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RELATED APPLICATIONS
[0001] This application is a divisional of prior U.S. patent application Ser. No. 11/131,847 filed May 18, 2005, and claims the benefit of and priority to U.S. patent application Ser. No. 11/131,847 which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] This invention relates to vehicle recovery systems and, in particular, a vehicle locating unit of such a system with improved power management techniques.
BACKGROUND OF THE INVENTION
[0003] The applicant's successful and popular vehicle recovery system sold under the trademark LoJack® includes a small electronic vehicle locating unit (VLU) with a transponder hidden within a vehicle, a private network of communication towers each with a remote transmitting unit (RTU), one or more law enforcement vehicles equipped with a vehicle tracking unit (VTU), and a network center with a database of customers who have purchased a VLU. The network center interfaces with the National Criminal Information Center. The entries of that database comprise the VIN number of the customer's vehicle and an identification code assigned to the customer's VLU.
[0004] When a LoJack® product customer reports that her vehicle has been stolen, the VIN number of the vehicle is reported to a law enforcement center for entry into a database of stolen vehicles. The network center includes software that interfaces with the database of the law enforcement center to compare the VIN number of the stolen vehicle with the database of the network center which includes VIN numbers corresponding to VLU identification codes. When there is a match between a VIN number of a stolen vehicle and a VLU identification code, as would be the case when the stolen vehicle is equipped with a VLU, and when the center has acknowledged the vehicle has been stolen, the network center communicates with the RTUs of the various communication towers (currently there are 130 nationwide) and each tower transmits a message to activate the transponder of the particular VLU bearing the identification code.
[0005] The transponder of the VLU in the stolen vehicle is thus activated and begins transmitting the unique VLU identification code. The VTU of any law enforcement vehicles proximate the stolen vehicle receive this VLU transponder code and, based on signal strength and directional information, the appropriate law enforcement vehicle can take active steps to recover the stolen vehicle. See, for example, U.S. Pat. Nos. 4,177,466; 4,818,988; 4,908,609; 5,704,008; 5,917,423; 6,229,988; 6,522,698; and 6,665,613 all incorporated herein by this reference.
[0006] Since the VLU unit is powered by the vehicle's battery, power management techniques must be employed in the VLU to ensure the VLU does not drain the vehicle's battery. One prior technique employed by the applicant includes programming the VLU to “wake up” and check for messages from the communication towers only periodically, e.g., every 8 seconds for 0.2 seconds. The timing of the sleep and wake-up modes was synchronized to the transmission schedule of one communication tower. See U.S. Pat. No. 6,229,988.
[0007] But, if the vehicle equipped with the VLU so programmed moves out of the transmission range of that tower, when the VLU wakes up, no signal will be received from that tower. According to prior methods, the VLU must wake up for a longer time in order to be sure to receive a tower transmission since the VLU has no memory of which time slot the tower is likely to transmit. This results in increased power consumption.
BRIEF SUMMARY OF THE INVENTION
[0008] It is therefore an object of this invention to provide a vehicle locating unit with improved power management technique.
[0009] It is a further object of this invention to provide such a vehicle locating unit whose wake-up and sleep modes are synchronized to the communication source transmitting the strongest signal.
[0010] It is a further object of this invention to provide such a vehicle locating unit which continuously updates its memory to store the identity of one or more communication towers with the strongest signals.
[0011] The subject invention results from the realization that a more effective power management subsystem for a VLU is configured to alternately enter sleep and wake-up modes, to synchronize the wake-up mode to the communication source (e.g., tower) transmitting the strongest signal, and to test the signal strength of at least one additional communication source in sequence.
[0012] The subject invention, however, in other embodiments, need not achieve all these objectives and the claims hereof should not be limited to structures or methods capable of achieving these objectives.
[0013] The subject invention features a vehicle locating unit with improved power management. A receiver receives a signal from a network of communication sources and a signal strength monitoring subsystem determines which of the communication sources are transmitting the strongest signals. The power management subsystem is responsive to the signal strength monitoring subsystem and is configured to: alternatively enter sleep and wake-up modes, synchronize the wake-up mode to the communication source transmitting the strongest signal, and test the signal strength of at least one additional communication source according to a predefined sequence.
[0014] Typically, the power management subsystem is configured to test and store the identity of two communication sources with the two strongest signals, switch to synchronization with any communication source having a signal stronger than the strongest signal of the two stored communication sources, and store the identity of any communication source with a signal stronger than the signal of any previously stored communication source.
[0015] In one embodiment, there are n (e.g., eight) communication sources each transmitting a signal at a different time every n seconds. Preferably, the power management system is configured to include a start-up mode wherein all communication sources are tested. In one preferred embodiment, the power management subsystem is implemented in a microcontroller which is configured to power down the receiver during the sleep mode and to power up the receiver during the wake-up mode. One example of a signal strength monitoring subsystem includes a demodulation circuit embodied in a transceiver.
[0016] A method of checking messages from a network of communication sources in accordance with this invention includes initially testing the signal strength of a plurality of communication sources, storing the identity of the communication sources with the two strongest signals, alternatively entering a sleep mode and a wake-up mode, the wake-up mode synchronized to the communication source with the strongest signal, testing the signal strength of one additional communication source, switching synchronization to the additional communication source if said source presents a signal stronger than the signal of the stored communication source with the strongest signal, and replacing the identity of any stored communication source if an additional communication source tested in sequence presents a signal stronger than the signal of said stored communication source.
[0017] For VLUs and other electronic receivers which receive a signal from a network of communication sources, a signal strength monitoring subsystem determines which of the communication sources are transmitting the strongest signals. A power management subsystem is responsive to the signal strength monitoring subsystem and is configured to: alternatively enter sleep and wake-up modes, synchronize the wake-up mode to the communication source transmitting the strongest signal, and test the signal strength of at least one additional communication source to ensure the wake-up mode is synchronized to the communication source transmitting the strongest signal.
[0018] One embodiment features a vehicle locating unit power management system comprising a memory, and a controller configured to alternatively output sleep and wake-up mode signals, store in said memory the identity of at least a first communication source presenting the strongest signal, test the signal strength of at least one different communication source during the wake-up mode, synchronize the wake-up mode to the communication source identified in said memory, and update the memory to store the identity of a different communication source presenting a signal stronger than the first communication source.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0019] Other objects, features and advantages will occur to those skilled in the art from the following description of a preferred embodiment and the accompanying drawings, in which:
[0020] FIG. 1 is a schematic block diagram showing the primary components associated with a vehicle recovery system in accordance with the subject invention;
[0021] FIG. 2 is a block diagram showing the primary components associated with a vehicle locating unit in accordance with the subject invention;
[0022] FIG. 3 is a flow chart depicting the primary steps associated with one example of the programming of the microcontroller of the vehicle locating unit shown in FIG. 2 as it relates to power management; and
[0023] FIG. 4 is a schematic timing diagram showing a time slot synchronization pattern for an example of a communication network including eight communication towers.
DETAILED DESCRIPTION OF THE INVENTION
[0024] Aside from the preferred embodiment or embodiments disclosed below, this invention is capable of other embodiments and of being practiced or being carried out in various ways. Thus, it is to be understood that the invention is not limited in its application to the details of construction and the arrangements of components set forth in the following description or illustrated in the drawings. If only one embodiment is described herein, the claims hereof are not to be limited to that embodiment. Moreover, the claims hereof are not to be read restrictively unless there is clear and convincing evidence manifesting a certain exclusion, restriction, or disclaimer.
[0025] As discussed in the background section above, the applicant's successful and popular vehicle recovery system sold under the trademark LoJack® includes a small electronic vehicle locating unit (VLU) 10 , FIG. 1 , with a transponder 12 hidden within a vehicle 14 , a private network of communication towers 16 each with a remote transmitting unit (RTU) 18 , one or more law enforcement vehicles 20 equipped with a vehicle tracking unit (VTU) 22 , and network center 24 .
[0026] When a LoJack® product customer reports that her vehicle has been stolen, the VIN number of the vehicle is reported to law enforcement center 26 for entry into database 28 of stolen vehicles. Network center 24 includes software that interfaces with database 28 of law enforcement center 26 to compare the VIN number of the stolen vehicle with database 30 of network center 24 which includes VIN numbers corresponding to VLU identification codes. When there is a match between a VIN number of a stolen vehicle and a VLU identification code, as would be the case when stolen vehicle 14 is equipped with VLU 10 , network center 24 communicates with the RTUs 18 of the various communication towers 16 and each tower transmits a message to activate transponder 12 of VLU 10 bearing the particular identification code.
[0027] Transponder 12 of VLU 10 in stolen vehicle 14 , once activated, begins transmitting a unique VLU identification code. VTU 22 of law enforcement vehicle 20 proximate stolen vehicle 14 receives this VLU transponder code and, based on signal strength and directional information, the appropriate law enforcement vehicle can take active steps to recover stolen vehicle 14 .
[0028] VLU 10 ′, FIG. 2 , in accordance with the subject invention includes transceiver 40 or, in another example, a receiver without transmission capabilities. Signal strength monitoring subsystem 42 , in one embodiment, is a demodulator circuit on a chip within transceiver 40 and outputs a signal identifying and characterizing the signal strength of all signals received by transceiver 40 via antenna 44 from the communication network and one or more communication towers 16 , FIG. 1 .
[0029] Microcontroller 46 , FIG. 2 , (e.g., a Texas Instrument microcontroller model No. MSP430) receives the output of subsystem 42 , is programmed to evaluate the signal strength of all signals received by transceiver 40 , and is also programmed to alternatively cause transceiver 40 to enter sleep and wake-up modes to save battery power by outputting a signal to power supply unit circuitry 48 in accordance with the flow-chart of FIG. 3 . Memory 47 , FIG. 2 , is shown separate from controller 47 but many microcontrollers, as is known by those skilled in the art, have internal memories including the controller example above.
[0030] In the following example, there are eight communication sources or LoJack® towers A-H, FIG. 4 , transmitting signals to VLU 10 ′, FIG. 2 . Each transmits a synchronization signal at a different time t 0 -t 7 each eight seconds and possibly a message (in the case of a reportedly stolen vehicle) in which instance microcontroller 46 , FIG. 2 would activate transponder 12 .
[0031] But, transceiver 40 , if continuously left on to check for such a message, would more quickly drain the battery of the vehicle. According to the subject invention, microcontroller 46 at start-up, step 60 , FIG. 3 , tests the signal strength of towers A-H by analyzing the output of signal strength monitoring subsystem 42 . In this test mode, the signal strength of each tower is noted and if any signal carries a message, the message is acted upon.
[0032] The identity of the two strongest tower signals is stored in memory 47 , FIG. 2 , step 62 , FIG. 3 , and the wake-up mode is then synchronized, step 64 , to the strongest of these two signals. Next, the sleep mode is entered and when the wake-up mode is activated in synchronization with the communication tower presenting the strongest signal, the signal strength of the two previously stored towers is tested as is the signal strength of one additional communication tower, in sequence.
[0033] As an example, suppose towers A and B, FIG. 4 , are transmitting the strongest signals by virtue of their proximity to VLU 10 , FIG. 2 . If tower A's signal is assumed to be stronger than tower B's signal, the wake-up mode synchronization is in accordance with tower A's signal. Thus, in each cycle, (typical wake up times are 8 sec. apart), controller 46 would power up transceiver 40 by signaling power supply unit circuit 48 at time t 0 , FIG. 4 , and sleep between times t 1 -t 7 , steps 66 - 68 . At the next wake-up time, the signal strength of the two previously stored towers (A and B) is tested for strength as is the signal strength of the next tower according to a predefined sequence which, in this example, is tower C, step 70 . In this way, if at any time due to movement of the vehicle a different tower in the sequence A-H presents a stronger signal than a) the tower upon which controller 46 synchronizes the wake-up mode or b) the stored identity of the tower with the second strongest signal, the identity of the new tower is stored in memory 47 , FIG. 2 , steps 72 - 74 , FIG. 3 , and synchronization to the tower with the strongest signal is ensured at step 64 .
[0034] Suppose, however, that tower C does not present a stronger signal than either towers A or B and that the wake up and sleep modes are still synchronized to tower A in step 66 . At steps 68 and 70 towers A, B, and now D are tested and if tower D's signal strength is not stronger than either tower A or B and once again the sleep mode is entered, step 66 . Upon entering the wake-up mode at step 68 , still synchronized to tower A, the signal strength of towers A, B, and now E is checked, step 70 .
[0035] Now, if the signal strength of tower E is stronger than the signal strength of tower B, but not tower A, the identity of tower E is stored in memory 47 , FIG. 2 at step 74 , FIG. 3 , replacing tower B. But at step 64 the wake-up mode is still synchronized to the strongest tower, namely tower A at steps 64 - 68 .
[0036] So, next, the signal strengths of towers A, E, and F are tested, step 70 ; and suppose at step 72 the signal strength of tower F is stronger than tower A and E but tower A is still stronger than tower E. Now, synchronization will be according to tower F at step 64 and at step 70 , towers F, A, and G are tested, and so on.
[0037] In another example, imagine towers C and D initially present the strongest first and second signals to the VLU. The wake up mode is initially synchronized to tower C and the identity of towers C and D are stored in memory. After the first sleep mode, the signal strength of towers C, D, and E are tested, and next towers C, D, and F, and then towers C, D, and G, and then towers C, D, and H, and so on—one additional tower during each subsequent wake-up mode. If during this wake-up/sleep mode cycle, towers C and D remain the strongest two towers, synchronization remains with tower C and the memory continues to store the identity of towers C and D. If during the next cycle, when tower A is tested and is found to present a signal stronger than tower D but not C, the memory is updated to store the identity of towers C and A, synchronization continues according to tower C's transmission schedule, and during each subsequent wake-up mode the signal strength of towers C, A, and B; C, A, and D; C, A, and E; C, A, and F . . . and so on is tested.
[0038] In this way, the identity of the towers which transmit the two strongest signals is always stored and controller 46 , FIG. 2 in sequence checks another tower in the wake-up mode to maintain in storage 47 , FIG. 2 , the identity of the two towers emitting the strongest signals. Also, controller 46 ensures the wake-up mode is synchronized to only the tower emitting the strongest signal. Power is conserved but now in a way which ensures no communication message from any tower in the network is missed. To enter the sleep mode, microcontroller 46 sends a signal to power supply unit 48 which then powers down transceiver 40 . To enter the wake-up mode, microcontroller 46 sends a signal to power supply unit 48 which then again provides power to transceiver 40 so that it can receive signals via antenna 44 .
[0039] The example presented above in reference to FIGS. 3-4 assumes eight towers in a given region, continuous storage of the two strongest tower signals, and testing of an additional tower in a specific sequence, but this is an example only and not a limitation of the subject invention: any number and combination of towers and storage of tower combinations can be used. The example above also assumes that the power management method of the subject invention applies to a VLU of a vehicle recovery system but the invention hereof may find applicability to battery powered electronic devices other than VLUs.
[0040] Thus, although specific features of the invention are shown in some drawings and not in others, this is for convenience only as each feature may be combined with any or all of the other features in accordance with the invention. Moreover, the words “including”, “comprising”, “having”, and “with” as used herein are to be interpreted broadly and comprehensively and are not limited to any physical interconnection. Also, any embodiments disclosed in the subject application are not to be taken as the only possible embodiments. Other embodiments will occur to those skilled in the art and are within the following claims.
[0041] In addition, any amendment presented during the prosecution of the patent application for this patent is not a disclaimer of any claim element presented in the application as filed: those skilled in the art cannot reasonably be expected to draft a claim that would literally encompass all possible equivalents, many equivalents will be unforeseeable at the time of the amendment and are beyond a fair interpretation of what is to be surrendered (if anything), the rationale underlying the amendment may bear no more than a tangential relation to many equivalents, and/or there are many other reasons the applicant can not be expected to describe certain insubstantial substitutes for any claim element amended.
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A method of checking messages from a network of communication sources includes initially testing the signal strength of a plurality of communication sources, storing the identity of the communication sources with the two strongest signals, and alternatively entering a sleep mode and a wake-up mode, the wake-up mode synchronized to the communication source with the strongest signal. The method further includes testing the signal strength of one additional communication source, switching synchronization to the additional communication source if said source presents a signal stronger than the signal of a stored communication source with the strongest signal, and replacing the identity of any stored communication source if an additional communication sources tested in sequence presents a signal stronger than the signal of said stored communication source.
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BACKGROUND OF THE INVENTION
This invention relates to tire bead seating and inflating apparatus.
As is well-known, before tubeless tires can be inflated, it is necessary to set their beads against the wheel rim on which they are mounted to preclude air introduced into the tire through the valve from escaping between the bead and the rim. Over the years, a variety of devices for accomplishing the bead seating requirement have evolved. For example, various hoop-like devices have been employed for peripherally engaging the tire tread and forcing the same inwardly to cause the beads to seat. Such devices, while suitable for their intended purpose in most instances, are not susceptible to easy use with weak-walled tires such as radial ply tires. Moreover, they require manual placement and orientation about the periphery of the tire tread.
In attempts to improve on such prior art structures, collar-like sealing devices adapted to establish a seal between one sidewall of a tire and the edge of the corresponding rim were developed. Such structures are shown, for example, in U.S. Pat. No. 2,874,760 to Bishop and U.S. Pat. No. 2,874,761 to Varvaro. Such devices also work well for their intended purpose but are susceptible to difficulties in use either because of the fact that the collar must be manually placed as is the case with the Varvaro device or, the apparatus mounting the collar as disclosed by Biship is, for all intents and purposes, susceptible only to use as a bead seating and inflating device and cannot be used for other tire servicing purposes, thus requiring extensive manipulation of a wheel from one apparatus to another where more than simply bead seating and inflating is required.
Still another method of seating the beads of tires and inflating is that of creating a pressure differential across a tire sidewall. U.S. Pat. No. 3,552,469 to Corliss and U.S. Pat. No. 2,874,759 to Ranallo illustrate apparatus employing this princple but, in each instance, inflexibility of use of the apparatus or the requirement of manually locating the device prior to use is a significant drawback.
The difficulties attendant the use of the Corliss and Ranallo apparatus mentioned in the preceding paragraph have, in a large part, been overcome by the proposal of Strang et al in commonly assigned application Ser. No. 179,298, filed Sept. 10, 1971, entitled "Tire Bead Seating and Inflating Apparatus". But, even with such equipment, manual effort is required to move the bead seating and inflating apparatus to and from operative positions.
It has also been proposed that apparatus of the type disclosed by Corliss be mounted on the table of a conventional tire changing apparatus, thus eliminating any need for manual orientation of the device between operative and inoperative positions or, when a tire is to be placed on or removed from the tire changing device. However, this proposal is overly simplistic in its approach and some difficulty may be experienced with the same in terms of inflating tires on different size rims. Moreover, the same fails to contemplate peripheral equipment associated with such a bead seating and inflating device that may be of great assistance to the operator of such apparatus in maximizing the efficiency of the tire changing operation including the seating of the beads of the tire and the inflation thereof.
SUMMARY OF THE INVENTION
It is the principal object of the invention to provide a new and improved tire bead seating and inflating apparatus. More particularly, it is an object of the invention to provide such an apparatus which does not require manual manipulation during operation and which may be advantageously employed in conjunction with tire changing equipment, which operates on the pressure differential principle, is operative with a wide range of varying rim sizes, includes a variety of peripheral equipment to maximize the efficiency of the operation, and which is configured such that it may be installed on tire changing stands at a factory as original equipment or, alternatively, easily installed on existing tire changing equipment in the field as a kit.
The exemplary embodiment achieves the foregoing objects by a construction including an arcuate tube or air ring which may be mounted on the table of a conventional tire changing apparatus in a relation concentric with the usual spindle found thereon. Preferably, the tube is intended for mounting on tables of the type where at least a part of the rim receiving surface is generally frusto-conical. In such an instance, the air nozzles on the tube are directed upwardly and inwardly at an angle such that streams of air issuing therefrom will be generally parallel to corresponding portions of the frusto-conical surface whereby air will be directed at a tire in the same direction regardless of the rim size thereof.
To facilitate conversion of tire changing apparatus already in the field, the invention contemplates a housing which may be secured to such tire changing apparatus. The housing in turn mounts a surge tank which may serve as a source of air under pressure for both the air ring and an air chuck which may be affixed to a valve stem on a wheel rim received on the table of the tire changing stand. The housing may mount a pressure gauge having an indicator on the external portion of the housing as well as an air relief valve having an operator exteriorly of the housing. A pair of valves are provided with the assemblage along with means for securing the same to a tire changer and the valves are provided with a common actuator. One of the valves is interconnected between the surge tank and the air ring to control the flow of air through the nozzles of the latter. The other valve is connected between the surge tank and the air chuck to control the flow of air to the air chuck. The air relief valve and the pressure indicator are connected to a conduit extending between the valve controlling flow of air to the air chuck and the air chuck itself so that when the valve is closed, pressure in the tire may be monitored and, if necessary, the relief valve operated to selectively relieve air from the tire.
The common actuator for the two valves is arranged to be movable through three positions. A first of the positions is such that both valves are closed, while a second position is such that air will be allowed to pass to the air chuck only. The third position permits the passage of air to both the air ring and the air chuck. Thus, through a single actuator, an operator of the apparatus can easily control the same throughout the bead seating and inflating operation.
Other objects and advantages will become apparent from the following specification taken in conjunction with the accompanying drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a conventional tire changing stand having an embodiment of the invention affixed thereto;
FIG. 2 is a vertical section illustrating the arrangement of an air ring with respect to a portion of the tire changing stand table and further illustrates the relation of air jets issuing from the air ring to a variety of rims of different sizes, several shown in dotted lines;
FIG. 3 is a plan view of a portion of a kit made according to the invention with parts broken away for clarity;
FIG. 4 is a plan view of another portion of a kit made according to the invention; and
FIG. 5 is a somewhat schematic illustration of a common actuator for a pair of valves employed in one embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to FIG. 1, an examplary embodiment of the invention is shown in connection with a tire changing stand, generally designated 10, which may be of the type disclosed in Strang et al U.S. Pat. No. 3,255,800. Of course, the invention is also suited for use with a variety of other types of stands as well. As is known, such a tire changing stand 10 includes a tire changing table, generally designated 12, which will normally be formed as a heavy metal stamping and which includes portions 14 having frusto-conical configurations. That is, if the opposite portions 14 illustrated in FIG. 1 were continued about the entire periphery of the table 12, a generally frusto-conical surface would be defined thereby.
Extending upwardly from the center of the table 12 is a center post or spindle 16 which may receive the central aperture in a tire rim along with a plunger 18 which may be disposed in a lug hole in a wheel rim for purposes well known.
The assemblage further includes a lower bead breaking assembly, generally designated 20, and an upper bead breaking assembly, generally designated 22. The equipment also includes an internally threaded cone member 24 which is employed on the spindle 16 in a manner well known as well as a control pedal 26 for controlling operation of the stand 10.
The interrelation of the various components described thus far is described in greater detail in the above-identified Strang et al U.S. Pat. No. 3,255,800 and reference may be had thereto for additional details.
With continued reference to FIG. 1, the invention with which the instant application is concerned includes an air ring, generally designated 28, which is mounted in concentric relation to the table 12 relative to the spindle 16 in any suitable manner. Preferably, eye brackets 30 formed of sheet metal may be employed for this purpose. The air ring 28 is circular and has a peripheral extent greater than the majority of a circle and which is limited only by the presence of the lower bead breaking assembly 20. That is, the ends of the air ring 28 terminate short of the lower bead breaking assembly 20 so as to not interfere with operation of the same. Additionally, there is provided a front console, generally designated 32, which mounts a variety of components for controlling the bead seater and inflating apparatus of the invention and which, at its lower end, has an outwardly projecting foot pedal 34 operable to control the operation.
A second housing or console, generally designated 36, is adapted to be secured to the left side of the tire changing stand 10 and serves as a securing means for a source of air under pressure, namely, an air surge tank 38. The console 36 mounts a pressure gauge, generally designated 40, as well as an operator 42 for an air release valve. As a last basic component, the invention includes a conventional air chuck 44 which, as is well known, may be placed in operative relation on a valve stem on a wheel rim to cause air under pressure to pass through such valve stem.
With reference now to FIG. 2, the table 12 is seen to be supporting a tire rim 50 having a central opening 52 through which the spindle 16 extends. About the rim 50 is a tire carcass 54 and the rim further includes a conventional valve stem 56 in fluid communication with the air chuck 44 and the interior of the tire carcass 54. The air ring 28 is seen to be comprised of a tube 58 having a plurality of inwardly and upwardly directed air nozzles 60 therein. That is, the air nozzles are directed inwardly toward the spindle 16 and upwardly toward the rim 50 resting on the table 12.
The air nozzles 60 may be easily formed simply by punching apertures in the tube 58, but it is highly desirable that the upward inclination be such that the individual air streams 62 issuing from the nozzles are parallel to the underlying portions of the surface of the frusto-conical portions 14. Stated another way, the nozzles 60 should be configured such that the air streams 62 will define a conical configuration which is the same as the cone that would be defined by the frusto-conical portions 14 if a full cone were to encompass those postions. For example, if the frusto-conical portions 14 are at an angle 45° to the horizontal, the air streams 62 should leave the air ring 28 at an angle approximately 45° to the horizontal.
As can be seen, an upper bead 64 of the tire carcass 54 has been seated against the upper boundary of the rim 50 while a lower bead 66 of the tire has not been seated and the air streams 62 with the nozzles 60 configured in relation to the frusto-conical portions 14, as mentioned above, will be directed at the interface of the lower bead 62 and the tire rim 50 and passed between the two into the interior of the tire to inflate the same in accordance with the well-known pressure differential principle. Thee resulting inflation will cause the bead 66 to progressively move downwardly until finally it too seats against the rim 50. At this time, further inflation may be maintained soley through the air chuck 44.
It will further be appreciated that the above-described arrangement of the air nozzles 60 with respect to the frusto-conical portions will result in the air streams 62 having the same angle of attack on a rim and a tire carcass regardless of rim size. For example, if a smaller rim indicated in dotted lines at 50' is employed the angle of attack will remain the same, while if a larger rim, indicated in dotted lines at 50" is employed the angle of attack again will be the same. Thus, the arrangement permits an optimum angle of attack for the air streams to be employed for a variety of different sizes of rims.
Turning now to FIG. 3, the surge tank 38 is seen to be secured to the second console 36 by four brackets 70 (only two of which are shown) and, includes a portion 72 extending through an opening in a side wall of the console 36. Within that portion 72 of the surge tank 38 within the console 36 is a fitting 74 which may be connected to an air conduit 76 which, in turn, terminates in a fitting 78 exterior of the console 36 for connection to a compressor or the like. The conduit 76 serves to deliver air under pressure to the interior of the surge tank 38.
As may be ascertained from FIGS. 1 and 3, the underside of the surge tank 38 includes a depending elbow 80 which is connected to a large conduit 82 which delivers air from the source, the surge tank 38, to the air ring 28 and the air chuck 44 via a control system to be described in greater detail hereinafter.
The console 36 on its upper side 84 mounts the pressure gauge 40 which has an indicating portion 88 on the exterior surface of the console. Also within the console 36 is an air release valve 90. Also within the console 36 is an air release valve 90. As will be recalled from the description of FIG. 1, an actuator 42 for the air release valve 90 is located exteriorly of the console 36.
At the lower end of the console 36 there is a pair of inwardly extending rails 92 formed of angle irons. The horizontal portions of the rails 92 include a plurality of apertures 94 through which bolts or the like (not shown) may be passed to secure the console 36 to the underside of the tire changing stand 10 in the configuration illustrated in FIG. 1.
The assemblage is completed by conduits 96, 98 and 100. The conduit 96 extends from the control system, to be described in greater detail hereinafter, and directs air through the air release valve 90, when the latter is closed, to both the conduit 98 and the conduit 100. The conduit 100 is connected to the air chuck so that when air under pressure is being passed through the conduit 96 and the air release valve 42 is closed, a tire on the stand may be inflated through the air chuck 44.
