the generation of electricity have been known for many years; however, their use has not been cost competitive except for limited applications because of the lack of thermoelectric materials having the needed thermoelectric properties.
A good thermoelectric material is measured by its "figure of merit" or Z, defined as
Z=S.sup.2 /ρK
where S is the Seebeck coefficient, ρ is the electrical resistivity, and K is the thermal conductivity. The Seebeck coefficient is further defined as the ratio of the open-circuit voltage to the temperature difference between the hot and cold junctions of a circuit exhibiting the Seebeck effect, or
S=V/(T.sub.h -T.sub.c).
Therefore, in searching for a good thermoelectric material, we look for materials with large values of S, and low values of ρ and K.
Thermoelectric materials currently in use today include the materials listed below with their figures of merit shown:
______________________________________ThermoelectricMaterial Peak Zeta, Z (at temperature shown) ZT______________________________________Lead telluride 0.9 × 10.sup.-3 /°K. at 500° K. 0.9Bismuth telluride 3.2 × 10.sup.-3 /°K. at 300° K. 1.0Silicon germanium 0.8 × 10.sup.-3 /°K. at 1100° K. 0.9______________________________________
Workers in the thermoelectric field have been attempting to improve the figure of merit for the past 20-30 years with not much success. Most of the effort has been directed to reducing the lattice thermal conductivity (K) without adversely affecting the electrical conductivity.
Experiments with superlattice quantum well materials have been underway for several years. These materials were discussed in an paper by Gottfried H. Dohler which was published in the November 1983 issue of Scientific American. This article presents an excellent discussion of the theory of enhanced electric conduction in superlattices. These superlattices contain alternating conducting and barrier layers. These superlattice quantum well materials are crystals grown by depositing semiconductors in layers whose thicknesses is in the range of a few to up to about 100 angstroms. Thus, the layers can be as thin as only a few atoms thick. There has been speculation that these materials might be useful as thermoelectric materials. (See articles by Hicks, et al and Harman published in the Proceedings of 1992 1st National Thermoelectric Cooler Conference Center for Night Vision & Electro Optics, U.S. Army, Fort Belvoir, Va. FIG. 1 has been extracted from the Hicks paper and is included herein as prior art. It projects theoretically very high ZT values as the layers are made progressively thinner.) The idea being that these materials might provide very great increases in electric conductivity without adversely affecting the Seebeck coefficient or the thermal conductivity. Harmon of Lincoln Labs, operated by MIT has claimed that he is close to producing a superlattice of layers of (Bi,Sb) and Pb(Te,Se), but to the best of Applicants' knowledge, he has not been successful in producing quantum wells. He claims that his preliminary measurements suggests ZTs of 3 to 4 are possibly feasible. Most of the thermoelectric efforts to date with superlattices have involved alloys such as BeTe which are known to be good thermoelectric materials for cooling, many of which are difficult to manufacture as superlattices because the stoichiometry of the alloys have to be very carefully controlled which is very difficult in vapor deposition techniques. Bulk SiGe is not a good thermoelectric material at low temperatures. Superlattices tend to diffuse at high temperatures and lose their superlattice qualities.
Researchers investigating opto-electronic properties of multilayer quantum well structures have considered the effects of strain in the layers. These researchers (e.g., Abstrater, et al., Phy. Lett. S4, 2441 (1985)) report increased electron mobility due to the strain effect.
What is needed are thermoelectric materials with improved ZT values which permit a simplified manufacturing process.
SUMMARY OF THE INVENTION
The present invention provides thermoelectric elements having a very large number of alternating layers of semiconductor material, the alternating layers all having the same crystalline structure. This makes the vapor deposition process easy because the exact ratio of the materials in the layers is not critical. The inventors have demonstrated that materials produced in accordance with this invention provide figures of merit more than six times that of prior art thermoelectric materials. A preferred embodiment is a superlattice of Si, as a barrier material, and SiGe, as a conducting material, both of which have the same cubic structure. Another preferred embodiment is a superlattice of B--C alloys, the layers of which would be different stoichiometric forms of B--C but in all cases the crystalline structure would be alpha rhombohedral. In a preferred embodiment the layers are grown under conditions as to cause them to be strained at their operating temperature range in order to improve the thermoelectric properties.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing the theoretical thermoelectric properties of superlattice materials.
FIG. 2 is simple drawing showing an apparatus for making superlattice materials.
FIG. 3 shows a thermoelectric eggcrate arrangement.
FIG. 4 shows how the thermoelectric elements are cut from the substrate on which grown.
FIG. 5 shows a portion of a thermoelectric device to show current flow through the elements.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The present inventors have demonstrated a revolutionary thermoelectric material, with ZT values in excess of 6. This material is comprised of very thin layers of silicon and a solid solution of silicon and germanium. These very thin layers may be forming quantum wells which are know to greatly increase electron mobility which in turn increase electrical conductivity. The principal advantage of the inventors' material over many others that have been suggested is that Si and Ge both have the same crystalline structure so that when the layers Si and SiGe (solid solution) are grown the atoms fit together to form the well ordered lattices.
Making the n-Type Superlattice
Si.sub..8 Ge.sub..2 /Si layers were grown on (100) Si substrates by codeposition from two electron beam evaporation sources in a molecular beam epitaxy. The fluxes from the Si and Ge electron beam sources were separated, sensed and controlled to yield a total deposition rate of 5 A/sec. Prior to deposition, substrates were chemically cleaned, then argon sputtered in situ and annealed at 800°-850° C. Above 500° C., annealing and growth temperatures were measured directly by infrared pyrometry. Then the layers could be alternatively deposited on top of each other to make Si.sub..8 Ge.sub..2 /Si superlattices with each layer being about 50 A thick.
The actual deposition configuration is illustrated schematically in FIG. 1. Five substrates 2 are mounted on the bottom of platen 4 which rotates at a rate of 1 revolution per second. The platen is 50 cm in diameter and the substrate wafers are each 125 mm in diameter. Two deposition sources 6 and 8 are mounted on a source flange 7 such that their deposition charges are about 20 cm from the axis 5. Deposition source 6 is pure silicon and deposition source 8 is germanium doped to ˜10 16 carriers per cc. The rotating platen is positioned 23 cm above the sources. An Airco Temescal electron beam is used for evaporation. We use one 150 cc source of pure silicon and a 40 cc source of germanium. We alternate the beams so layers of silicon only and silicon and germanium are deposited. Dopants may be mixed with the germanium.
The apparatus is computer controlled to evaporate the sources alternatively at intervals appropriate to achieve the desired thicknesses while the platen rotates above. Layer thicknesses are monitored by two electroluminescent deposition meters 9 at the side of platen 4. Layers will continue to build on the substrates until we have a wafer with about 250,000 layers and a thickness of about 0.254 cm. which is the thickness needed for a preferred thermoelectric device. The wafer is then diced into chips as indicated in FIG. 2.
Making the p-Type Superlattice
We make the p-type material exactly as discussed above except we use a p-type dopants for the SiGe layers. These layers are boron doped for p-type material and antimony doped for n-type material.
Other Techniques for Making n-Type and p-Type Material
Molecular beam epitaxy equipment for making the n-type and p-type layered material is commercially available from several suppliers such as Instruments SA Inc., Riber Div. with offices in Edison, N.J. The material can also be prepared using sputtering techniques. Sputtering equipment adequate for making these materials is also commercial available from suppliers such as Kurt J. Lesker Co. with offices in Clairton, Pa.
Sputtering is done in a manner similar to the techniques used for the fabrication of X-ray optics. Vacuum is established and maintained by a two-stage mechanical roughing pump and a high-capacity cryogenic pump. The system usually achieves base pressures of approximately 10 -9 torr after bake-out and before sputtering. Substrates are mounted on a rotating carousel driven by a precision stepper motor.
Substrates can be heated or cooled by the carousel during sputtering. Heating of the substrate during deposition and subsequent annealing is used as a means of controlling the structure and orientation of individual crystalline layers, as well as means of reducing the number of defects in the films. (We can also control the temperature in order to enhance strain within the layers as a function of temperature as discussed later.) One of the essential conditions for epitaxial film growth is a high mobility of condensed atoms and molecules on the surface of the substrate. Two 1 kW magnetrons, each having a 2-5-inch diameter target and a 1 kW power supply, are used to deposit films. The sputter sources are operated at an argon pressure between 0.001 and 0.1 torr. Argon is admitted to the system by a precision flow controller. All functions of the system, including movement of the carousel, rates of heating and cooling, magnetron power, and argon pressure, are computer controlled.
Making the Thermoelectric Element
The p-type and the n-type chips are formed into an egg crate configuration in a manner standard in the industry. Metal contacts are applied then all n and p legs are electrically shorted. The n and p couples are electrically isolated by lapping the surface until the insulating egg crate is visible and a series circuit of n and p elements is produced. In FIG. 3 elements shown are n-type thermoelectric elements 10, p-type thermoelectric elements 12, aluminum electrical connectors 14, eggcrate electrical barrier 16 and molybdenum diffusion barrier 18. FIG. 4 shows how the chips are cut from the silicon substrate. FIG. 5 is another view showing how the n elements 10 and p elements 12 are connected to produce electric power from hot and cold sources. Arrows 30 show current flow. Insulators are shown as 22 and electrical conductors are shown as 14.
Test Results
Materials produced in accordance with the teachings of this invention have been tested by the inventors. The tested thermoelectric properties of both n-type and p-type samples of Si.sub..8 Ge.sub..2 /Si are compared in Table I with the properties of bulk material with the same ratios of Si and Ge:
TABLE I__________________________________________________________________________ Electrical Seebeck Carrier Power Figure of Resistivity Coef. Conc. Factor Merit Z(Abs Temp)Sample ρ α n α2/ρ Z (T = 300° K.)Si.sub..8 Ge.sub..2 /Si (mΩ-cm) (μV/oC) (1/cm) ((/1000) (1/K) ZT__________________________________________________________________________Sample 1 N 0.52 -260 10.sup.16 120 1.6 × 10.sup.-3 0.5Sample 2 N 4 -1250 10.sup.19 391 5.1 × 10.sup.-3 1.5Sample 3 P 1.44 +850 10.sup.15 293 3.8 × 10.sup.-3 1.2Sample 4 P 1.94 +850 10.sup.19 218 2.9 × 10.sup.-3 0.9Sample 5 P 1.74 +850 10.sup.20 243 3.2 × 10.sup.-3 1.0Sample 6 P 1.4 +850 5 × 10.sup.20 302 4.0 × 10.sup.-3 1.2Bulk Si.sub..8 Ge.sub..2 P 1 +130 10.sup.20 17 .3 × 10.sup.-3 0.1Bulk Si.sub..8 Ge.sub..2 N 2 -200 10.sup.20 20 .33 × 10.sup.-3 0.1__________________________________________________________________________
The data reported in Table 1 was obtained with thin samples of about 10 alternating layers deposited on a silicon substrate. All measured values were corrected for the effect of the silicon substrate for a total thickness of about 1,000 A. These Z values in the range of 1.6×10 -3 /K to 5.1×10 -3 /K are amazingly high, approximately an order of magnitude higher than Si.8 Ge.2. These results are also amazing in view of a prediction in 1991 that the maximum possible Z for SiGe was about 1.7×10 -3 for p-type elements and about 1.9×10 -3 /K for n-type elements. (See Slack and Hussain, "The maximum possible conversion efficiency of silicon-germanium thermoelectric generators", J. Appl. Phys. 70 (5), 1 Sep. 1991.)
Strain Effect
Applicant's have concluded that strain in the layers can have a very beneficial effect on the thermoelectric properties of the multi-layer elements. In-plane stresses cause tensile strains in the Si layers and compressive strains in the SiGe layers, with opposite strains in the direction normal to the layer plane. The strain induce splittings and shifts of the conduction-band minima. This helps assure that the conduction band of the wider-gap material, Si, is lower in energy than that of the conduction band material, SiGe. The net effect is that the electron mobility in the multi-layer element is enhanced. These types of strain would have a temperature dependency of T 3 . Because of the positive contribution of strain to electron mobility, we prefer to tailor our fabrication process to assure that at the planned operating temperature of the elements the layers are under strain as indicated above. One method of assuring that this is the case is to fabricate the multi-layer elements at a temperature at least 200 C. above the planned operating temperature. Other methods for creating this strain will be apparent to persons skilled at molecular beam epitaxy and sputtering techniques.
Similar High Temperature Lattices
The Si/SiGe superlattice is not stable at very high temperatures for very long periods (i.e., above about 500° C.); therefore, there is a need for a similar superlattice which can be operated at these high temperatures. Boron and Boron-Carbon alloys are also expected to perform as excellent p-type thin-layer (possibly quantum well) materials. The same alpha rhombohedral crystal structure exists over a wide range of composition from B 4 C to B 11 C. As the B content is increased in going from B 4 C to B 11 C the B atoms substitute for C atoms. As a result of this progressive change in composition without a change in structure it should be possible to grow epitaxial layers of various B--C compositions on one another. From data generated on bulk B--C alloys one should be able to fabricate a device by using compositions close to B 11 C as the insulating layer and compositions close to B 4 C as the more conducting layer. Also pure alpha boron which is rhombohedral could be used as the insulating layer. The B--C alloys are of further interest because these alloys exhibit extremely low diffusion rates at temperatures at which they would be used as thermoelectric materials. For example, the B--C alloys of interest melt at temperatures in excess of 2400° C. yet they will only be operated up to about 1100° C. By using materials such as B--C alloys the thin layers will remain intact at elevated temperatures and not be subject to degradation by adjacent layers diffusing together with time. This annihilation of the two adjacent layers via diffusion is of serious concern with the lower melting alloys such as Si/SiGe, PbTe based alloys, and (Bi,Sb) 2 (Se,Te) 3 based alloys and limits their usefulness in high temperature applications.
While the above description contains many specificities, the reader should not construe these as limitations on the scope of the invention, but merely as exemplifications of preferred embodiments thereof. For example, the SiGe ratio could be any composition between about 5 percent Ge to about 95 percent Ge; however, the preferred composition is between about 10 percent Ge and about 40 percent Ge. Those skilled in the art will envision many other possible variations are within its scope. Persons skilled in the thermoelectric art are aware of many different dopants other than the ones discussed above which would produce similar effects. Examples of n-type dopants include phosphorus and arsenic. Examples of p-type dopants in addition to boron are aluminum and antimony. Persons skilled in the art will recognize that is is possible to produce quantum layers having the same crystalline structures from materials having different crystal structures. For example, epitaxial layers of GeTe and PbTe could be fabricated even though PbTe and GeTe differ slightly in crystalline structure. Accordingly the reader is requested to determine the scope of the invention by the appended claims and their legal equivalents, and not by the examples which have been given.
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A thermoelectric element having a very large number of alternating layers of semiconductor material. The alternating layers all have the same crystalline structure. The inventors have demonstrated that materials produced in accordance with this invention provide figures of merit more than six times that of prior art thermoelectric materials. A preferred embodiment is a superlattice of Si, as a barrier material, and SiGe, as a conducting material, both of which have the same cubic structure. Another preferred embodiment is a superlattice of B--C alloys, the layers of which would be different stoichiometric forms of B--C but in all cases the crystalline structure would be alpha 0. In a preferred embodiment the layers are grown under conditions as to cause them to be strained at their operating temperature range in order to improve the thermoelectric properties.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of copending International Application No. PCT/AT01/00260, filed Aug. 1, 2001, which designated the United States and was not published in English.
BACKGROUND OF THE INVENTION
Field of the Invention
[0002] the invention relates to a flocculant or binder composition, a slurry containing the flocculant or binder composition, a method for making ceramics using the slurry, and ceramic products made therefrom.
[0003] When producing ceramics products, inorganic base materials that are mostly inorganic fiber materials are introduced into an aqueous sludge referred to as a slurry. The addition of flocculants and/or binders, and optionally other components, will cause the formation of flocks. After the separation of the formed flocks, the moist cake is at first dried and then baked into ceramics using different thermal processes.
[0004] In order to prepare suitable slurries, a great number of additives are required, including flocculants and/or binders, by which the inorganic materials contained in the slurry are brought into a form/distribution that is suitable for the final heat treatment.
[0005] Due to the increasing concern for environmental protection of the last decade, there has been great interest in using, for the manufacture of ceramics, flocculants and/or binders that do not produce environmentally relevant noxious matter during the final heat treatment, which is also called carbonization if inorganic substances are used. Aromatic compounds such as, for instance, phenolic resins were frequently used in former times, as in German published, non-prosecuted patent application DE 32 31 100 A1, for the production of shaped articles of silicon carbide. Starch-containing products have recently been successfully employed for that purpose.
[0006] Therefore, flocculants and binders based on starch have been widely applied on the ceramics sector. This is of special importance, because flocculants and binders based on starch are of natural origin and hence more environment-friendly. Thus, no hazardous substances that might have impacts on the environment are released during carbonization.
[0007] Thus, the use of potato, corn and wheat starch derivatives is described in U.S. Pat. No. 5,618,767, which indicates the merits of starch during carbonization. In particular, this patent describes the use of the above-mentioned starches in the manufacture of ceramics products based on silicon carbide.
[0008] U.S. Pat. No. 3,224,927 deals extensively with the potentialities of cationic starches in the manufacture of heat-resistant products. This patent emphasizes the advantages of those starch products and their optimal integration into a system of fibers and the binder silica sol. The starches described include commercially available cationic starches from National Starch, which have to be initially gelatinized during flocculation.
[0009] International PCT publication WO 99/15322 describes the vacuum-forming process technique for the production of ceramic shaped bodies. In that process, flocculants are preferably added, with cold-water soluble cationic starches being above all applied. Commercially available products based on cornstarch or conventional potato starch are emphasized.
[0010] European Patent Application EP-094 731 A teaches the production of shaped ceramics. This application also teaches binders made from starch and, in particular, corn starch and also rice starch, tapioca starch, and conventional potato starch.
[0011] In the prior art described, starch products are, thus, used as flocculants or binders in native, degraded, modified, and derivatized forms.
[0012] Starch is a natural plant product. It essentially includes a glucose polymer that, as a rule, is a composition of two components, namely amylopectin and amylose. These are, in turn, not uniform substances, but mixtures of polymers having different molecular weights. Amylose essentially includes unbranched polysaccharides in which glucose is present in an alpha-1,4-bond. Amylopectin, on the other hand, is a strongly branched glucose polymer in which the glucose moieties on the branching points are contained in 1,6-bonds in addition to alpha-1,4-bonds.
[0013] Natural starches, as a rule, have amylose contents ranging from 15 to 30%; only corn varieties of the waxy type yield starches that are formed almost exclusively of amylopectin. The field of application of this starch, which is called waxy corn starch, primarily pertains to the food industry. There, it is particularly appreciated that amylose-free starch tends to threading during gelatinization to a largely less extent, thus giving a more pleasant mouthfeel. In addition, amylopectin starch exhibits fewer retrogradation phenomena, i.e. tends less strongly to reunifying already separated chains, than starch rich in amylose.
[0014] The cultivation of waxy corn is hardly practical or possible from an economical point of view in cold or tempered climes that are found in Austria, Germany, Belgium, the Netherlands, Great Britain, Poland, etc. Therefore, waxy corn could not find acceptance in those areas for cost reasons. By contrast, potatoes are common starch sources in those countries. Compared to cereal starch, potato starch has a lower content of lipids and proteins and contains considerable amounts of phosphate ester groups. A comparative representation in this respect, which takes into account the amylopectin potato starch presently claimed, is set out in the experimental part of the description of the present invention.
[0015] Methods for reducing the amylose content of starch by physical or chemical methods are known. Yet, these involve considerable expenditures and are feasible only when justified from an economical point of view.
[0016] These methods for reducing amylose contents, however, require treatments at elevated temperatures (usually above approximately 140° C.), which will inevitably result in the formation of degradation products. Yet, such degradation products may have adverse effects with many applications. Moreover, the fractionation process is very complex and cost-intensive; this has so far prevented such products from being successful in large-scale applications. In the context of the present invention, amylopectin potato starches prepared by fractionation are referred to as fractionated amylopectin potato starches (FAP-PSs).
[0017] Due to the successful genetic modification of potatoes achieved during the last decade, which was aimed at providing a starch free of amylose, completely new types of starch could be made accessible (See international PCT publication WO 92/11376 A). As a result, it became, for instance, feasible for the first time to obtain an amylose-poor or amylose-free potato starch in which the three-dimensional amylopectin structure typical of potato starch is completely retained without involving the formation of degradation products or deviations of the three-dimensional network from the native structure (cf. international PCT publication WO 92/11376). In this manner, an amylopectin potato starch is provided, which is not only substantially more defined, but also particularly well apt for derivatization processes (cf. again international PCT publication WO 92/11376 A).
[0018] Although a plurality of applications have been proposed for these novel starch products, only little is known about the actual technical exploitability of these starch products on account of the small amounts available so far. Thus, waxy cornstarch is still the only starch product rich in amylopectin that has so far been used on an industrial scale in the prior art. Waxy cornstarch has already gained ground on the market because of its ready availability as compared to FAP-PS or other waxy cereal starches that can be obtained from mutants of common cultigens.
[0019] The above-mentioned amylopectin-rich starches with native amylopectin patterns (cf. international PCT publication WO 92/11376) have already been proposed for some applications as pointed out above, yet not for the manufacture of ceramics products. These starches are produced by selectively manipulating the amylose-forming enzymes contained in the potato and are referred to as amylopectin potato starches (AP-PS) for the purposes of the present invention.
SUMMARY OF THE INVENTION
[0020] It is accordingly an object of the invention to provide a flocculant or binder composition, a slurry containing the flocculant or binder composition, a method for making ceramics using the slurry, and ceramic products made therefrom that overcome the hereinafore-mentioned disadvantages of the heretofore-known devices of this general type by providing a flocculant or binder composition that includes amylopectin potato starch (AP-PS).
[0021] In the production of ceramics products, amylopectin potato starch surprisingly exhibited properties substantially superior to those of products proposed so far for this purpose and, in particular, in comparison with other starch products. In the context of the present invention, it was, in fact, possible to achieve a decisive improvement particularly over fractionated amylopectin potato starch (FAP-PS) as well as over waxy corn starch and, of course, also over conventional potato starch as well as over products derived from these starch derivatives.
[0022] Amylopectin-rich starch has so far been proposed only for applications in fields where its properties have come to light at room temperature or at slightly elevated temperatures such as, for instance, in the textile and paper industries (cf., e.g., U.S. Pat. No. 5,582,670). However, in the ceramics sector, the use of AP-PS in the course of production processes has neither been proposed nor encouraged. Accordingly, the completely surprising positive properties of AP-PS as against related products and, in particular, other starches rich in amylopectin such as FAP-PS or waxy corn starch, also have not yet been revealed.
[0023] By the term “ceramics”, products made of clay minerals are understood both in everyday usage and according to the invention. The diversity of ceramic materials, as well as their applications, have largely increased during the past decades such that, in addition to clay minerals, also carbides, nitrides, oxides, or silicides are used today amongst others. Concurrently with this development, refractory ceramics became established on the market. According to DIN 51060, the term refractory materials serves to denote nonmetallic materials like high-melting oxides, refractory silicates, etc. (yet including those containing defined metal portions like, for instance, cermets), which have Seger cone falling points of at last 1500° C. These products stand out for being usable at temperatures exceeding 800° C. over extended periods of time.
[0024] According to the ISO recommendation R 1109, they are classified as follows:
[0025] 1. Products rich in alumina group 1: >56% Al 2 O 3
[0026] 2. Products rich in alumina group 2: 45-56% Al 2 O 3
[0027] 3. Fireclay refractories: 30-45% Al 2 O 3
[0028] 4. Acidic fireclay refractories: 10-30% Al 2 O 3 , <85% SiO 2
[0029] 5. Siliceous refractories: 85-93% SiO 2
[0030] 6. Silica products: >93% SiO 2
[0031] 7. Basic refractories: with variable amounts of magnesite-chromite
[0032] 8. Special products based on carbon, graphite, Zi-silicate, nitrides, borides, cermets
[0033] Ceramics products offer a large and wide field of application. Typical examples include their use in the car industry, in industrial blast furnaces for refractory materials, or high-temperature filters.
[0034] Ceramics products are above all characterized by their porosity. The porosity is achieved especially by using starch-containing flocculants or binders.
[0035] Although, in principle, starch has been used as a flocculant in other fields (for instance in paper production), the ceramics industry makes very special demands on a flocculant. On the one hand, the demands are attributed to the preparation of slurries of inorganic materials. On the other hand, the demands are explained by the drying/forming and firing processes following subsequently.
[0036] “Flocculant” is meant to include those substances that influence the zeta potential (electrokinetic potential) of colloidal particles to cause the formation of aggregates, such as, for instance, flocks. The zeta potential of dispersed particles is reduced or neutralized by flocculants. In order to enable flocculation at all, the flocculant must overcome the electrostatic repulsion of the particles that are mostly negatively charged in the solvent, primarily water.
[0037] Starches or starch derivatives cause solids particles to agglomerate to large units (flocks). Bridging causes the agglomeration to suspended particles. According to accepted teachings, the effectiveness of a flocculant is a function of the ionic character, on the one hand, and of the molecular chain length, on the other hand. It has not yet been recognized that the nativity of the amylopectin structure might play an important role in this respect. Moreover, starch may also have a binding function in the field of ceramics products. It may, for instance, constitute an important binding link between fibers and other auxiliary substances or binders like silica sol. On account of its organic nature, starch is a temporary binder that is converted into carbon by heat treatment, thus forming a stable three-dimensional network structure (porous matrix) with the silicon present.
[0038] It has been shown by the invention that it is exactly AP-PS that imparts special properties on the produced ceramics product by that conversion. Then there are the properties that are enhanced during the preparation process of the slurry.
[0039] AP-PS is preferably obtained from potatoes in which the starch granule-bound starch synthase I (GBSS I), which is responsible for the -1,4-glycosidic bond to the linear amylose molecule, is limited in its activity or totally inactivated, for instance by a suitable antisense technology as described in international PCT publication WO 92/11376. The inhibition of GBSS I, for instance, allows for the production from potatoes, of native AP-PS with an amylopectin content that is largely increased as compared to that of natural potato starch, without having to put up with the disadvantage of fractionated amylopectin potato starch (degradation products; thermal treatment).
[0040] Therefore, AP-PS having a content of at least 95%, preferably at least 98%, of amylopectin, based on the overall starch quantity, is used in a preferred manner.
[0041] Preferably, AP-PS is obtained from a potato modified by breeding or by molecular-biological or genetic-engineering techniques for the purpose of amylose inhibition. Above all, the AP-PS to be used according to the invention is obtained from a potato inhibited by the antisense inhibition of a GBSS gene or by co-suppression in respect to amylose formation. In doing so, the synthesis of amylose is preferably impeded or inhibited, with the amylopectin branching being preferably left unchanged. After all, this is readily feasible from a technical point of view, since the synthesis of amylose and the formation of amylopectin branching patterns are two completely independent processes occurring in the plant. The participating enzymes are specific for both processes and can each be influenced in their activities in a mutually independent and specific manner, for instance by genetic-engineering interventions. Thus, AP-PS can be obtained as a known starch (potato starch) with a modified amylose/amylopectin ratio at an otherwise completely unchanged quality (regarding its branching degree). As opposed to the preparation of FAP-PS, the starch quality in recombinantly produced AP-PS is unambiguously definable and hence accessible to a precise success control, whereby the industrial availability of AP-PS is safeguarded.
[0042] Starches obtained from genetically manipulated potatoes in which the branching degree of amylopectin has been modified (optionally at an equally high portion of amylose; see international PCT publication WO 96/19581) turned out to be disadvantageous in the context of the present invention and, therefore, are not to be considered as AP-PSs in the sense of the present invention—because of their high amylose contents alone.
[0043] Other important characteristics of amylopectin potato starch are its molar mass distribution and its mean molecular weight.
[0044] The differences from waxy starches such as, for instance, waxy corn starch, or a potato starch amylopectin prepared by physical or chemical methods, become particularly apparent by size exclusion chromatography (SEC) measurements. The respective data are set out in the experimental part.