The conduit 98 extends to the pressure gauge 40 so that the latter, with its indicator 88, may provide an indication of the pressure of the air within the conduits 96 and 100. It will be appreciated that as a result of the foregoing construction, even when air is not flowing through the conduit 96, the presence of the conduit 98 will result in the pressure gauge 40 giving a reading corresponding to the air pressure in a tire on the stand if the chuck 44 is fitted on the valve stem 56 thereof. The system may be used to monitor the inflation pressure of such a tire such that bead seating and inflating operation may be temporarily stopped and the pressure monitored. If the pressure is in excess of the desired pressure, the manual actuator 42 may be operated to open the air release valve 90 to release some air. This procedure may be repetitively accomplished until the pressure in an inflated tire is at the desired level.
Turning now to FIGS. 4 and 5, the control components of the invention will be descirbed. As generally alluded to previously, the same are housed in the first console 32 which may be formed of sheet metal or the like and secured to the front of the tire changing stand 10 by any suitable means such as self-tapping screws or the like. The conduit 82 from the surge tank 38 is led to the console 32 and enters the same in any suitable manner. Within the console 32, the conduit 82 is connected to a relatively large, normally closed, spring loaded valve 102. At approximately the point of connection of the conduit 82 to the valve 102, a fitting 104 is located and a conduit 106 is secured thereto and connected to a smaller valve 108, also within the console 32 and, again, of the normally closed, spring loaded variety. The conduit 96 which, it will be recalled, is connected to the air release valve 90, has its opposite end connected to the valve 108.
A conduit 110 is connected, within the housing, to the valve 102 and emerges through an aperture 112 in the upper side thereof to be connected to the air ring 28. Thus, it will be appreciated that the valve 102 controls the flow of air to the ring 28 while the valve 108 controls the flow of air to the air chuck 44.
the foot pedal 34 is operative to selectively open both of the valves 102 and 108. In particular, the same is movable through three positions. In the first position, both of the valves 102 and 108 will be in their normally closed configuration. In a second position intermediate the first and the third positions, the foot pedal is operative to open the valve 108 while permitting the valve 102 to remain closed. In this position, air will flow to the air chuck 44 only. In the third position, the foot pedal 44 is operative to cause both valves to be opened so that air will flow both to the air chuck 44 and to the air ring 28.
The structure by means of which the foregoing is accomplished is best illustrated in FIG. 5. In particular, a stamped metal channel bracket 114 is secured to the underside of the console 32 and includes openings 116 and 118 through which valve operators 120 and 122 for the valves 102 and 108 respectively extend. As mentioned previously, both of the valves 102 and 108 are of the normally closed variety and are spring loaded such that their operators 120 and 122 are biased outwardly from the valve bodies (downwardly as shown in FIG. 5).
It will also be recalled that the valve 102 is a larger valve than the valve 108 and as a practical matter, manufacturers of such valves, employ larger springs in larger valves than in smaller ones. Thus, there will be a greater biasing force tending to close the valve 102 than the biasing force tending to close the valve 108 with the result that a greater force must be exerted upwardly on the operator 120 for the valve 102 to open the latter than need be applied to the operator 122 for the valve 108. Advantage is taken of this fact as will be seen.
The foot pedal 34 is generally in the form of an inverted channel and the sides thereof include aligned apertures 124 through which a pivot rod, normally a bolt, 126 extends. The bolt also extends through aligned apertures (not shown) in the sides of the channel bracket 114 so that the foot pedal 34 is secured thereto for pivotal movement about the axis defined by the bolt 126.
The foot pedal 34 also includes a second set of aligned apertures 128 near its innermost end for receiving a pivot rod 130.
The assemblage is completed by a pedal bracket 132 formed in the shape of a channel and having a cut-out 134 in both sides thereof in the vicinity of the bolt 126 so as to preclude interfering contact between the tow. The width of the channel of the pedal bracket 132 is slightly greater than the width of the pedal 34 so that the sides of the former may be interposeed between the sides of the latter and the sides of the channel bracket 114.
Adjacent the cut-outs 134, the sides of the pedal bracket 132 include aligned apertures (not shown) which receive the ends of the pivot pin 130 so as to pivotally secure the pedal bracket 132 to the innermost end of the pedal 34. The arrangement of the various components is generally shown in FIG. 5, it being of some significance that the location of the pivot axis defined by the pivot pin 130 be between vertical planes parallel to such pivot axis and extending through the operators 120 and 122 for the valves 102 and 108.
Also of some significance is the location of the bolt 126. Firstly, the same must be on the large valve side of the pivot pin 130 and secondly, is preferably located just inside the aforementioned vertical plane extending through the operator 120 for the valve 102 although, depending upon dimensions of the other components, a fair amount of deviation from this relation is allowable.
With the foot pedal 34 in its first position, namely, that wherein both valves are closed, the assemblage will have the configuration illustrated in FIG. 5 with the web of the pedal bracket 132 in contact with the lowermost ends of the valve operators 120 and 122. The spring biasing of the valves will cause the assemblage to assume this configuration whenever a downward force is not applied to the left-hand end of the foot pedal 34.
When the pedal 34 is partially depressed i.e., the pedal 34 is pivoted counterclockwise about the bolt 126, the pivot pin 130 will be elevated along with the pedal bracket 132. However, the greater resistance posed by the heavier spring loading of the valve 102 and conveyed to the left-hand end of the pedal bracket 132 via valve operator 120 will result in pivoting of the pedal bracket 132 about the pivot axis defined by pin 130 on the pedal 34, also in a counterdclockwise direction so that once the pedal 34 has been depressed to the second of its positions, the web of the pedal bracket 32 will assume the dotted line position designated by the legend "SECOND POSITION" whereat only the operator 122 for the valve 108 will have been moved to open that valve. Thus, in such a position, the valve 102 will remain closed while the valve 108 will be open.
Further pivotal movement of the pedal 34 in the counterclockwise direction will result in the opening of the valve 102 as follows. Specifically, the right-hand end of the web of the pedal bracket 132 will be blocked from further movement in an upwardly direction by a portion of the valve body. Thus, continued elevation of the pivot pin 130 will result in pivotal movement of the pedal bracket 132 in a clockwise direction about pivot pin 130 to raise the left-hand end of the web thereof against the force applied by the operator 120 to open the valve 102. When such has occurred, the web of the pedal bracket 132 will be in the dotted line position designated by the legend "THIRD POSITION" and both valves 102 and 108 will be opened.
The invention may be used as follows. A tire rim with an unseated tire carcass 54 thereon may be placed on the tire changing stand and secured in place through the use of the cone 24. The operator may lift up the tire carcass 54 to partially seat the upper bead 54. The air chuck 44 may then be applied to the valve stem 56 and the pedal 34 depressed from its first position to its third position. This will result in the opening of both of the valves 102 and 108 so that the air ring 28 will be operative to force air into the tire through the interface of the rim and the lower bead 62 while additional air will be forced into the tire through the air chuck 44. At some point, inflation will be sufficient to cause the lower bead 66 to seat. At this time, the operator may allow the foot pedal 34 to move from the third position to the second position, at which time, the valve 102 will be closed ceasing operation of the air ring 28 but causing the valve 108 to remain open to cause further inflation via the air chuck 44. When the operator believes the tire to be sufficiently inflated, he may then release the pedal 34 completely so that it will return to its first position, at which time both valves 102 and 108 will be closed and the pressure in the tire may be checked via the indicator 88 of the pressure gauge 40. Should the tire be underinflated, the pedal 34 may be depresssed to its second position to cause further admission of air. In the event the tire is overinflated, the actuator 42 for the air release valve 90 may be manually manipulated to release air in the tire to bring pressure with the tire down to a desired value.
It will be appreciated from the foregoing that the invention provides many advantages over various devices heretofore known. For example, by use of the surge tank 38, during inoperative periods, sufficient pressure may be built up within the apparatus itself so as to insure the presence of sufficient air under pressure to rapidly complete a bead seating and inflating operation. It will also be appreciated that the use of a single operator for the two control valves permits the operator to have substantially more freedom in performing the operation. The presence of the pressure gauge and the air release valve allow rapid monitoring of inflation pressure and release of pressure in the case the tire is overinflated. And, the construction of the various consoles is such that the invention may be easily embodied on new tire changing stands at their point of manufacture and before shipping or, alternately, may be embodied on existing tire stands already out in the field with a minimum of labor. The orientation of the air nozzles with respect to the configuration of the table optimizes the bead seating portion of the operation for any of a variety of differing sizes of rims. And, finally, the tire changing stand on which the invention may be employed is fully usable for its conventional function such that tire changing as well as bead seating and inflating may be accomplished on but a single apparatus without the need for relocating various components during different steps of the combined operations.
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Tire bead seating and inflating apparatus of the type employing an arcuate tube having its interior connected to a source of air and including inwardly directed nozzles for directing a high volume of air under pressure toward the interface between a tire rim and a tire sidewall while air is simultaneously being applied to the interior of the tire through a conventional valve stem. The invention specifically contemplates a kit whereby such an apparatus, along with desired peripheral equipment, may be easily affixed to existing tire changing stands.
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RELATED APPLICATIONS
[0001] This application claims priority to the co-pending provisional application having Ser. No. 60/624,736, which was filed on Nov. 3, 2004. The provisional application having Ser. No. 60/624,736 is herein incorporated by reference in its entirety.
[0002] The application is also related to the subject matter disclosed in U.S. application Ser. No. 10/228,385, filed 26 Aug. 2002, the subject matter of which is herein incorporated by reference.
FIELD OF THE INVENTION
[0003] The present invention relates to apparatus and methods for monitoring fatigue, structural response and operational limits in structural components. More particularly the present invention relates to apparatus and methods for installation of monitoring systems on marine and land structural members.
DESCRIPTION OF THE RELATED ART
[0004] All structures respond in some way to loading, either in compression, tension, or combinations of various loading modes. While most structures and systems are designed to accommodate planned loading, it is well known that loads exceeding design limits or continued cyclical loading may induce fatigue in the structure. While some structures may be readily monitored for signs of fatigue, others are not easily monitored. Examples include subsea structures, such as pipelines, risers, wellheads, etc.
[0005] In most instances, monitoring systems are installed when the structure is installed or constructed. However, there exists a system of subsea risers, pipelines and other structures that have already been installed without the benefit of monitoring systems. These subsea components are subject not only to normal planned current or wave loading, but met ocean events, such as hurricanes, or sustained cyclical loading from vortex induced vibration (VIV) loading.
[0006] A major concern in all offshore operations is the operational life of subsea components. A fatigue-induced failure can result in a substantial economic loss as well as an environmental disaster should produced hydrocarbons be released into the sea. When a subsea production structure is nearing the end of its serviceable life or has suffered substantial fatigue, producing companies are likely to shut-in production rather than run the risk of a catastrophic failure. This can result in substantial financial losses to the producing company.
[0007] Currently, most subsea structures, such as risers and pipelines, including steel catenary risers, are not monitored. Structural integrity of such bodies is modeled, based on known loading factors, sea state data, and boundary conditions. Because there is no direct measurement of strain or fatigue in these structures, high safety factors, on the order of 10 to 20, are factored into these models. It will be appreciated that as the models indicate that a structure is nearing the end of its serviceable life or has undergone unacceptable fatigue, the choice for the production company is to repair or replace the structure or to shut-in production. In some instances, the structural integrity is far better than the models may predict. This means that the producing companies may be incurring substantial expense in repairing or replacing the structures or losses from shutting in production. The alternative, a loss of containment of produced hydrocarbons, would, however, subject any producing company to far greater liability costs when compared to repair, replacement or shut-in.
[0008] Recently efforts have been made to develop monitoring systems for subsea structures. U.S. Patent Publication 2004/0035216, published 26 Feb. 2004, U.S. Application 10/228,385, entitled Apparatuses and Methods for Monitoring Stress in Steel Catenary Risers, which is herein incorporated by reference in its entirety, describes an apparatus and method for monitoring subsea structures utilizing a series of fiber optic Bragg grating (FBG) sensors to measure strain in several directions on a subsea structure. The design and use of FBG sensors is discussed within the '385 application. Multiple fiber optic strands from a centralized fiber bundle have a Bragg grating applied to them and are attached to the subsea structure. Small gratings are etched on the fibers where attached to the structure. As a light is applied to the fiber a return signal is received. As a strain is applied to the structure, the grating is likewise strained and the returned signal undergoes a frequency shift that is proportional to the strain. The aforementioned application discloses the performance of the FBG sensors and a means for attaching them to the structure. It will be appreciated that by obtaining actual strain data, the models used to determine serviceable life are more accurate and the safety factors can be reduced to manageable levels. As, such, producing companies are more likely to reduce repair/replacement costs or shut-in losses without substantially increasing environmental risk.
[0009] Thus, there exists a need for an improved method and apparatus to permit retrofit of an FBG or other sensor monitoring system that can be adapted to structures already in place.
SUMMARY OF THE PRESENT INVENTION
[0010] The present invention is directed to a means of retrofitting sensors to installed marine elements. More particularly, the present invention utilizes a set of collars that may be remotely installed on subsea structures. One or more fiber optic sensors and umbilicals leading to a system are affixed to the structure by means of multipart collars. The collars may be hingeable for ease of installation or may be assembled as separate items. The umbilical acts as a protective sleeve for the fiber optic sensor and its fiber optic communication line. The sensors may be bonded internal to the the umbilical. Moreover, the fiber optic sensors may be of the FBG type previously disclosed, or may be of the Fabry Perot (FP) interferometer type. The nature of FP sensors is well known to those of ordinary skill in the art. In a Fabry Perot sensor, light is reflected between two partially silvered surfaces. As the light is reflected, part of the light is transmitted each time it reaches the surface, resulting in multiple offset beams that set up an interference. The performance of FP sensors is similar in that relative movement between the two silvered surfaces will result in a change of wavelength of the light.
[0011] The present invention contemplates that the fiber optic sensors and their umbilicals are secured to the collars or other support structures. The support structure is then deployed subsea and installed on an existing subsea structure. The umbilicals may be removably attached to the support structure. This permits subsequent replacement of a sensor/umbilical in the event of failure. Alternatively, it permits installation of the sensor/umbilical following attachment of the support structure to the structure. In the present invention, multiple sensor/umbilical pairs may be attached to a single support structure. When the support structure is attached to the subsea structure, the sensors are fixed in position relative to the subsea structure. It will be appreciated that multiple support structures/umbilical/sensor assemblies may be attached to the subsea structure, thereby permitting strain monitoring along the length of the subsea structure. The flexibility of support structure design and attachment scheme of the sensor/umbilical pairs permits the user to design a custom monitoring system for the subsea structure.
[0012] In one application, the present invention may provide a large and dense array of sensors over a relatively small portion of the structure. In the case of a subsea pipeline or a riser, this type of deployment could be used to determine not only strain from physical forces (physical loading and current forces) but may be used to detect large volumes of denser production (slugs) as they pass through the monitored section. As the slugs pass through a pipeline, the internal pressure within the pipe increases, resulting in detectable strain in the pipe internal and external walls. This strain may be detected by the sensors arrayed to measure hoop strain and may be recorded by the monitoring system. As the slug passes down a pipeline, it will be detected by subsequent sensors. The design of a sensor array and its placement along a pipeline section may be used to characterize the slug velocity and size.
[0013] In another application, the present invention may provide for multiple support structures over long spans of the structure. In the case of SCRs, it would permit monitoring strain across the touch down zone. This type of application would also permit monitoring of the effects of temperatures on a subsea element. It will be appreciated that high temperature/high pressure well production may have hydrocarbon production temperatures in the range of 200° to 350° F. This production may be rapidly cooled as it passes through subsea flow lines to production risers. The effect of this rapid temperature change on subsea equipment is poorly documented. It will be appreciated that the failure of a piece of subsea equipment due to temperature failure would have a disastrous effect on the environment.
[0014] While the foregoing and following discussion focuses on the use of fiber optic FBG and FP sensors, it will be appreciated that the sensors described herein may include hybrid sensors, i.e., fiber optic sensors in combination with other types of transducers including a means for converting the transducer signal for transmission through a fiber optic medium.
[0015] The foregoing summary has outlined rather broadly the features and technical advantages of the present invention so that the detailed description of the preferred embodiment that follows may be better understood. Additional features and advantages of the invention will be described hereinafter, which form the subject of the invention. It should be appreciated by those skilled in the art that the conception and the specific embodiments disclosed might be readily used as a basis for modifying or designing other apparatuses and methods for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth and claimed herein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The accompanying drawings, which are incorporated in and form a part of the specification, illustrate the embodiments and applications of the present invention, and, together with the detailed description, serve to explain the invention. In the drawings:
[0017] Figs. 1A and 1B are side and top views, respectively, of a cutaway section of a tubular showing one embodiment of the present invention;
[0018] FIGS. 2A and 2B are side and top views, respectively, of a cutaway section of a tubular showing another embodiment of the present invention;
[0019] FIG. 3 is a perspective view of an application of the present invention showing spaced collars having multiple sensors on each fiber optic cable on an SCR;
[0020] FIG. 4 is a side view of another application of the present invention is which the sensor umbilical is wound helically between the collars so as to sense vortex induced vibration;
[0021] FIGS. 5A and 5B are side and top views of another embodiment of the present invention utilizing two locking collars;
[0022] FIGS. 6A and 6B are side and top views of another two collar embodiment of the present invention;
[0023] FIGS. 7A and 7B are top and side views of another embodiment of the present invention utilizing a bladder contact system;
[0024] FIGS. 8A-8C are detailed views of the bladder and sensor contact system of FIGS. 7A and 7B ;
[0025] FIGS. 9A-9C are top, cross-sectional and detailed views of another embodiment of the present invention;
[0026] FIGS. 10A and 10B are side and cross-sectional views of another embodiment of the present invention; and
[0027] FIGS. 11A and 11B are cross-sectional and detailed views of another embodiment of the present invention as applied to concrete or cement coated structures; and
[0028] FIGS. 12A and 12B are side and cross-sectional views of the present invention as applied to a tubular connection.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0029] In one embodiment the structure to which the monitoring system is attached is discussed in terms of a tubular subsea element. However, it will be appreciated that the structure need not be tubular. The specific geometry of the support structure and the means of securing it about the structure may be readily varied to the geometry of the structure. Moreover, the structure need not be limited to a subsea element, as the same principles would operate with a horizontal or vertical structure, subsea or on the land.
[0030] In FIGS. 1A and 1B , a cutaway of a subsea element 10 is shown with one embodiment of the monitoring system of the present invention mounted thereon. A collar 20 is shown comprised of two collar sections 22 A and 22 B. The collar sections 22 A and 22 B each have a hinge portion built therein and are pinned together by pin 24 , thus allowing the collar sections 22 A and 22 B to open and close tightly about the vertical element 10 . It will be appreciated that a deformable material such as rubber or plastic may be placed on the internal surfaces of collar sections 22 A and 22 B. The material is deformed against the outer surface of the subsea element 10 when the collar 20 is closed thereabout, thereby further securing the collar 20 against movement relative to the subsea element 10 . The pin 24 may be secured by any number of means known to those skilled in the art, including, but not limited to cotter pins, snap rings, etc. In Fig. 1B , a collar latch 26 is depicted as holding collar sections 22 A and 22 B in a closed position about the vertical element 10 . The collar latch 26 may be readily selected by those skilled in the art from any number of latch designs that are capable of being operated underwater, either manually or by remotely operated vehicle (ROV). Collar sections 22 A and 22 B are provided with at least one groove or notch section 28 , which will serve to provide a placement point for the fiber optic umbilical, to be discussed below. It will be appreciated that the collar sections 22 A, 22 B, the pin 24 and latch 26 may be readily fabricated from metal, fiberglass, thermoplastic or other material suitable for the marine environment. Moreover, the collars may be coated with copper or other anti-fouling coating to prevent marine growth on the collars.
[0031] Multiple fiber optic umbilicals 40 are shown as being installed in collar 20 . The fiber optic umbilical 40 provides an appropriate shield for the one or more fiber optic fibers 42 within each umbilical 40 . The umbilical 40 may be constructed from an appropriate material, such as thermoplastic or other material. Each of the fibers 42 has at least one sensor 44 integrated therein and secured to the inner wall of the umbilical 40 by epoxy or some other suitable means. As noted above, the sensor 44 may be of the FBG or FP type. While fiber optic fibers 42 of FIG. 1A are shown with a single sensor 44 , multiple sensors may be placed on a single fiber. This may be achieved by designing the FBG or FP sensor 44 to have an initial different wavelength response to the same light source as other FBG or FP sensors 44 . Accordingly, any measurement of strain from the multiple sensors could be distinguished one from the other. The sensor umbilicals 40 are depicted as being within grooves 28 within the collar sections 22 A and 22 B. The umbilicals 40 are secured within the grooves 28 and to the collar sections 22 A and 22 B by means of umbilical latches 50 . The latch 50 may be readily selected by those skilled in the art from any number of latch designs that are capable of being operated underwater, either manually or by ROV. It will be appreciated that the number of umbilicals 40 that may be deployed on collar 20 and may be a simple matter of engineering design. The sensor umbilicals 40 are then connected to a system (not shown) designed to monitor and record strains on the element 10 . Moreover, the umbilical 40 may be used to shield multiple fibers 42 , each having multiple sensors 44 thereon.
[0032] The collar 20 with umbilicals 40 already installed thereon may be lowered on a heave-resistant line from an appropriate work vessel. At the selected depth, the collar 20 and umbilicals 40 may be maneuvered into position about structure 10 . The collars 20 may then be opened and closed about the structure 10 by means of divers or ROVs, depending upon the depth of installation. Further, installation of the collar or other support structure may be achieved utilizing an ROV together with a special installation system designed to permit the installation of multiple support structures in a single trip. U.S. Pat. No. 6,659,539, incorporated herein by reference in its entirety, describes a method and apparatus for installing multiple clamshell devices, such as collar 20 , using Shell's RIVET™ system, commercially available from one or more Shell Companies. Utilizing the RIVET™, the collars 20 and umbilicals 40 would be loaded into the RIVET™, lowered to the desired position next to the structure 10 and RIVET™ arms would be activated to close the collar 20 sections about the marine element 10 . An ROV can be used to activate the RIVET™ structure or it may be remotely activated. The ROV may also be used to close the collar latch 26 , if required. Alternatively, a self-closing latch 26 may be used on collar sections 22 A and 22 B.
[0033] The monitoring system may be located on a structure or vessel above the water line. However, in many instances, the sensors may not be readily adjacent to a surface structure, making it impractical to have umbilicals 40 lead back to the surface structure for connection to the monitoring system. It is contemplated with respect to the present invention that the monitoring system may further include a subsea-based system. The subsea system would analyze and record the strain information much like a surface system. The information could be stored for periodic transmission from the subsea system to a surface based system or retrieval of data from the subsea system. This may be accomplished by means of short range electromagnetic transmission, acoustic transmission via transponders and receivers or simple data retrieval utilizing an ROV system. Alternatively, the monitoring and recording system could be based in a surface buoy tethered to the marine element. The surface buoy could be battery and/or solar powered to provide power for the monitoring system. Further, the surface buoy system could transmit information to a remote station. Thus, it would be possible to support a remote monitoring system away from a structure. It will be appreciated that the remote monitoring system disclosed therein could be utilized with any of the embodiments discussed herein.
[0034] FIGS. 2A and 2B depict side and vertical cutaways of another embodiment of the present invention. A collar 20 , comprised of collar sections 22 A and 22 B, each having a mating hinge section incorporated therein are secured about marine element 10 by means of hinge pin 24 and latch 26 . In the embodiment depicted in FIGS. 2A and 2B , a single groove 28 is incorporated into collar 20 . An umbilical 40 is shown as being placed in groove 28 and secured within the collar 20 by means of a suitable latch 50 . Whereas the umbilical 40 of FIGS. 1A and 1B had but a single fiber therein, the embodiment shown in FIGS. 2A and 2B depict multiple fiber optic fibers 42 therein, each having a sensor 44 bonded to the inside wall of the umbilical 40 . The embodiment shown in FIGS. 2A and 2B depict each of the sensors 44 at approximately the same axial position within the umbilical 40 . It will be appreciated that each fiber optic fiber 42 need not have its sensor bonded to the inside of the umbilical 40 wall in the same axial position. Moreover, more than one sensor 44 may be placed on a single fiber optic cable 42 , as discussed above. The sensors 44 may be spaced azimuthally inside umbilical 40 . Motion by marine element 10 in a specific direction will affect each sensor FIG. 3 . is a perspective view of a marine element 60 , in this case an SCR, on which a plurality of collars 20 and umbilicals 40 have been mounted in the touch down zone (TDZ), i.e., that portion of the riser where it comes into contact with the seabed 70 . The implementation depicted in FIG. 3 utilizes multiple sensors 44 on a single fiber optic fiber 42 within umbilical 40 . It will be appreciated, however, that the ability to detect a frequency shift created by FBGs, and therefore the strain seen by a particular sensor 44 , will decrease as the number of sensors on a single fiber optic fiber increases. As a result, it may be desirable as the number of collars 20 installed on a structure increases, to have separate umbilicals 40 and/or fibers 42 on the collars 20 .
[0035] FIG. 4 depicts a series of collars 20 placed on a vertical element 10 . Unlike the alignment in shown in FIG. 1A , the umbilicals 40 are shown as being deployed in a helical manner by indexing each umbilical 40 over to the adjacent groove 28 in collar sections 22 A and 22 B. As noted previously, the umbilicals 40 are secured to the collar 20 by means of an umbilical latch 50 . The umbilicals 40 may then be installed on collars 20 in a helical manner as shown in FIG. 4 using ROVs to place the umbilical 40 and close latch 50 to secure them to the collar 20 . It is well known to those skilled in art that the installation of helical bodies about a larger body will have the result of suppressing VIV. At the same time, it will be appreciated that a single umbilical 40 /sensor 44 combination that has failed during its operational life may be replaced by sending down an ROV to open the appropriate latch 50 on each collar to remove the defective umbilical 40 /sensor 44 and replace it with an operational one.
[0036] Another embodiment of the present invention is depicted in FIGS. 5A and 5B , in which a dual collar system utilizing spacer members placed between the collars. A marine element 70 is shown having two collars 101 placed at two different locations along the longitudinal axis of the tubular 70 . Each of the collars 101 are comprised of collar halves 100 A and 100 B and are free to rotate about pin 102 . Each collar 101 is also equipped with a latch 104 to secure the collar halves 100 A and 100 B together. Strips of spacers 109 are show as being affixed to and connecting collars 101 . The spacers 109 depicted in FIGS. 5A and 5B are shown as rectangular strips in compression between the collars 101 . The spacers may also have other geometric configurations and may made from ABS plastic, PVC plastic, or other thermo plastics, soft metals, fiberglass or other materials that would permit the spacers 109 to flex sufficiently to place them in compression between collars 101 . A fiber optic umbilical 110 attached to a surface monitoring system (not shown) is shown as being connected to fiber optic junction 112 . Junction 112 may be affixed to one of the collars 100 A or 100 B or may be affixed to the spacer 109 . The junction 112 shown in FIG. 5A is shown as being “daisy-chained” through fiber optic umbilical 113 to other similar junctions 112 mounted on the spacers 109 . Each junction 112 further has a fiber optic sensor lead 114 leading away from the junction 112 and terminating in a FBG or FP sensor 116 . FIG. 5A shows the sensor 116 as being mounted on the inside of spacer 109 to protect it from current borne objects. The sensor 116 may further be protected by means of epoxy, plastic or other suitable marine resistant coating. With the spacers 109 being under compression, any strain seen by marine element 70 will result in a change in the compression of the spacers 109 . These changes may be detected by the sensors 116 and transmitted to the monitoring system. While FIG. 5A shows multiple junctions 112 , it will be appreciated that a single fiber optic junction having multiple fiber optic sensor leads 114 may be used to place multiple sensors 116 on the spacers 109 .