[0045] AP-PS in the flocculant or binder composition according to the invention is preferably modified and, in particular, cationically modified. In this context, amylopectin potato starches including nitrogen-containing groups and, in particular, electropositively charged quaternary ammonium groups, have proved particularly beneficial.
[0046] According to a particularly preferred embodiment, the amylopectin potato starch according to the invention is an amylopectin potato starch sulfamate.
[0047] Depending on the nature of the organic fibers used, both an anionically charged amylopectin potato starch and a cationically charged amylopectin potato starch may, however, be required. In special cases, also an amphoteric amylopectin potato starch may constitute a preferred variant.
[0048] From the literature, a plurality of derivates is known, the preparation of which is readily apparent, inter alia, from “Starch: Chemistry and Technology”, R. L. Whistler, Chapters X and XVII, 1984, and from “Modified Starches: Properties and Uses”, edited by O. B. Wurzburg, Chapters 2-6 and 9-11, CRC Press, 1986. In general, distinction is made among anionic, cationic, and amphoteric starch derivates, the following derivatization options for other starch types belonging to the prior art.
[0049] Under anionic modification of amylopectin potato starch, those derivatives are summarized where the free hydroxyl groups of the starch are substituted by anionic groups. Unlike waxy cornstarch, amylopectin potato starch includes naturally bound anionic groups such that, in the true sense, one has to speak of an additional anioinic modification. These are naturally chemically bound phosphate groups that impart an additional specific polyelectrolytic property on the amylopectin potato starch.
[0050] Basically, there are two ways of carrying out anionic derivatization:
[0051] a) Modification is effected in a manner so as to induce the esterification of amylopectin potato starch. Modification agents include inorganic or organic heterovalent, mostly bivalent, acids or salts thereof or esters or anhydrides thereof. Thus, the following acids are suitable amongst others, their enumeration being only exemplary: o-phosphoric acid, m-phosphoric acid, poly-phosphoric acid, various sulfuric acids, various silicic acids, various boric acids, oxalic acid, succinic acid, glutaric acid, adipic acid, phthalic acid, citric acid, etc. Mixed esters or anhydrides may be used as well. When esterifying amylopectin potato starch, this may also be effected several times so as to produce, for instance, distarch phosphoric esters.
[0052] b) Modification is effected in a manner so as to induce the etherification of amylopectin potato starch. Modification agents include inorganic or organic—substituted acids or salts thereof or esters thereof. This type of reaction results in the cleavage of the—substituent while forming an ether group.
[0053] Consequently, the amylopectin potato starch is additionally substituted, for instance, by phosphate, sulfate, sulfonate, or carboxyl groups. This is accomplished, for instance, by the reaction of amylopectin potato starch with—halocarbonic acid, chlorohydroxy alkyl sulfonates, or chlorohydroxy alkyl phosphonates.
[0054] Under cationic modification of amylopectin potato starch, those derivates are summarized where a positive charge is introduced into the starch by substitution. Cationization methods are carried out by the aid of amino, imino, ammonium, sulfonium, or phosphonium groups. Methods for preparing cationized starches are, for instance, described in D. B. Solareck: Cationic Starches, in the book by O. B. Wurzburg (Ed.): Modified Starches: Properties and Uses, CRC Press Inc., Boca Raton, Fla. (1986), pp 113-130. Such cationic derivatives preferably contain nitrogen-containing groups, in particular primary, secondary, tertiary, and quaternary amines, or sulfonium and phosphonium compounds, respectively, which are bound via ether or ester bonds. The use of cationized amylopectin potato starches containing electropositively charged quaternary ammonium groups is preferred.
[0055] In detail, also the sulfamates of amylopectin potato starch are to be mentioned herein, their production likewise falling within the scope of the present invention. This new amylopectin potato starch derivative is obtained by reaction of the presently claimed amylopectin potato starch with ammonium, earth alkali, or alkali sulfamates. An exemplary description of the preparation of this derivative will also be found in the experimental part.
[0056] Another group is represented by amphoteric starches. They contain both anionic and cationic groups, their applications thus being highly specific. These are usually cationic starches that are additionally modified either by phosphate groups or by xanthates. The preparation of such products is also described by D. B. Solareck: Cationic Starches, in the book by O. B. Wurzburg (Ed.): Modified Starches: Properties and Uses, CRC Press Inc., Boca Raton, Fla. (1986), pp 113-130.
[0057] Esters and ethers of amylopectin potato starch are of great importance. Distinction is made between simple starch esters and mixed starch esters, with different ester substituent(s) being conceivable: in the ester residue RCOO—, the residue R may be an alkyl, aryl, alkenyl, alkaryl, or aralkyl residue having 1 to 17 carbon atoms, preferably 1 to 6 carbon atoms and, in particular, 1 or 2 carbon atoms. These products include the following derivatives: acetates (prepared from vinyl acetate or acetic anhydride), propionates, butyrates, stearates, phthalates, succinates, oleates, maleinates, fumarates, and benzoates.
[0058] Etherifications are mainly realized by reactions with alkylene oxides containing 2 to 6 carbon atoms, preferably 2 to 4 carbon atoms and, in particular, by using ethylene and propylene oxides. Yet, also methyl, carboxymethyl, cyanoethyl, and carbamoyl ethers may be prepared and used. Further products include alkyl hydroxyalkyl, alkyl carboxyalkyl, hydroxyalkyl carboxymethyl, and alkyl hydroxy alkyl carboxymethyl derivatives.
[0059] Besides said esters and ethers, amylopectin potato starch can also be crosslinked to different extents. Crosslinking is preferably effected by reaction with a crosslinker such as epichlorohydrin or 1,3-dichloro-2-propanol, optionally mixed with (poly)amines, furthermore with phosphoroxychloride, sodium trimetaphosphate, di- or polyepoxides, mixed anhydrides of carbonic acids with di- or tribasic acids such as, for instance, a mixed anhydride of acetanhydride with adipic acid, aldehydes or aldehyde-releasing reagents such as, for instance, N,N′-dimethylol-N,N′-ethyleneurea.
[0060] Pastes of these crosslinked starches at lower degrees of crosslinking exhibit rapidly increasing viscosities which, however, decrease again with crosslinking increasing. Yet, retrogradation is very low in both cases, for which reason crosslinked amylopectin potato starch is also highly advantageous with a view to obtaining a long flocculation stability. Moreover, crosslinked amylopectin potato starches additionally modified by the compounds described above also constitute advantageous starch materials.
[0061] Finally, amylopectin potato starch may also be present as a graft polymer or a graft copolymer, for instance with products from the group of polyvinyl alcohols, acrylamides, or monomers or polymers derived from petroleum hydrocarbons. In this case, the amylopectin potato starch graft (co)polymer preferably may be present as an emulsion polymer.
[0062] All the above-mentioned modifications of amylopectin potato starch are obtainable not only by reacting native starches, but also by employing degraded forms. The degradation procedures can be realized in a mechanical, thermal, thermochemical or enzymatic manner. Thus, it is not only feasible to structurally modify amylopectin potato starch, but the starch products can also be made soluble or swellable in cold water.
[0063] Cold water soluble degraded amylopectin potato starch, in particular, can be prepared with or without pre-gelatinization by drum drying, spray drying, etc. The degree of dissociation is of great relevance to the optimum development of the properties of starch or starch derivatives soluble in cold water. Amylopectin potato starch or its derivatives do not show any lump formation, dust development and tendency to demixing during their dissociation and subsequent use and are, therefore, perfectly processable in the practical application of a suitable paste-based dry product upon stirring into water. A very special method in this context is extrusion. It offers the possibility to degrade modified amylopectin potato starch to different extents by physical action and, at the same time, convert it into a product soluble or swellable in cold water. Moreover, this technology also renders feasible the direct derivatization of amylopectin potato starch in a cost-saving manner.
[0064] When producing starch derivatives, the elevated grain stability of amylopectin potato starch allows for a simpler production technology than does conventional potato starch. The realization of reactions, for instance, in slurries is more efficient, yielding higher reaction rates. Besides, amylopectin potato starch is less sensible to alkalis and temperatures than conventional starches. Derivatization reactions like, for instance, etherification or esterification reactions, as well as many other reactions preferably used for the derivatization of starches, can thus be intensified at shorter reaction times while the use of gelatinization protection salts can be markedly reduced. The saving of reaction time and the marked reduction of chemicals employed is reflected not only economically by reduced production costs, but also in terms of ecology. Thus, for instance, the salt and CSB loads of reaction waste waters are considerably reduced.
[0065] The flocculant or binder composition according to the invention further may include sedimentation accelerators, stabilizers, dispersants, antifoaming agents, softeners, non-starch-based adhesives or adhesive precursors, buffers, salts, preserving agents or other common additives, optionally in combination. The selection and quantity of the aforementioned additives are, above all, functions of the intended use of the flocculant or binder composition, primarily in view of the inorganic fibers employed.
[0066] According to another aspect, the present invention relates to the use of AP-PS as a flocculant or binder in the production of ceramics products and the use of a flocculant or binder composition according to the invention for the production of ceramics products.
[0067] Ceramics products are generally performed according to the following method. First, an aqueous suspension of inorganic fibers is prepared. Added to the aqueous suspension is an inorganic binder, usually in the form of colloidal silica sol, as well as the starch (according to the invention, that is the amylopectin potato starch), mostly in the positively charged state. Depending on the property of the product, additives and fillers may also be added. In general, the flock-containing mixture has a pH of 4 to 8. Decanting the liquid phase through a screened shaped body separates the formed flocks. The moist cake obtained by this procedure, which is generally referred to as green body, is initially dried and then baked to ceramics after various thermal procedures such as, for instance, sintering. The aim in any event is to carbonize the starch in order to thereby impart the desired porosity on the ceramic material. A general description for the manufacture of ceramics is to be found in “Coagulation and Flocculation”, edited by Bohuslav Dobias, Chapter 11 (1993).
[0068] The slurry necessary for the production of ceramics products in most cases has a solids content of about 0.3-6% usually composed as follows (the data indicated below referring to the overall weight of the slurry):
[0069] The portion of inorganic fibers is around 0.5-4%, preferably at a concentration of 0.5-2%. In addition, organic or inorganic fillers are also added, which are usually employed at concentrations of 0-3%, preferably 0.1-2%. The binder is added in an amount of <2%, mostly <0.5%. The amylopectin potato starch is present at a concentration of from 0.001 to 0.5%, preferably 0.01 to 0.3%. Besides, up to 1% of additives such as, for instance, sedimentation accelerators, dispersants, antifoaming agents, softeners and many others may also be added, provided these additives have no adverse effects on the flocculation procedure. The large remainder in the slurry is water.
[0070] The inorganic fiber employed is of great relevance to the quality and demand of the ceramics product. The used fibers in most cases include aluminum silicates and are available on the market under various trade names. Examples of known product groups include the following fibers: Fiberfrax (available from Unifrax), Kaowool (Thermal Ceramics) or Maxsil (McAllister). Fibers made of zirconium, magnesium, calcium, yttrium, titanium, and other metals or oxides are primarily used for high-temperature applications. Yet, also whiskers or tabular oxides are used amongst others.
[0071] In the production of ceramics products, also fillers may be added. These substances preferably include oxides of aluminum or aluminum silicates, but also chalk. Moreover, organic fibers such as, for instance, celluloses or polyethylene are applied.
[0072] The flocculation process proper is then realized according to the invention by the addition of amylopectin potato starch or a derivative thereof.
[0073] Accordingly, the present invention also relates to a slurry for the production of ceramics products, which is characterized in that it includes a flocculant or binder according to the invention.
[0074] The invention preferably provides a slurry including AP-PS at a concentration of 0.001 to 0.5 weight percent.
[0075] With the objects of the invention in view, there is also provided a slurry that includes the following: inorganic fibers, in particular fibers based on aluminum silicates; fillers, in particular oxides of aluminum or aluminum silicates or chalk; organic materials, in particular organic fibers made of celluloses or polyethylene; inorganic binders, in particular colloidal silica; or mixtures of these ingredients as well as other common additives.
[0076] With the objects of the invention in view, there is also provided a method for producing ceramics products that includes the following steps: preparation of a slurry according to the invention, and thermal treatment at a temperature of above 300° C., in particular above 500° C.
[0077] A good distribution of the fibers and fillers is required for the flocculation process to proceed in the optimum manner. The addition of amylopectin potato starch, as a rule, can be accomplished in three different ways. If cooking starch is added, the slurry must be heated until boiling in order to initiate the flocculation process. It is only by heat that the starch will be gelatinized and hence brought into a water-soluble state. Alternatively, a derivative that is soluble in cold water can be introduced into the system in powdery form under moderate stirring so as to cause the amylopectin potato starch to enter into solution without lumps. A third option is to prepare a concentrated starch paste first and add it to the slurry.
[0078] It has been shown that amylopectin potato starch and, in particular, cationic amylopectin potato starch soluble in cold water, can be admixed in powdery form very quickly and, above all, free of lumps and in a completely dissolved state, what has proved to be particularly beneficial especially in the context of the present invention. The solution dynamics of amylopectin potato starch as well as the flocculation rate, in particular, could be markedly improved upon those of conventional starch derivatives. Yet, also the capacity could be substantially raised. Agglomeration or lump formation as they repeatedly occur with conventional cationic starches have not been observed at the application of amylopectin potato starch. Consequently, also possible predissolving of modified starch may be obviated, thus saving both time and equipment. It was, moreover, shown that upon introduction of the amylopectin potato starch into the system the formed flocks were extremely uniform and exhibited a markedly improved stability, particularly during extended processing times. The formed flocks surprisingly exhibit an excellent shearing stability even by the continuous agitation at an elevated speed in the reaction vessel. By using amylopectin potato starch, also inorganic fibers are wetted more effectively, thus becoming more fluid. Because of naturally chemically bound phosphate groups, amylopectin potato starch additionally offers specific polyelectrolytic properties clearly enhancing the fixation of the subsequently introduced binder on the fiber. In addition, the quantitative ratio between binder and amylopectin potato starch can be better regulated.
[0079] A further important factor resides in the clarity of the amylopectin potato starch paste, which is markedly higher. Comparative measurements with conventional cationic starch products by measuring light transmission on a conventional spectrophotometer revealed considerable advantages. Moreover, amylopectin potato starch derivative pastes show less tendency to retrogradation and are also viscostable over extended periods of time. Comparative measurements in this respect are set out in the experimental part.
[0080] In order to optimize the production of ceramics products, the addition of an inorganic binder is also favorable. In most cases, colloidal silica, which is generally referred to as silica sol, is used as an inorganic binder. As a rule, silica sols are 30-60% aqueous solutions whose turbidity is a function of the size of the SiO 2 particles contained therein. Silica sol is usually applied within a wide particle size distribution, the particle size strongly depending on the ceramics product to be produced. Silica sols are commercially available under various trade names such as MEGASOL® from
[0081] Wesbond Corporation or LUDOX® from DuPont Corporation. Silica sol is usually employed at a ratio of 3:1 to 2:1 relative to the starch. When using amylopectin potato starch, its quantity can be reduced as compared to conventional starches, thus enabling the ceramics end product to be produced at an elevated strength and lower shrinkage. Besides, any possible coagulation of the silica sol is prevented by the use of amylopectin potato starch. Alternatively, the silica sol may be replaced with a binder such as polyvinyl alcohol, polyvinyl acetate or natural or synthetic waxes, or used in combination therewith.
[0082] Various operating techniques are available for removing the flocks from the system, such as, for instance, “tape casting”, “slip casting” or “colloidal filtration” to name but a few examples. In most cases, the formed flocks are discharged into a mold by filtration or suction through pressure application. When using amylopectin potato starch, the optimum orientation of the fibers will be obtained, which is again extremely beneficial for the quality of the ceramics product. The filtrate itself is clear and free of turbid matter. It does not contain any starch residues such that this water can be repeatedly used within the production cycle without any risk. The thus produced moist cake (green body) is initially dried at about 120° C. After this, the green body is converted into a ceramics product by firing. This procedure basically occurs under slow and progressive heating so as to avoid destruction of the ceramics.
[0083] By using amylopectin potato starch, carbonization without residues can be guaranteed, which means that no toxic or environmentally damaging substances will be released. Moreover, the use of amylopectin potato starch gives rise to a particularly stable three-dimensional structure, which is also reflected in the strength values measured. Due to the fact that amylopectin potato starch exhibits an excellent solubility, which prevents the formation of agglomerated particles during the flocculation process, it is also impossible for undesired hollow spaces to form in the ceramic material during firing. Such hollow spaces would otherwise be occupied by silica, which would in turn markedly reduce the strength of the ceramics. Amylopectin potato starch, in particular, also functions as a porosity control. Due to its large hydrodynamic volume, the starch is able to develop and interact more properly. Its porosity can be readily controlled by varying inputs, thus enabling the manufacture of ceramics products having graduated product properties.
[0084] In the context of the method according to the invention, the slurry is preferably prepared through the following steps: providing an aqueous suspension of inorganic fibers; and adding an inorganic binder, in particular silica sol, and a flocculant and binder according to the invention as well as optionally further additives and fillers.
[0085] In accordance with a further object of the invention, a drying step is also provided prior to the thermal treatment step. The drying step is preferably carried out at 100 to 200° C. and, in particular, about 120 to 140° C.
[0086] The thermal treatment step preferably includes a sintering step. Preferred temperatures to be applied during the thermal treatment step as maximum temperatures range from 800 to 2500° C., preferably 1500 to 2000° C. and, in particular, are about 1800° C., which is primarily due to the nature of the inorganic fibers and the demands made on the ceramics product to be produced.
[0087] If desired, the thermal treatment step and optionally also the drying step are preceded by mechanical water removal. Likewise preferred is the provision of a forming step prior to the thermal treatment step, wherein the slurry or the green body is introduced into a suitable mold in a manner known per se.
[0088] An alternative to the direct carbonization of amylopectin potato starch resides in the manufacture of ceramically reinforced products. In this case, the green bodies produced from fibers, binder, and flocculant are penetrated with molten metal and/or metal alloys during forming without destroying the three-dimensional structure (matrix). During this procedure, the starch is baked out and a fiber-reinforced product is finally obtained. By using amylopectin potato starch, it is feasible to substantially raise the amount of porosity and to even better control the distribution. Moreover, the starch also functions perfectly as a binder between the mixed fibers and metals, which helps to further increase the stability.
[0089] In a preferred manner according to the invention, the thermal treatment step is therefore realized by the penetration of liquid metals or liquid metal alloys.
[0090] Ceramics products produced by the use of AP-PS according to the invention stand out particularly for their high strength, strong chemical and thermal resistance, excellent corrosion-resistant properties, special heat conductivity and altogether excellent overall porosity.
[0091] Accordingly, the present invention in a further aspect also relates to ceramics products that are obtainable by the production method according to the invention, i.e., by using AP-PS.
[0092] Other features that are considered as characteristic for the invention are set forth in the appended claims.
[0093] Although the invention is illustrated and described herein as embodied in a flocculant or binder for the ceramics sector, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
[0094] The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0095] [0095]FIG. 1 is a graph illustrating the viscosity development of different starches by plotting viscosity versus time; and
[0096] [0096]FIG. 2 is a graph comparing amylopectin potato starch with amylopectin-rich potato starch prepared by fractionation.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Example 1
Preparation of Cationic Amylopectin Potato Starch
[0097] Native amylopectin potato starch is mixed into a 40% slurry. After the addition of sodium sulfate, a pH of about 11.5 is adjusted by adding 3% soda lye. Cationization is started by admixing 2,3-epoxypropyltrimethyl ammonium chloride. After 18 hours at 34° C., the reaction is stopped by neutralizing the slurry. The cationic starch was washed with water and carefully dried.
[0098] The wash-out degree of the cationic amylopectin potato starch must be very high in order to ensure that the product contains only small quantities of alkali and earth alkali traces. It is known that the elements sodium, potassium, calcium, and magnesium, but also iron and manganese, induce higher shrinkage during the carbonization of a ceramics workpiece. This effect constitutes a problem particularly with high-temperature-resistant ceramics. Consequently, the following quality demands should apply to the washing out of cationic amylopectin potato starch:
Sodium: <0.1% Calcium: <0.01% Potassium: <0.01% Magnesium: <0.01%
[0099] When using amylopectin potato starch, the removal of salt loads was rapidly feasible using smaller amounts of water than with derivativse of conventional starches.
Example 2
Preparation of an Amylopectin Potato Starch Sulfamate
[0100] A 40% slurry of amylopectin potato starch is supplemented with 10% ammonium sulfamate (based on the starch). The reaction mixture is reacted by the gelatinizion of the starch. The paste product is subsequently drum-dried.
Example 3
Variants for the Preparation of Amylopectin Potato Starch Soluble in Cold Water
[0101] The preparation of a derivatized amylopectin potato starch soluble in cold water may be accomplished in various ways. Two typical process variants are given as examples.
[0102] A) Drum-Drying
[0103] Depending on the quality and viscosity desired of the cold water soluble end product, two method variants suggest themselves. Either the slurry of the cationic starch is dried directly on the drum, or the starch is initially gelatinized and drum-dried only subsequently. Both products are scaly.
[0104] B) Extrusion
[0105] By this method, the derivatized starch is converted into a cold water soluble product under the influence of mechanical forces and temperature in the presence of a small amount of water, the dry substance of the reaction mixture in the extruder usually being 70 to 90%. The starch obtained is present in granular form.
Example 4
Viscosity Development
[0106] The viscosity development is an experimental setup to describe the dissolution rate of a cold water soluble cationic starch.
[0107] To this end, 4.5% cationic starches were stirred in at 1000 rpm for 3 minutes. The results are illustrated in FIG. 1
[0108] The curves clearly indicate that amylopectin potato starch derivatives have completed their viscosity development much earlier than conventional potato starch products. The tests, in particular, also revealed that amylopectin potato starch was clearly superior to conventional potato starch already at a low degree of substitution of 0.03, which advantage could be compensated for by conventional potato starch only through a higher nitrogen substitution.
Example 5
Structural Analytics of Amylopectin Potato Starch
[0109] In order to characterize the amylopectin potato starch, both the mean molecular weight and the molar mass distribution were determined. Both analytical methods are extensively described in the literature such as, for instance, by Chi-san Wu in Handbook of Size Exclusion Chromatography; Chromatographic Science Series, Vol. 69 (1995), Marcel Dekker Inc., New York.
[0110] In order to more clearly characterize the amylopectin potato starch, the amylopectin of a conventional potato starch was obtained by enrichment for comparative purposes. A number of methods are available for this method step, the present assay having been based on the fractionation according to the method described by J. Potze in “Starch Production Technology”, Chapter 14, pp 257-271. This method entails the heating of the starch to 155° C. and the selective precipitation of amylopectin by the aid of magnesium sulfate.
[0111] For the comparative representation of the mean molecular weight, also the measuring values of two conventional starches, namely waxy corn starch and conventional potato starch, were determined.
TABLE 1 Comparative Representation of Different Cooking Starches AP-PS PS WCS FAP-PS Mean molecular 190.10 6 48.10 6 64.10 6 43.10 6 weight
[0112] From the above comparison, it is readily apparent that amylopectin potato starch (AP-PS) clearly distinguishes itself from other starches. There is a pronounced difference between amylopectin potato starch and fractionated amylopectin potato starch (FAP-PS) prepared by chemical/physical methods.
[0113] In order to more clearly depict the differences between amylopectin potato starch (AP-PS) and fractionated amylopectin potato starch (FAP-PS), also the molar mass distribution was determined through size exclusion chromatography. In addition, the surface ratio of the measured distribution was characterized (cf. FIG. 2).
Retention time AP-PS FAP-PS >41 min 69.0% 34% <41 min 31.0% 66%
[0114] While amylopectin potato starch (AP-PS) exhibits a significantly uniform molar distribution, fractionated amylopectin potato starch shows a much obscurer picture. What is, above all, typical is the portion of molar masses at a retention time of <41 minutes. With amylopectin potato starch, this is twice as large as with fractionated amylopectin potato starch. Due to the separation process involved in fractionation, the starch was degraded whereby also the properties of the products were changed.
Example 6
Comparative Analytical Characterization of Amylopectin Potato Starch (AP-PS) in View of Waxy Corn Starch (WCS), Corn Starch (CS), and Conventional Potato Starch (PS)
[0115] The values indicated in the Table below were taken from “Starch—Chemistry and Technology” by Roy L. Whistler et al., (1965), Academic Press, and supplemented with in-house experimental values.
MS PS WCS AP-PS % Amylose 26-31 23-27 <2 <2 % Lipid 0.5-0.9 0-0.1 0.5-0.9 0-0.1 % Protein 0.2-0.4 0.05-0.2 0.1-0.35 0.05-0.2 % 0.01-0.02 0.04-0.13* 0-0.02 0.04-0.15* Phosphorus
[0116] From the comparative representation of some specific analytical data, the differences between amylopectin potato starch (AP-PS) and the three conventional starches are clearly apparent. Compared to waxy corn starch and corn starch, amylopectin potato starch contains slighter amounts of lipids and proteins, whereas the high portion of naturally bound phosphate is very typical. The difference from conventional potato starch is reflected by the content of amylose. Due to the fact that amylopectin potato starch contains up to 100% amylopectin, its viscosity, for instance, or also the turbidity behavior of pastes, differ strongly. Thus, it was found that amylopectin potato starch exhibits a constant paste clarity even over an extended period of time, while conventional starches show noticeable turbidities. It is exactly on an industrial scale that the stability of starch or starch derivatives is of relevance to the quality of flocculation and the production of green bodies.
Example 7
Dissolution Behavior of Starch Sulfamates and Cationic Starches
[0117] An important characteristic of cold water soluble starches is their dissolution behavior. The manufacture of ceramics products calls for an unrestrictedly complete solubility without involving the formation of, for instance, agglomerations or lumps. In order to be able to examine the solubility of cold water soluble derivatized starches at all, the following experimental array was chosen, which is very similar to real life.
[0118] A container was filled with 15 L water under stirring at 700 rpm, and 15 g starch are rapidly admixed within a few seconds. The paste is stirred at room temperature for 3 minutes under the conditions indicated and subsequently filtered over an 800 m sieve. Paste residues on the stirrer as well as sieve residues were subjectively assessed to evaluate solubility. The following results were obtained:
TABLE 2 Cationic starches Production Sieve process* DS** residues Paste on stirrer commercial PS WATRO 0.03 +/− +/− commercial PS WATRO 0.1 +/− − AP-PS WATRO 0.03 + + AP-PS WATRO 0.1 + + WCS WATRO 0.03 − +/− WCS WATRO 0.1 − +/− FAP-PS WATRO 0.03 +/− +/− FAP-PS WATRO 0.1 +/− − PS extruded 0.03 +/− +/− PS extruded 0.1 +/− − AP-PS extruded 0.03 + + AP-PS extruded 0.1 + + Starch sulfamates Sieve Production process* residues Paste on stirrer Commercial PS WATRO +/− +/− AP-PS WATRO + + WCS WATRO − +/− FAP-PS WATRO +/− −
[0119] The dissolution tests clearly demonstrated that the amylopectin potato starch derivatives exhibited a solubility far better than that of conventional derivatives of potato starch, waxy corn starch or fractionated amylopectin potato starch obtained by enrichment. Comparative studies, furthermore, revealed that cationic products of amylopectin potato starch were clearly superior to conventional commercial products, which is again of great advantage in the manufacture of ceramics products.
Example 8
Ceramics Production
[0120] To a slurry of 210 g aluminum silicate fibers of the Kaowool brand and 25 L water are added 90 g of a filler like, for instance, mullite. Then, 13 g of a cold water soluble cationic amylopectin potato starch (DS=0.03) are introduced. Within a short period of time, the starch is dissolved and distributed in the system to the optimum degree. The optimum flock size and flock distribution could, in fact, be obtained by the addition of this starch. After this, 96 g of a commercially available 40% silica sol are added, briefly stirred, and subsequently the flock mass is sucked off via a screened mold upon application of vacuum. The shaped body is dried at about 120° C. and baked at about 1800° C.