[0037] A variation of this spacer system for monitoring is shown in FIGS. 6A and 6B . Instead of flexible spacers 109 as used in FIGS. 5A and 5B , multiple spacer bars 120 are used as spacers between collars 100 A and 100 B secured about marine element 70 . The spacer bars 120 may be placed in tension, compression or an unloaded condition between collars 100 A and 100 B. A fiber optic umbilical 110 , attached to a surface monitoring system (not shown) is shown as being connected to a single fiber optic junction 112 . Multiple fiber optic sensor leads 114 lead away from junction 112 and terminate in FBG or FP sensors 116 placed on the inside of spacer bars 120 . Alternatively, multiple junctions 112 may be used similar to those depicted in FIGS. 5A and 5B . Strain seen by the marine element 70 will be transmitted via collars 100 A and 100 B to the spacer bars 120 . The strain may be detected by the sensors 116 , transmitted through junction 112 , and fiber optic cable 110 to the surface system or another system, where it may be recorded. It will be appreciated that implementations depicted in FIGS. 5A, 5B and 6 A, 6 B may be installed utilizing the aforementioned RIVET™ system.
[0038] An alternative to mounting sensors on intermediate objects attached to a marine element is to mount the sensor directly on the marine element. However, retrofitting sensors directly to an installed marine element is generally difficult in assuring (a) placement and (b) contact between the sensor and marine element. FIGS. 7A and 7B depict the design of a collar system that permits a sensor to be directly in contact with an installed marine element. A single collar 200 is comprised of collar halves 202 A and 202 B pivoting about pin 206 . The collar halves 202 A and 202 B are secured about the marine element utilizing a latch 204 , for example a self-locking latch. Each collar half 202 A and 202 B may have at least one recess 212 therein for the mounting of an inflatable bladder 210 A and 210 B which is placed between the inside of the collar halves 202 A and 202 B and the marine element 70 . Each of the collar halves 202 A and 202 B is provided with an injection port 208 A and 208 B which are depicted in greater detail in FIGS. 9A-9C .
[0039] Collar 202 B is shown in section and detail in FIGS. 8A-8C . It will be appreciated that collar 202 A has similar detail but is not shown for the sake of brevity. Collar 202 B has an annular chamber 212 machined azimuthally about the interior of the collar 202 B. Inflatable bladder 210 B is mounted in the recess 212 and is in fluid communication with port 208 B. It will be appreciated that a check valve (not shown) may be placed in the fluid passage between bladder 210 B and port 208 B. A fiber optic umbilical 214 is depicted passing through access port 216 in collar 202 B. The access port 216 may be sealed to the marine environment by means of epoxy, potting compound or other suitable substance. Chamber 212 B further includes a flexible, non-corrosive carrier plate 220 B bearing fiber optic strand 215 B which terminates in a FBG or FP sensor 222 B. As depicted in FIGS. 8A-8C , the carrier plate 220 B is retained within the chamber by placing part of the plate within relief grooves 218 formed in the chamber 212 . Other methods for retaining the carrier plate 220 B may used such as leaf springs or other suitable retaining systems. A vent port 224 B is further drilled in collar 202 B and may further be provided with a check valve (not shown) to permit the flow of water from chamber 212 B to the marine environment but prevent water from the marine environment from flowing back into the chamber 212 B.
[0040] In operation, the collar 200 may be installed about a marine element 70 by a diver, ROV or ROV and RIVET™ system. As noted above, the latch 204 is designed to be self-locking to tightly fit collar 200 about the marine element 70 . Following securing the collar 200 about the marine element 70 , a diver or ROV may be sent down to the collar 200 . An epoxy may be pumped into port 208 B, which is in fluid communication with the bladder 210 B. As can be seen in FIG. 8B , as the epoxy 240 enters the bladder 210 B, the bladder 210 B expands and starts to deflect towards the marine element 70 , pulling the carrier plate 220 B out of grooves 218 B. Alternatively, the carrier plate 220 B may be scored adjacent to where it is affixed to chamber, rendering it frangible across the scoring allowing it to part and move toward the marine element 70 as the bladder 210 B is inflated by pumping in the epoxy 240 . In FIG. 8C , the bladder 210 B is shown as fully inflated with the sensor 220 B in contact with the marine element 70 . It will be appreciated that as bladder 210 B is inflated, that it will displace water originally in annulus between chamber 212 B and marine element 70 . Accordingly vent port 224 B is provided to permit the displacement of the water and the addition of a check valve can prevent the return of water back into the annulus through port 224 . The pump is disconnected from port 208 B and the epoxy 240 is allowed to cure. With fiber optic cable 214 in communication with a surface monitoring system, this embodiment provides for a direct contact between the marine element 70 and the sensor 222 B. It will be appreciated that multiple carrier plates 220 and sensors 222 may be installed in the chamber 212 B, either utilizing multiple cables 214 or a single cable and a fiber optic junction that leads to multiple sensors. While FIGS. 7A, 7B and 8 A- 8 C depict two azimuthal bladders 210 A and 210 B, it will be appreciated that small individual bladders may be used for one or more sensors. This type of arrangement would require additional pumping ports or a flow system that permits selection and inflation of the individual bladders without over-pressurizing other bladders that could result in damage to the sensor. Other systems may be readily designed to advance the sensor 222 into contact with the marine element upon injection of epoxy or some other bonding fluid. For example, sensor 222 may be mounted on a rod recessed in a sleeve in port 208 . Upon injection of epoxy through port 208 , the rod bearing the sensor is advanced into contact with the marine element as epoxy continues to fill cavity 212 displacing any water through port 224 . It will be appreciated that the embodiments depicted in FIGS. 1, 2 and 7 - 8 are designed to be secured around an existing marine element in a hinged or clamshell fashion that may use the RIVET™ tool for installation.
[0041] In other instances, a marine element may be horizontal or lying at or along the ocean bottom or partially embedded in the ocean bottom. It will be appreciated that it would be difficult, if not impossible, to install a fully encircling collar of the types disclosed above. Accordingly, there exists yet another embodiment to permit retro-fitting to horizontal and/or partially embedded marine elements. An embodiment for monitoring a partially embedded marine element 70 is depicted in FIGS. 9A-9C . FIG. 9A is a top view of the marine element having a shroud 300 disposed over the top of the marine element 70 . The shroud 300 may be fabricated from fiberglass, thermoplastic, metal or other materials suitable for a marine environment. The shroud 300 may be lowered onto the marine element 70 from a surface vessel with the assistance of a diver or an ROV. The shroud 300 is secured to the marine element 70 by at least one spring-loaded (springs not shown), locking balls 302 installed in the interior of the shroud. As the shroud 300 lowered over the marine element 70 , the spring loaded balls 302 are pushed back into shroud 300 . As the shroud 300 is further lowered, the locking balls 302 pass the diameter of the marine element 70 and are then biased outwardly by the springs, thereby affixing the shroud 300 to the marine element 70 . It will be appreciated that other retaining methods may be used to secure the shroud 300 to the marine element, including screws passing through shroud 300 that may be tightened about the marine element by a diver or an ROV. Alternatively, spring-loaded or screw-activated locking dogs may be used to secure the shroud 300 to the marine element 70 . A sensor assembly 304 , including fiber optic umbilical 310 , is mounted atop the shroud 300 . The fiber optic umbilical 310 is connected to an instrumentation system (either surface or subsurface) that is used to monitor and record the data.
[0042] The sensor assembly is shown in greater detail in FIG. 9C , which is a cross sectional view of the sensor assembly 304 and marine element 70 . The shroud 300 is provided with a slotted hole 320 , having slot portion 322 therein. A slotted sensor module 308 is designed to fit within threaded slotted hole 320 . The module 308 has a key 306 manufactured therein and cooperates with slot 322 to align and limit the module 308 movement toward the marine element 70 . The module 308 may be comprised of a potted epoxy thermoplastic, metal or other marine resistant material. The fiber optic umbilical 310 may be potted as part of the module and terminates in a FBG or FP sensor 312 mounted at the end of the module. Alternatively, a hole in the sensor module 308 or shroud 300 may be provided for passing the fiber optic cable 310 to the end of the sensor module. The sensor assembly 304 may further be provided with a grommet 324 or protective other means to protect sensor 312 . The sensor module 308 is secured in slotted hole 320 by a lock down screw or bolt 314 that mates with the threads in slotted hole 320 . The module 308 and grommet 324 may be designed to bring the grommet 324 into contact with the marine element 70 and thus permit the sensor 312 to directly monitor strain. Alternatively, if the sensor 312 is not in direct contact with the marine element 70 , it will still be capable of monitoring the marine element 70 as large mechanical strains placed on the marine element will be passed to the sensor 312 through shroud 300 . The illustrated embodiment thereby provides for a means for monitoring strains in elements that are horizontally situated or partially embedded.
[0043] In other instances, it may be desirable to monitor the strain placed on a tubular or other connection. A system for carrying out monitoring is depicted in FIGS. 10A and 10B , which are side and cross-sectional views of such a system. Two tubular elements 70 are joined in a pin and box connection 400 in which the male threaded end of one of the tubulars is screwed into sealing engagement with the box end of the other tubular. In this embodiment collar halves 402 A and 402 B rotate about pin 404 . In this instance, the assembly is made up of two collar sets, each disposed on one side of the connection 400 . The respective collars may be secured by latches, bolts, machine screws 406 or other suitable retaining mechanism. A sensor support connection 408 is attached to each of the collars 402 by epoxy or other suitable means. The connections 408 are aligned to permit the attachment of a sensor support 410 prior to deployment. A fiber optic umbilical (not shown) is introduced such that a sensor 420 may be disposed in between the sensor support 410 and pin and box connection 400 . This permits sensor 420 to directly monitor strain incurred by pin and box connection 400 . While a single sensor is depicted in FIGS. 10A and 10B , it will be appreciated that multiple sensor supports 410 and sensors may be deployed using junction boxes and shown in FIGS. 5A and 5B .
[0044] In some instances, a marine element 70 , such as a pipeline, is coated with concrete to add extra weight and to prevent the pipeline from moving in response to near bottom currents. The present invention contemplates yet another embodiment to permit monitoring of concrete coated marine elements. In cross-sectional view FIG. 11A , a marine element 70 having a concrete coating 72 thereabout is shown in a horizontal position partially embedded in the surface. A sensor assembly 340 is depicted in FIG. 11A and shown in greater detail in FIG. 11B . A hole 342 is drilled and/or milled through the concrete coating 72 . This may be accomplished by a diver or by using a work ROV equipped with a drill. It will be appreciated that a masonry drill and/or mill that is less capable of cutting into the steel of the marine element 70 may be used to prevent damaging marine element 70 . Upon completion of drilling, a threaded, slotted sensor housing 344 may be inserted in the hole 342 . The slotted sensor housing 344 is designed to receive a sensor module 346 having keyed portion 350 designed to mate with the slotted sensor housing 344 to align and position the sensor module 344 . As with the embodiment of FIGS. 10A and 10B , the module 346 may be made of any suitable marine resistant material. The module 346 provides a pass-through or potted fiber optic cable 348 that terminates in a FBG or FP sensor 352 on the bottom of module 346 . The module 346 is retained in the housing 344 utilizing a set screw 354 or other suitable means. The module 346 itself is retained within the concrete coating 72 by a quick setting epoxy 356 that is pumped into the annulus between the housing 344 and hole 342 . Alternatively, a tapered sleeve or other friction retaining means may be used to retain the housing 344 within the hole 342 . As will be noted in FIG. 11B , as illustrated, the sensor 352 is not in direct contact with the marine body 70 . Rather, any strains will be transmitted through the cement coating 72 , to the housing 344 and to the sensor module 346 and sensor 352 .
[0045] FIGS. 12A and 12B are cross-sectional and detailed views, respectively, of another single collar embodiment of the present invention. Two collar halves 80 and 82 pivot about pin 83 . The collar halves 80 and 82 may be made of metal, thermoplastic or other materials suited to long term marine exposure. They are positioned about marine element 70 closed and secured by a suitable latch 84 . A sensor base 86 is affixed to one of the collar ( 80 or 82 ) halves. The base 86 may be attached utilizing adhesives, resins, or may be welded to the selected collar half. One or more fiber optic cable grooves 92 are formed or machined in the sensor base 86 . A locking latch arm 90 pivots about pin 86 , which is in turn connected to sensor base 86 . The locking latch arm 90 is drilled and threaded to receive contact pin 94 . The contact pin 94 is used to insure that the fiber umbilical optic 94 having fiber optic cable 95 and FBG or FP sensor (not shown) remain in contact with the sensor base 86 . In this instance, the collar may be installed on the tubular 70 prior to being installed in its location. The fiber optic umbilical 94 may be installed after the marine element 70 has been installed.
[0046] The present application has disclosed a number of different support structures that may be used to retrofit existing, in place marine structures with fiber optic monitoring equipment. As noted above, the fiber optic sensors may be used for the purpose of strain measurement, slug detection and temperature measurement. Various modifications in the apparatus and techniques described herein may be made without departing from the scope of the present invention. It should be understood that the embodiments and techniques described in the foregoing are illustrative and are not intended to operate as a limitation on the scope of the invention.
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Sensors, including fiber optic sensors and their umbilicals, are mounted on support structures designed to be retro-fitted to in-place structures, including subsea structures. The sensor support structures are designed to monitor structure conditions, including strain, temperature, and in the instance of pipelines, the existence of production slugs. Moreover the support structures are designed for installation in harsh environments, such as deep water conditions using remotely operated vehicles.
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BACKGROUND OF INVENTION
The present invention relates to pallets, primarily to pallets that can be assembled and disassembled, and pallets moved by fork trucks.
Many products and goods are moved and stored on pallets. The majority of these pallets are constructed of wood and remain assembled after use because they cannot easily be taken apart. Other pallets constructed of plastic or paperboard cannot be disassembled at all. When not in use the pallets are usually stored and/or shipped back to their originator. Pallets, which cannot be collapsed or disassembled, require a large amount of space for storage and trucking. In addition, if a portion of the pallet is damaged, the whole pallet is discarded and a replacement procured. Space, material and time cost money to a business. Storage and transport of empty pallets has associated costs that can be reduced by keeping pallets unassembled while not in use. In addition, pallets constructed of matching parts and easily disassembled have the advantage of only requiring replacement of damaged parts. The pallet assembly also must not take a substantial amount of time to put together or take apart, the cost of which may be recovered from the savings in storing, return shipping, and replacement.
SUMMARY OF INVENTION
It is the intent of the present invention to provide an easily assembled and disassembled pallet manufactured of plastic or other suitable material and constructed of a number of specific parts. The pallet would be delivered to a user in the unassembled form. Varying the lengths of associated parts will also make pallets of different sizes.
The general purpose of the present invention is a pallet assembly can easily be assembled and unassembled.
It is an object of the present invention to have the storage of the pallet in an unassembled form thereby requiring less space for storing and shipping. Smaller trucks may be used to transport the pallets; or more can be transported in the same size truck.
Another object of the present invention is to provide a versatile pallet by varying the sizes of associated parts and not requiring a separate top sheet.
A further object of the present invention is to provide like parts for all pallets of the same size and load rating. Which allows easy replacement of damaged parts.
Another object of the present invention is to enable the assembly or disassembly to be accomplished within a few minutes without tools.
BRIEF DESCRIPTION OF DRAWINGS
All 8 views are viewed from the same direction.
FIG. 1 is a perspective rendition of the completely assembled pallet.
FIG. 2 is a perspective rendition of the runners.
FIG. 3 is a perspective rendition of the joist.
FIG. 4 is a perspective rendition of the retainer bar.
FIG. 5 is a perspective rendition of the support member.
FIG. 6 is a perspective rendition of the end fastener.
FIG. 7 is a perspective rendition of the support member and end fastener.
DETAILED DESCRIPTION
FIG. 1 shows a perspective of a completed easily assembled pallet having two opposed and parallel runners 1 , at least one joist 2 connected at either end to runners 1 , two retainer bars 3 one each inserted in runners 1 to hold the joists 2 in place vertically so that a flat surface is formed by the top surfaces of the runners 1 and joists 2 . At least one support member 4 to provide additional strength and support for joists 2 , and two end fasteners 5 to hold the support member 4 in place (only one end fastener is visible in this figure). The parts of the pallet may be constructed of different types of plastic, any other suitable material, or a combination of materials. The material used needs to be selected for required strength, resiliency, and durability, ease of manufacture, cost, and other such considerations. The height of the runners 1 and support member 4 are such that forks of a lift truck will easily slide below the joists 2 . And, the spacing apart of runners 1 and support member 4 is such that a lift truck fork will pass between the support member 4 and runner 1 . The support member 4 may not be required for light loading or small pallets.
A pair of runners 1 is shown in FIG. 2 . For a given pallet size the runners are made identical in size and with the same number and spacing of keyways 7 so that they may be used interchangeably on either side. The at least one keyway 7 are formed as part of, or affixed to, the runner 1 , and spaced such that there is minimal spacing between joists 2 . The keyway 7 is shown as “T” shaped as can be seen in the enlarged view but can be any number of shapes. The keyway 7 contacts the inside surface of runner side 10 . The top of the keyway 7 is also in contact with the runner top underside 11 of the runner 1 . Depressor 6 is formed as part of, or affixed to, runner bottom 12 . Depressor 6 is sloped to aid the placement of retainer bar 3 and to hold retainer bar 3 in place when assembled. To allow depressor 6 to be retractable from the retainer bar 3 during assembly and disassembly, slots are cut into runner bottom 12 along each side of depressor 6 . A spring-loaded depressor 6 could be used if the runner material is inelastic. Slot 8 is cut completely through each of ends 13 and 14 . Hole 9 is cut through surface 10 , aligned with and above depressor 6 .
FIG. 3 shows a joist 2 with ends 15 , flanges 16 and 17 , and web 18 . At least one joist 2 is required when assembling a pallet. The joist end 15 is a key shown in the shape of a “T” matching the runner keyway 7 so the joist end 15 can be slip fit into the runner keyway 7 . The joist top flange 16 is shorter on each end than the bottom flange 17 by an amount to allow the top flange to fit between the runner top surfaces 11 . Thus, the length of the joist top flange 16 is limited to the spacing of the runners 1 . This allows all top surfaces of the pallet to be flush and a tight fit can occur between the ends of flange 16 and runner top 11 . If a tight fit is not required the top flange 16 length can be shorter. The end 15 is flush with the end of the bottom flange 17 . When joist end 15 is inserted into runner keyway 7 , joist end 15 and the end of flange 17 are to fit tightly against runner inside surface 10 . Each end of the joist 2 are constructed the same so the joist 2 can be inserted into either runner 1 . The joist 2 so installed forms the top surface of the pallet, therefore, no top sheet is required for a continuous surface. If a contiguous top pallet surface is not required some joists 2 can be left out of the assembly.
FIG. 4 shows in detail one retainer bar 3 having tongue ends 19 , recess 20 , top surface 24 , bottom surface 25 , front surface 26 , and back surface 27 . The retainer bar 3 must be flexible to allow a slight bending to take place during assembly. The overall length of retainer bar 3 , including the two tongue ends 19 is the same length as runner 1 overall length from outside runner surface 13 to outside runner surface 14 . Retainer bar 3 fits inside runner 1 . Runner slot 8 and tongue 19 are of substantially the same size and shape with runner slot 8 being slightly larger to allow a slip fit with tongue 19 . Recess 20 is provided for clearance of runner depressor 6 with additional finger clearance for removal of retainer bar 3 during disassembly. To avoid having to bend the retainer bar 3 the tongue ends 19 could be replaced with spring loaded tongues or pins; or the ends could be without tongues and held in place with screws or clamps.
FIG. 5 shows the support member 4 having a top surface 30 . At each end of the support member 4 is formed a hole 31 and a slot 32 which is tapered from inside adjacent hole 31 towards the support member 4 free end as can be seen in enlarged view of FIG. 5 (Top portion above slot of support member 4 is shown removed for clarity). The height of slot 32 is the same as the diameter of hole 31 .
FIG. 6 is a detail of the end fastener 5 . The end fastener 5 has two pins 33 formed as part of, or attached to, and extending from the inside surfaces of end fastener 5 having a clearance between the free ends of pins 33 slightly larger than the small end width of the support member tapered slots 32 or the thickness of the support member between the end depth of the holes 31 . The height of pins 33 are slightly less than the height of the support member slot 32 and hole 31 to allow the pins 33 to slide within the slot 32 and engage the hole 31 . The pins are shown round but any suitable shape can be used. Spring-loaded pins can be used if material is inelastic. A pin can be construed to mean a dowel, rod, bar, dimple, nipple, or the like. Slot 38 of end fastener 5 is of size and shape to fit over joist flange 17 . The bottom of slot 38 is on the same plane as the top of support member 4 . The end fasteners 5 when pushed into place engaging a support member 4 and joist flange 17 will lock the support member 4 to the bottom of joist 2 as shown in FIG. 1 . Many other means of fastening the end fastener 5 to the support member 4 can be contrived which may or may not require the use of tools. Such as, drilling holes in the end fastener sides and through the support member 4 ends then passing a bolt through and securing with a nut.
FIG. 7 shows the end fasteners 5 mounted on the support member 4 .
Assembly and disassembly does not require any tools.
To assemble, set two runners 1 on a flat surface nearly parallel with inside surfaces facing each other. Insert a joist end 15 into an end slot 7 of one runner 1 , next insert the opposite joist end 15 into the end slot 7 of the second runner 1 . Similarly insert a second joist 2 , if required, at the opposite end of the runners forming a rectangular shape. Continue inserting additional joists as needed until the required number of slots 7 are connected between the two runners 1 .
After all the joists 2 are installed in runners 1 , the retainer bar 3 , with front surface 26 facing toward the inside of the pallet, is installed by inserting one tongue 19 into runner end 13 slot 8 . With the one tongue 19 inserted in a runner slot 8 , the retainer bar 3 is slightly bent until the retainer bar clears the runner end 14 allowing the free end tongue 19 to be inserted in the adjacent runner slot 8 . As the tongue 19 enters runner slot 8 in runner end 14 , apply pressure to retainer bar surface 26 (thereby causing depression of depressor 6 ) until surface 26 clears runner depressor 6 . Runner depressor 6 moves back up to original position when retainer bar 3 is in place, thereby locking retainer bar 3 in place within runner 1 . When retainer bar 3 is in the assembled position the retainer top surface 24 fits tightly against the bottom surface of joist bottom flange 17 . Repeat the procedure to install the second retainer bar 3 on the opposite side of the pallet.
When the runners 1 , required joists 2 , and retainer bar 3 are in place the support member 4 with two end fasteners 5 can be installed. The support member 4 is set in place at approximately the center of the pallet, parallel to runners 1 , and against joist bottom flange 17 . The two end fasteners 5 are next installed one at each end of support member 4 . As the end fastener 5 is pushed into place, the sides having the pins 23 attached bend outwardly, distorting until pins 33 reach hole 31 thereby sliding into hole 31 . At the same time slot 38 of end fastener 5 slides over and encompasses flange 17 . After repeating this procedure with the second end fastener 5 the support member 4 is locked in place with the two end joists 2 and the support member top surface 30 is flush with the bottom of joist flange 17 . Repeat if additional support members are required. Support member 4 is used when additional support of joists 2 is needed. When assembled the bottom of the support member 4 is on a parallel plane with the bottom of runners 1 (all 3 sit flat and touch the floor).
Disassembly is accomplished in reverse order of assembly. Remove support member end fasteners 5 by slightly spreading the sides apart and sliding the end fasteners 5 off. Then remove the support member 4 (repeat for additional support members). Remove the retainer bar 3 by applying pressure to runner depressor 6 and to retainer bar back surface 27 by pushing through runner hole 9 causing the retainer bar 3 to bend releasing tongues 19 . Repeat this procedure to remove the second retainer bar 3 . The joists 2 can now be easily removed from the runners 1 .
Assembling and disassembling would be easier with the pallet upside down with top of the pallet resting on a flat surface.
The phrase “formed as part of” as used herein applies to the use of a material where pieces can be manufactured as one piece. If the material used does not allow forming of parts then some attachment means can be substituted such as welding, screwing, bolting, clamping or the like.
While a preferred form of the invention has been shown in the drawings and described, since variations in the preferred form will be apparent to those skilled in the art, the invention should not be construed as limited to the specific form shown and described, but instead is as set forth in the following claims.
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An easily assembled pallet, having two runners set apart and opposed, joists slidibly attached between the runners, and two retainers slidibly connected to each of the runners and contacting the joist end bottom surface thereby keeping the joists in proper location in the runners. Whereby the top of the joists forms the pallet's top flat surface. In addition, a support bar can be attached to the bottom of the joists between the runners to provide additional support and stiffness to the joists.
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FIELD OF INVENTION
This invention relates to dense matrix composites suitable for high temperature applications. More particularly, this invention relates to SiC fiber reinforced reaction bonded SiC composites wherein the SiC fibers are coated with a ceramic material.
BACKGROUND OF THE INVENTION
Reinforced ceramic matrix composites are well suited for structural applications because of their potential toughness, thermal resistance, high temperature strength and chemical stability. These composites can be produced by the addition of whiskers, fibers or platelets to a ceramic matrix. The non-brittle nature of these composites provides the much needed reliability that is otherwise lacking in monolithic ceramics.
Fabrication of ceramic matrix composites reinforced with sintered continuous fibers is more difficult than fabrication of dense monolithic ceramics. Conventional sintering of a green ceramic matrix reinforced with sintered fibers is not possible if the green ceramic matrix has rigid inclusions. Densification can, however, be achieved by chemical vapor infiltration (CVI) or reaction bonding. Reaction bonding is the preferred method because it is less time consuming and more often produces a fully dense body than the CVI process. For high temperature applications, full densification is necessary to prevent rapid oxidation degradation of the reinforcements or reinforcement coating.
Densification by reaction bonding, described in U.S. Pat. No. 3,205,043 to Taylor, involves infiltrating molten silicon through the pores of a green body containing SiC and carbon. The silicon reacts with the carbon to form SiC, which then bonds the SiC grains together. In the absence of carbon, the infiltrated molten silicon solidifies upon cooling, thereby filling the pores of the SiC bonded SiC body. This process is known as siliconization. The resulting fully dense end product contains SiC and residual free silicon. Since reaction bonding does not involve shrinkage of the green body as does conventional sintering, the final dense product is a near net shape.
Fracture resistance of ceramic matrix composites is achieved through crack deflection, load transfer, and fiber pull-out. Fiber pullout, which is well established as central to the toughness of ceramic fiber composites, is achieved by having little or no chemical bonding between the fibers and matrix. The fibers must be able to readily debond and slide along the matrix for increased fracture toughness of the composite.
It is known that many fiber-matrix combinations undergo extensive chemical reaction or interdiffusion between the fiber and matrix material, each of which is likely chosen for the contribution of specific mechanical and/or physical properties to the resulting composite. Such reaction or interdiffusion can lead to serious degradation in strength, toughness, temperature stability and oxidation resistance. The fibermatrix interface is therefore very important to preventing or minimizing chemical reactions and interdiffusion.
Surface modification of the fibers is an effective means to control the fiber-matrix interface. This can be accomplished by coating the fibers with a suitable ceramic to inhibit the fibers from reacting or bonding with the matrix. The ceramic coating allows the fiber to pull out from the matrix and slide along the matrix, thus increasing the fracture toughness of the composite.
Coated silicon carbide fibers and whiskers are known reinforcements for composite materials. U.S. Pat. No. 4,929,472 to Sugihara et al. discloses SiC whiskers having a surface coated with a thin, 7-100 Å, carbonaceous layer and SiC whiskers coated with a Si 3 N 4 layer which is 15-200 Å thick. These surface coated whiskers are used as a reinforcing material for ceramics such as SiC, TiC, Si 3 N 4 , or Al 2 O 3 .
U.S. Pat. No. 4,781,993 to Bhatt discloses a SiC fiber reinforced reaction bonded Si 3 N 4 matrix wherein the SiC fibers are coated with an amorphous carbon layer and an overlayer having a high silicon/carbon ratio covering the amorphous layer.