[0121] In order to elucidate the advantages of the use of amylopectin potato starch, comparative tests were carried out with conventional cold water soluble cationic starches. In the course of these tests, the flocculation time, the turbidity of the circulating water after 20 passes as well as the physical parameters of the ceramics end product were determined.
TABLE 3 PS ** WCS AP-PS FAP-PS Measurements during production Flocculation 3 min 3.5 min 2 min 3 min time Turbidity * 19 FTU 12 FTU 4 FTU 11 FTU Analytics of ceramics end products Density 350 m 3 /kg 372 m 3 /kg 410 m 3 /kg 347 m 3 /kg Shrinkage 2.0% 2.4% 0.9% 1.9%
[0122] The measurements carried out with amylopectin potato starch revealed significantly reduced flocculation times as against conventional starches; moreover, the flocculation stability was considerably higher. The latter is reflected, in particular, by the clear reaction water, which is still clear and free of turbid matter even after 20 production passes. The enhanced processability of the ceramics products obtained by the use of amylopectin potato starch is apparent from the analytical data of the end products. The density of the products was significantly higher when using amylopectin potato starch, the shrinkage of the three-dimensional body was clearly reduced.
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A flocculant or binder composition can be used to form a slurry, which in turn, is usable in methods of producing ceramics and ceramic products. The flocculant or binder composition includes amylopectin potato starch (AP-PS).
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FIELD
The present invention is directed to a carrier for a reticle used in semiconductor manufacturing.
BACKGROUND
The manufacturing of semiconductor chips is an extremely exacting and difficult process. Each chip has many layers and a reticle or photomask is required for each layer that is printed on the wafer. These reticles should have no contamination or dust, in order to avoid defects in the pattern which is formed on the wafer. Traditionally, light has been shined through the photomask in order to form the pattern on the wafer. However, as the patterns on the wafers have gotten smaller and closer together, it is no longer possible to effectively use regular light to form these patterns. That is, the wavelength of regular light is too long to clearly form such small patterns. In order to extend the use of this process to even smaller patterns, other types of light such as deep ultraviolet (248 nm or 193 nm), vacuum ultraviolet (157 nm) and EXTREME ultraviolet (13.4 nm) are being used or are being considered. However, even this shorter wavelength radiation has limits.
Because of the problem of dust and other impurities landing on the reticle during transport, and the possibility of scratches, it is important to have a protective layer. Typically, a pellicle, which is a membrane, is used for this purpose. The use of such a membrane protects the reticle during the transportation and exposure process. However, the use of the pellicle produces additional problems when shorter wavelength radiation is utilized. The shorter wavelength radiation causes the standard pellicle material to burn off or otherwise be destroyed. Thus, if shorter wavelength radiation is to be utilized, it is necessary to find other ways to protect the reticle from the high intensity radiation without destroying the pellicle.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and a better understanding of the present invention will become apparent from the following detailed description of example embodiments and the claims when read in connection with the accompanying drawings, all forming a part of the disclosure of this invention. While the foregoing and following written and illustrated disclosure focuses on disclosing example embodiments of the invention, it should be clearly understood that the same is by way of illustration and example only and that the invention is not limited thereto. The spirit and scope of the present invention are limited only by the terms of the appended claims.
The following represents brief descriptions of the drawings, wherein:
FIG. 1 is an example advantageous embodiment of the present invention;
FIG. 2 is an example advantageous embodiment of the present invention in exploded form.
DETAILED DESCRIPTION
Before beginning a detailed description of the subject invention, mention of the following is in order. When appropriate, like reference numerals and characters may be used to designate identical, corresponding or similar components in differing figure drawings. Further, in the detailed description to follow, example sizes/models/values/ranges may be given, although the present invention is not limited to the same.
In the processing of semiconductor wafers it is common to have a manufacturing apparatus which holds dozens of reticles at a time so that it is unnecessary to remove the wafer or reticles from the apparatus while several different layers are being formed. This allows the internal atmosphere of the apparatus to be sealed. This is very important since the apparatus includes a very clean, class 1 environment, to prevent any dust or other imperfections from landing on the wafer and also to protect the reticles. By storing a number of reticles at a time, it is possible to process the wafer without removing it and exposing it to the atmosphere.
The present invention provides a reticle carrier and protection device 10 , as shown in FIG. 1 . This carrier includes a bottom 12 and a top 14 . The top includes a transparent window portion 16 . A cover 18 can also be used which is removable when necessary but which otherwise protects the window. An input port 20 and exit port 22 are provided, so that nitrogen or other gas may be used to purge the reticle carrier to prevent impurities from settling on the reticle. Filters (not shown) may also be provided to help remove impurities.
As mentioned previously, it is difficult to provide a pellicle to protect the reticle when using lower wavelength radiation (below 193 nm such as 157 nm). Thus, traditional soft pellicles which are polymer membranes are damaged by lower wavelength radiation. The present invention solves this problem by having a removable pellicle. That is, the pellicle is left in place during transport and during inspection. However, during the exposure step, where the lower wavelength radiation is utilized, the pellicle is removed to avoid any damage thereto.
Thus, in the normal handling of the reticle, the protective lid over the transparent window 16 is closed during transportation. However, the lid may be opened for inspection utilizing DUV (deep ultraviolet) radiation. The transparent window is not harmed by this type of radiation. In addition, it may also be utilized with VUV (vacuum ultraviolet) in the process of photochemical cleaning. By having the transparent window as part of the top of the carrier, it is possible to perform the steps of inspection and photochemical clean without removing the reticle from the carrier.
When the reticle is used to produce a pattern on the semiconductor, the carrier is opened and the reticle removed and used. As soon as exposure is completed, the reticle is returned to the carrier and the top and cover reinstalled. The removal of the reticle and its reinstatement is all done automatically within the class one or better clean environment. By using this system, it is possible to use the transparent window for all the necessary steps except the exposure, which is handled by removing the reticle from the carrier.
FIG. 2 shows an exploded version of the carrier shown in FIG. 1 . As seen, the top 14 including window 16 is placed over reticle 13 and on top of bottom 12 . The parts are placed together and the top and bottom closed around the reticle. The cover 18 may also be placed over the top cover. The various parts of the carrier should be made of non-out gassing material that generates no particles. The carrier can use mechanical clamping or magnetic sealing to protect a reticle during transport.
Ports can be provided to introduce nitrogen gas or other inert gases to purge and filter any impurities. The ports shown in FIG. 1 may be connected to a single input for each reticle carrier, or a plurality of ports can be connected to a single source.
The carrier may have other design features such as electrostatic dissipation and may have a design which minimizes contact from the reticle surface.
While the device as device described above has a transparent window in the top cover, it would also be possible to provide transparent windows in both the top and bottom if inspection were necessary for the bottom of the reticle.
While the above mentioned wavelengths for the various type of ultraviolet light are those preferred, other wavelengths may also be utilized. For example, for the inspection steps, 266 nm or 193 nm may be utilized.
The reticle carrier described can use any type of top and bottom cover that provides a tight seal.
In concluding, reference in the specification to “one embodiment”, “an embodiment”, “example embodiment”, etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the purview of one skilled in the art to effect such feature, structure, or characteristic in connection with other ones of the embodiments. Furthermore, for ease of understanding, certain method procedures may have been delineated as separate procedures; however, these separately delineated procedures should not be construed as necessarily order dependent in their performance, i.e., some procedures may be able to be performed in an alternative ordering, simultaneously, etc.
This concludes the description of the example embodiments. Although the present invention has been described with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this invention. More particularly, reasonable variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the foregoing disclosure, the drawings and the appended claims without departing from the spirit of the invention. In addition to variations and modifications in the component parts and/or arrangements, alternative uses will also be apparent to those skilled in the art.
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A reticle carrier used in semiconductor manufacture. The carrier includes a bottom cover and a top cover having a transparent window. A protective lid may also be included. The box includes ports to allow nitrogen gas to enter and purge the inside. The transparent window is used for inspection and photochemical clean. However, since no material is available which can suitably handle smaller wavelength radiation, the reticle is removed from the carrier when exposure at these wavelengths is required.
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This application is filed under 35 U.S.C. 371 and based on PCT/EP98/00891, filed Feb. 17, 1998.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a process for the contact drying of aqueous surfactant pastes in a horizontal thin-layer evaporator or dryer.
2. Discussion of Related Art
Anionic and amphoteric or zwitterionic surfactants are important ingredients of solid detergents and bar soaps. The detergents are normally produced by spraying an aqueous, generally highly alkaline slurry of the ingredients and drying the slurry with hot inert gases flowing in countercurrent. However, since this conventional spray drying process is accompanied by serious pollution of the waste air with organic material, there is a need for alternative, ecologically more favorable drying processes. These include in particular the contact drying of water-containing surfactant pastes in thin-layer dryers which leads to dry products which can then be processed with the other dried detergent ingredients, for example in mixers, to form the end product.
European patent application EP-A1 0 572 957 (Kao) describes a process for drying alkyl or alkyl ether sulfates in which dilute surfactant pastes are first concentrated to an active substance content of 60 to 80% by weight and are then dried in vacuo at temperatures of 50 to 140° C. in a vertical thin-layer evaporator. However, a major disadvantage of this process is that, because drying is carried out under reduced pressure, the end product has to be removed from the circuit using complicated equipment suitable for operation in a vacuum. The continuous contact with the hot product means that there is always a danger of caking and, hence, operational disturbances which necessitate a complete stoppage of production so that cleaning can be carried out. Another major disadvantage is that the use of a vertical thin-layer evaporator with wall contact of the rotor blades means that a flowable product film has to be maintained on the wall of the evaporator over its entire length in continuous operation in order to avoid mechanical overloading of the evaporator. Accordingly, the process is not suitable for the direct production of a powder, but only for the production of a concentrated hotmelt which has to be separately crystallized (for example in a flaking roller or the like) and then size-reduced.
By contrast, International patent application WO 96/06916 (Unilever) proposes a process for drying water-containing anionic surfactant pastes in a horizontal thin-layer evaporator which operates under a light vacuum to almost normal pressure and at temperatures above 130° C. Another feature of this process is the use of a very high peripheral speed of the stirrers used of at least 15 m/s which virtually rules out direct wall contact and leads to products of satisfactory color. However, in the drying of water-containing anionic surfactant pastes, more particularly aqueous pastes of alkyl sulfates or alkyl ether sulfates, there is basically a risk of unwanted hydrolysis in the product. Even brief reduction of the pH value leads in the presence of water to rehydrolysis, to the formation of inorganic sulfate and to a reduction in the content of washing-active substance. In following the teaching of WO 96/06916, applicants found that a hydrolysis-free product could not be reproducibly obtained over an operating period of several hours.
Accordingly, the complex problem addressed by the present invention was to provide a process for the contact drying of water-containing anionic surfactant and/or amphoteric surfactant pastes which would not have any of the disadvantages mentioned above and which, despite minimal outlay on equipment, would lead under production conditions to hydrolysis-free, free-flowing granules of satisfactory color distinguished by high bulk densities and a uniform particle size distribution.
DESCRIPTION OF THE INVENTION
The present invention relates to a process for the production of solid detergent raw materials by simultaneously drying and granulating water-containing pastes of anionic and/or amphoteric surfactants in a horizontal thin-layer evaporator or dryer with rotating fittings, characterized in that drying is carried at a temperature in the range from 120 to 130° C.
It has surprisingly been found that free-flowing granules of satisfactory color can be obtained only and precisely when the drying temperature is kept in the range mentioned. Even minor upward deviations lead to an unwanted increase in the content of inorganic sulfate while slight downward deviations lead to products with unsatisfactory flow properties. The invention includes the observation that the tendency towards hydrolysis can be further suppressed by carrying out the contact drying process in the presence of (a) 0.05 to 0.5% by weight of alkali metal carbonate and/or (b) an alkaline gas stream. The water is removed preferably by a gas stream and not by applying a vacuum. Another advantage of the process according to the invention is that it gives products of high bulk density (above 600 g/l) which, irrespective of the surfactant paste used, have a very uniform particle size distribution.
Surfactants
Typical examples of anionic surfactants which can be dried by the process according to the invention are soaps, alkyl benzenesulfonates, alkane sulfonates, olefin sulfonates, alkyl ether sulfonates, glycerol ether sulfonates, α-methyl ester sulfonates, sulfofatty acids, alkyl sulfates, fatty alcohol ether sulfates, glycerol ether sulfates, hydroxy mixed ether sulfates, monoglyceride (ether) sulfates, fatty acid amide (ether) sulfates, mono- and dialkyl sulfosuccinates, mono- and dialkyl sulfosuccinamates, sulfotriglycerides, amide soaps, ether carboxylic acids and salts thereof, fatty acid isethionates, fatty acid sarcosinates, fatty acid taurides, N-acyl amino acids such as, for example, acyl lactylates, acyl tartrates, acyl glutamates and acyl aspartates, alkyl oligoglucoside sulfates, protein fatty acid condensates (more particularly vegetable wheat-based products), alkyl (ether)phosphates and sulfates of ring-opening products of olefin epoxides with water or alcohols. Where the anionic surfactants contain polyglycol ether chains, they may have a conventional homolog distribution although they preferably have a narrow homolog distribution. Typical examples of amphoteric or zwitterionic surfactants are alkyl betaines, alkyl amidobetaines, aminopropionates, aminoglycinates, imidazolinium betaines and sulfobetaines. The surfactants mentioned are all known compounds. Information on their structure and production can be found in relevant synoptic works, cf. for example J. Falbe (ed.), “Surfactants in Consumer products”, Springer Veriag, Berlin, 1987, pp. 54-124 or J. Falbe (ed.), “Katalysatoren, Tenside und Mineralöladditive”, Thieme Verlag, Stuftgart, 1978, pp. 123-217.
In the context of the invention, water-containing pastes are understood to be aqueous preparations of the surfactants which have an active substance content of 5 to 80% by weight and preferably 10 to 70% by weight. For energy-related and rheological reasons, it is of advantage to use pastes which have a solids content of at least 30% by weight and preferably 50% by weight and at most 70% by weight. The anionic surfactants are used in the form of their alkali metal, alkaline earth metal, ammonium, alkylammonium, alkanolammonium, glucammonium salts. In other preferred embodiments of the process, alkyl and/or alkenyl (ether)sulfates, sulfosuccinates and/or betaines are dried and processed to light-colored, free-flowing granules.
Alkyl and/or Alkenyl Sulfates
In the context of the invention, alkyl and/or alkenyl sulfates, which are also often referred to as fatty alcohol sulfates, are understood to be the sulfation products of primary alcohols which correspond to formula (I):
R 1 O—SO 3 X (I)
where R 1 is a linear or branched, aliphatic alkyl and/or alkenyl group containing 6 to 22 and preferably 12 to 18 carbon atoms and X is an alkali metal and/or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium. Typical examples of alkyl sulfates which may be used in accordance with the present invention are the sulfation products of caproic alcohol, caprylic alcohol, capric alcohol, 2-ethylhexyl alcohol, lauryl alcohol, myristyl alcohol, cetyl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, arachyl alcohol gadoleyl alcohol, behenyl alcohol and erucyl alcohol and the technical mixtures thereof obtained by the high-pressure hydrogenation of technical methyl ester fractions or aldehydes from Roelen's oxosynthesis. In addition, Guerbet alcohols containing 16 to 32 carbon atoms may also serve as raw materials. The sulfation products may advantageously be used in the form of their alkali metal salts, especially their sodium salts. Alkyl sulfates based on C 16/18 tallow fatty alcohols or vegetable fatty alcohols with a comparable C chain distribution in the form of their sodium salts are particularly preferred.
Alkyl and/or Alkenyl Ether Sulfates
Alkyl and/or alkenyl ether sulfates (“ether sulfates”) are known anionic surfactants which are industrially produced by SO 3 or chlorosulfonic acid (CSA) sulfation of oxoalcohol or fatty alcohol polyglycol ethers and subsequent neutralization. Ether sulfates suitable for the purposes of the invention correspond to formula (II):
R 2 O—(CH 2 CH 2 O) m SO 3 X (II)
where R 2 is a linear or branched alkyl and/or alkenyl group containing 6 to 22 carbon atoms, m is a number of 1 to 10 and X is an alkali and/or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium. Typical examples are the sulfates of addition products of on average 1 to 10 and, more particularly, 2 to 5 moles of ethylene oxide with caproic alcohol, caprylic alcohol, 2-ethylhexyl alcohol, capric alcohol, lauryl alcohol, isotridecyl alcohol, myristyl alcohol, cetyl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, arachyl alcohol, gadoleyl alcohol, behenyl alcohol, erucyl alcohol and brassidyl alcohol and technical mixtures thereof in the form of their sodium and/or magnesium salts. Adducts of ethylene oxide with Guerbet alcohols containing 16 to 32 carbon atoms may also be used as raw materials. The ether sulfates may have both a conventional homolog distribution and a narrow homolog distribution. A particularly preferred embodiment comprises using ether sulfates based on adducts of on average 2 to 3 moles of ethylene oxide with technical C 12/14 or C 12/18 cocofatty alcohol fractions in the form of their sodium and/or magnesium salts.
Sulfosuccinates
Sulfosuccinates, which are also referred to as sulfosuccinic acid esters, are known anionic surfactants which may be obtained by the relevant methods of preparative organic chemistry. They correspond to formula (III):
where R 3 is an alkyl and/or alkenyl group containing 6 to 22 carbon atoms, R 4 has the same meaning as R 3 or X, p and q independently of one another stand for 0 or for numbers of 1 to 10 and X is an alkali metal or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium. They are normally produced from maleic acid, but preferably from maleic anhydride, which in a first step is esterified with optionally ethoxylated primary alcohols. The monoester-to-diester ratio can be adjusted at this stage by varying the quantity of alcohol and the temperature. The second step comprises the addition of bisulfite which is normally carried out in methanol as solvent. Fairly recent overviews of the production and use of sulfosuccinates have been published, for example, by T. Schoenberg in Cosm. Toil. 104, 105 (1989), by J. A. Milne in R. Soc. Chem. (Ind. Appl. Surf. II) 77, 77 (1990) and by W. Hreczurch et al. in J. Am. Oil. Chem. Soc. 70, 707 (1993). Typical examples are sulfosuccinic acid monoesters and/or diesters in the form of their sodium salts which are derived from fatty alcohols containing 8 to 18 and preferably 8 to 10 or 12 to 14 carbon atoms. The fatty alcohols may be etherified with on average 1 to 10 and preferably 1 to 5 moles of ethylene oxide and may have both a conventional and—preferably—a narrow homolog distribution. Di-n-octyl sulfosuccinate and monolauryl-3EO-sulfosuccinate in the form of their sodium salts are mentioned as examples.
Betaines
Betaines are known surfactants which are mainly obtained by carboxyalkylation, preferably carboxymethylation, of aminic compounds. The starting materials are preferably condensed with halocarboxylic acids or salts thereof, especially sodium chloroacetate, 1 mole of salt being formed per mole of betaine. Another suitable method is the addition of unsaturated carboxylic acids, for example acrylic acid. Information on the nomenclature and above all on the difference between betaines and “true” amphoteric surfactants can be found in the article by U. Ploog in Seifen-Öle-Fette-Wachse, 198, 373 (1982). Other overviews on this subject have been published, for example, by A. O'Lennick et al. in HAPPI, November 70 (1986), by S. Holzman et al. in Tens. Det. 23, 309 (1986), by R. Bibo et al. in Soap Cosm. Chem. Spec. Apr. 46 (1990) and by P. Ellis et al. in Euro Cosm. 1, 14 (1994). Examples of suitable betaines are the carboxy-alkylation products of secondary and, more particularly, tertiary amines corresponding to formula (IV):
in which R 5 represents alkyl and/or alkenyl groups containing 6 to 22 carbon atoms, R 6 represents hydrogen or alkyl groups containing 1 to 4 carbon atoms, R 7 represents alkyl groups containing 1 to 4 carbon atoms, x is a number of 1 to 6 and Y is an alkali metal and/or alkaline earth metal or ammonium. Typical examples are the carboxymethylation products of hexyl methyl amine, hexyl dimethyl amine, octyl dimethyl amine, decyl dimethyl amine, dodecyl methyl amine, dodecyl dimethyl amine, dodecyl ethyl methyl amine, C 12/14 cocoalkyl dimethyl amine, myristyl dimethyl amine, cetyl dimethyl amine, stearyl dimethyl amine, stearyl ethyl methyl amine, oleyl dimethyl amine, C 16/18 tallow alkyl dimethyl amine, Guerbet amines and technical mixtures thereof.
Also suitable are carboxyalkylation products of amidoamines which correspond to formula (V):
where R 8 CO is an aliphatic acyl group containing 6 to 22 carbon atoms and 0 or 1 to 3 double bonds, y is a number of 1 to 3 and R 6 , R 7 , x and Y are as defined above. Typical examples are reaction products of fatty acids containing 6 to 22 carbon atoms, namely caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, palmitoleic acid, stearic acid, isostearic acid, oleic acid, elaidic acid, petroselic acid, linoleic acid, linolenic acid, elaeostearic acid, arachic acid, gadoleic acid, behenic acid, erucic acid, Guerbet acids, and technical mixtures thereof, with N,N-dimethylaminoethyl amine, N,N-dimethylaminopropyl amine, N,N-diethylaminoethyl amine and N,N-diethylaminopropyl amine which are condensed with sodium chloroacetate. A condensation product of C 8/18 cocofatty acid-N,N-dimethylaminopropyl amide with sodium chloroacetate is preferably used.
Other suitable starting materials for the betaines to be used in accordance with the invention are imidazolines. These substances are also known substances which may be obtained, for example, by cyclizing condensation of 1 or 2 moles of fatty acid with polyfunctional amines, for example aminoethyl ethanolamine (AEEA) or diethylenetriamine. The corresponding carboxyalkylation products are mixtures of different open-chain betaines. Typical examples are condensation products of the above-mentioned fatty acids with AEEA, preferably imidazolines based on lauric acid or C 12/14 cocofatty acid which are subsequently betainized with sodium chloroacetate.
Alkyl and/or Alkenyl Oligoglycosides
In one particular embodiment of the invention, the anionic or amphoteric surfactants are dried together with nonionic surfactants of the alkyl and/or alkenyl oligoglycoside type which correspond to formula (VI):
R 9 O—[G] p (VI)
where R 9 is an alkyl and/or alkenyl radical containing 4 to 22 carbon atoms, G is a sugar unit containing 5 or 6 carbon atoms and p is a number of 1 to 10. They may be obtained by the relevant methods of preparative organic chemistry, for example by acid-catalyzed acetalization of glucose with fatty alcohols. The alkyl and/or alkenyl oligoglycosides may be derived from aldoses or ketoses containing 5 or 6 carbon atoms, preferably glucose. Accordingly, the preferred alkyl and/or alkenyl oligoglycosides are alkyl and/or alkenyl oligoglucosides. The index p in general formula (VI) indicates the degree of oligomerization (DP), i.e. the distribution of mono- and oligoglycosides, and is a number of 1 to 10. Whereas p in a given compound must always be an integer and, above all, may assume a value of 1 to 6, the value p for a certain alkyl oligoglycoside is an analytically determined calculated quantity which is generally a broken number. Alkyl and/or alkenyl oligoglycosides having an average degree of oligomerization p of 1.1 to 3.0 are preferably used. Alkyl and/or alkenyl oligoglycosides having a degree of oligomerization of less than 1.7 and, more particularly, between 1.2 and 1.4 are preferred from the applicational point of view.
The alkyl or alkenyl radical R 9 may be derived from primary alcohols containing 4 to 11 and preferably 8 to 10 carbon atoms. Typical examples are butanol, caproic alcohol, caprylic alcohol, capric alcohol and undecyl alcohol and the technical mixtures thereof obtained, for example, in the hydrogenation of technical fatty acid methyl esters or in the hydrogenation of aldehydes from Roelen's oxosynthesis. Alkyl oligoglucosides having a chain length of C 8 to C 10 (DP=1 to 3), which are obtained as first runnings in the separation of technical C 8-18 coconut oil fatty alcohol by distillation and which may contain less than 6% by weight of C 12 alcohol as an impurity, and also alkyl oligoglucosides based on technical C 9/11 oxoalcohols (DP=1 to 3) are preferred. In addition, the alkyl or alkenyl radical R 9 may also be derived from primary alcohols containing 12 to 22 and preferably 12 to 14 carbon atoms. Typical examples are lauryl alcohol, myristyl alcohol, cetyl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, arachyl alcohol, gadoleyl alcohol, behenyl alcohol, erucyl alcohol, brassidyl alcohol and technical mixtures thereof which may be obtained as described above. Alkyl oligoglucosides based on hydrogenated C 12/14 coconut oil fatty alcohol having a DP of 1 to 3 are preferred.
The co-drying process may be carried out by mixing and homogenizing the aqueous pastes of the various surfactants beforehand and then introducing the resulting homogenized mixture into the thin-layer evaporator. However, the pastes may also be separately introduced and mixed in situ. The ratio by weight between the anionic/amphoteric surfactants and alkyl and/or alkenyl oligoglycosides can be in the range from 10:90 to 90:10, based on the washing-active substance content, and is preferably in the range from 25:75 to 75:25. Mixtures of sulfosuccinates and alkyl oligoglucosides in a ratio by weight of 40:60 to 60:40 are particularly preferred and, after drying, are eminently suitable for the production of bar soaps.
Drying and Granulation in a Flash Dryer
The simultaneous drying and granulation are carried out in a horizontally arranged thin-layer evaporator or dryer with rotating fittings of the type marketed, for example, by the VRV Company under the name of “Flashdryer” or by the VOMM Company under the name of “Turbodryer”. In simple terms, these dryers are tubes which can be heated to different temperatures over several zones. The paste-form starting material which is introduced by a pump is projected by one or more shafts equipped with blades or plowshares as rotating fittings against the heated wall on which drying takes place in the form of a thin layer typically between 1 and 10 mm thick. According to the invention, it has proved to be of advantage to apply a temperature gradient from 130 (product entry) to 20° C. (product exit) to the thin-layer evaporator. This can be done, for example, by heating the first two zones of the evaporator to 120-130° C. and cooling the last zone to 20° C. The thin-layer evaporator or dryer is operated at atmospheric pressure. Air, but preferably an alkaline gas stream, for example ammonia, is passed through in countercurrent (throughput 50 to 150 m 3 /h). The gas entry temperature is generally in the range from 20 to 30° C. while the gas exit temperature is in the range from 90 to 110° C. The throughput of the surfactant pastes is of course dependent on the size of the dryer and amounts, for example, to between 5 and 25 kg/h. It is advisable to heat the pastes to 40 to 60° C. as they are fed into the dryer and to add alkali metal carbonate, preferably sodium carbonate, to them in quantities of 0.05 to 0.5% by weight, based on the solids content, in order to avoid hydrolysis processes.
Another preferred embodiment of the process according to the invention comprises mixing the water-containing surfactant with already dried end product on the hot contact surface. To this end, a partial stream of the product of about 10 to 40% by weight and preferably 15 to 25% by weight, based on the mass flow of the paste used, is removed at the dryer exit and directly re-introduced into the apparatus in the immediate vicinity of the paste entry point by means of a solids metering screw. It is possible by applying this measure to reduce the tackiness of the water-containing surfactant and to establish better wall contact of the product over the entire available surface. This makes product transport more uniform and intensifies drying of the product. At the same time, the particle size distribution of the granules can be shifted under control towards coarser products, i.e. the unwanted fine particle component can be significantly reduced, by the addition of the end product. This measure provides for an increase in throughput, based on analogous process conditions with no recycling of solids.
After drying, it has also proved to be of considerable advantage to transfer the granules, which still have a temperature of about 50 to 70° C., to a conveyor belt, preferably in the form of a vibrating chute or the like, and rapidly to cool them, i.e. in 20 to 60 seconds, to temperatures of around 30 to 40° C. using ambient air. In order to improve their resistance to unwanted water absorption, the granules of particularly hygroscopic surfactants may also be powdered or dusted with silica in a quantity of 0.5 to 2% by weight.