U.S. Pat. No. 4,642,271 to Rice discloses BN coated ceramic fibers embedded in a ceramic matrix. The fibers may be composed of SiC, Al 2 O 3 or graphite, while the matrix may be composed of SiO 2 , SiC, ZrO 2 , ZrO 2 -TiO 2 , cordierite, mullite, or coated carbon matrices.
U.S. Pat. No. 4, 944,904 to Singh et al. discloses a composite containing boron nitride coated fibrous material. Carbon or SiC fibers are coated with BN and a silicon-wettable material and then admixed with an infiltration-promoting material. This mixture is then formed into a preform which is then infiltrated with a molten solution of boron and silicon to produce the composite.
Teusel et al. in "Aluminum Nitride Coatings Silicon Carbide Fibres, Prepared by Pyrolysis of a Polymeric Precursor", J. Mat. Sci., 25 (1990) 3531-3534, discloses a method of coating SiC fibers. Nicalon (SiC) fibers, Nippon Carbon Co. Ltd., were thermally pretreated in nitrogen and dip coated with a solution of metallic aluminum in an organic electrolyte. The fibers were then calcined at 900° C. under anhydrous ammonia. The authors found that a thin coating, about 0.5 microns, produced a smoother and more uniform surface than thicker coatings. The performance of these AlN coated SiC fibers in a SiC matrix was not discussed in the Teusel et al. article.
A specific problem encountered with SiC reinforced SiC composites is that the SiC fibers or coatings on the SiC fibers may react with the matrix during formation of the composite, resulting in a strong fiber-matrix bond. This strong interfacial bond leads to decreased fracture toughness. It is an object of the invention, therefore, to provide a process for incorporating SiC fibers into a SiC matrix while controlling the fiber-matrix interface to achieve high fracture toughness. It is also an object of the invention to provide a process for producing a SiC composite possessing high temperature strength.
SUMMARY OF THE INVENTION
The present invention has resulted from the discovery that a reaction bonded silicon carbide composite reinforced with coated silicon carbide fibers can produce a dense ceramic composite suitable for high temperature applications. AlN, BN and TiB 2 coatings were found to limit both mechanical and chemical bonding with the matrix to improve the strength and toughness of the composite material.
The present process for producing SiC fiber reinforced SiC composites includes the steps of coating SiC fibers with a composition selected from the group consisting of AlN, BN and TiB 2 ; treating the surface of the coated fibers with a mixture of SiC powder, water and a non-ionic surfactant; preparing a slurry comprising SiC powder and water; vacuum infiltrating the coated fibers with the slurry to form a cast; drying the cast to form a green body; and reaction bonding the green body to form a dense SiC fiber reinforced reaction bonded matrix composite.
The SiC reinforced SiC composite of the present invention includes a reaction bonded SiC matrix, a SiC fiber reinforcement possessing thermal stability at temperatures of at least 1420° C., preferably 1500° C. and an interface coating on the fibers having chemical and mechanical compatibility with the SiC matrix and with the SiC fibers.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are 1000 times and 1500 times magnified microscopic photographs showing the fracture surfaces of AlN coated SiC fibers.
FIGS. 3 and 4 are micrographs of the reinforced composite manufactured in accordance with the process of the present invention.
FIG. 5 is a 200 times magnified microscopic photograph showing fiber pull out at the fracture surface of a reaction bonded SiC matrix composite incorporating AlN coated SiC fibers.
FIG. 6 is a 200 times magnified microscopic photograph showing fiber pull out at the fracture surface of a reaction bonded SiC matrix composite incorporating BN coated SiC fibers.
FIG. 7 is a photograph showing the stable crack growth of a reaction bonded SiC composite containing BN coated SiC fibers.
FIG. 8 is a graph showing the load-deflection curves for both a BN coated SiC fiber reinforced reaction bonded SiC composite according to the present invention and a monolithic reaction bonded SiC.
FIGS. 9a and 9b are 50 times and 250 times magnified microscopic photographs of the fracture surface of uncoated SiC fiber reinforced reaction bonded SiC matrix composite showing no fiber pull-out.
DETAILED DESCRIPTION OF THE INVENTION
The subject invention relates to a process for producing SiC fiber reinforced reaction bonded SiC matrix composites wherein the fibers are coated with a non-oxide ceramic material and the article thus produced. The matrix material provided in the present invention is reaction bonded SiC which possesses net shape processing capability and ease of fabrication.
The SiC fibers employed in the present invention are sintered polycrystalline SiC fibers from The Carborundum Company, Niagara Falls, N.Y. However, other SiC fibers, such as those produced by chemical vapor deposition or other processes could be used if they are suitable for use in the reaction bonding process, especially those possessing thermal stability at 1420° C. or higher. Most of the existing commercial precursor-derived SiC fibers such as Nicalon (Nippon Carbon Company) and Tyranno (UBE Industries, Japan) are not suitable for this application because they lack the thermal stability necessary for use in reaction bonded SiC composite fabrication.
To achieve the desired composite properties, namely, high temperature strength and fracture toughness, it is necessary that there is a suitable interface coating between the matrix and the fiber. To provide non-catastrophic failure of the composite, the fracture energy must be dissipated by the fiber pulling out from the matrix and sliding along the matrix. The frictional sliding expends the energy, thereby providing increased fracture toughness. If uncoated SiC fibers are incorporated into a matrix of reaction bonded SiC, fiber pull out is not achieved because of the bonding of the SiC fiber with the SiC matrix. Thus, any crack that occurs in the surface of the composite will propagate through the matrix and continue through, i.e., transverse to, the fiber resulting in the typical brittle fracture behavior of conventional monolithic ceramics.
The preferred non-oxide ceramic coatings for the SiC fiber reinforcements are AlN, BN and TiB 2 and combinations thereof. A further preferred fiber coating is AlN because AlN exhibited the most desirable fiber pull out behavior with the reaction bonded SiC matrix.
The non-oxide ceramic can be coated onto SiC fibers by several methods, including, (1) chemical vapor deposition, (2) evaporation of aluminum, followed by chemical conversion with NH 3 , and (3) deposition of an Al 2 O 3 coating through sol-gel, followed by chemical conversion with NH 3 . Chemical vapor deposition is the preferred method because it is most convenient and thus far has produced the most uniform coatings.
An AlN coating thickness of between about 1-15 microns on the SiC fibers is desired. A BN coating thickness of between about 0.1 to 10 microns is desired. The preferred thickness of BN is between about 0.5 to 2 microns. We have found that thin AlN coatings, less than 1 micron, were inadequate because the AlN actually dissolved in and reacted with the molten silicon during the infiltration process. After incorporating thinly coated fibers into the reaction bonded SiC matrix, no AlN coating nor fiber pull out could be detected. However, when sintered fibers coated with a thicker layer of AlN were incorporated into the reaction bonded SiC matrix and fractured in a four-point bending test, fiber pull out could be observed. This is demonstrated in FIGS. 5 and 6. Although some AlN may react or dissolve in molten silicon during reaction bonding, fiber pull out will still occur as long as there remains some unreacted AlN coating on the SiC fibers. The AlN coating remaining on the SiC fibers after reaction bonding is between 0.1 to 15 microns thick.
A green body of coated SiC fiber reinforced SiC composite is preferably produced by a slurry filtration process. In this process, the slurry is prepared by ball milling SiC powder (for example, submicron SiC powder marketed by Arendal Smelteverk A.S., Norway) in water. To ensure good dispersion of the powder, the pH of the slurry is adjusted to between 8 and 10 by adding ammonium hydroxide to the slurry. A small amount, about 0.5 wt %, of sodium silicate may be used as a binder. Other binders that can be used include PVA, sucrose syrup, phenolic, acrylic latex and other water soluble binders. The solid content of the slurry is preferably between 20 and 80 wt %. The slurry is then poured into a mold.
An appropriate amount of sintered SiC fiber in the form a bundle is dipped into a mixture of SiC powder and water (solid content of 10-50 wt. %) containing about 2% or less of a non-ionic wetting agent, such as 2 wt % Triton x-100 surfactant, comprising iso-octylphenoxypolyethoxyethanol. The surfactant treated fiber bundle is then laid in the SiC slurry and infiltrated and dewatered. The resulting cast is allowed to fully dry to form the green body. The green body is then completely densified by conventional siliconization/reaction bonding. The temperature range for siliconization/reaction bonding is between 1420° C. (the melting point of silicon) and 2400° C., and preferably between 1500° and 1600° C. The process is preferably carried out under vacuum to prevent oxidation, but can be carried out in atmospheric pressure. Complete densification is achieved at temperatures as low as 1500° C. in 1/2 to 1 hour under vacuum for small test samples. Densification time and temperature depend on the size of the article and on the carbon content in the slurry.
Carbon as particulate carbon, colloidal carbon, or carbon-yielding resins may also be added to the SiC slurry. However, it is important that the rheology and chemistry of the slurry is not severely altered. The added carbon can help achieve good wicking of molten silicon during the reaction bonding process and help minimize residual silicon in the dense body by reacting with the Si to form SiC.
Composites with fiber volume fraction as high as 0.44 were also produced. Composites produced without the addition of wetting agent to the slurry had regions where veins of silicon were present. However, when the wetting agent is used, these silicon veins were absent and a uniform microstructure was obtained.
A fracture toughness of about 13 MPa m 1/2 was calculated from the fiber pull out lengths for a reaction bonded SiC matrix composite having about 40 vol. % of AlN coated fibers. Similar fiber pull out for BN coated SiC fibers in a reaction bonded SiC matrix has been observed, as is demonstrated in FIG. 6. Because AlN has a higher oxidation resistance than BN, it is expected that the AlN coated SiC fiber reinforced composite will have a higher oxidation resistance than the BN coated SiC fiber reinforced composite.
The SiC fiber reinforced reaction bonded composite of the present invention possesses thermal stability up to 1420° C.
The examples which follow are intended to illustrate and not to limit the inventive concepts presented herein.
SPECIFIC EXAMPLES
Example 1
SiC fibers were coated with AlN by a chemical vapor deposition (CVD) process. The CVD coating process involved the use of AlCl 3 and NH 3 as precursors. Solid AlCl 3 was heated to about 120°-150° C. and the AlCl 3 vapor that was generated was transported by hydrogen gas flow to the hot zone where the NH 3 was introduced. The AlCl 3 react with Nh 3 to produce AlN. The typical deposition temperature was about 850°-1000° C. The pressure in the deposition chamber was about 50 torr. The resulting AlN coating thickness varied from 5-15 microns. FIGS. 1 and 2 show these AlN coated SiC fibers.
A green body of AlN coated SiC fiber reinforced composite was fabricated by a slurry filtration process. The slurry was prepared by ball milling SiC powder (Submicron Arendal) in water. The solids content of the slurry was about 75 wt %. The pH of the slurry was adjusted to 9 by adding ammonium hydroxide. About 0.5 wt % of sodium silicate was used as a temporary binder. Mixing was accomplished by ball milling for 24 hours. About 4 grams of slurry was poured into a glass mold 0.25×0.25×1 inch which was placed over filter paper in a Buchner funnel.
About 1.75 grams of AlN coated SiC fibers in the form of a bundle was dipped into a diluted SiC/water slurry with 50 wt % SiC and 0.1 wt % Triton X-100 surfactant to surface treat the fibers and facilitate infiltration. The treated bundle was then placed into the glass mold containing the undiluted slurry. A vacuum was drawn on the funnel containing the mold until the cast was fairly dry.
The cast was allowed to fully dry. The cast was then placed in a furnace and completely densified by conventional reaction bonding/siliconization. Complete densification was obtained at 1500° C. in 1 hour under vacuum.
The volume percent of coated fibers for this sample was estimated to be about 30%. The sample was fractured in a standard four point bend test. Fiber pull-out was observed as shown in FIG. 5.
Example 2
SiC fibers were coated with BN by a CVD process. The average coating thickness was about 2 microns. The composite was fabricated substantially in accordance with Example 1. The volume percent of coated fibers was about 12%.
The composite sample was fractured in a standard four point bend test. Fiber pull-out was observed as shown in FIG. 6.
To test the crack deflection of the composite, a notch was cut in a composite sample having the dimensions 1/8"×1/4"×2". The sample was then subjected to a four point bend test. Stable crack growth was observed as shown in FIG. 7. In FIG. 8, the load-deflection characteristics for a BN coated SiC fiber reinforced reaction bonded SiC composite were compared to those of a monolithic reaction bonded SiC composite. The SiC fiber reinforced composite shows stable crack growth as evidenced by the non-linear composite behavior. The monolithic reaction bonded SiC composite, on the other hand, shows catastrophic failure at a load of around 33 lbs. The stable crack growth of the SiC fiber reinforced SiC reaction bonded matrix is attributed to fiber pull-out.
Comparative Example 3
A composite was fabricated substantially in accordance with Example 1, except that uncoated SiC fibers were incorporated into the reaction bonded SiC composite. No fiber pull-out was observed as shown in FIGS. 9a and 9b.
The foregoing examples are not intended to limit the subject invention, the breadth of which is defined by the specification and the claims appended hereto, but are presented rather to aid those skilled in the art to clearly understand the invention defined herein.
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The invention provides silicon carbide fiber-reinforced, reaction-bonded silicon carbide composites suitable for high temperature applications in which the silicon carbide fiber is coated with AlN, BN or TiB 2 . The composites offer superior fracture toughness which is ascribed to fiber pullout. The invention also includes a process for making the composites.
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FIELD OF THE INVENTION
[0001] This application relates to stressed membrane structures and to opening or door assemblies for such enclosures.
BACKGROUND OF THE INVENTION
[0002] Stressed membrane structures have been in use for many years and, in many situations, offer advantages over conventional structures. One area where such structures are very attractive is for use as aircraft hangars.
[0003] In order to function effectively as aircraft hangars, it is necessary that wide opening doors be provided for ingress and egress of aircraft.
[0004] There has been an ongoing need for doors which will meet this objective of wide opening doors for hangers and many other applications within the structural limitations of stressed membrane structures. It is preferable that such doors retain the relocatability which has been the hallmark of tensioned membrane structures, while meeting structural criteria such as wind resistance.
[0005] The present invention arises against this background.
PRIOR ART
[0006] Applicant's prior U.S. Pat. No. 5,283,993 illustrates a door arrangement for tensioned membrane structures.
SUMMARY AND OBJECTS OF THE INVENTION
[0007] The present invention provides an opening or a door arrangement whereby an end of a stressed membrane structure can be partly or fully opened while maintaining a tensioned condition of the membrane of the opened part.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] In the drawings which illustrate embodiments of the invention:
[0009] [0009]FIG. 1 is a plan view, partially cut away, of a stressed membrane structure, showing an airplane in ghost lines;
[0010] [0010]FIG. 2 is a plan view of the structure of FIG. 1 with an opening assembly in an open position;
[0011] [0011]FIG. 3 is a plan view of the structure of claim 1 with the opening assembly in a partially opened condition;
[0012] [0012]FIG. 4 is a cross-section through the opening assembly of FIG. 1 with the tensioned membrane removed;
[0013] [0013]FIG. 5 is a perspective view illustrating a support frame for the opening assembly;
[0014] [0014]FIG. 6 illustrates detail of bracing for a part of the support frame of FIG. 5;
[0015] [0015]FIG. 7 is an elevation of a pivot assembly for the opening assembly;
[0016] [0016]FIG. 8 is a plan view of the pivot assembly of FIG. 7;
[0017] [0017]FIG. 9 illustrates an inner tie-down for securing the opening assembly;
[0018] [0018]FIG. 10 illustrates an outer tie-down for securing the opening assembly;
[0019] [0019]FIG. 11 illustrates a closure lock plate for securing a pair of opening assemblies in a closed position;
[0020] [0020]FIG. 12 illustrates the closure plate of FIG. 11 in a partially opened position;
[0021] [0021]FIG. 13 is a plan view of a skid plate and alignment pipes for aligning a pair of opening assemblies during closing; and
[0022] [0022]FIG. 14 is an elevation of the skid plate and alignment pipes of FIG. 13.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] Stressed membrane structure 10 comprises a framework including structural members 12 which support tensioned membrane 14 .
[0024] Various bracing arrangements, such as cable bracing 16 , may be utilized where required in structure 10 .
[0025] Structure 10 may be provided with doors such as personnel doors 18 and sliding door 20 . Various other features, such as skylight 22 , may be included.
[0026] Structure 10 will generally have a substantially semi-circular end 34 , and it is desirable that at least a part of end 34 can be opened to allow access to the structure for large objects. Thus end 34 is divided into two end parts 24 and 26 . In the preferred case, both end parts 24 and 26 are rotatable so that the entire end 34 of structure 10 can be opened to the full width of the structure 10 . For this purpose, end parts 24 and 26 are pivotally associated with but separated from structure 10 by pivot assemblies 28 and 30 .
[0027] Stressed membrane structures normally have rounded or arcuate ends or ends which extend outwardly of the plane across the end of the normal full width of the structure. While this is not always true for these structures, the present invention is applicable to those which do have at least one such end.
[0028] The rounded or arcuate end part has a number of advantages which include the ability to stress the membrane continuously around the structure without substantial special attention to the end treatment. As well, such end structures contribute to the very important ability of the structure to withstand wind and associated environmental effects.
[0029] It is possible that other shapes might be used but all such protruding or extended ends are considered to be under the general heading of extended ends. Such extended shapes are to be contrasted specifically with a normal flat door configuration.
[0030] In guiding the opening and closing of end parts 24 and 26 , pivot assemblies 28 and 30 are preferably positioning and guiding pivots only and are not intended to support any part of the weight of the associated end part.
[0031] [0031]FIG. 3 illustrates the positioning of the main frame members 36 that would normally be a part of an end 34 of a structure 10 .
[0032] The door arrangement of the present invention preferably provides a support structure 38 associated with each structural member 36 . As illustrated in FIG. 4, the support structure 38 comprises horizontal beam 40 , vertical beam 42 and diagonal beams 44 and 46 .
[0033] Each support structure 38 is preferably provided with transport members which may be in the form of rollers which are preferably wheel assemblies and preferably at least two wheel assemblies 48 and 50 for each horizontal beam 40 .
[0034] It is the combination of the support structures 38 and wheels 48 and 50 which support the weight of end parts 24 and 26 in opening and closing the end parts. Pivot assemblies 28 and 30 are non-weight bearing.
[0035] [0035]FIG. 5 illustrates an essentially complete frame for each of end parts 24 and 26 . This consists of the normal structural members 36 of structure 10 and, as well, usual structural members 52 , extending between structural members 36 .
[0036] In addition, FIG. 5 illustrates transverse bracing arrangements 54 between vertical beams 42 and shown consisting of horizontal members 56 and diagonal structure 58 . Diagonals 58 may comprise cables and the cables may be adjustable in tension.
[0037] End parts 24 and 26 are thus each self-supporting structures and each maintains its membrane in a stressed condition at all times.
[0038] It is noted that bracing structure is required to provide rigidity and tension to the end parts 24 and 26 , and variations on the support structure are therefore permissible so long as those criteria are maintained. Thus the bracing structure may vary for different environments.
[0039] [0039]FIGS. 7 and 8 illustrate details of pivot assemblies 28 , 30 . Pivot post 60 comprises pipe 62 which passes through the structure's concrete pad 64 and is embedded in concrete pile 66 . Pipe 62 may be filled with concrete 68 .
[0040] Brackets 74 and 76 are fixed to structure member 36 . Each bracket includes a cylindrical sleeve 78 .
[0041] In assemblies structure 10 , the sleeves 78 are slid over post 60 to form the pivot.
[0042] Each horizontal structural beam 40 is provided with wheel assemblies 48 and 50 . The wheel assemblies support the weight of the end parts so that the pivot assemblies do not carry the weight of the end parts. Additional wheel assemblies may be used if required.
[0043] Connecting and/or sealing means (not shown) are preferably provided between beams 39 and 41 in the closed position and between beams 37 and 43 and beam 45 main part 32 of structure 10 when the end parts are in the closed position.
[0044] In order to actually activate opening or closing of the assemblies 24 and 26 around pivot assemblies 28 and 30 , tow-bar attachments are provided at the bases 80 and 82 of the central arches 39 and 41 , which are the arches which will be adjacent when the door is in the closed position. An aircraft tug or other small motorized vehicle may then be used to open and close the assemblies.
[0045] As well, an integral drive arrangement (not shown) may be mounted on the opening assemblies for opening and closing parts 24 and 26 .
[0046] [0046]FIGS. 13 and 14 illustrate alignment pipe and skid plate assemblies 84 and 85 . The assemblies are mounted at selected locations between the arches 39 and 41 , which are located adjacent each other when the opening assemblies are in the closed position, and also between the end rib 45 of the stationary part of the stressed membrane structure and the adjacent ribs 37 and 43 of the opening assemblies when in the closed position.
[0047] Assemblies 84 and 85 comprise skid plates 86 and 88 and respective pairs of alignment pipes 90 and 92 . As the opening assembly is moved into the closed position, the camming angles 94 on pairs of pipes 90 and 92 ride alone skid plates 86 and 88 to align the adjacent beams.
[0048] The effect of the alignment is to transfer some of the load from the rolling sections of the assemblies to the overall structure to thus provide greater structural stability of the system. The skid plates also provide some friction between the opening assemblies and the stressed membrane structure to further facilitate load transfer from the opening assembly to the stationary structure.
[0049] [0049]FIGS. 11 and 12 illustrate a lock plate assembly 96 for holding doors in a locked position. The assembly 96 comprises fixed plates 98 and 100 from which project pins 102 and 104 . Lock plate 106 rotates on pin 104 . Lock plate 106 includes camming surface 108 which, during closing of the assemblies, rides up and over pin 102 . Recess 110 at the end of surface 108 then drops over pin 102 to lock the assemblies in the closed position.
[0050] Parts 24 and 26 are preferably additionally stabilized in the open and closed positions by the use of conventional aircraft tie-down systems.
[0051] [0051]FIGS. 9 and 10 illustrate inner and outer tie-down assemblies 112 and 114 respectively. Tie-down assemblies 112 and 114 include earth anchors 116 and 118 implanted below surface 119 . Cables 120 and 122 project from earth anchors 116 and 118 above surface 119 . The opening assemblies are provided with brackets 124 and 126 to correspond in positioning with projecting cables 120 and 122 respectively. When the opening assemblies are in position and ready for tie down in either the open or the closed position, load binders 128 or 130 are installed between the brackets and the projecting cable ends.
[0052] The inner tie-down is intended for installation on interior beam members while the outer tie-down is intended for installation on the outer arches.
[0053] Clearly, the tie-downs will vary in size, type, location, and quantity depending on door size and environmental conditions. In short, any kind of tie-down may be used depending on circumstances.
[0054] Suitable flashing will be installed along the line where the two halves of the opening assembly meet in the closed position and along the line between the two parts of the opening assembly and the stationary structure in the closed position.
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There is provided an opening assembly for an extended end of a stressed membrane structure having a fixed part, said opening assembly comprising: at least a part of said end separated from said fixed part and moveable relative to said fixed part; a pivot assembly for permitting movement of said at least a part of said extended end between an open and a closed position relative to said structure; a support frame for maintaining the integrity of said part in stressed membrane condition at all times during said movement and when in said open and closed position; rolling transport means for supporting said frame and said assembly during said movement.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an image forming method of using an aqueous liquid containing a dye to deposit the dye electrochemically, thereby forming an image, an image forming apparatus suitable for the image forming method, and a method for manufacturing a color filter using the image forming method.
2. Description of the Related Art
Methods for recording an image onto a recording medium such as paper based on an electric or optical signal, which are currently utilized in printers or the like include the dot impact recording method, the thermal transfer recording method, the thermal sublimation recording method, the ink jet recording method, and the electrophotographic method. These methods are roughly classified into three main groups.
The methods, which are included in the first group are methods of bringing a sheet in which dye molecules are dispersed, such as an ink ribbon or a donor film, into contact with a medium such as paper and then the dye molecules are transferred to the paper by a mechanical impact or heating, and include the dot impact recording method, the thermal transfer recording method, and the thermal sublimation recording method. In these methods, however, consumption articles other than ink and electric power are necessary. Energy efficiency is also low, and running costs are high. Furthermore, apart from the thermal sublimation recording method, the image quality obtained in these methods is poor.
The methods, which are included in the second group, are non-contact methods, and include an ink jet recording method of jetting ink from a ink head onto paper. The ink jet recording method does not require consumption articles other than ink and electric power. However, it is difficult to control the size of the ink dots, the flying direction thereof, or the like completely. Moreover, the ink jet recording method is not high in energy efficiency.
The methods, which are included in the third group, are methods of forming an image on paper via an intermediate transferring member, and include the electrophotographic method, in which toner is adhered onto a latent image on a photosensitive member which is formed by laser spots and then this latent image is transferred onto paper to form an image. In the electrophotographic method, a relatively sharp and fine image can be formed. However, in the electrophotographic method, high voltage is necessary for forming a latent image on the photosensitive member, absorbing the toner by the photosensitive member, and transferring the absorbed toner onto paper. Therefore, there occur problems such as a large amount of power is consumed and ozone and nitrogen oxides are generated.
All of the methods in the first, second and third groups also have the problem that, in general, the noise of the operation of forming an image is quite loud.
Furthermore, a method is known in which a solution, in which a pigment or a dye is dispersed in a polymer having electrodepositing ability, is used to form a electrodeposited film, although it is not as common as the above-mentioned methods.
Those of the methods as disclosed in, for example, Japanese Patent Application Laid-Open (JP-A) No. 60-23051 (Color Printing Apparatus), Japanese Patent Application Laid-Open (JP-A) No. 4-165306 (Method for Making a Color Filter), and Japanese Patent Application Laid-Open (JP-A) No. 7-5320 (Patterning Method, Electrodepositing-Master for Using the Method, and Method for Making a Color Filter And Optical Recording Medium). The electrodeposition film formed in these methods contains a dye which is fixed inside a polymer film as a supporting matrix. The dye content in the ectrodeposition film does not exceed 30%. Therefore, an image having only a low density proportional to the energy consumed energy can be obtained so as to resulting in problems about energy efficiency and cost. Furthermore, in such a method, the same number of dye-applying baths as the number of primary colors used in an additive color method or a subtractive color method are necessary for obtaining a color image or a color filter, and a single electrodeposition step is essential for every primary color.
In view of the above respective properties, an object of the present invention is to provide an image forming method in which a dye can be used to realize high image quality, and in which the density and color of an image can be adjusted, which has excellent safety, is environmentally friendly, and has low energy consumption.
Another object of the present invention is to provide an image forming method which makes the electrodepositing operation for obtaining a color image easier.
Still another object of the present invention is to provide an image forming apparatus using the above-mentioned image forming method.
A further object of the present invention is to provide a method for making a color filter using the above-mentioned image forming method.
SUMMARY OF THE INVENTION
The inventors paid attention to the fact that there are molecules, among water-soluble dye molecules, which can be independently precipitated by an electrochemical reaction from the aqueous solution in which they are dissolved, so as to complete the following present invention.
The first image forming method according to the present invention comprises the step of applying a voltage between a first electrode and a second electrode,
the first electrode being immersed into or brought into contact with an aqueous solution in which a group of two or more dyes having same polarities, and including at least one dye which can be independently precipitated from this aqueous solution by an electrochemical reaction, are dissolved and coexist at a specified pH, and the second electrode being provided so as to cooperate with the first electrode in causing the electrochemical reaction,
thereby forming on the first electrode a mixed color image which is composed of the group of dyes.
In this method, the dye which can be independently precipitated by an electrochemical reaction from the aqueous solution in which it is dissolved (the dye is referred to as a dye having a electrodeposition film forming ability, hereinafter) is deposited on the first electrode, while incorporating the other dyes, to form on the first electrode a mixed color image.