COMMERCIAL APPLICATIONS
The granules obtainable by the process according to the invention may subsequently be mixed with other ingredients of powder-form surface-active compositions, for example tower powders for detergents. The powders may also readily be incorporated in water-based preparations. In fact, there are no differences in performance properties between the powders on the one hand and the aqueous starting pastes on the other hand. The granules may readily be incorporated, for example together with fatty acids, fatty acid salts, fatty alcohols, starch, polyglycols and the like, in bar soaps of the combination bar or syndet type and toothpastes or may be used for the production of emulsifiers for emulsion polymerization.
EXAMPLES
Examples 1 to 5
The granules were produced in a flash dryer of the type manufactured by VRV S.p.A. of Milan, Italy. This dryer is a horizontally arranged thin-layer evaporator (length 1100 mm, internal diameter 155 mm) with 4 shafts and 22 blades which are arranged at a distance of 2 mm from the wall. The dryer has three separate heating and cooling zones and a total heat-exchange surface of 0.44 m 2 . It is operated at normal pressure. Water-containing surfactant pastes (solids content 70% by weight) optionally containing 1% by weight of sodium carbonate as additive and heated to 50° C. were pumped by a vibrating pump (throughput 11.5 kg/h) into the thin-layer evaporator in which heating zones 1 and 2 had been adjusted to 125° C. and cooling zone 3 to a temperature of 20° C. The speed of the rotors was 24 m/s. Air or a 1:1 mixture of air and ammonia was passed through the flash dryer (ca. 110 m 3 /h). The gas exit temperature was ca. 65° C. The predried granules, which still had a temperature of about 60° C., were transferred to a vibrating chute (length 1 m), exposed to ambient air and cooled in 30 seconds to a temperature of around 40° C. The granules were then dusted/powdered with about 1% by weight of silica (Sipernat® 50 S). Dry, pure white granules were obtained and remained free flowing, i.e. did not form any lumps, even after prolonged storage in air. The characteristic data of the granules are set out in Table 1.
TABLE 1
Characteristic data of the flash dryer granules (percentages = % by
weight)
Particle size distribution [%] in
Surfactant
mm
RW
BD
Ex.
paste
>0.8
>0.4
>0.2
>0.1
<0.1
[%]
[g/l]
1
Sodium Lauryl
11.1
19.0
24.2
31.0
14.7
1.3
610
Sulfate 1)
2
Sodium
11.8
21.0
26.3
35.5
5.4
1.2
615
Laureth
Sulfate 1)
3
Sodium
12.0
13.4
27.1
34.0
13.5
1.3
620
Laureth
Sulfo-
succinate 2)
4
Cocoamido-
12.2
12.7
23.5
33.7
17.9
1.3
610
propyl Betaine
5
Sodium
11.9
12.5
22.9
32.7
20.0
1.3
600
Laureth
Sulfo-
succinate/
Coco
Glucosides
(1:1) 2)
1) Addition of sodium carbonate to the paste, air/ammonia gas stream
2) Addition of sodium carbonate to the paste
RW = Residual water content of the granules
BD = Bulk density
Examples 6 to 11
Alkyl sulfate pastes were dried in the same way as described in Example 1 except that a partial product stream (Examples 7, 8 and 11) was removed at the dryer exit and directly returned to the dryer in the immediate vicinity of the paste entry point by means of a solids metering screw. The results are set out in Table 2.
TABLE 2
Drying of AS pastes with recycling (percentages = % by weight)
Parameter
6
7
8
9
10
11
Starting material
1
1
1
2
2
2
Drying temperature [° C.]
128
Flow rate of paste [kg/h]
8.5
11.5
13.5
8.5
11.3
11.3
Flow rate of solids [kg/h]
—
3.5
1.7
—
—
1.7
Water content of end product
0.4
0.4
0.4
0.7
1.3
1.0
[%]
Bulk density [g/l]
557
593
654
657
Particle size distribution [%]
>0.8 mm
11.1
29.4
0.8
0.7
>0.4 mm
19.0
30.2
3.0
9.1
>0.2 mm
24.2
23.9
7.2
19.7
>0.1 mm
31.0
13.1
32.2
45.7
<0.1 mm
14.7
3.4
56.8
24.8
1) Cocoalkyl sulfate sodium salt, 35% by weight active substance
2) Lauryl sulfate sodium salt, 35% by weight active substance
Examples 6 to 8 show that, for the same water content of the end product, the throughput of paste was increased from 8.5 to 13.5 kg/h when the powder was recycled. The quantity recycled can be varied within wide limits (Examples 7 and 8). The product of Example 8 is much coarser than the product of Example 1. Examples 9 and 10 show that an increase in throughput without any recycling of powder can lead to an increase in the water content of the product from 0.7 to 1.3% by weight. Recycling of the powder (Example 11) reduced product moisture and again led to powders with a smaller dust content.
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A process for producing solid detergent granular materials is presented involving (a) forming an aqueous surfactant paste of an anionic surfactant, an amphoteric surfactant or mixtures thereof, and (b) drying and granulating the aqueous paste in a horizontal thin-layer evaporator or dryer having rotating fittings, wherein the drying is carried out at a temperature of 120° C. to 130° C. The process produces granules having a bulk density greater than 600 grams/liter and a uniform particle size distribution.
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BACKGROUND OF THE INVENTION
The present invention relates generally to a shutter mechanism for automatically opening and closing a port and, in particular, relates to a shutter mechanism which ensures that the sealing/unsealing movement and the rotational movement of a shutter are mutually independent.
The need to control gas or moisture passing through a port is widespread. One specific application where such a requirement is in demand is in analytical instrument, e.g., an infrared spectrophotometer In many analytical instruments a compartment containing the optical elements of the instrument is purged with an inert gas to maintain an optimum ambient for IR transmission a well as to protect the optical surfaces from condensation, contamination or other degrading effects. During such purging the sample compartment is often contaminated by gas or moisture leaks. It is imperative to maintain the sample compartment of an analytical instrument, particularly a sensitive analytical instrument, as clean as possible.
It is known in the art and, in particular, in the analytical instrument field, to seal the ports to the sample compartment during the period of time that the optical compartment is opened or undergoing a purging. This can be accomplished by many mechanisms, such as, for example, sealing the port with tape or with a sponge-like material. However, such techniques provide either insufficient seals or contaminate the sample compartment in and by themselves.
One analytical instrument which is extremely sensitive to the type of problem discussed above is a Fourier Transform Infrared (FT/IR) spectrophotometer. In such an instrument the sample compartment is isolated from the remainder of the instrument except for two ports through which the light beam passes through the sample. Because of the high sensitivity of such a spectrophotometer the cleanliness of the sample compartment is crucially important. To date, conventional techniques used to seal the beam path openings on either side of a sample compartment generally suffer from such difficulties as, for example, short lifetime, failure to seal sufficiently, or the like.
SUMMARY OF THE INVENTION
Accordingly, it is one object of the present invention to provide a shutter mechanism which can open and sealingly close a port in a reliable repeatable manner.
This object is achieved, at least in part, by a shutter mechanism the sealing face of which is displaceable in two different planes and which is adapted so that simultaneous movement in both planes is excluded.
Other objects and advantages will become apparent to those skilled in the art from the following detailed description read in conjunction with the appended claims and the drawing attached hereto.
BRIEF DESCRIPTION OF THE DRAWING
The drawing, not drawn to scale, includes:
FIG. 1 which is a plan view of a shutter mechanism, embodying the principles of the present invention, in a fully opened position;
FIG. 2 which is a plan view of the shutter mechanism shown in FIG. 1 but wherein the shutter is at an intermediate sealing position;
FIG. 3 which is a cross-sectional view of the shutter mechanism shown in FIG. 2 taken along the line 3--3 thereof;
FIGS. 4A-4C are front, side and top views of one element (24) in the shutter mechanism shown in FIG. 1;
FIGS. 5A-5C are front, top and side views of another element (22) of the shutter mechanisms shown in FIG. 1; and
FIG. 6 is a detailed view of a portion of the shutter arm (18) shown in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
A shutter mechanism, generally indicated at 10 in the drawing and embodying the principles of the present invention, includes a shutter plate 12 having an annulus 14 of resilient sealing material affixed to one face 16 thereof (FIG. 3). The opposite face 20 of plate 12 is affixed to one end 40 of a shutter arm 18 by means of a universal joint as hereinafter described. The shutter mechanism 10 also includes a shutter arm carrier plate 22 to which the shutter arm 18 is pivotably affixed, as at 19 a manner also hereinafter described. Further included in mechanism 10 is a shutter control member 24 rotatable between a first position 26 (FIG. 1), whereat a port 28 through a wall 30, e.g., a sample compartment wall, is fully opened, and a second position 32 (FIG. 2), whearat the port 28 is sealed by the shutter plate 12. The mechanism 10 further includes a means 34 for interlocking the shutter arm carrier plate 22 with the shutter control member 24 only during a first portion of the distance rotated between the first position and the second position. In addition, the shutter mechanism 10 includes a means 36 for releasing the shutter arm carrier plate 22 from the shutter control member 24 during a second portion of the distance rotated between the first position and the second position. Still further, the shutter mechanism 10 includes means 38 for pivoting the shutter arm 18 only during the second portion of the total distance rotated between the first position and the second position.
In one preferred embodiment, the mechanism 10 is located within the optical compartment of a Fourier Transform Infrared (FT/IR) spectrophotometer adjacent the sample compartment wall 30. A number of ports 28, only one of which is shown in FIG. 1, through the wall 30 are about 40 mm in diameter and are situated to allow the incident IR radiation beam to enter and exit the sample compartment.
The shutter plate 12, in one embodiment, has an outside diameter of about 5 centimeters, and the annulus 14 of sealing material, e.g., plastic foam, is affixed to the face 16 thereof, has a thickness of about 0.3 centimeters and an outside radius of about 2.5 centimeters. The shutter plate 12 is connected to one end 40 of the shutter arm 18 by means of, for example, a ball and socket joint which allows uniform pressure to be applied against the wall 30 by the shutter plate 12 when in the closed position.
The shutter arm 18 is pivotably secured to the shutter arm carrier plate 22. As best appears in FIG. 5A, shutter arm carrier plate 22 is generally formed in the shape of a circular sector and includes a tab 42, preferably rectangular, extending from the sector arc 44 away from the pivot point. The shutter arm 18 is secured between a pair of pins 46 about which it can rotate, which pins are affixed to a pair of blocks 48 protruding from the tab 42. Referring to FIG. 6, the other end 50 of the arm 18, in the preferred embodiment, carries a roller bearing 52 which is in the shape of a cone segment. The bearing 52 rotates in an opening 54 in end 50 of the arm 18 and protrudes slightly therefrom. As more fully discussed below, the bearing 52 acts in conjunction with a ramp 56 protruding from the shutter control member 24 to cause end 40 of the shutter arm 18 to pivot toward the wall 30.
The shutter arm carrier plate 22, shown in FIGS. 5A through 5C, is rotatably affixed to the sample compartment wall 30. In the preferred embodiment, the shutter arm carrier plate 22 is a sector having an included angle of 70 degrees and bounded by radii of about 6 centimeters. The shutter arm carrier plate 22 rotates about a point 58 which is located along a radius bisecting the included angle. The sector arc 44 includes a first portion 60 of about 45 degrees and a second portion 62 of about 25 degrees. The first portion 60 is bounded by radii of about 6 centimeters and the second portion 62 is bounded by radii of about 5 centimeters. The first portion 60 and the second portion 62 interface near the arc periphery to form a first notch 64. The first portion 60 of the carrier plate 22 includes a protruding rim 66 along the arc thereof which rim 66 includes a gap 68 therein. In the preferred embodiment, the protruding rim 66 includes a rim extension 70 extending along the sector boundary radius downwardly away from the arc 44. Preferably, the rim extension 70 extends along the radius a distance of about 1 centimeter. As more fully discussed below, the rim extension 70 serves as part of the means 34 for interlocking the shutter arm carrier plate 22 and the shutter control member 24.
The shutter control member 24, shown in FIGS. 4A through 4C, is rotatably affixed to the sample compartment wall 30 and spaced apart therefrom by the shutter carrier plate 22. Preferably, the shutter control member 24 is also a sector having an included angle of about 30 degrees and bounded by radial edges 74 of about 5.5 centimeters in length. The shutter control member 24 rotates about point 58 on a radius bisecting the included angle. In the preferred embodiment, the shutter control member 24 and the shutter arm carrier plate 22 rotate about a common axis at point 58. The shutter control member 24 has a first surface 76 proximate the wall 30 and an opposing surface 78 generally parallel to and spaced apart from the first surface 76. Preferably, the shutter control member 24 is about 1 centimeter thick. Surface 76 includes an indentation 80 therein which extends into the first surface 76 to a depth of about 0.3 centimeters and arcuately extends from one edge 82 of the member 24 about 14 degrees. The indentation 80, forming a segment 81 of the sector, uniformly extends away from the sector arc 74 about 0.25 centimeters to provide a release track 84. The member 24 further includes the shutter arm engaging ramp 56 protruding from the second face 78 thereof. The ramp 56 extends about 15 degrees arcuately and rises from a zero depth at one end 86 to a thickness of about 0.4 centimeters at the other end 88. Preferably, the other end 88 of the ramp 56 co-terminates with the radius of the sector distal the indentation 80.
For reasons more fully explained below, a retainer plate 90 is provided and affixed to the wall 30. The retainer plate 90 is affixed such that the tab 42 of the shutter arm carrier plate 22 extends above the outer peripheral edge 92 thereof. Additionally, sufficient clearance is provided to allow the carrier plate 22 to rotate. The retainer plate 90 includes an arcuate track 94 which is substantially uniformly spaced apart from the protruding rim 66 of the shutter carrier plate 22. The track 94 includes an interlocking means receiving notch 96 therein having an arcuate length of about 15 degrees and a depth of about 0.2 centimeters. The track 94 includes a downwardly protruding stop 98 at one end thereof proximate the notch 96. In one embodiment, the retainer plate 90 includes an overhanging lip 100, which is, for clarity, shown in cutaway only in FIG. 2, and which, for reasons more fully explained below, overhangs the shutter control member 24.