The dyes are provided in the form of an aqueous solution, and do not have harmful effects on the environment or the human body. Further, consumption articles such as ribbons are unnecessary, except for the dye and electric power. The voltage applied in forming an image is only from about 0.6 to about 3 V, therefore a very small amount of electric power is consumed. Thus, running costs are low. Moreover, a high density, good quality image can be obtained, since the image can contain a large amount of dye. In this method, the density of an image can also be controlled by controlling the voltage between the electrodes or the period of time the voltage is applied.
The second image forming method of the present invention comprises the step of applying voltage between a first and second electrode,
the first electrode being immersed into or brought into contact with an aqueous solution in which a group of two or more dyes having different polarities, and including at least one dye which can be independently precipitated from this aqueous solution by an electrochemical reaction, are dissolved and coexist at a specified pH, and the second electrode being provided so as to cooperate with the first electrode in causing the electrochemical reaction,
thereby forming, on at least the first electrode, a first mixed-color image composed of the group of dyes, or another mixed-color image composed of the group of dyes and whose colors are different to those of the first mixed-color image, or a single-color image composed of a single dye.
In the second image-forming method, a first mixed-color image, or another mixed-color image whose colors are different to those of the first mixed-color image, or a single-color image, and which is composed of the group of dyes, is formed on at least the first electrode. The specific mechanism of forming the mixed color image is not clear, but it is supposed that it occurs when a dye with one polarity is incorporated into a dye with a different polarity.
According to the second image forming method, it is possible to form an image having two colors from a single type of solution, reduce the steps of forming a color image, and make the operations for forming an image simple. It is also possible to adjust the density or color of an image by controlling the voltage between the electrodes or the period of time the voltage is applied.
The image forming apparatus according to the present invention comprises:
a bath for holding an aqueous solution in which a group of two or more dyes, including at least one dye which can be independently precipitated from this aqueous solution by an electrochemical reaction, are dissolved and coexist at a specified pH,
a first electrode which can be immersed into or brought into contact with the aqueous solution,
a second electrode provided so as to cooperate with the first electrode in causing the electrochemical reaction, and
a voltage applying means for applying voltage between the first and second electrodes.
The apparatus may also comprise a transferring means for transferring the image onto a recording medium.
This image-forming apparatus has the above-mentioned advantages, and makes it possible to form a dye image pattern on the electrode, and if desired, transfer the dye image onto a medium suitable for one's needs so as to form documents.
According to the color filter formation method of the present invention, a color filter can be formed in which an electrodeposited film serving as a single color image or a mixed color image is formed on a transparent electrode serving as the first electrode, using the above-mentioned image forming method.
This method makes it possible to form a color filter, with the above-mentioned advantages. That is, the formation method is greatly simplified in comparison to the prior art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic structured diagram of an apparatus used in the present invention.
FIG. 2 shows an absorption spectrum of an aqueous solution of Pro Jet Fast Yellow 2, which is an anionic dye used in the present invention.
FIG. 3 shows an absorption spectrum of a thin film of Pro Jet Fast Yellow 2, which is an anionic dye used in the present invention.
FIG. 4 shows an absorption spectrum of an aqueous solution of Cathilon Pure Blue 5GH, which is a cationic dye used in the present invention.
FIG. 5 shows an absorption spectrum of a thin film of Cathilon Pure Blue 5GH, which is a cationic dye used in the present invention.
FIGS. 6A and 6B are diagrams explaining the principle of the situation in which different electrodeposited films are formed according to the polarity of the electrodes.
FIG. 7 is a graph showing the relationship between the ratio of Y-peak to C-peak and values/polarities of the voltages applied to the electrodes.
FIG. 8 shows an absorption spectrum of a mixed color film.
FIG. 9 is a schematic structural diagram of an apparatus used in another embodiment according to the present invention.
FIG. 10 shows a substrate in which electrodes in a matrix form are formed on a supporting member used in the present invention.
FIG. 11 is a schematic structural diagram of an apparatus for simultaneously forming an electrodeposited film having two colors on the substrate shown in FIG. 10.
FIG. 12 is a schematic structural diagram of an apparatus for forming electrodeposited films having two colors one by one on the substrate shown in FIG. 10.
FIG. 13 is a schematic structural diagram of an apparatus for transferring the electrodeposited film having two colors formed on the substrate shown in FIG. 10.
FIG. 14 is a schematic structural diagram of an apparatus which is used in the present invention and makes it possible to form an image and transfer the image.
FIG. 15 is a schematic structural diagram of apparatus which is used in another aspect of the present invention and makes it possible to form an image and transfer the image.
FIG. 16 shows an absorption spectrum of a mixed film of a color filter, being a mixed film which is composed of Pro Jet Fast Yellow 2 and Cathilion Pure Blue 5GH, formed on a transparent substrate.
FIG. 17 shows an absorption spectrum of an electrodeposited film of a color filter, being an electrodeposited film which is composed of Cathilion Pure Blue 5GH formed on a transparent substrate.
FIG. 18 illustrates a pattern having two colors obtained from the substrate shown in FIG. 11.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will be explained in detail below.
In the present invention, there is used an aqueous liquid in which a group of two or more dyes are dissolved and coexist at a specific pH value, the dyes including at least one dye which can be independently precipitated from this aqueous solution wherein the dye is dissolved by an electrochemical reaction.
For example, Rose Bengal and eosin, which are fluorescein type dyes, are water-soluble when the pH is 4 or more, but are oxidized to be water-insoluble and be precipitated when the pH is lower than 4. Similarly, diazo-based, Pro Jet Fast Yellow 2 (manufactured by Zeneca Colours Marking Inc.) is water-soluble when the pH is 6 or more, but is precipitated when the pH is lower than 6. For reference, FIG. 2 shows the absorption spectrum of an aqueous solution of Pro Jet Fast Yellow 2 having a concentration of 20 μM.
When a solution, in which such a dye has been dissolved in pure water, is energized (pH 6 to 8), the dye is oxidized to be water-insoluble, thereby forming an electrodeposited film composed of the dye molecules on the anodic electrode. When a voltage is applied between electrodes so that the electrode on which the electrodeposited layer is formed becomes the cathode or when this electrode is immersed into an aqueous solution having a pH of 10 to 12, the dye in the electrodeposited film is reduced to be eluted in the aqueous solution again. For reference, FIG. 3 shows the absorption spectrum of an electrodeposited film of Pro Jet Fast Yellow 2 formed on a transparent electrode of ITO.
An oxazine type of basic dye Cathilon Pure Blue 5CH (C.I. Basis Blue 3) [manufactured by Hodogaya Chemical Co., Ltd.], which is a quinoneimine dye, or a thiazine type of basic dye, Methylene Blue (C.I. Basis Blue 9) is water-soluble when the pH is 10 or less, but is reduced to be water-insoluble and precipitated when the pH is higher than 10. Cathilon Pure Blue 5GH is easily dissolved into pure water so as to be present therein as a cation, but is water-insoluble and precipitated when the pH is 11 or more. For reference, FIG. 4 shows the absorption spectrum of an aqueous solution of Cathilon Pure Blue 5GH having a concentration of 20 μM.
When such a dye is dissolved in pure water and energized, the dye is reduced to form an electrodeposited film composed of the dye molecules on the cathodic electrode. When a voltage is applied between the electrodes so that the electrode on which the electrodeposited film is formed becomes an anode or when this electrode is immersed into an aqueous solution having a pH of 8 or lower, the dye in the electrodeposited film is oxidized to be eluted in the aqueous solution again. For reference, FIG. 5 shows the absorption spectrum of an electrodeposited film of Cathilon Pure Blue 5GH formed on a transparent electrode of ITO.
As the dye which can be independently precipitated from the aqueous liquid wherein the dye is dissolved, and be used in the present invention (the dye is referred to as a "a dye having electrodeposition film forming ability" hereinafter), there is used a color former which can exhibit a color-developing structure under external stimulation from an acid, a base, and the like. Examples thereof include triphenylmethanephthalide, phenoxazine, phenothiazine, fluoran, indolylphthalide, spiropyran, azaphthalide, diphenylmethane, chromenopyrazole, leucoauramine, azomethine, rhodaminelactam, naphtholactam, and triazene types, more specifically rose Bengal, Pro Jet Fast Yellow 2, and Cathilon Pure Blue 5GH.
The dyes having the chemical structure represented by the general formula (1) have the above-mentioned characteristic.
In the image recording method of the present invention, as the dye which can be independently precipitated from the aqueous solution in which the dye is dissolved,
General formula (1): ##STR1##
In the general formula (1), Ar 1 and Ar 2 each independently represent an aryl or substituted aryl group. At least one of Ar 1 and Ar 2 has at least one substituent selected from a --COSH group and a --COOH group. J 1 and J 2 each independently represent a group expressed by the formulas (1), (2), or (3) shown below. L represents a bivalent organic linking group. X independently represents a carbonyl group or a group expressed by the formulae (4), (5) or (6). R 1 to R 4 each independently represent an alkyl or substituted alkyl group. The symbol "n" is 0 or 1. ##STR2##
In the formulae (1) to (3), R 5 represents a group selected from H, an alkyl group, a substituted alkyl group, an alkoxy group, a halogen atom, --CN, a ureido group, and --NHCOR 6 wherein R 6 represents H, an alkyl group, a substituted alkyl group, an aryl group, a substituted aryl group, an aralkyl group, or a substituted aralkyl group. T represents an alkyl group. W represents a group selected from the group consisting of H, --CN, --CONR 10 R 11 , a pyridinium group, and --COOH; m represents an alkylene chain having 2 to 8 carbon atoms; and B represents H, an alkyl group or --COOH, in which R 10 and R 11 each independently represent an alkyl or substituted alkyl group. ##STR3##
In the formulae (4) to (6), Z represents --OR 7 , --SR 7 , or --NR 8 R 9 ; Y represents H, Cl, or CN; and E represents Cl or CN, in which each of R 7 , R 8 , and R 9 represents an alkyl or substituted alkyl group, an alkenyl or substituted alkenyl group, an aryl or substituted aryl group, an aralkyl or substituted aralkyl group, and R 8 and R 9 may constitute a 5 or 6-membered ring together with a bonded N atom.
Specific examples of the dye represented by the general formula (1) relating to the present invention are shown below, but the dyes which can be used are not limited to the specific examples having the following chemical structures.
Compound (Example-1) ##STR4## Compound (Example-2) ##STR5## Compound (Example-3) ##STR6## Compound (Example-4) ##STR7## Compound (Example-5) ##STR8## Compound (Example-6) ##STR9## Compound (Example-7) ##STR10## Compound (Example-8) ##STR11## Compound (Example-9) ##STR12## Compound (Example-10) ##STR13## Compound (Example-11) ##STR14## Compound (Example-12) ##STR15## Compound (Example-13) ##STR16## Compound (Example-14) ##STR17## Compound (Example-15) ##STR18## Compound (Example-16) ##STR19## Compound (Example-17) ##STR20## Compound (Example-18) ##STR21## Compound (Example-19) ##STR22## Compound (Example-20) ##STR23## Compound (Example-21) ##STR24## Compound (Example-22) ##STR25## Compound (Example-23) ##STR26## Compound (Example-24) ##STR27## Compound (Example-25) ##STR28## Compound (Example-26) ##STR29## Compound (Example-27) ##STR30## Compound (Example-28) ##STR31## Compound (Example-29) ##STR32## Compound (Example-30) ##STR33##
As a dye which has no electrodeposition layer forming ability and may be used together with a dye having a electrodeposition layer forming ability, any ionic dye can be selected. Examples of the ionic dye include acridine, azaphthalide, azine, azulenium, azo, azomethine, aniline, amidinium, alizarin, anthraquinone, isoindoline, indigo, indigoid, indoaniline, indolylphthalide, oxazine, carotenoid, xanthine, quinacridon, quinazoline, quinophthalone, quinoline, quinone, guanidine, chrome chelate, chlorophyll, ketone imine, diazo, cyanine, dioxazine, bisazo, diphenylmethane, diphenylamine, squarilium, spiropyran, thiazine, thioindigo, thiopyrilium, thiofluoran, triallyl methane, trisazotriphenyl methane, triphenly methane, triphenylmethanephthalide, naphthalocyanine, naphthoquinone, naphthol, nitroso, bisazooxadiazole, bisazo, bisazostilbene, bisazohydroxyperinone, bisazofluorenone, bisphenol, bislactone, pyrazolone, phenoxazine, phenothiazine, phthalocyanine, fluoran, fluoren, flugid, perinone, perylene, benzimidazolone, benzopyran, polymethine, porphyrin, methine, merocyanine, monoazo, leucoauramine, leucoxanthine, and rhodamine type synthesized dyes; and natural dyes such as a turmeric, gardenia, red-malt, scallion, grape vine, beet, perilla, berry, corn, cabbage, and cacao.
In the present invention, the pH of the aqueous solution is adjusted so that two or more dyes can coexist without producing a complex or precipitation.
When the dyes contained in the aqueous solution have the same polarity (that is, are all anionic dyes, or cationic dyes), the above-mentioned coexistence can be easily accomplished.
However, when an anionic or cationic dye aqueous solution (e.g., an aqueous solution of anionic Rose Bengal) is mixed with a dye aqueous solution containing a polymer compound (e.g., polyethyleneimine) having a polarity different from the anionic or cationic dye aqueous solution, they are neutralized producing a precipitate. However, since a dye having a electrodeposition film forming ability is used in the present invention to form an image, a polymer compound is not an essential requirement. Dyes having different polarities can also coexist easily in the aqueous solution.
According to the present invention, an aqueous solution in which two or more dyes coexist is energized thus forming an image.
When a mixture solution, in which two dyes having the same polarity are mixed, is energized, an electrodeposited film having the same color as that of the mixture solution is formed on the electrode having the opposite polarity to that of the dyes. When, for example a mixture solution of Rose Bengal (red), which is an anionic dye having a electrodeposition film forming ability, and Brilliant Blue (blue), which is an anionic dye not having this ability, are energized, a purple electrodeposited film, which is the same color as the mixture solution, is formed on the anode. This is because Rose Bengal is oxidized to be deposited on the anode while incorporating the ions of the Brilliant Blue. In such a way as described above, a mixed-color image is generally obtained if dyes having the same polarity are mixed. As understood from this example, it is sufficient if only one dye has the electrodeposition film forming ability when two dyes having the same polarity are mixed.
On the contrary, when a solution, in which two dyes having different polarities are mixed, is energized, different images can be formed dependently according to the polarity of the voltage applied to electrodes.
When dyes having different polarities are used, it depends on the properties of the dyes whether a single-color image is formed or a mixed-color image resulting from the mixed dyes is formed. For this reason, it is important to combine the optimal dyes for forming an image of the desired color.
In the case of an aqueous solution in which, for example, Pro Jet Fast Yellow 2 (yellow), which is an anionic dye having the electrodeposition film forming ability, is mixed with Cathilon Pure Blue 5GH (blue), which is a cationic dye having the electrodeposition film forming ability, the color of the solution is green. This is the color resulting from the mixture of these two colors. As shown in FIG. 6A, when this solution is energized, the anionic dye A (Pro Jet Fast Yellow 2) is oxidized to be deposited on an anode E1 while taking in the cationic dye C (Cathilon Pure Blue 5GH), thereby forming an electrodeposited film F1 having the same color (i.e., green) as the mixture solution. On the other hand, as shown in FIG. 6B, a blue electrodeposited film F2 is formed on a cathode E2. This blue color is substantially the same as that of Cathilon Pure Blue 5GH, i.e., the cationic dye C alone (in forming the film, the light yellow results from faded Cathilon Pure Blue 5GH). As understood from this, in the case of a mixture solution containing a mixture of two dyes having the electrodeposition film forming ability and different polarities, this ability of the respective dyes is not lost. When this solution is energized, electrodeposited films having different colors can be formed on the respective electrodes. In this example, at least one of each of the dyes having same polarity has the electrodeposition film forming ability. However, only one of the dyes having either polarity may have the electrodeposition film forming ability.
The amount of dye to be deposited on the electrode changes according to Faraday's law. Therefore, the thickness of the electrodeposited film can be changed successively by controlling at least one of the applied voltage, the applied electric charge, or the applied current in forming a film, or the length of time any one of them is applied. In other words, the density of the electrodeposited film (i.e., the image density) can be changed by controlling, for example, the applied voltage.
In the present invention, the color of the electrodeposited film (i.e., the image color) can be changed by controlling, for example, the applied voltage. FIG. 7 is a graph showing the relationship between the value/polarity of the voltage applied to electrodes and the ratio of the Y-peak (see below) to the C-peak, in the present invention method using a 1:1 mixture solution of Cathilon Pure Blue 5GH and Pro Jet Fast Yellow 2. The Y-peak and the C-peak represent the height of the absorption maximum point in the absorption spectrum of a Pro Jet Fast Yellow 2 electrodeposited film, and that in the absorption spectrum of a Cathilon Pure Blue 5GH electrodeposited film, respectively (see FIG. 7). FIG. 7 demonstrates that the ratio of the Y-peak to the C-peak, that is, the color of the electrodeposited film can be changed by changing the value and the polarity of the voltage applied to the electrodes.
In the present invention, the total concentration of dyes in a solution is usually from 0.1 mM to 1 M. The percentage of each of the dyes is not limited. In the case where a dye which does not have the electrodeposition film forming ability is included, the ratio of this dye to the dye having the ability may be, for example, from 1/99 to 10/1.
FIGS. 1 and 9 illustrate apparatuses for forming an image on an electrode by the method according to the present invention.
In the apparatus illustrated in FIG. 1, the first and second electrodes 1 and 2 are connected to a non-illustrated power supply, the electrodes 1 and 2 being platinum electrodes, and immersed into an aqueous solution 3 in which two sorts of dyes are dissolved. A saturation calomel electrode 5 as a reference electrode is immersed into a KCl saturated aqueous solution 4 electrically connected to aqueous solution 3 through a salt bridge 6. The saturation calomel electrode 5 is connected to the power supply through a non-illustrated potentiometer. If the aqueous solution 3 is, for example a mixture solution of Rose Bengal (red) and Brilliant Blue (blue) in this apparatus, when a voltage is applied between the platinum electrodes 1 and 2 so that the platinum electrode 1 is an anode, a purple electrodeposited film is formed on the platinum electrode 1. If the aqueous solution 3 is a mixture of Pro Jet Fast Yellow 2 (yellow) and Cathilon Pure Blue 5GH (blue), a green electrodeposited film is formed on the platinum electrode which has functioned as an anode, and a blue electrodeposited film is formed on the platinum electrode which has functioned as a cathode.
On the contrary, in the apparatus shown in FIG. 9, only the first electrode, i.e., the platinum electrode 1 is immersed into the aqueous solution 3, and the second electrode, that is, the plutonium electrode 2 is immersed into a KCl saturated aqueous solution 8 electrically connected to the aqueous solution 3 through a salt bridge 7. The platinum electrodes 1 and 2 are connected to a non-illustrated power supply. The saturation calomel electrode 5 as a reference electrode is immersed into the KCl saturated aqueous solution 4 electrically connected to a KCl saturated aqueous solution 8 through the salt bridge 6. The saturation calomel electrode 5 is connected to the power supply through a non-illustrated potentiometer. If the aqueous solution 3 is, for example a mixture solution of Rose Bengal (red) and Brilliant Blue (blue) in this apparatus, when a voltage is app lied between the platinum electrodes 1 and 2 so that the platinum electrode 1 is an anode, a purple electrodeposited film is formed on the platinum electrode 1. If the aqueous solution 3 is a mixture solution of Pro Jet Fast Yellow 2 (yellow) and Cathilon Pure Blue 5GH (blue), when a voltage is applied between the platinum electrodes 1 and 2 so that the platinum electrode 1 is an anode, a green electrodeposited film is formed on the platinum electrode 1. When a voltage is applied between the platinum electrodes 1 and 2 so that the platinum electrode 1 is a cathode, a blue electrodeposited film is formed on the platinum electrode 1. In this way, dye films of the two colors can be obtained from a single type of mixture solution merely by changing the polarity of the voltage applied to the electrodes.
In the apparatuses shown in FIGS. 1 and 9, the voltage applied between the electrodes 1 and 2 is usually from 0.6 to 3 V.
As shown by a substrate 80 in FIG. 10, in order to form an image having two colors on the same substrate, it is necessary to beforehand separate a surface area of a substrate into an area to which a positive voltage is to be applied and an area to which a negative voltage is to be applied. The electrode substrate 80 has a supporting body 82 composed of an insulator such as glass, and electrodes (e.g., platinum electrodes) 84 in a matrix on the supporting body 82. Preferably, the respective electrodes 84 are arranged and wired so that the desired positive or negative voltage is independently applied to the respective electrodes 84.
The substrate 80 is used as shown in FIG. 11. That is, the two electrodes or areas on the substrate 80 are connected to each other through a direct current power supply 81, and the substrate 80 is immersed into an aqueous solution 86 in which two or more dyes having different polarities are dissolved. When a voltage is applied between the electrodes or the areas, two images are simultaneously formed, one of the images being a single color image composed of the single dye, and the other being a mixed color image composed of the two or more dyes. FIG. 11 illustrates the substrate 80 wherein the single color image is formed on areas P and the mixed color image is formed on areas N. This method uses the same principle that is used in the apparatus shown in FIG. 1, and the substrate 80 has the first and second electrodes.
On the other hand, as shown in FIG. 12, a counter electrode 92, two direct current power supplies 94 and 95, and a switch 93 are prepared, and then the switch 93 is connected to the counter electrode 92, a nd power supplies 94 and 95 so that the counter electrode 92 can be connected to the negative side of the power supply 94 or the positive side of the power supply 95. The positive side of the power supply 94 and the negative side of the power supply 95 are connected to an arbitrary electrode or areas on the substrate 80, and then the substrate 80 is immersed into an aqueous solution in which two or more dyes having different polarities are dissolved. When the switch 93 is switched to the side of the power supply 94, a single color image or a mixed color image is formed on the arbitrary electrode or area on the substrate 80. When the switch 93 is switched to the side of the power supply 95, a mixed color image or a single color image is formed on the arbitrary electrode or area on the substrate 80. According to this method, a single color image and a mixed color image can be formed successively. In this case, the counter electrode 92 may be immersed into the aqueous solution, together with the substrate 80, or be immersed into an aqueous solution different from the aqueous solution into which the substrate 80 is immersed, by using a salt bridge. In the present method, the plurality of electrodes on the substrate 80 and the counter electrode 92 correspond to the first electrode and the second electrode, respectively.
According to the present invention, when a transparent substrate is used as the electrode in the above-mentioned apparatus, a color filter can be made wherein a single or a mixed color electrodeposited film is formed on the transparent substrate.
In the present invention, an image formed on the electrode may be transferred onto an image receiving medium such as paper. Conventional methods for such transfer include using static electricity, pressure, adhesion, chemical bonding force, wettability, or the like to transfer an image formed on an electrode by a deposition phenomenon. According to the present invention, the two following methods are preferred for transferring an image formed on the electrode onto an image receiving medium. The first is a method of bringing the electrode having a formed image into contact with the image receiving medium and pressing them to transfer the image from the electrode to the medium. As shown in FIG. 13, the other is a method of arranging the substrate 80 having a formed image and the counter electrode 92 so that they face each other, arranging an image receiving medium 96 between the substrate 80 and the counter electrode 92, and applying a voltage between the electrode 84 and the counter electrode 92 so that the polarity of the electrode 84 on the substrate 80 will be opposite to the polarity at the time the image film was formed. In this method, the dye adhering to the electrode 84 is moved toward the counter electrode 92, to transfer the dye onto the image receiving medium 96 arranged between the electrode 84 and the counter electrode 92. When the image on the electrode has a difference in density, that is, light and shade, it is possible to forma transferred image corresponding to this image. The density of the transferred image may be adjusted by controlling, for example, the applied voltage during the formation of an image film and accordingly adjusting the density of the image on the electrode, as described above. Alternatively, the density of the transferred image may be adjusted by controlling at least one of the voltage, the electric charge and the electric current applied in the transfer, or the length of time for which they are applied.
The apparatus according to the present invention may have a means for removing any image-constituting particles remaining on the surface of the image supporting member (the remaining deposited dye particles) after the transfer. The method for removing the particles may be any known method including using a blade, a fur brush, an elastic roller, a cleaning web, or an air knife.
FIG. 14 shows the schematic structure of a apparatus for forming an image on an electrode and transferring the formed image onto an image receiving medium by press. The apparatus shown in FIG. 14 has a roll 115 which can rotate along the direction shown by an arrow B. On the outer surface of the roll 115, a plurality of the first electrodes are formed which are divided into fine sections. Below the roll 115, a bath 114 containing a mixture solution 113 of dyes is arranged so that the electrodes positioned at the bottom of the roll 115 contact the mixture solution 113 or are immersed into the solution 113. The second electrode 112 is immersed into the bath 114. A transferring roll 116 is located over the roll 115. A paper 117 is fed between both the rolls 115 and 116. A cleaning blade 118 for removing dyes remaining on the roll 115 is provided at the downstream side, which is viewed from the transferring roll 116, of the rotation direction of the roll 115. The apparatus of FIG. 14 also has a controller 119 connected to the respective first electrodes arranged on the outer surface of the roll 115, and the second electrode 112. By control of the controller 119, a voltage is applied between the first electrodes on the roll 115 and the second electrode 112, so that the respective electrodes on the roll 115 will independently function as anodes or cathodes.
In this apparatus, an electrodeposited film 111 formed on the first electrodes on the roll 115 is transferred by pressing the transferring roll 116 onto the paper 117 fed between the film 111 and the transferring roll 116 when the first electrodes on which the film 111 is formed are shifted to the top of the roll 115.
FIG. 15 illustrates the schematic structure of a apparatus for forming an image on an electrode and then transferring the formed image onto an image receiving medium by applying a voltage. This apparatus is different from the apparatus shown in FIG. 14 in that a transferring roll 120 whose outer surface is composed of a conductive material is connected to the controller 119. In this apparatus, a voltage is applied between the electrode on which the electrodeposited film 111 and the transferring roll 120 so that the polarity of the electrodes will be opposite to its polarity at the time an image was formed. Thus, the electrodeposited film 111 is transferred onto the paper 117. In this apparatus, water having the desired pH value may be applied to the paper 117 during the transfer of the image.
As illustrated in FIGS. 14 and 15, images can be formed successively by arranging a plurality of the first electrodes on a roll.
To print a color image having three or more colors according to the present invention, an apparatus composed of combination of the apparatus shown in FIG. 14 or FIG. 15 with the same apparatus, or an apparatus having a roll, two baths containing two different sorts of mixture solutions, each of which contains two or more sorts of dyes, and a washing bath containing washing water may be used.
In the present invention, the raw materials of the first and second electrodes are not limited, and may be a metal, or an organic or inorganic semiconductor. An electrochemically stable material, such as a noble metal is preferred, for example, platinum or gold, or carbon. The transparent substrate for manufacturing a color filter may be one wherein an electrode made of, e.g., ITO or a conductive polymer, is formed on a transparent support made of, e.g., glass or a transparent film.
EXAMPLES
The following describes the present invention on the basis of specific examples.
Example 1
In the apparatus shown in FIG. 9, an aqueous solution (pH=7.2) was used which was a mixture of a 0.02 M Rose Bengal aqueous solution (red) and a 0.02 M BRILLIANT BLUE aqueous solution (blue). When voltage was applied between the platinum electrodes 1 and 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was +1.0 V, a purple (a mixed color) thin film was formed on the platinum electrode 1. The platinum electrode 1 was withdrawn from the aqueous solution, and then, using the apparatus shown in FIG. 13 paper was interposed between the counter electrode 92 and the platinum electrode 1. When a voltage of -2.0 V was applied between these electrodes, an image composed of a purple thin film was formed on the paper.
This example demonstrates that an mixed color electrodeposited film can be formed from the mixture solution of a dye having a electrodeposition film forming ability and a dye having the same polarity as the first dye but not having this ability, and that the image can be transferred onto paper by applying a voltage to the first electrode and the counter electrode so that the polarity of the first electrode will be opposite to the polarity which it had during formation of the film.