All the components of the mechanism 10 can be formed using the conventional manufacturing techniques. Preferably the parts hereof are formed 40% carbon fiber filled polyphenelene sulfide except for the conical bearing 52 which is preferably formed from acetal.
In operation, a disk 102, having a diameter on the order of about 0.65 centimeters and a thickness on the order of about 0.3 centimeters, effectively constitutes the interlocking means 34. The disk 102 is positioned in the notch 64 in the shutter control member 24 and projects into the gap 68 in the protruding rim 66 of the sample carrier plate 22 during the rotation of the shutter control member 24 through the first portion of the complete distance of its travel. The shutter control member 24 is affixed to a movable arm 104 which causes it to rotate about its pivot point 58. In the preferred embodiment, the moveable arm 104 is controlled by a pneumatic piston although other forms of movement such as a reciprocating motor or the like could also be used.
As shown in FIG. 1, which represents the shutter mechanism 10 being in the fully opened position, the disk 102 is retained between the indentation 80 in the shutter control member 24 and in the gap 68 of the shutter carrier plate 22. Thus, when the control member 24 is urged to rotate by the moving arm 104, the shutter carrier plate 22 is carried therewith. The member 24 and the plate 22 remain interlocked until the notch 96 in the retainer plate 90 is reached whereupon the downwardly protruding edge 98 of the retainer plate 90 stops any further rotation of the shutter carrier member 22. The disk 102 is, at that point in time, aligned with the notch 96 extending into the retainer plate 90 and is pushed thereinto by the continued rotation of the shutter control member 24. As a consequence, the control member 24 is allowed to continue its rotation whereas the shutter carrier member 22 is retained in position. Simultaneously with the singular continued motion of the shutter control member 24, the conical bearing 52 of the shutter arm 18 contacts the ramp 56 protruding from the second surface 78 of the control member 24 and, as the rotation continues, pivots the shutter plate 12 toward the port 28. As a consequence, when the control member 24 is in its second position, i.e., the fully closed position, the conical bearing 52 is at approximately the maximum height of the ramp 56 thereby providing maximum force to the shutter plate 12 against the wall 30 about the port 28.
As shown in FIG. 2, during the second portion of the rotation of the control member 24, the disk 102 is secured in the notch 96 of the retainer plate 90 by the outer peripheral arc 74 of the control member 24.
When the port 28 is to be opened, the control member 24 is rotated clockwise to thereby remove the ramp 56 from underneath the conical bearing 52 and allow the shutter plate 12 to move away from the port 28. At this stage, i.e. once the conical bearing 52 is released from the ramp 56, the disk 102 moves through the gap 68 of the protruding rim 66 carrier plate 22 into the indentation 80 of the control member 24. Simultaneously, the control member 24 contacts the rim extension 70 protruding downwardly along the radius of the carrier plate 22 and causes the carrier plate 22 to rotate with the control member 24.
The present invention has been described herein by means of a specific exemplary embodiment. Other configurations and arrangements may be made by persons skilled in the art without departing from the spirit and scope of the present invention which is considered defined only by the appended claims and the reasonable interpretation thereof.
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A shutter mechanism which includes simultaneous translation of a shutter in two planes of motion prolongs the life of the sealing material of the shutter as well as ensures that, when open, an optical beam passes through a sample compartment without interference or disruption. A further advantage of such a mechanism lies in the positive sealing of a port with sufficient pressure applied via the shutter plate to prevent vapor or fluid communication across the port.
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BACKGROUND OF THE INVENTION
This invention provides novel compositions and methods for the inducement of cytokines production in humans.
In U.S. Pat. No. 4,761,490, the applicants disclosed that certain tellurium derivatives will induce the production of cytokines such as lymphokines.
The known types of lymphokines include, in addition to Interleukin-2 (IL-2), B-cell factors, Macrophage activation factor (MAF), Interleukin-3 (IL-3), Colony Stimulating Factor (CSF), Tumor Necrosis Factor and other factors produced by monocytes such as Interleukin-1 (IL-1) and Gamma Interferon. All of these factors are elaborated by white blood cells and are collectively known as cytokines.
The present invention is based on the discovery that tetravalent tellurium halides are capable of stimulating the production of cytokines when they are administered to a human. This discovery makes possible a novel chemotherapeutic approach to the treatment of immune deficiencies, autoimmune diseases and infectious diseases using the tetravalent tellurium halides as adjuvants or as primary therapeutic agents.
Accordingly, it is an object of this invention to provide a novel method for producing in vitro cytokines such as lymphokines.
It is also an object of this invention to provide a novel method for producing in vivo cytokines such as lymphokines.
It is also an object of this invention to provide novel methods for the treatment of immune deficiencies, autoimmune disease and infectious diseases.
These and other objects of the invention will become apparent from a review of the specification.
SUMMARY OF THE INVENTION
The novel compositions of the invention comprise a tellurium tetravalent halide and a pharmaceutically acceptable carrier. The tetravalent tellurium tetrahalides include tellurium tetrachloride, tellurium tetrabromide, tellurium tetraiodide and tellurium tetrafluoride.
The compositions of the invention may be administered to mammals for treatment of immune deficiencies, autoimmune diseases and infectious diseases using amounts of the composition that are effective in each condition. The treatment will alleviate the symptoms of these diseases by causing the mammalian body to produce increased amounts of lymphokines. The invention also contemplates the in vitro production of increased amounts of cytokines such as lymphokines and or their receptors and the use of these materials as therapeutic agents to be administered to mammals for the alleviation of cancer, immune deficiencies and infectious diseases. It is contemplated that the composition of the invention may be administered in combination with other anti-cancer chemotherapeutic agents such as AZT cyclophosphamide, methotrexate, interferon, 5-fluorouracil and the like.
The term is used to include leukemia and solid tumors that arise spontaneously or in response to a carcinogenic agent, by irradiation or by oncoviruses. These conditions are well known to those who are skilled in the art and include such conditions as adrenal tumors, bone tumors, gastrointestinal tumors, brain tumors, skin tumors, lung tumors, ovarian tumors, genitourinary tumors and the like. The Merck Manual 13th Edition, Merck & Co. (1977) describes many of these conditions. Pages 647-650; 828-831; 917-920; 966; 970-974; 1273; 1277; 1371-1376; 1436-1441; 1563; 1612-1615 of that publication are incorporated herein by reference.
The term immunodeficiency diseases is used to describe a diverse group of conditions such as Acquired Immunodeficiency Syndrome (AIDS) characterized chiefly by an increased susceptibility to various infections with consequent severe acute, recurrent and chronic disease which result from one or more defects in the specific or nonspecific immune systems. Pages 205-2330 of the Merck Manual 13th Edition describe these conditions and they are incorporated herein by reference.
The term autoimmune diseases includes disorders in which the immune system produces autoantibodies to an endogenous antigen, with consequent injury to tissues. Pages 241-243 of the Merck Manual 13th Edition describe these conditions and they are incorporated herein by reference.
The term infectious diseases includes those pathologic conditions that arise from bacterial, viral or fungus organisms that invade and disrupt the normal function of the mammalian body. Pages 3-147 of the Merck Manual 13th Edition describe these conditions and they are incorporated herein by reference.
The compositions may be administered orally, parenterally, transcutaneously, topically or by contacting mucous membranes. The compositions may be administered orally with or without a carrier although if oral administration is employed, the composition may be administered in capsules or tablets using conventional excipients, binders, disintegrating agents and the like. The parenteral route is presently preferred and compositions may be prepared by dissolving the compound in a suitable solvent such as water, aqueous buffer, glycerol or PBS. The parenteral route may include the intramuscular, intravenous, intradermal using a sustained release carrier and subcutaneous route. The concentration of the compositions in the pharmaceutical carrier is not critical and is a matter of choice. Remingtons Practice of Pharmacy, 9th, 10th and 11th Ed. describe various pharmaceutical carriers and is incorporated herein by reference.
It is believed that the tellurium tetrahalides will decompose in water to form various tellurium derivatives. For this reason when solutions employed, it is preferred to use freshly prepared solutions although solutions which are not freshly prepared will be biologically active.
The dosage of the compositions used to stimulate lymphokine production or treat a specific disease condition described herein may be varied depending on the particular disease and the stage of the disease. Generally, an amount of the compound may be administered which will range from 0.01×10 -3 to 1×10 -3 g/Kg of body weight and preferably from 0.02×10 -3 to 0.5×10 -3 g/Kg of body weight. For example a dosage of about 2-8 mg. preferably every other day for a 75 Kg. mammal is contemplated as a sufficient amount to induce the production of lymphokines but the dosage may be adjusted according to the individual response and the particular condition that is being treated. For the treatment of AIDS about 1.0-9.0 mg/m 2 may be given three times a week. In addition, the compound may be given concomitantly with other anti-AIDS agents such as 9-(1,3-dihydroxy-2-propoxymethyl) guanine (DHPG); and/or AZT. These agents may be administered at conventional dosages which are known to those who are skilled in the art.
In addition to the treatment of the mammalian disorders described hereinabove, the compounds may be utilized for veterinary purposes in the treatment of viral and immune diseases that afflict horses, ungulates and fowl as well as other species. These disorders may be treated using the dosages set forth hereinabove for the treatment of mammalian disorders.
For in vitro use, cells may be stimulated to produce lymphokines by use of 1×10 -8 to 1×10 -4 , preferably 1×10 -7 to 1×10 -5 g of compound per about 10 6 cell/ml. Plant bacterial infectious such as crown gall may be treated by the application of a solution containing an effective amount of the composition of the invention, preferably containing about 0.1% of the active component.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following examples are given to illustrate the invention and it is understood that it does not limit the scope of the invention.
EXAMPLE 1
The compound tellurium tetrachloride was tested for its effect on the proliferation of splenocytes in vitro. Spleen cells were obtained from male Balb-C mice 6-8 weeks of age. The spleens were removed and the spleen cells were pushed through stainless steel 60 mesh nets (United States standard) resting in 5 mm Petri dishes containing PBS in order to separate the cells. The cells were then collected into centrifuge tubes and spun at 1000 rpm for 10 minutes. The supernatant was discarded and cells were treated with 5 ml of hypotonic buffer (0.15M NH 4 Cl; 0.01M KHCO 3 dissolved in double distilled water, pH 7.2) for exactly two minutes. Thereafter, PBS was added to the cells and the test tubes were centrifuged for 10 minutes at 1000 rpm. The cells were rinsed twice and counted in a heamocytometer using trytan blue to test for viability. The cells were brought to a concentration of 10 6 viable cells/ml using enriched RPMI with 10% fetal calf serum. The cells were placed in a 96 well culture plate (0.1 ml cells) containing the stated amounts of tellurium tetrachloride and Control to which was added 20 ng/ml PMA (Phorbol Myristic Acetate). The cells were incubated for 48 hours, labelled for an additional 24 hours with 1 u Ci/well of 3 H-thymidine and harvested. The results are set forth in Table I.
TABLE 1______________________________________ TeCl.sub.4 Control*μg/ml CPM______________________________________5 1,093 2922.5 267 3271.25 280 1,4570.6 447 4,1870.3 5,597 56,1950.1 73,475 66,4550.07 45,342 38,1420.03 -- 13,573PMA alone - 18,796 PBS alone - 1800______________________________________ *ammonium trichloro(dioxoethylene0,0')tellurate
These results show that TeCl 4 is capable of inducing the proliferation of mouse spleen cells in vitro.
EXAMPLE 2
Tellurium tetrachloride was tested for its effect on proliferation of human MNC in vitro. MNC were obtained by layering buffy coats from normal human donors on a Ficoll-Hypaque gradient. Cells were rinsed, brought to a concentration of 10 6 cells/ml, divided into wells of a 96 well culture plate and incubated for 72 hours with varying concentrations of TeCl 4 or Control. Plates were labelled for an additional 24 hours with 3 -H-thymidine and harvested. The results are set forth in Table II.
TABLE II______________________________________ TeCl.sub.4 Control*μg/ml CPM______________________________________2.5 1,027 2751 -- 5,0270.7 6,883 6,4070.3 8,762 8,4130.1 9,383 13,9520.07 3,843 3,3000.03 2,779 2,943PMA alone - 1,020______________________________________ *ammonium trichloro(dioxoethyle0,0')tellurate
These results show that TeCl 4 can stimulate human MNC to proliferate in vitro.
EXAMPLE 3
Tellurium Tetrachloride (TeCl 4 ) and Control were tested for their effect on IL-2 production from mouse spleen cells in vitro. Spleen cells were obtained as described in Example 1. The cells were brought to a concentration of 5×10 6 /ml using enriched RPMI with 10% fetal calf serum. Cells were placed in a 24 well culture plate containing the stated amount of tellurium tetrachloride or the Control, to which was added 20 ng/ml PMA (Phorbol Myristic Acetate). Cultures were incubated for 24 hours at 37° C. Supernatants were collected and tested for IL-2 content. The results are presented in Table IIIa (50% Supernatant) and Table IIIb (25% Supernatant).
TABLE IIIa______________________________________(50% Supernatant) TeCl.sub.4 Control*μg/ml CPM______________________________________5 160 6,1151 743 6,1250.5 19,746 43,0530.1 49,995 13,413PMA alone - 4,993 PBS alone - 1,200______________________________________
TABLE IIIb______________________________________(25% Supernatant) TeCl.sub.4 Control*μg/ml CPM______________________________________5 1,229 2,9021 4,273 24,9120.5 16,422 51,5670.1 27,680 28,877PMA alone - 4,993 PBS alone - 1,200______________________________________ *ammonium trichloro(dioxoethylene0,0')tellurate
These results show that TeCl 4 is capable of inducing the production of IL-2 in vitro.
______________________________________PBS contains:______________________________________NaCl 8.0 gKCl 200 mgNa.sub.2 HPO.sub.4 1150 mgKH.sub.2 PO.sub.4 200 mgCaCl.sub.2 (anhyd.) 100 mgMg Cl.sub.2 6H.sub.2 O 100 mg/LH.sub.2 O sufficient to make 1 liter______________________________________
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The present invention provides a method for the stimulation of the production of lymphokines which comprises the administration of an effective amount of a tellurium tetrahalide.
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