Example 2
In the apparatus shown in FIG. 9, an aqueous solution (pH=7.2) was used which was a mixture of a 0.02 M Pro Jet Fast Yellow (manufactured by Zeneca Colour Marking Inc.) aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH (manufactured by Hodogaya Chemical Co., Ltd.) aqueous solution (blue). When voltage was applied between the platinum electrodes 1 and 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was become +2.0 V, a green (a mixed color) thin film was formed on the platinum electrode 1. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a green thin film on the paper.
In the apparatus shown in FIG. 9, voltage was applied between the platinum electrodes 1 and 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was -2.0 V, a light yellow thin film was formed on the platinum electrode 1. After one minute, the color of the thin layer turned to blue. Subsequently, the platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a blue thin film on the paper.
This example demonstrates that images having two colors can be obtained from a mixture solution of two sorts of dyes having different polarities and that the images can be transferred onto paper by pressure.
Example 3
In the apparatus shown in FIG. 9, an aqueous solution was used which was a mixture of a 0.02 M Pro Jet Fast Yellow aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH aqueous solution (blue). When voltage was applied between the platinum electrodes 1 and 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was +2.0 V, a green (a mixed color) thin film was formed on the platinum electrode 1. The platinum electrode 1 was withdrawn from the aqueous solution, and then, using the apparatus shown in FIG. 13, paper was interposed between the counter electrode 92 and the platinum electrode 1. When a voltage of -2.0 V was applied between these electrodes, an image composed of a green thin film was formed on the paper.
In the apparatus shown in FIG. 9, volt age was applied between the platinum electrodes 1 and 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was -2.0 V, a blue thin film was formed on the platinum electrode 1. The platinum electrode 1 was withdrawn from the aqueous solution, and then, using the apparatus shown in FIG. 13, paper was interposed between the counter electrode 92 and the platinum electrode 1. When a voltage of +2.0 V was applied between these electrodes for 30 seconds, an image composed of a blue thin film was formed on the paper.
This example demonstrates that images having two colors can be obtained from a mixture solution of two sorts of dyes having different polarities and that the image can be transferred on paper by applying a voltage between the first electrode and the counter electrode so that the polarity of the first electrode will be opposite to the polarity it had during formation of the film.
Example 4
In the apparatus shown in FIG. 9, in which an ITO electrode formed on a glass substrate was used as the first electrode, an aqueous solution was used which was a mixture of a 0.02 M Pro Jet Fast Yellow aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH aqueous solution (blue). When voltage was applied between the ITO electrode and the platinum electrode 2 for 30 seconds so that the potential difference between the saturation calomel electrode 5 and the ITO electrode/platinum electrode 2 was +2.0 V, a green (a mixed color) thin film was formed on the ITO electrode. The absorption spectrum of this film at this time is shown in FIG. 16.
When voltage was applied between the ITO electrode and the platinum electrodes 2 for 90 seconds so that the potential difference between the saturation calomel electrode 5 and the ITO electrode/platinum electrode 2 was -1.0 V, a blue thin film was formed on the ITO electrode. The absorption spectrum of this film at this time is shown in FIG. 17.
This example demonstrates that it is possible to form a dye film which can be used as a color filter on a transparent electrode. The absorption spectra clearly demonstrate that the resultant dye films are different depending on the polarity of the applied voltage.
Example 5
In the apparatus shown in FIG. 9, an aqueous solution was used which was a mixture of a 0.02 M Pro Jet Fast Yellow aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH aqueous solution (blue). When voltage was applied between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 for periods of 20 seconds, so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 rose from 0 V to +3.0 V at intervals of +0.5 V, green (a mixed color) thin films having different dye densities were formed on the platinum electrode 1 depending on the applied voltages. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a green thin film having an image density depending on the applied voltage on the paper.
Subsequently, in the apparatus shown in FIG. 9, when voltage was applied between the saturation calomel electrode 5 and the platinum electrodes 1, 2 for periods of 20 seconds, so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 rose from 0 V to -3.0 V at intervals of -0.5 V, blue thin films having different dye densities were formed on the platinum electrode 1 depending on the applied voltages. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a blue thin film having an image density depending on the applied voltage on the paper.
This example demonstrates that images having two colors can be obtained from a mixture solution of two sorts of dyes, and that the thickness of the dye films, that is, the density of the images is changed by the applied voltage to obtain transferred images having different image density.
Example 6
In the apparatus shown in FIG. 9, an aqueous solution was used which was a mixture of a 0.02 M Pro Jet Fast Yellow aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH aqueous solution (blue). Voltage was applied between the saturation calomel electrode 5 and the platinum electrodes 1 and 2, so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was +2.0 V. This was repeated while the period of time the voltage was applied was increased from 0 to 50 seconds at intervals of 10 seconds. As a result, green (a mixed color) thin films having different dye densities were formed on the platinum electrode 1 depending on the period the voltage was applied for. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image on the paper composed of a green thin film having an image density depending on the period the voltage was applied for.
Subsequently, in the apparatus shown in FIG. 9, a voltage was applied between the saturation calomel electrode 5 and the platinum electrodes 1 and 2, so that the potential difference between the saturation calomel electrode 5 and the platinum electrodes 1 and 2 was -2.0 V. This was repeated while the period of time the voltage was applied for was increased from 0 to 50 seconds at intervals of 10 seconds. As a result, blue thin films having different dye densities were formed on the platinum electrode 1 depending on the period the voltage was applied for. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image on the paper composed of a blue thin film having an image density depending on the period the voltage was applied for.
This example demonstrates that images having two colors can be obtained from a mixture solution of two types of dyes, and that the thickness of the dye films, that is, the density of the images is changed by the period of time the voltage is applied to obtain transferred images having different image densities.
Example 7
In the apparatus shown in FIG. 9, an aqueous solution was used which was a mixture of a 0.02 M Pro Jet Fast Yellow aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH aqueous solution (blue). When a platinum electrode 1 was energized in 10 second periods, so that the electric current flowing through the platinum electrode 1 (whose surface area is 2 cm 2 ) increased from 0 mA to +10 mA at intervals of +1 mA, green (a mixed color) thin films having different dye densities were formed on the platinum electrode 1 dependent on the amperage of the energizing electric current. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a green thin film having an image density dependent on the amperage of the energizing electric current on the paper.
Subsequently, in the apparatus shown in FIG. 9, when a platinum electrode was energized in 10 second periods, so that the electric current flowing through the platinum electrode 1 increased from 0 mA to -10 mA at intervals of -1 mA, blue thin films having different dye densities were formed on the platinum electrode 1 dependent on the amperage of the energizing electric current. The platinum electrode 1 was withdrawn from the aqueous solution, and then was brought into contact with paper under pressure so as to form an image composed of a blue thin film having an image density dependent on the amperage of the energizing electric current on the paper.
This example demonstrates that images having two colors can be obtained from a mixture solution of two sorts of dyes, and that the thickness of the dye films, that is, the density of the images is changed by the amperage of the energizing electric current to obtain transferred images having different image densities.
Example 8
By sputtering, a substrate 80 shown in FIG. 10 was made which had a platinum electrode in a matrix form on a glass base. The electrode on the base was separated into an area for marking in a green color (the first electrode) and an area for making in a blue color (the second electrode) .AS shown in FIG. 11, the first and the second electrodes were connected to each other and then the electrodes were immersed into a mixture of a 0.02 M Pro Jet Fast Yellow (manufactured by Zeneca Colour Marking Inc.) aqueous solution (yellow) and a 0.02 M Cathilon Pure Blue 5GH (Hodogaya Chemical Co., Ltd.) aqueous solution (blue). When voltage of 4 V was applied between the electrodes of both areas for 20 seconds in such a way that the electrode of the area for marking in a green color would be an anode, a thin film having a green color (a mixed color) was formed on the anode. Alternatively, a thin film having a blue color was formed on the cathode. After that, the substrate 80 was brought into contact with paper under pressure so as to form at the same time a pattern on the paper having both green and blue colors, as shown in FIG. 18.
This example demonstrates that an image having two colors can be obtained from a mixture solution of two sorts of dyes by applying a voltage once and that an image having two colors can be obtained by a single transfer.
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A voltage is applied between a first and second electrode, the first electrode being immersed into an aqueous solution in which a group of two or more dyes having different polarities, and including at least one dye able to be independently precipitated from this aqueous solution by an electrochemical reaction, are dissolved and coexist at a specified pH, and the second electrode being provided so as to cooperate with the first electrode in causing the electrochemical reaction, thereby forming a first mixed color image which is composed of the group of dyes, or another mixed color image whose colors are different to those of the first mixed color image and which is composed of the group of dyes, or a single color image which is composed of a single dye on the electrode. Thus, it is possible to realize a high quality image using dyes and safely and simply record an image at a high levels of flexibility. It is also possible to adjust the density of an image easily, and reduce the effects on the environment and energy consumption.
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This application claims the priority of Provisional Patent Application No. 61/972,642 filed on Mar. 31, 2014.
BACKGROUND OF THE INVENTION
Field of the Invention
The present invention relates to the manufacture of nonwoven materials and, more particularly, to a new and improved method and apparatus for producing nonwoven materials of any suitable thickness and/or composition.
Description of the Background Art
At the present time, substantially all needle looms for producing nonwoven materials such as felt have a maximum opening between the stripper plate for the needles and the upper surface of the supporting bed having holes for receiving the needles of about 3½ inches. Accordingly, the maximum thickness of needle felts produced by existing needle looms is about 1¾ inches and the maximum density is about 170 oz per square yard of product. This is because the number and pattern of needles is limited for the reason that the present needle looms are constructed so that the needles pass through the product to be needled and into aligned openings in the upper surface of the supporting bed. The number and pattern of needles, therefore, is limited by the pattern of openings in the supporting bed.
Current needle looms are constructed so that the vertical movement of the needle bed is limited to 1 9/16 inches to 3 inches.
Also, the speed of the material being advanced through the current needle looms is limited by the fact that the needles extend through the material into the openings in the supporting bed. Because the needles enter the openings in the supporting bed, they are subject to breakage if, for some reason, they are not properly aligned with the openings in the support bed.
As a result of the current needle loom constructions, the production of needle felts or nonwoven materials is limited to materials of small thickness, such as 1¾ inches maximum and this limitation limits the uses of such needle felts or nonwoven materials.
A need has risen, therefore, for a new and improved method and apparatus for producing needle felts and other nonwoven materials that can be used for any suitable or desired applications. The present invention meets this need and allows the creation of any density or oz per sq yd to any thickness requirement above the standard needling of 170 oz per sq. yard and 1¾″ thick. It also allows any desired or suitable synthetic fibers to be added to needle felts throughout the build, such as, e.g., ceramic fiber, high-purity alumina, zirconia, silica spun ceramic fibers or a base rayon viscose or cellulose base product prior to carbonization.
BRIEF SUMMARY OF THE INVENTION
In accordance with the present invention, a carded batt of any suitable material or combination of materials is advanced from a roll or in flat form on a feed apron into a needle loom that is constructed to vary the opening between the stripper plate or bed for the needles and the supporting bed for the batt to any suitable or desired size, e.g., a few inches to many feet as desired. As the batt is advanced through the needle loom, the needles in any suitable or desired pattern and density are reciprocated at any suitable or desired speed to penetrate the batt to tangle the fibers together and make the batt thinner, more compact and tighter as a result of the reciprocating movement of the needles generally in accordance with known technology. In the apparatus of the present invention, however, the needles do not extend completely through the batt into any holes in the supporting bed. Accordingly, the supporting bed may be of lighter construction, the needles may have limited lateral movement without worrying about breakage, and the reciprocating speed of the needles can be increased over the speed used in current needle looms. The needles may be of any suitable construction depending on the materials in the batt.
The distance between the stripper plate or needle bed and the support bed is adjusted to accommodate the thickness of the batt and the desired needle penetration thereof. The adjustment is accomplished by vertical movement of the support bed for the batt or vertical movement of the bed supporting the needles.
After the batt is needled and leaves the needle loom, it may be conveyed on a take up apron or the like to an apparatus for lifting the batt, turning it over to an inverted position and moving it again to the feed apron to be advanced into the same needle loom or another needle loom such that the batt is needled from the opposite side in both directions in a manner similar to that of the first needle penetration of the batt.
Thereafter, the double needled batt is removed from the needle loom by a suitable take up apron or the like and is moved to a position wherein it can be fed to the same or a different needle loom. Before advancing the double needled batt into the needle loom, another batt of any desired or suitable material is positioned on the double needled batt, the distance between the stripper plate or needle bed and the support bed of the needle loom is increased and the two batts in overlapped relation are advanced through the needle loom wherein the reciprocating needles extend through the upper batt into the lower batt short of the supporting bed to connect the two batts together. After the overlapped batts are removed from the needle loom by a take up apron or the like, the overlapped batts may then be lifted, inverted and transported to a feed apron or the like for movement into the same or a different needle loom wherein they can be needled from both directions in a manner as hereinbefore described.
Within the scope of the present invention, any suitable or desired number of batts of any suitable material, density or thickness may be added in overlapping relation to a needled batt as described herein without inverting the needled batt or the overlapped batts so that they are needled together from one direction only and not from both directions. The new and improved method and apparatus of the present invention, therefore, may be used to produce layered batts of any suitable thickness that are needled from one and/or two directions in any desired manner.
Thereafter, in accordance with the present invention, any suitable number of batts can be added to the needled batts, the opening between the stripper plate or needle bed and the support bed can be adjusted accordingly and the overlapped batts can be moved and needled in any desired manner to produce a multilayered batt of any suitable thickness limited only by the construction of the needle loom and the size of the opening between the stripper plate or needle bed and the support bed thereof.
In accordance with the method and apparatus of the present invention, the feed apron, needle loom and take up apron and devices are constructed and operate to insure for each cycle of operation that the needle beam movement and the movement of the batt or overlapped batts into, through and out of the needle loom is uniform and does not vary in speed.
With the improved method and apparatus of the present invention, layered and needled felts or nonwoven materials of any suitable or desired thickness can be constructed of any suitable material or materials and can be used for any desired application wherein lightweight strong materials are required such as in space or aircraft applications or any other desired applications.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic side elevational view of an apparatus for conveying a carded batt of one or more materials through a needle loom;
FIG. 2 a is an enlarged schematic side elevational view of a portion of an apparatus for conveying one or more layers or batts of a selected material or materials through a needle loom in accordance with the present invention, showing the needle bed at the upper end of its reciprocating movement;
FIG. 2 b is a side elevational view similar to FIG. 2 a showing the needle bed at the lower end of its reciprocating movement;
FIG. 3 is a side elevational view of one embodiment of a movable support bed for the apparatus shown in FIGS. 2 a and 2 b;
FIG. 4 is a side elevational view of a portion of a needling apparatus showing another embodiment of a movable support bed;
FIG. 5 a is a perspective view of one embodiment of a needle loom with a movable support bed like the one shown in FIG. 4 ;
FIG. 5 b is an enlarged perspective view of a portion of the needle loom shown in FIG. 5 a;
FIG. 6 is a side elevational view of a portion of a needling apparatus showing a further embodiment wherein the support bed is fixed and the needle bed and associated portions of the apparatus are movable;
FIG. 7 is a perspective view of a further embodiment of a needle loom having a movable needle bed like that shown in FIG. 6 ;
FIG. 8 is a schematic view of a needle from a needle loom extending through a stripper plate on its down stroke into the fiber of one or more batts in a needle loom of the present invention;
FIG. 9 is a view similar to FIG. 8 showing the needle at the bottom of its stroke through the batt;
FIG. 10 is a view similar to FIGS. 8 and 9 showing the needle on its upstroke through the fiber of the batt;
FIG. 11 a is a side elevational view of one embodiment of a needle for use in the needle loom of the present invention;
FIG. 11 b is an enlarged side elevational view in section of a portion of the needle shown in FIG. 11 a;
FIG. 12 is a perspective view of an apparatus for conveying a batt or layers of batts through a needle loom with a movable needle bed and for lifting a needled batt or layers of batts exiting the needle loom and conveying them to a feed apron in an inverted or another position so that they can be again conveyed through the needle loom;
FIG. 13 is a side elevational view of a portion of the apparatus shown in FIG. 12 ;
FIG. 14 is a perspective view similar to FIG. 12 of an apparatus for conveying a batt or batts through a needle loom having a movable support bed;
FIG. 15 is a perspective view of a crane for moving and/or inverting or turning over a needled batt or batts showing a track system for moving the crane;
FIG. 16 is a perspective view of a portion of the apparatus shown in FIG. 14 wherein the crane is positioned to pick up a needled batt or batts from the take up apron;
FIG. 17 is a perspective view similar to FIG. 16 wherein the crane has lifted the needled batt or batts from the take up apron;
FIG. 18 is a perspective view of a portion of the apparatus shown in FIG. 14 showing the crane at the beginning of the feed apron with the needled batt or batts supported on the crane being rotated to be inverted;
FIG. 19 is a perspective view similar to FIG. 18 showing the needled batt or batts supported by the crane being turned over completely;
FIG. 20 is a perspective view similar to FIGS. 18 and 19 wherein the turned over or flipped needled batt or batts are again positioned on the feed apron for movement into the needle loom for additional needling in the opposite direction and on the opposite side thereof;
FIG. 21 is a perspective view of a portion of a feed apron or conveyer for a needle loom in accordance with the present invention;
FIG. 22 is a perspective view of a portion of the feed apron shown in FIG. 21 showing a holding or pushing rail and associated operational devices;
FIG. 23 is an exploded perspective view of the feed apron components shown in FIG. 22 ;
FIGS. 24 a , 24 b and 24 c show various views of the slats of the feed apron shown in FIG. 21 ; and
FIG. 25 shows enlarged perspective views of portions of the take up apron and associated apparatus shown in FIGS. 12 and 13 .
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1 , a batt B is fed by a feed apron 10 into a needle loom 12 of any suitable construction wherein the batt is engaged by a predetermined number and pattern of reciprocating needles (not shown) for the purpose of compacting and tightening the fibers of the batt. The batt B is then removed from the needle loom 12 by a take up apron 14 and associated apparatus of any suitable construction for storage, shipping or further processing. In accordance with the present invention, the batt B may be positioned on a needled batt or overlapped batt layers B 1 that are positioned on the feed apron 10 for passage through the needle loom 12 in overlapped relation, as will be further explained in more detail hereinafter.
As shown schematically in FIGS. 2 a and 2 b , the new batt B and/or the underlying needled batts B 1 can be conveyed through the needle loom 12 wherein they are engaged by needles 13 on a vertically reciprocating needle bed 16 and are supported by a bed 18 that is vertically movable by a hydraulic device or any other suitable device to vary the spacing between the support bed 18 and the stripper plate 19 to accommodate one or more layers of batts to be needled of different thicknesses. In accordance with one embodiment of the invention, a hydraulic cylinder 20 may be located in a pit 22 of any suitable size or depth that is positioned beneath the needle loom 12 and operates to move the support bed 18 vertically, as shown in FIG. 3 .
Referring to FIG. 2 b , on the down stroke of the needle bed 16 , the needles 13 pass through the stripper plate 19 and penetrate the batt B or batts B 1 . As will be explained hereinafter, in accordance with the present invention, the needles 13 do not enter the support bed 18 .
In accordance with another embodiment of the invention shown in FIGS. 4, 5 a and 5 b , the support bed 18 is slidably mounted on the frame 21 of the needle loom 12 for vertical movement in relation to the needle bed 16 and stripper plate 19 . The needle bed 16 is mounted on the frame 21 for limited vertical reciprocating movement thereon. The frame 21 is fixed in position on the floor and thus is not movable to vary the spacing between the needle bed 16 or stripper plate 19 and the support bed 18 . A jack support system 23 of any suitable construction mounted on the frame 21 is connected to the support bed 18 and is operable mechanically or hydraulically to vary the spacing between the support bed 18 and the stripper plate 19 up to about two feet.
FIGS. 6 and 7 illustrate a further embodiment of the present invention wherein a new and improved needle loom 100 comprises a needle bed 102 that is mounted for reciprocal movement on the frame 104 secured to a plurality of vertically extending legs 106 that are telescopically mounted on vertically extending supports 108 secured to base pads 110 that include any suitable type of shock absorbing devices. The legs 106 are vertically movable on the supports 108 by any suitable type of hydraulic or mechanical drive means (not shown).
The upper portion of the needle bed 102 comprises a suitable type of drive apparatus 112 for the vertical reciprocal movement of the needle bed 102 and needles 103 connected thereto.
A support bed 114 is positioned under the needle bed 102 and is fixedly mounted on base girders 116 of any suitable type.
The sturdy construction of the needle loom 100 enables the vertical spacing between the support bed 114 and the stripper plate 119 to be varied a significant amount, e.g., up to ten feet or more, by vertical movement of the frame 104 secured to the support legs 106 that are vertically movable on the supports 108 . This construction also minimizes any vibration that may occur from reciprocating movement of the needle bed 102 . In cases where the needle loom 100 is constructed for significant vertical spacing between the support bed 114 and the needle bed 102 , additional support legs 106 and supports 108 may be provided on the needle loom 100 .
FIGS. 8-10 illustrate schematically the reciprocating movement of a needle in accordance with the principles of the present invention. As shown in FIG. 8 , on the down stroke of a needle N of any suitable or desired construction, the needle extends through an aligned aperture in a stripper plate 200 of a needle loom (not shown) and engages the fibers of a batt 202 formed of one or more layers being advanced between the stripper plate 200 and the support bed or plate 204 of any suitable construction. During the downstroke of the needle N, fiber gathers inside of barbs on the needle that continue to grab strands of fiber and draw them down towards the support bed 204 . At the bottom of the stroke of the needle N, as shown in FIG. 9 , the needle stops short of the support bed 204 and therefore does not enter into the plane of the support bed 204 in accordance with the present invention. In this manner, the support bed 204 may be of simple lightweight construction without any apertures therethrough and the needle N may be free to move laterally to a limited extent in any direction without any danger of breakage by not being aligned with apertures in the support bed 204 . Depending on the type of needle N used in the needle loom and the type of fibers in the batt 202 , the use of a stripper plate 200 on the needle loom (not shown) may not always be necessary.
On the upstroke of the needle N as shown in FIG. 10 , the fibers of the batt 202 begin to tangle together, the thickness of the batt 202 is reduced and the batt becomes more compact and tighter. As more needle penetrations occur, the tightness of the batt will increase and its thickness will decrease up to a certain point which is controlled by the penetration depth of the needle, the number of barbs on the needle, and the number of penetrations of the needle.
FIGS. 11 a and 11 b illustrate one example of a needle N that may be used in a needle loom constructed in accordance with the present invention. The needle N comprises a plurality of barbs 206 in its lower portion that grab strands of fibers 208 and push them downwardly on the downstroke of the needle N through a batt being advanced between a stripper plate and a support bed of a needle loom.
In accordance with the present invention, any suitable needle construction may be used in a needle loom depending on many factors such as the composition and thickness of the batt or layers of batts being advanced through the needle loom and the depth and reciprocating speed of penetration of the needles into the moving batt.
FIGS. 12-20 illustrate different embodiments of an apparatus 300 for performing the new and improved method of the present invention comprising the following basic steps:
1. Advancing a carded batt of a selected material or materials through a needle loom between the stripper plate and support bed of a needle loom which is constructed in accordance with the present invention to vary the vertical spacing between the stripper plate and support bed a significant amount to accommodate a batt or layers of batts of significant thickness, e.g., up to ten feet or more; 2. Adjusting the vertical spacing between the stripper plate and the support bed for a predetermined penetration of the batt or layers of batts by the needles on the needle bed; 3. Limiting the downward movement of the needles on the needle bed through the advancing batt such that the needles do not penetrate or contact the support bed which allows the needles to be mounted for limited lateral movement in any direction to reduce needle breakage; 4. Removing the needled batt from the needle loom onto a take up apron of any suitable construction; 5. Lifting the needled batt from the take up apron, and moving it in the same or an inverted position to a feed apron for the needle loom or another needle loom; 6. Advancing an inverted needled batt through the needle loom so that it is needled in the opposite direction and on the opposite side thereof; 7. Removing a double needled batt from the needle loom onto a take up apron and moving it again to a feed apron; 8. Positioning a second carded batt over a single or double needled batt on the feed apron and advancing and connecting the batts in overlapped relation through a needle loom which has been adjusted to increase the spacing between the stripper plate and the support bed to accommodate the increased thickness of the overlapped batts; 9. Moving the layered, needled and secured batts to the take up apron for the needle loom and lifting and moving them in the same or an inverted position to a feed apron for the same or another needle loom for a repeat of the same cycles as hereinbefore described which can be repeated a desired or selected number of times to produce a layered batt of any suitable thickness.
Referring to FIGS. 12-20 , the apparatus 300 generally comprises a feed apron 302 , a needle loom 304 or 304 a , pinch rolls 306 , a take up apron 308 and an overhead crane 310 that is movable longitudinally over the feed apron, needle loom and take up apron.
The feed apron 302 may be of any suitable construction and, in one embodiment of the present invention, comprises upstanding bars 312 for engaging the rear portion of a batt and overlying clamp arms 314 or the like for holding the batt on the feed apron 302 as will be more fully disclosed hereinafter.
The needle loom 304 may be of any suitable construction in accordance with the present invention, such as the construction shown in FIG. 5 a or 7 wherein the vertical distance between the stripper plate and the support bed can be varied to a significant extent as hereinbefore explained.
The pinch rolls 306 may be of any suitable construction for advancing the needled batt or batts in a uniform manner onto the take up apron 308 which also may be of any suitable construction and may comprise movable clamp arms 316 for holding the batt B on the take up apron. To insure that a needled batt or batts of certain materials, such as viscose or cellulose fibers used in a carbon/carbonization process, are metal free, the apparatus 300 also comprises a magnet 307 and metal detector 309 positioned between the needle loom 304 and the take up apron 308 .
As shown in FIG. 15 , a crane 310 is longitudinally movable over the feed apron 302 , the needle loom 304 and the take up apron 308 in any suitable manner, such as by mounting it for movement on a track 318 or the like. The crane 310 comprises a frame 320 having support arms 322 slidably mounted on the upper portion thereof for lateral movement. Each arm 322 comprises vertically moveable legs 324 having a clamp mechanism 326 rotatably mounted on the bottom portion thereof. The vertically movable legs 324 may be of any suitable construction, such as a telescoping construction, and may be movable by any suitable hydraulic or mechanical means (not shown).
Each clamping device 326 may be of any suitable construction to enable it to engage and pick up a batt or layered batts on the take up apron 308 when the crane 310 is positioned over the take up apron and to deposit them on the feed apron in the same or an inverted position when the crane is moved to a position over the feed apron.
In an illustrative embodiment, each clamp mechanism 326 comprises an inwardly extending fixed bottom plate 328 and an inwardly extending top plate 330 that is vertically movable with respect to the bottom plate 328 .
In the operation of the apparatus 300 in accordance with the method of the present invention, the crane 310 is movable over the take up apron 308 to engage and pick up a needled batt or layers of batts B that have been moved onto the take up apron 316 from the needle loom 304 , as shown in FIG. 12 . This is accomplished by moving the support arms 322 outwardly, moving the support legs 324 downwardly so that the fixed bottom plate 328 of each clamp device 326 can be inserted under the adjacent batt or layers of batts on the take up apron 308 , moving the support arms 322 inwardly to insert the fixed bottom plates 328 under the batt or layers of batts B, moving the top plates 330 downwardly into engagement with the top of the batt B and moving the support arms 324 upwardly to lift the batt B upwardly from the take up apron 308 , as shown in FIGS. 16 and 17 .
The crane 310 is then moved to a suitable position wherein the clamp devices 326 may be rotated approximately 180° on the support legs 324 when it is desired to invert or turn the supported batt B over on its opposite side as shown in FIGS. 18 and 19 .
Thereafter, as shown in FIG. 20 , the crane 310 is moved to a position over the feed apron 302 , the support arms 324 are moved downwardly to position the movable plates 330 on the clamp devices 326 on the feed apron 302 , the movable plates 330 are moved away from the fixed plates 328 of the clamp devices 326 , the support arms 322 are moved laterally outwardly to remove the movable plates 330 from the supported batt B so that the batt B rests on the feed apron 302 in the same or an inverted position. An inverted batt B can then be advanced into the needle loom 304 so that it is needled in the opposite direction and also on the opposite side.
The described operation of the apparatus 300 can then be repeated in the manner shown in FIGS. 12-20 to pick up batts or layers of batts from the take up apron 308 and deposit them in the same or an inverted position on the feed apron 302 . In this manner, layers of batts B can be needled together in the same or different directions and on different sides, if desired, to produce a layered batt of any desired thickness and composition, and the spacing between the stripper plate and the support bed of the needle loom 304 can be increased to accommodate the increases in thickness of the layered batts, as hereinbefore described.
For the operation of the method and apparatus of the present invention, it is essential that a batt or layered batts be moved into, through and out of the needle loom at a constant speed. To accomplish this, the apparatus of the present invention comprises a new and improved feed apron, take up apron and associated devices.
Referring to FIGS. 12 and 21-24 c , the feed apron 302 is formed of slats 303 that are connected by hinges 305 and have longitudinal grooves 311 on the inner surfaces thereof that are engaged by teeth 313 on supporting end rollers 315 for moving the feed apron 302 between and over the end rollers 315 . The feed apron 302 is supported at its upper portion by a plurality of support rollers 317 .
A plurality of holding or pushing rails 319 are movably mounted on the slats 303 for engaging a batt or overlapped batts on the feed apron 302 to advance the batt or batts on the feed apron 302 at a constant speed into a needle loom 304 and 304 a . The apparatus for moving the rails 319 is illustrated in FIGS. 22 and 23 and generally comprises an air cylinder 321 or the like, guide devices 323 , 325 and gearing 327 .
As an alternative, the fed apron may comprise upstanding bars 312 and overlying clamp arms 314 as shown in FIG. 12 that are operated in any suitable manner.
The take up apron 308 shown in FIGS. 12 and 25 generally comprises a movable conveyor belt 329 and movable clamp arms or pinch rollers 316 for holding a batt or overlapped batts and moving them at a constant speed out of the needle loom 304 , 304 a.
Drive rollers 331 are positioned at the exit end of the needle loom 304 , 304 a and pinch rollers 306 are positioned above them to hold a batt or batts down on the drive rollers 331 and move them at a constant speed out of the needle loom 304 , 304 a and onto the take up apron 308 .
A removable table 333 may be positioned between the drive rollers and the take up apron 308 when the batt or batts cannot be rolled.
From the foregoing description, it will be readily seen that the new and improved method and apparatus of the present invention can be used to produce a needled batt of any suitable material or materials and of any desired thickness and size for use in any desired field of use. Because layered needled batts of lightweight, strong and heat resistant materials of any suitable thickness can be effectively produced by the method and apparatus of the present invention, such layered batts are especially useful in aerospace and space applications, high temperature environments, marine applications or any other desired fields.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention is not to be limited to the disclosed embodiments, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
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A method of producing a needled product of a selected material or materials of a desired thickness and size. A first carded batt of a selected material or materials is moved from a feed support into a needle loom between a vertically reciprocating needle bed and a support bed located beneath and in spaced relation to the needle bed. The needle bed and/or the support bed are vertically movable to vary the spacing therebetween. The upper surface of the first carded batt is penetrated by the needles in the needle loom so that the needles do not reach an upper surface of the support bed and are able to flex laterally. The needled first batt is then lifted and moved to the feed support or a feed support for another needle loom. Thereafter, a second batt is positioned over the first batt in overlapping relation, the needle bed or support bed is moved to increase the vertical spacing therebetween to accommodate the overlapped batts, and the batts are moved through the needle loom and connected. This method may be repeated to add additional overlapped batts to produce a layered product of any suitable thickness.
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BACKGROUND OF THE INVENTION
The present invention relates to heating liquids at remote campsites or in the field, and more particularly, to a compact, self-contained portable stove.
Even the heartiest outdoorsmen often enjoy a cup of coffee or other hot beverage prepared at the campsite. Many instant or dehydrated foods can be prepared using a cup or two of hot water. Open camp fires and portable gas stoves have long been used by hikers, campers, and backpackers for heating liquids such as water at remote campsites where electricity generally is not available. However, these methods are less than ideal for heating small quantities of liquid in a remote camp site where the camper must either carry in or locate fuel.
The oldest and most widely used method for heating liquids is to place the liquid in a pot and suspend or support the pot over an open fire to transfer heat to the liquid. Open campfires, however, are dangerous and difficult to control. Fuel may be scarce and difficult to ignite. Equipment for using a fire generally includes a pot and some means for supporting the pot, though logs or rocks may be adequate. Fuel, such as wood, must be provided or tools, such as an ax, for cutting wood on site.
Another known method for heating liquids in the field is the portable gas stove. This device is typically fueled by liquid propane, carried in a fuel bottle separate from the stove. Some models include an integral fuel tank for storing white gasoline or, most recently, even unleaded automobile gasoline. Although a portable gas stove can be small in size, a fuel supply and a container or pot to hold the liquid to be heated are also required for a complete liquid heating system. These necessary components are awkward to carry, and can be quite bulky. Equally important, the space occupied by the stove and other components could be used for some other important piece of camping gear where space is limited. The weight of these various components also is a drawback to a hiker, backpacker or equestrian.
Other disadvantages of using a gas stove include the exposed flame of the burner, and the time it takes to set up, use, and then take apart. Known portable stoves are inefficient because of heat lost to heating a pot or other container, and because the heat transfer site, primarily the bottom of a pot, has very limited area, and is remote from the water near the top of the pot. A short pot with a larger area provides more heat transfer area, but at the expense of increased water surface area leading to faster cooling.
Even where electricity is available, use of an electric power source for heating liquids also requires the additional components of a stove or heating element and a pot or container to hold the liquid. Thus, like the gas stove, valuable space is taken by a heating system that requires numerous components.
Accordingly, a need remains for a way to heat liquids in the field that is convenient and easy to use, compact and lightweight, simple.
SUMMARY OF THE INVENTION
An object of the present invention is to eliminate the a camper's need to carry more than one implement to a remote area to heat a liquid.
Another object is to reduce the size and weight of equipment necessary for heating a liquid in the field. Yet another object is to improve efficiency in a portable stove.
The present invention includes a camp stove that combines a heat source and a pot into a single compact unit for heating a liquid. The unit comprises an upright enclosure having an open top end and a closed sidewall. The interior of the enclosure is divided into an upper chamber and a lower chamber. The upper chamber acts as a reservoir to hold the liquid. The lower chamber houses a fuel source. To transfer heat to the liquid, a hollow elongated chimney, open at both ends with a closed sidewall, extends through the upper chamber at least to the top end of the enclosure, so that liquid in the upper chamber substantially surrounds the chimney. The bottom end of the chimney is open to the lower chamber to allow heated air to rise through the chimney. The chimney is formed of a thermally conductive material to allow maXimum heat transfer to the liquid.
A fuel plate is located in the lower chamber below the bottom end of the chimney to support solid fuel material. In operation, as the solid fuel combusts, surrounding air heated by the combusting fuel flows from the lower chamber up through the chimney and out of the top end of the of the chimney and heat transfers through the chimney sidewall to heat the liquid.
One advantage of the present invention is that it operates efficiently on small amounts of solid fuel thereby eliminating the need to use valuable space to carry bulkier liquid fuel. Also, the stove's operation on solid fuel makes the unit much safer than a conventional gas stove that operates on highly flammable liquid propane.
A second advantage is that the flame is out of sight and touch thus substantially reducing the likelihood of starting unwanted fires. The fuel is shielded by the enclosure so that the stove is operable despite adverse weather conditions such as rain or snow.
A third advantage is that its reservoir can be used for storage when the stove is not in use.
The foregoing and additional objects, features, and advantages of the present invention will be more readily apparent from the following detailed description of a preferred embodiment which proceeds with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view of a portable stove according to the present invention, showing the lid raised, and the door in an opened position.
FIG. 2 is a vertical sectional view of the portable stove of FIG 1.
FIG. 3 is a cross-section taken along line 3--3 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIGS. 1-3 depict a portable stove 50 for heating liquids in the field. Referring to FIG. 2, a cylindrical enclosure 12 is made of a rigid, heat resistant material, preferably stainless steel. It is open at the top end and has a closed sidewall 13 and a flat, closed bottom end for supporting the stove upright on an underlying surface when in use. The enclosure 12 surrounds an upper chamber (A) for holding a liquid, and a lower chamber (B) located below the upper chamber for enclosing a heat source. The sidewall 13 includes a plurality of holes (not visible in the drawing) located about the lower chamber to allow the free flow of air into the lower chamber for combustion. Further, a rectangular portion of the sidewall adjacent the lower chamber is removed to form an access passage to the lower chamber to allow inserting, positioning and igniting a solid fuel material.
A circular bottom plate 22, made of like material, is fixed to the inside of the enclosure 12, oriented generally parallel to the top end of the enclosure. Plate 22 has an outside diameter substantially equal to the inside diameter of the enclosure. The peripheral edge of the plate is continuously sealed along the sidewall to form a water tight connection, thereby dividing the enclosure to form upper chamber (A) and the lower chamber (B). The bottom plate 22 includes a central aperture 23, discussed below.
A hollow elongated chimney 14 is symmetrical about its vertical axis and open at a top end 15 and bottom end 16. The chimney is preferably made from a material with superior conductive properties so that heat is efficiently transferred to the liquid, i.e., a metal such as stainless steel. Chimney 14 includes a closed sidewall, tapered to define a truncated cone shape. In addition, the chimney 14 includes corrugations 19 extending lengthwise to maximize its surface area, as best seen in cross section in FIG. 3. The chimney extends vertically through the upper chamber about the enclosure axis from the bottom plate, at least to the top end of enclosure -2, and preferably extends slightly higher than top end 15. The chimney has a bottom end 16 sized and shaped corresponding to aperture 23 in the bottom plate. The chimney is attached to the plate 22 along the inside peripheral edge of the plate and is continuously sealed to form a water tight reservoir and to provide support for the chimney.
In an alternative embodiment, the bottom end of the chimney is circular, having a diameter equal to the inside diameter of the enclosure. The bottom end of the chimney is continuously sealed along the inside of the enclosure sidewall so that the chimney sidewall separates the upper and lower chambers. Such an embodiment obviates bottom plate 22.
A cylindrical outer shell 10, made from like material, concentrically surrounds the enclosure 12 and has an approximate diameter of one half inch greater than that of the enclosure 12 to provide a uniform one-quarter inch insulating space between the shell 10 and the enclosure 12. The insulating space optionally may be filled with thermally insulating material, for example, a closed-cell foam material, to increase insulation of the upper chamber from the ambient environment. The height of shell 10 is approximately the same as the height of the enclosure 12. Additionally, and similar to the enclosure 12, a shell 10 includes a plurality of holes 36 to allow for the free flow of air to the lower chamber (B). Further, a rectangular portion of the outer shell is removed and registered with the same in the enclosure, to allow access to the lower chamber.
The shell 10 and the enclosure 12 are fixed together by an upper ring 20, a lower ring 24, and by a common base plate 30. The upper ring 20 and lower ring 24 are employed to attach the shell 11 to the enclosure 12. The outside diameter of each ring 20, 24 is equal to the inside diameter of the outer shell. Similarly, the inside diameter of both rings is substantially equal to the outside diameter of the enclosure. Both rings are flat and made of heat resistant material, preferably stainless steel. The upper ring is positioned adjacent the top end of the enclosure and shell. The lower ring is positioned approximately level with the plate 22. The outer edge of each ring is intermittently attached to the shell and the inner edge of each ring is intermittently attached to the enclosure.
Base plate 30 provides a common surface for the support of both the shell and the enclosure. Base plate is a solid, flat plate having an outside diameter substantially equal to the inside diameter of the outer shell. The bottom edge of the shell and the bottom edge of the enclosure are each intermittently connected to the base.
A fuel plate 22 is disposed within the lower chamber (B), spaced above the base 30 by a plurality of legs. The fuel plate 22 provides a surface for placement of a solid fuel material. The solid fuel may be a tab formed of, for example, trioxane or hexamine. One such fuel tab is military spec. F-10805C. The fuel is utilized to warm surrounding air in the lower chamber (B). The warm air rises up through the chimney 14 by convection and out the top end 15. The portable stove thus provides for indirect heating of a volume of liquid contained in the upper chamber from within the volume of liquid.
A door 32 is slidingly mounted to the outer surface of the outer shell 10. The door is located near the base for covering the access passage to the lower chamber when access is not needed. The door 32 includes a plurality of holes 38 to allow for the free flow of air for combustion. The door is moveably attached to the outer shell, for example, by two small screws 34.
A circular, flat lid 17, made from similar heat resistant material, has an outside diameter equal to the outside diameter of the shell 10. Lid 17 includes a central aperture sized and shaped to receive a top portion of the chimney 14 so that, when the lid is positioned covering the top end of the enclosure, the top portion of the chimney extends through the aperture, thereby maintaining said positioning of the lid.
In an alternative embodiment (not illustrated), the chimney is not corrugated, but simply defines a truncated-cone shape. The aperture in the lid accordingly is round, sized to receive a top portion of the chimney. In such an embodiment, provision also may be made for locking the lid to the stove by positioning the lid covering the top end of the enclosure and rotating the lid to a locked position. Details of such an arrangement are known.
In one example of an operative embodiment of the invention, the apparatus is formed of stainless steel and has an overall height of approximately 9 inches (23 cm.) and an outside diameter of approximately 4 inches (10 cm.). The upper chamber is about 71/2 inches high (19 cm.), and the lower chamber is about 11/2 inches high (4 cm.). There is a space of about 1/4 inch (0.6 cm.) between the enclosure and the outer shell. The access passage measures about 1 inch high by 2 inches across (2.5 cm. by 5 cm.). The chimney is about 1 inch (2.5 cm.) in diameter at the top end and about 21/2 inches (6.3 cm.) diameter at the bottom end.
In an alternative embodiment, a single-wall construction may be used, in which the enclosure and the outer shell essentially are combined into one. Single-wall construction is simpler, and therefore cost is reduced, but at the expense of sacrificing insulation, with the result that the apparatus may become to hot in use to comfortably handle it with the bare hand, and liquid remaining in the upper chamber will cool more quickly. In winter, however, users will appreciate the hand-warming benefit of the stove.
Operation
In operation, the user fills the upper chamber with a liquid to be heated. Following this, the user positions and tightens the lid 16 over the enclosure. The user then opens the door 32 to access the lower chamber and positions a solid fuel tab 28 in the lower chamber on the fuel plate. The fuel tab is ignited by extending a burning match through the access passage into contact with the fuel. The user then slides the door downward until it is closed. Cleaning the stove 10 is easily accomplished by rinsing the surfaces that were in contact with the heated liquid.
A standard military type fuel tab, measuring approximately 3/4 inch diameter by 1/2 inch high, provides enough fuel to warm about 2 cups of water sufficiently to make coffee or hot tea. The tab burns completely in about 5-7 minutes, leaving virtually no residue.
Having illustrated and described the principles of my invention in a preferred embodiment thereof, it should be readily apparent to those skilled in the art that the invention can be modified in arrangement and detail without departing from such principles, I claim all modifications coming within the spirit and scope of the accompanying claims;
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A portable camp stove has an upper chamber for holding a liquid to be heated and an integral lower chamber disposed below the upper chamber. An elongated chimney with corrugated sidewall extends from the lower chamber up through the upper chamber so that, in use, the liquid in the upper chamber surrounds the chimney. A solid fuel material is combusted within the lower chamber to warm surrounding air which flows upwardly through the chimney. Heat transfer through the corrugated chimney sidewall warms the liquid. The camp stove is compact and portable, obviating the need to carry bulky stoves, fuel bottles and pot or tea kettle.
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This application claims the benefit of provisional application 60/263,349 filed Jan. 22, 2001.
BACKGROUND OF THE INVENTION
The concept of placing a cover enclosure over a rotational doorknob, to prevent rotation of the doorknob, and concurrent dislodging of the associated locking bolt, and, finally, opening of an associated door, is, generally known. U.S. Pat. No. 4,285,221, to Atchisson, discloses a retrofit doorknob lock apparatus, in which a shroud is placed over the doorknob and the doorknob shaft and a clevis fits through slots in the shroud to retain the shroud in place. The clevis is locked in place with a separate exterior lock, on the same side of the door. Similarly, U.S. Pat. No. 3,739,608, to Young, discloses an auxiliary door lock including a doorknob cover, a resilient band along the inner wall surface of the cover, and a locking means, again on the same side of the door, utilizing a separate, exterior lock. The door lock of U.S. Pat. No. 4,876,867, to Leneave, again discloses a cover, comprised of a tubular casing, which fits over a doorknob, on one side of the door, with a locking lever, utilizing a separate lock, again, on the same side of the door. U.S. Pat. No. 5,425,256, to Crosby, for a doorknob security device, also utilizes a cover mechanism, kept in place by a separate lock, on the same side of the door. The lockable doorknob enclosure of U.S. Pat. No. 5,560,235, to Aucoin, again deals with an enclosure which fits over a doorknob to prevent rotation of the knob, and which has an incorporated locking mechanism, requiring a separate key, again, on the same side of the door as the mechanism.
As is indicated from review of the referenced prior art, all of the mechanisms shown for disabling a doorknob require an additional locking mechanism, either with an incorporated lock and key, or by requiring a separate, external lock, which would require either a combination or key to open. None of the devices shown in the prior art allow the disabling function to be completed by simply placing the door ajar, fitting the device into place, and closing the door, thereafter allowing entry only by activation of the doorknob from the opposite side. Correspondingly, the devices of the prior art do not permit removal of the device, once locked in place, simply by opening the associated door from the opposite side and removing the device by simple reverse sequence of its installation, without the need to separately unlock a separate attached security device.
Accordingly, a need exists for a doorknob disabling device, of a two piece construction, which may be put in place in a simple sequence, by placing the associated door ajar, placing a cover over the doorknob and mating a retaining mechanism with the doorknob cover, by movement of the retaining mechanism toward the cover, and closing of the door, so that the cover and retaining mechanism may not be disassociated while the door is closed, because of the position of the associated door jam, and its contact with the retaining mechanism, and the associated doorknob and its contact with the cover.
A need for such a device is particulary apparent in industries such as the mobile home sales industry, to prevent prospective customers from unnecessarily opening, and leaving unlocked, different access doors, during the course of their investigation of the product.
Likewise, the prior art does not provide a doorknob disabling device which may be placed over a knob on a associated door, on the side for gaining entry, and closed by a person temporarily occupying the interior space to which the door provides access, when there is a need for personal security in such space.
The present invention is directed toward a device with a minimum of components and moving parts, which does not require a separate locking mechanism, and addresses the shortcomings of the prior art.
SUMMARY OF THE INVENTION
The present invention is directed to a locking device, generally, and, in particular, to a doorknob disabling device which is utilized with a standard doorknob, which may or may not have a key on the knob on the side of the door from which access may still be gained, and, in some cases, having a manual locking or unlocking device on the portion of the doorknob on the interior or opposing side of the door. The device may, however, be utilized on any doorknob, even one without locks on either side, to disable the doorknob from the side of the door on which the device is affixed, when the door is closed within its associated doorjamb.
The device is designed, primarily, to be utilized to cover the knob on the side of the door which does not require a key, and from which the door may be manually locked or unlocked, so that, when the door is closed, the door may only be unlocked, as a prelude to opening, by utilizing the key from the exterior side of the door.
The device may be constructed of an rigid, non-permeable material. It is ideally constructed of metal. Plastic, acrylic or other material may be utilized. The device consists of a hollow cylinder, cup, or other enclosure having an open end, in which to accept a doorknob, and being otherwise, externally closed. This member is constructed, generally, so that it has the appearance of a cylinder, glass, or cup, but, in theory, may be of any shape, so long as there is a unitary, rigid exterior surface, completely enclosing the doorknob, when the doorknob is inserted or covered through the open end. The enclosure may be of a variation of sizes, and is generally configured to fit as snugly as desired over a doorknob, so that the open end rests against the planar surface of the door upon which the knob is attached. The cylinder may be long enough to accommodate varying doorknobs while maintaining contact with the door. While the interior portion of the closed end of the covering enclosure may touch the outer surface of the doorknob when the open end of the enclosure is in contact with the planar surface of the door, it is not necessary that it do so, and the device works equally well when the interior of the enclosure is actually contacting the knob, or where there is a space between the exterior knob surface and interior surface of the enclosure.
The device may constructed in different sizes, to accommodate different diameters of doorknobs, but the device will operate as intended, so long as the interior portion of the enclosure is of greater diameter than the diameter of the doorknob. If desired, rings or spacers may be placed around the interior of enclosure to make the interior diameter of the enclosure more closely conform to the outer diameter of the knob, if a close fit is particularly desired. As stated, it is not necessary for this fit to be close in any particular relative dimension, other than that the space between the exterior circumference of the knob and the interior surface of the enclosure must be less than the distance of the insertion of the mating extension from the enclosure into the female mating receptacle on the retention device, so that sideways movement of the enclosure will be impeded by the knob, prior the point where the mating relationship may be disengaged.
The enclosure has an opening, which is basically formed by a truncated section, so that the opening has an edge surface, substantially in a singular plane, which corresponds with and contacts the planer surface of the associated door. Either in the same plane, or in a plane parallel thereto, the enclosure member has a mating extension which extends outward toward the outer edge of the door, when the enclosure is in place over the doorknob.
A second detachable retaining member is conformed to fit over the width of the door edge approximate to the where the doorknob and lock assembly to be disabled is located. The retaining member is, preferably, a flat piece, conformed by bending to contact, by corresponding planar surfaces, the side of the door on which the knob to be disabled is located, the opposing side of the door, and the exterior edge of the door extending between them. The retaining member is fitted with a receptacle member, to accept and rigidly contain the extension from the enclosure, in a male-female relationship, when the enclosure is placed over the doorknob, and the retaining member is then placed over the edge of the door as described. The portion of the retaining member which forms the female receptacle portion of the mating relationship may be a complete enclosure, or may be partially cut away leaving overlapping flanges at the edges to hold extension firmly in place. The portion of the retaining member which contacts the planar edge of the door also is conformed to provide an opening sufficient for the locking bolt of the doorknob locking assembly to pass through.
The device is put in place when the associated door is ajar. Accordingly, when the associated door is closed, within its associated doorjamb, the enclosure may not be removed from the doorknob, because disassociating motion along the plane of the door is prevented by contact between the interior of the enclosure and the doorknob assembly and contact by the exterior portion of the retention member, and the associated doorjamb. Further, the enclosure may not be moved away from contact with the door, around the doorknob, because of the portion of the retaining member which is bent around the edge of the door, and which contacts the opposite surface of the door, and because of the dual retaining function provided when the locking doorknob assembly bolt passes through the opening in the retention member and locks into the associated receptacle in the doorjamb.
In another embodiment of the invention, the enclosure member alternatively is provided with two parallel pairs of apertures, with each pair aligned linearly parallel to the surface of the associated door and perpendicular to the plane of the exterior edge of the door, with a corresponding parallel pair of rods mounted on the retention member and fitting within and through the parallel pairs of apertures in male-female relationship.
Other objects, advantages and novel features of this invention will be set forth and will become apparent in the detailed description which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
The following detailed description is best understood with reference to the following drawings, in which:
FIG. 1 is a perspective view of the device, in mated position covering a doorknob and secured over the outer edge of an ajar door;
FIG. 2 is an exploded view of the components of the device showing the relationship between the device and an associated doorknob and door, as well as the mating association of the components of the device when in place;
FIG. 3 is a sectional top view of the device in place on an associated door;
FIG. 4 is perspective view of the an alternative embodiment of the device in place on an associated door, showing, in transparency, the relationship of the device with a doorknob on the associated door;
FIG. 5 is a sectional top-view of an alternative embodiment of the device in place on an associated door; and
FIG. 6 is a perspective view of the device, in mated position covering a doorknob and secured over the outer edge of a closed door.
FIG. 7 is a perspective view of the device in mated position covering a door knob and secured over the outer edge of a closed door, demonstrating the enclosure means in the shape if a truncated sphere.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The invention doorknob disabling device 10 , broadly considered, includes an enclosure member 20 and a retention member 30 . The doorknob disabling device is intended for use on an associated hinged door 40 having a doorknob assembly 41 which engages a locking bolt 42 . Such a door 40 generally has a planar interior surface 43 upon which the doorknob assembly 41 is mounted, a corresponding planar exterior surface 44 and a planar outer edge surface 45 , substantially perpendicular to the interior surface 43 and exterior surface 44 , and running between them. The locking bolt 42 extends from and retracts into the outer edge surface 45 , roughly proximate the doorknob assembly 41 .
Enclosure member 20 in the preferred embodiment is a hollow cylinder 21 , having a closed outer first end 22 and an open second end 23 . The cylinder 21 is truncated to form the open end 23 . Cylinder 21 has a rigid unitary outer surface 24 and a unitary inner surface 25 . The truncated open end 23 provides a continuous opening edge 26 of the outer surface 24 and inner surface 25 in a substantially singular plane as demonstrated in the cross-sectional views of FIGS. 3 and 5, which is proximate to and contacts the planar interior surface 43 of the associated door 40 . While the preferred embodiment of enclosure member 20 is a cylinder 21 , enclosure member 20 may be of varied exterior shapes, including, but not limited to, the shown cylinder 21 , a cup, or a truncated sphere, so long as the outer surface 24 is rigid and unitary, the edge 26 of the open end 23 is substantially planar, and the enclosure member 20 is sufficiently hollow to cover a doorknob 41 when the open end 23 is in contact with the associated door surface 43 , as shown in FIGS. 1, 2 , 3 , 4 , 5 and 6 .
Attached to enclosure member 20 is a rigid mating extension 27 , extending outward from member 20 proximate to opening 23 and substantially parallel to the plane thereof. In the preferred embodiment of the invention, extension 27 is a flat bar member having an upper edge 27 a , a lower edge 27 b , defining a height A, and a first end 27 c proximate to cylinder 21 and an outer second end 27 d , defining a length B. Extension 27 is of sufficient thickness or width 28 along its length B and height A to provide a rigid connection with retention member 30 when mated as shown in FIG. 1 . Extension 27 further has a flat outer surface 27 e and a flat inner surface 27 f.
Retention member 30 , in the preferred embodiment, is a flat bar unit, having an outer surface 31 and an inner surface 32 . Member 30 is conformed in a substantial “u” shape to provide a first side 30 a , a second, parallel, opposing side 30 b , and a bridging, perpendicular end section 30 c . Member 30 if further conformed to fit over the edge 45 of associated door 40 , with the inner surface 32 of first side 30 a in planar contact with interior surface 43 , inner surface 32 of opposing side 30 b in planar contact with exterior surface 44 , and inner surface 32 of end section 30 c in planar contact with outer edge surface 45 , when member 30 is moved into place as shown in FIGS. 1 and 2.
First side 30 a of retention member 30 is further configured to receive mating extention 27 in a rigid coupling relationship as shown in FIG. 1, by relative contacting movement as shown in FIG. 2 .
Retention member 30 has an upper edge 33 and lower edge 34 defining a height dimension C. In the preferred embodiment, upper edge 33 and lower edge 34 are each flanged to traverse the width 28 of extension 27 along upper edge 27 a and lower edge 27 b and a portion of the length B of outer surface 27 e.
Extension member 27 and first side 30 a are further conformed so that height dimension C is at least as long as height A, so that member 27 is slidably insertable within the flanged edges 33 and 34 and, when so inserted, is rigidly held there in a male-female relationship.
In another preferred embodiment the flanged ends 33 and 34 may be extended across height dimension C, and joined so that first side 30 a of retention member 30 completely encircles extension member 27 when coupled in male-female relationship. Extension member 27 may be configured as a rod or other shape so long as first side 30 a is correspondingly configured to provide a rigid male-female coupling when the outer second end 27 d is fully inserted into the receptacle of first side 30 a . In whatever configuration or shape extension member 27 and the first side 30 a of retention member 30 are provided, the mating movement between extension member 27 and first side 30 a is substantially in a singular plane parallel to the plane of opening edge 26 and perpendicular to planar outer edge surface 45 of the associated door.
In the preferred embodiment, an opening 35 is also provided in end section 30 c of retention member 30 . The opening 35 is provided large enough to permit passage through it of the locking bolt 42 when the locking bolt 42 is extended from outer edge surface 45 , as shown in FIG. 1 .
The device 10 is installed and made operative by placing the enclosure member 20 over the doorknob assembly 41 on the side of the associated door 40 , so that the open edge 26 is parallel to and in contact with the planar interior surface 43 , with the mating extension 27 extending outwardly and generally perpendicular to outer edge surface 45 . While the door 40 is ajar, retention member 30 is moved toward enclosure member 20 , until inner surface 32 of end section 30 c is in planar contact with outer edge surface 45 of door 40 , and positioned so that locking bolt 42 is moveable through opening 35 , extension member 27 inserted within the flanged edges 33 and 34 of first side by doorjamb 50 . Any substantial movement of enclosure member 20 in direction E is prevented by doorknob assembly 41 , and movement of both enclosure member 20 and retention member 30 away from contact with the associated door 40 is prevent by the dual functions of bolt 42 extending through opening 35 , and the contact of inner surface 32 of opposing side 30 b with exterior surface 44 . When the associated door 40 is opened and again ajar, the device may be removed by reverse sequence.
The entire device 10 may be constructed of metal or other rigid synthetic material such as plastic or acrylic matter.
An alternative embodiment of the device 10 is shown in FIGS. 4 and 5, wherein the mating function between enclosure member 20 and retention member 30 is provided by a pair of linear apertures 51 extending through enclosure member 20 , linearly aligned so as to be perpendicular to edge surface 45 above stem 41 a of doorknob assembly 41 , and a corresponding second pair of apertures 52 extending through enclosure member 20 linearly aligned parallel to linear apertures 51 and in the same plane parallel to the plane of opening edge 23 , with the distance G between the corresponding pairs 51 and 52 , being less than the largest diameter H of doorknob assembly 41 . Retention unit 30 is correspondly conformed to provide the parallel rods 53 attached to side 30 a with outer ends 53 a and 53 b linearly aligned to be insertable through aperture pairs 52 and 51 , respectively, when inner surface 32 of end section 30 c contacts outer edge surface 45 with aperture 35 centered to allow passage by locking bolt 42 . Motion in directions E & D is prevented in the same manner by doorjamb 50 and doorknob assembly 41 , while motion in direction F is additionally inhibited by contact of rods 53 a and 53 b against doorknob assembly 41 .
WHEREAS, a preferred embodiment of the invention has been illustrated and described in detail, it will be apparent that various and additional changes may be made in the disclosed embodiment without departing from the spirit of the invention.
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A device for temporarily disabling a doorknob attached to a hinged door. The device covers the doorknob with a rigid enclosure, preventing rotation of the doorknob to move the associated locking bolt. A retaining unit is mated with an extension from the rigid enclosure in a male-female relationship, simultaneously with fitting the retaining unit over the outer edge of the hinged door while ajar. Closure of the door into the associated doorjamb, with the enclosure over the doorknob, prevents parting movement between the enclosure and the retaining unit, providing a self-locking feature.
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TECHNICAL FIELD
[0001] The present invention relates to a rear wheel steering control system that can change the toe angles of rear wheels of a vehicle.
BACKGROUND OF THE INVENTION
[0002] It has been proposed to fit a four-wheeled vehicle with a rear wheel steering control system in addition to a more conventional front wheel steering system for the purpose of improving the driving stability of the vehicle. Typically, in association with each rear wheel is provided an electric linear actuator having an output rod that can be selectively extended and retracted so that the two rear wheels may be steered individually. See Japanese patent laid open publication No. 9-030438, for instance.
[0003] The linear actuator may be advantageously incorporated into one of the lateral arms that form a part of the wheel suspension system of the corresponding rear wheel. In such a case, changing the toe angle of the rear wheel is effected by changing the length of such a lateral arm. Therefore, as the toe angle of the rear wheel is changed, the geometry of the wheel, in particular the tread of the rear wheels, changes at the times of bump and rebound, and this may adversely affect the ride quality of the vehicle.
BRIEF SUMMARY OF THE INVENTION
[0004] In view of such problems of the prior art, a primary object of the present invention is to provide a rear wheel steering control system that can improve the ride quality of a vehicle fitted with a rear wheel steering control system.
[0005] A second object of the present invention is to provide a rear wheel steering control system which is highly simple and compact in structure.
[0006] According to the present invention, such objects can be at least partly accomplished by providing a rear wheel steering control system for a vehicle, comprising; an actuator for changing a toe angle of each rear wheel; a rear wheel steering control unit for activating the actuator according to a prescribed plan; and a road condition estimating unit for estimating a state of a road surface over which the vehicle is traveling; wherein the rear wheel steering control unit forces the toe angle of each rear wheel to a substantially neutral position or a slightly toe-in position when the road condition estimating unit has detected a rough road surface.
[0007] Thereby, when the vehicle is traveling over a rough road surface, the actuator is forced to the neutral position, and the rear wheels are brought to a neutral position so that the changes in the wheel geometry (tread and/or alignment) of the rear wheels at the time of a bump or a rebound can be avoided. Therefore, the ride quality of a vehicle equipped with the rear wheel steering control system is favorably maintained even when the vehicle is traveling over a road surface, and the rear wheels undergo large vertical displacements.
[0008] According to a preferred embodiment of the present invention, the vehicle is additionally fitted with an unsprung mass control unit, and the road condition estimating unit is enabled to determine the state of road condition from a manipulated variable of the unsprung mass control unit. Thereby, the state of the road surface can be accurately determined in a simple and inexpensive manner.
[0009] According to a particularly preferred embodiment of the present invention, the unsprung mass control system forms a part of a damper control system including a variable damping force damper, and is configured to supply a control current corresponding to a product of a stroke and a stroke speed of the damper to the variable damping force damper. The variable damping force damper may consist of a telescopic damper using MRF (magneto-rheological fluid) for the working fluid thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Now the present invention is described in the following with reference to the appended drawings, in which:
[0011] FIG. 1 is a diagram of a four-wheeled vehicle incorporated with a rear wheel steering control system embodying the present invention;
[0012] FIG. 2 is a fragmentary perspective view of a left rear wheel suspension system;
[0013] FIG. 3 is a vertical sectional view of a linear electric actuator of the rear wheel steering control system;
[0014] FIG. 4 is a block diagram of an essential part of an ECU used in the rear wheel steering control system; and
[0015] FIG. 5 is a flowchart showing the rear wheel steering control process of the illustrated embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] A preferred embodiment of the rear wheel steering control system of the present invention is described in the following with reference to FIG. 1 . In FIG. 1 , some of the components thereof are associated with each wheel, and such component parts are denoted with suffices fl, fr, rl and rr to indicate with which wheel the particular component is associated. For instance, a front left wheel is denoted with 3 fl , a front right wheel with 3 fr , a rear left wheel with 3 rl and rear right wheel with 3 rr . When a particular component is collectively referred to, it may be denoted with the corresponding numeral without the suffix. For instance, the wheels of the vehicle may be referred to simply as 3 depending on the situation.
[0017] Referring to FIG. 1 , the illustrated vehicle V has a vehicle body 1 which has four wheels 3 each fitted with a pneumatic tire 2 . Each wheel 3 is rotatably supported by a knuckle 7 which is in turn supported by wheel suspension system 5 including suspension arms, a spring and a variable damping force damper 4 . The variable damper 4 essentially consists of a telescopic piston and cylinder, and uses MRF (magneto-rheological fluid) for the working fluid thereof. By controlling a magnetic fluid valve incorporated in a piston of the damper 4 , the damping force for the given stroke speed thereof can be changed both quickly and continuously.
[0018] The vehicle V is fitted with a front wheel steering system 9 that allows the right and left front wheels 3 fl and 3 fr to be steered by turning a steering wheel 19 with the aid of a rack and pinion gear mechanism, and a rear wheel steering control system 6 that allows each rear wheel 3 rl , 3 rr to be steered individually by a corresponding electric actuator 8 l , 8 r provided in association with the corresponding rear wheel. Each electric actuator 8 consists of a linear actuator that has a housing attached to a part of the vehicle body 1 and an output rod connected to the knuckle 7 and configured to extend and retract according to an electric current supplied thereto.
[0019] The rear wheel steering control system 6 allows the toe-in and toe-out of the rear wheels 3 to be changes by steering the rear wheels in a mutually symmetric relationship in a corresponding direction, and the rear wheels to be steered by a same steering angle by extending the output rod of one of the actuators and retracting the output rod of the other actuator in an opposite direction by a same stroke.
[0020] The various onboard control systems including the dampers 4 rear wheel steering control system 6 are centrally controlled by an onboard ECU (electronic control unit) 20 which essentially consists of a microcomputer incorporated with ROM, RAM, interface circuits, input and output interfaces and drivers, and is connected to various sensors (which will be described hereinafter), the dampers 4 and the electric actuators 8 via a communication line such as CAN (controlled area network).
[0021] The vehicle V is provided with a steering angle sensor 10 for detecting a steering angle of the steering wheel 19 , a vehicle speed sensor 11 for detecting a traveling speed of the vehicle, a lateral G sensor 12 for detecting a lateral acceleration of the vehicle, a fore-and-aft acceleration sensor 13 for detecting a fore-and-aft acceleration of the vehicle and a yaw rate sensor 14 for detecting a yaw rate of the vehicle which are arranged in appropriate parts of the vehicle V. The vehicle V is additionally provided with a vertical G sensor 15 attached to a part of each wheel house for detecting a vertical acceleration of the corresponding part of the vehicle and a stroke sensor 16 for detecting a vertical stroke of each wheel. Each electric actuator 8 is provided with a position sensor (linear encoder) 17 for detecting the output stroke of the actuator, and the knuckle 7 of each rear wheel 3 rl , 3 rr carries an unsprung mass G sensor 18 for detecting the vertical acceleration of the knuckle 7 (unsprung mass acceleration).
[0022] FIG. 2 is a perspective view of a left rear wheel suspension system 5 rl . The right rear wheel suspension system 5 rr can be given as a mirror image of the left rear wheel suspension system 5 rl.
[0023] As shown in FIG. 2 , this rear suspension system 5 rl is of a double wishbone type, and comprises a knuckle 7 rotatably supporting the rear wheel 3 rl , an upper and lower arms 21 and 22 joining the knuckle 7 to the vehicle body in a vertically moveable manner, an electric actuator 8 l joining the knuckle 7 to the vehicle body so as to allow the toe angle of the rear wheel 3 rl to be varied, a suspension spring 4 a resiliently supporting the rear wheel to the vehicle body and a damper 5 to apply a damping force to the vertical movement of the knuckle 7 .
[0024] The upper arm 21 is attached to a part of the vehicle body 1 via a rubber bush joint 23 at the base end thereof and to an upper part of the knuckle 7 via a ball joint 25 , and the lower arm 22 is attached to a part of the vehicle body 1 via a rubber bush joint 24 at the base end thereof and to a lower part of the knuckle 7 via a ball joint 26 . The housing of the electric actuator 8 l is attached to the vehicle body 1 via a rubber bush joint 27 , and the output rod of the electric actuator 8 l is connected to a rear part of the knuckle 7 via a rubber bush joint 28 . The damper 4 is connected to the vehicle body 1 via a rubber bush not shown in the drawings at the upper end thereof, and to an upper part of the knuckle 7 via a rubber bush joint 29 at the lower end thereof.
[0025] Thus, when the output rod of the electric actuator 8 l is extended, the rear part of the knuckle 7 moves laterally outward so that a toe-in movement of the rear wheel 3 rl is effected. Conversely, when the output rod of the electric actuator 8 l is retracted, the rear part of the knuckle 7 moves laterally inward so that a toe-out movement of the rear wheel 3 rl is effected.
[0026] FIG. 3 is a vertical sectional view of the electric actuator 8 l of the illustrated embodiment. As shown in FIG. 3 , the electric actuator 8 l comprises a first housing 30 a integrally formed with the rubber bush joint (vehicle body) 27 , a second housing 30 b connected to the first housing 27 by a plurality of threaded bolts 31 and forming a whole housing 30 jointly with the first housing 20 a and an output rod 32 extending out of the second housing 30 b and having the rubber bush joint (knuckle) 28 formed at the free end thereof. The first housing 30 a receives therein a brushless DC motor 34 serving as a power source and fixedly attached to the first housing 30 a by using threaded bolts 35 . The second housing 30 b receives therein a planetary gear type reduction gear unit 36 , an elastic coupling 37 and a feed screw mechanism 38 using a trapezoidal thread.
[0027] When the DC motor 34 is actuated, the rotation of the output shaft 34 a thereof is reduced in speed by the reduction gear unit 36 , and is then converted into a linear motion of the output rod 32 by the feed screw mechanism 38 .
[0028] The position sensor 17 provided on the outer periphery of the second housing 30 b essentially consists of a magnet piece 41 fixedly attached to the output rod 32 by a threaded bolt 39 and a differential transformer 43 received in a sensor housing 42 which is in turn attached to the second housing 30 b so as to oppose the magnet piece 41 . The differential transformer 43 includes a primary winding and a pair of secondary windings, and a differential voltage produced between the secondary windings provides a measure of a linear displacement of the output rod 32 .
[0029] FIG. 4 is a block diagram of an essential part of the ECU 20 used in the illustrated embodiment. The ECU 20 includes a damping force control unit 52 for controlling the damping action of the dampers 4 , a rear wheel steering control unit 53 for controlling the steering action of the electric actuators 8 , an input interface 51 interfacing the various sensors 10 - 18 with the damping force control unit 52 and rear wheel steering control unit 53 , and an output interface 54 interfacing the damping force control unit 52 and rear wheel steering control unit 53 with the respective actuators.
[0030] The damping force control unit 52 comprises an attitude control unit 55 , a first control current setting unit 56 , an unsprung mass control unit 57 , a second control current setting unit 58 and a target current selecting unit 59 . The attitude control unit 55 comprises a skyhook control unit 60 , a roll control unit 61 and a pitch control unit 62 which produce a skyhook control target value Dsh, a roll control target value Dr and a pitch control target value Dp, respectively, according to the detection signals of the various sensors 10 - 16 . The first control current setting unit 56 selects one of the three control target values Dsh, Dr and Dp which is the same in sign as the stroke speed of the damper 4 and largest in absolute value as the first target damping force Dtgt1, and looks up a first control current Itb1 from a prescribed first control current map for the given first target damping force Dtgt1 and stroke speed obtained from the stroke sensor 16 .
[0031] The unsprung mass control unit 57 computes an unsprung mass control target value Dw for each damper 4 according to the vehicle speed obtained from the vehicle speed sensor 11 and stroke position obtained from the stroke sensor 16 . The second control current setting unit 58 sets the unsprung mass control target value Dw as the second target damping force Dtgt2, and looks up a second control current Itb2 from a prescribed second control current map for the given second target damping force Dtgt2 and stroke speed obtained from the stroke sensor 16 .
[0032] The skyhook control unit 60 is configured to control the oscillation of the sprung mass, and is effective in suppressing the resonant oscillation of the sprung mass which is about 1 Hz, but is relatively ineffective in suppressing the resonant oscillation of the unsprung mass which is about 10 Hz. In the unsprung mass control, when the damper stroke and stroke speed are high, an unsprung mass control current computed by multiplying a prescribed constant, the damper stroke speed and damper stroke is used instead of the skyhook control current (or added to the target current value required by the skyhook control) to provide the final target current for the damper. As a result, independently of the skyhook control, the resonant oscillation of the unsprung mass in a frequency range around 10 Hz can be effectively suppressed. For more details of the unsprung mass control, reference may be made to Japanese patent laid open publication No. 2006-321259, and U.S. Pat. No. 7,406,371.
[0033] The target current selecting unit 59 compares the obtained first control current Itb1 and second control current Itb2 with each other, and sets one of them having a greater absolute value as the target current Itgt, and supplies a drive current corresponding to the target current Itgt to the magnetic fluid valve of each damper 4 so that a desired damping control may be accomplished.
[0034] The rear wheel steering control unit 53 comprises a road condition estimating unit 63 , a target steering angle setting unit 64 , a target displacement setting unit 65 and a drive current setting unit 66 . The road condition estimating unit 63 estimates the state of the road surface on which the vehicle is traveling according to the unsprung mass control target value Dw computed by the unsprung mass control unit 57 , and forwards the estimated state of the road surface to the target steering angle setting unit 64 . The target steering angle setting unit 64 then determines a rear wheel target steering angle according to the detection signals of the steering angle sensor 10 and yaw rate sensor 14 and the estimated state of the road surface. The target displacement setting unit 65 determines a target displacement of the electric actuator 8 according to the difference between the target rear wheel steering angle and actual rear wheel steering angle obtained from the output of the position sensor 17 . The drive current setting unit 66 supplies a drive current for the electric actuator 8 according to the target displacement.
[0035] The mode of operation of the illustrated embodiment is described in the following. When the operation of the vehicle V has started, the ECU 20 executes the damping force control and a rear wheel steering control at a prescribed control interval (2 ms, for instance).
[0036] The damping control is executed by the damping force control unit 52 . Upon determining the operating condition of the vehicle according to the detection signals of the various sensors 10 - 16 , the damping force control unit 52 computes a skyhook control target value Dsh, a roll control target value Dr and a pitch control target value Dp for each wheel according to the determined operating condition of the vehicle V. The first control current setting unit 56 selects one of these target values which has the same sign as the stroke speed of the damper and the largest absolute value as a first target damping force Dtgt1, and looks up a first target current map to determine a first control current Itb1 according to the first target damping force Dtgt1 and the stroke speed of the damper 4 . The unsprung mass control unit 57 computes an unsprung mass control target value Dw according to the vehicle speed and stroke position of the damper 4 . The second control current setting unit 58 then sets the unsprung mass control target value Dw as a second target damping force Dtgt2, and looks up a second target current map to determine a second control current Itb2 according to the second target damping force Dtgt2 and the stroke speed of the damper 4 . The target current selecting unit 59 selects one of the first target damping force Dtgt1 and second target damping force Dtgt2 which is greater in absolute value as a target current Itgt which is supplied to the damper 4 for controlling the damping force thereof.
[0037] The rear wheel steering control of the illustrated embodiment is described in the following with reference to the flowchart of FIG. 5 . The rear wheel steering control is performed on each of the rear wheels 3 rr and 3 rl in a similar manner, and the following description is limited to that for the left rear wheel 3 rl for the convenience of description.
[0038] The ECU 20 executes the rear wheel steering control illustrated in the flowchart of FIG. 5 concurrently with the damping control described above. The road condition estimating unit 63 determines if the absolute value of the unsprung mass control target value Dw forwarded from the unsprung mass control unit 57 at a regular control interval is greater than a prescribed threshold value S 1 in step ST 1 . If the determination result is Yes, a current cumulative value I n is computed by adding “1” to the previous cumulative value I n−1 in step ST 2 . If the determination result is No, the current cumulative value I n is computed by subtracting “1” from the previous cumulative value I n−1 in step ST 3 . In the latter case, it is determined if the current cumulative value I n is smaller than zero in step ST 4 . If it is the case, the current cumulative value I n is set to zero in step ST 5 . Thus, the minimum value of the current cumulative value I n is zero owing to the process executed in steps ST 4 and ST 5 .
[0039] Following steps ST 2 , ST 4 or ST 5 , the road condition estimating unit 63 determines if the current cumulative value I n is greater than a second threshold value S 2 in step ST 6 . If the determination result of this step is Yes or if the vehicle V is traveling over a rough road surface, the absolute value of unsprung mass control target value |Dw|increases owing to the need to control the vibration of the unsprung mass. Therefore, the state of the road surface can be evaluated by determining if the current cumulative value I n has exceeded the second threshold value S 2 . The determination result of the road condition estimating unit 63 is forwarded to the estimated road surface signal to the target steering angle setting unit 64 .
[0040] When the estimated road surface signal indicates a rough road surface, the target steering angle setting unit 64 set the rear wheel target steering angle to zero in step ST 7 . Each actuator 8 is configured such that the rear wheel steering angle is zero when the actuator is in a neutral state without being extended or retracted. The target displacement setting unit 65 and a drive current setting unit 66 control each electric actuator 8 so that the rear steering angle is maintained at zero. As a result, when the vehicle is traveling over a rough a rough road surface, each electric actuator 8 is maintained in a neutral position so that the impairment of the ride quality which may be otherwise caused by the changes in the tread of the vehicle at the time bump and rebound conditions owing to the extension or retraction of the electric actuator 8 .
[0041] When the estimated road surface signal does not indicate a rough road surface, the rear wheel target steering angle is set in a normal way according to the detection signals of the steering angle sensor 10 and yaw rate sensor 14 in step ST 8 . The target displacement setting unit 65 and a drive current setting unit 66 control each electric actuator 8 so that the actual rear wheel steering angle agrees with the target rear wheel steering angle. When the vehicle is not traveling over a rough road surface, extending or retracting the electric actuator 8 does not cause changes in the tread at the time of bump or rebound, and the actuation of the electric actuator 8 does not impair the ride quality.
[0042] As a slightly modified embodiment of the present invention, the rear wheel target steering angle may be set to a slightly toe-in angle by extending the electric actuator 8 . By forcing the rear wheel target steering angle to a slightly toe-in angle from a normally controlled value, the changes in the tread at the time of the bump and rebound can be controlled, and the ride quality of the vehicle is prevented from being impaired.
[0043] Although the present invention has been described in terms of preferred embodiments thereof, it is obvious to a person skilled in the art that various alterations and modifications are possible without departing from the scope of the present invention which is set forth in the appended claims. For instance, the state of the road surface was estimated from the unsprung mass target value Dw in the foregoing embodiment, but may also be estimated from other data such as the detection signal of the vertical G sensor 15 and image information obtained by a camera.
[0044] The contents of the original Japanese patent application on which the Paris Convention priority claim is made for the present application, as well as the contents of any publications mentioned in this disclosure, are incorporated in this application by reference.
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In a rear wheel steering control system for a vehicle, a rear wheel steering control unit ( 53 ) forces the toe angle of each rear wheel ( 3 rl, 3 rr ) to a substantially neutral position or a slightly toe-in position when a road condition estimating unit ( 63 ) has detected a rough road surface. Thereby, when the vehicle is traveling over a rough road surface, the actuator is forced to the neutral position, and the rear wheels are brought to a neutral position so that the changes in the wheel geometry (tread and/or alignment) of the rear wheels at the time of a bump or a rebound can be avoided. Therefore, the ride quality of a vehicle equipped with the rear wheel steering control system is favorably maintained even when the vehicle is traveling over a road surface, and the rear wheels undergo large vertical displacements.
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FIELD OF THE DISCLOSURE
[0001] The instant disclosure relates to computer networks. More specifically, this disclosure relates to monitoring of computer systems on a computer network.
BACKGROUND
[0002] Computer systems, and servers in particular, form an information backbone upon which companies now rely on almost exclusively for data storage, data mining, and data processing. These systems are indispensable for the improved efficiency and accuracy at processing data as compared to manual human processing. Furthermore, these systems provide services that could not be realistically accomplished by human processing. For example, some computer systems execute physical simulations in hours that would otherwise take decades to complete by human computations. As another example, some computer systems store terabytes of data and provide instantaneous access to any of the data, which may include records spanning decades of company operations.
[0003] Monitoring these computers systems is a top priority for their operators and administrators to ensure that the computer systems are continuously available without interruption. These computer systems may demonstrate a coming problem, but if certain parameters of the computer system are not monitored, the corning problem may not be recognized in time for an administrator to take corrective action before a complete failure. For example, data channels in a computer system may experience a reduction in data rate prior to a complete failure of the data channel, However, conventionally there is no monitoring of the data channel data rate. Only after a complete failure would an administrator be alerted to a problem with the data channel, Even then, the administrator would likely not be aware of a problem until several users complained of the data channel failure. Waiting for a total failure of the data channel before taking corrective action causes downtime during which the data channel was unavailable and users were unable to access data.
SUMMARY
[0004] Computer systems, such as servers, may be monitored through a script engine executed on a client computer system remote from the servers. The computer system may execute a different operating system than the operating system executing on the server. The monitor may communicate with the server, issue scripts for execution on the server, parse results received from the server, and detect and/or correct conditions on the server that may lead to a failure.
[0005] Monitoring may be programmed once and deployed to any number of systems. The monitoring may continue 24 hours a day, 7 days a week, 365 days a year. In one embodiment, the monitoring may be performed by agentless monitoring. Unlike agents that consume memory, CPU, and disk space in their monitoring efforts, agentless monitoring is achieved at the cost of only a single additional (simulated) user on the target system. Commands submitted are those implemented by the primary system vendor, so customized programs need not me written and maintained. This further reduces monitoring cost and leads to a robust solution that may be evolved over time as needs change. Automated, agentless monitoring has very low impact (footprint) on the system as commands are submitted and the results examined.
[0006] One example of the monitoring includes detection of hardware degradation by monitoring data rates on data channels. Data channels connect a central processor to data sources, such as internal hard drives, internal solid state storage devices, external hard drives, external solid state storage devices, external tape drives, and/or other servers. When a hardware component begins to degrade, either the central processor, the storage device, or a bus processor between the central processor and the storage device, the data rate on the data channel decreases over time until a complete failure of the data channel. Previously, no human operator could repeatedly submit the commands necessary, perform the calculations required, and alert an administrator about the degradation of a data channel. Outright failure would occur before any problem was detected. Periodic console commands may be issued by an agentless monitor to probe a set of channels, average the combined data rates, and compare each channel in turn to this average actual rate. A degraded channel may thereby be identified, when its data rates are much lower than the others. Then, that data channel may be repaired or replaced. Automated detection flags a data channel problem within minutes of poor performance.
[0007] In one embodiment, the monitoring may be performed by generalized, modular code, which executes recursively through a list of channel names that need only be defined once within the compiled source code. This allows for easy maintenance when channel names change over time by allowing a simple mechanism to update their names within the code. To present an open-ended list of channel names to the code module, recursive list processing is employed using, for example, a simple pattern-matching language (SP-AMS). SP-AMS may be activated through use of a special Attribute Change Event Report, which may be implemented as a service and which may generate Message Event Reports in response to the Attribute Change Event Report. This processing may be implemented, in one embodiment, as an extension to the Shared Object Manager Application (SOMA), described in U.S. Pat. No. 6,154,787, which is hereby incorporated by reference. The SOMA may receive an Attribute Change Event Report of channels to examine (minus the channel currently being processed) from the channel monitoring solution and present a reduced list back to the solution as a Message Event Report. This SOMA-generated Message Event Report may appears as a typical console message to SP-AMS without causing disruption to normal console traffic. The effect is to recursively process all channel names, with the recursion being terminated after the last channel has been processed. Adding recursion to SP-AMS allows for elegant solution development, ease of maintenance, and may be applied to many other solutions in the future.
[0008] In one embodiment, channel data rates are expressed as large, 32-bit unsigned integers (e.g., 0 to 4294967296), but SP-AMS integer variables may only store 16-bit signed integers (e.g., −32768 to 32768). To accommodate data structures unable to store large-valued channel data rates an average of the accumulated data rates of all channels may be compared to each channel's individual data. rate and any channel with data rates far enough below this constantly-updated average may be flagged as potentially degraded. As the data rate disparity grows, the alert may be escalated and the alert's visibility enhanced by external notification, such as a text message or email message, 32-bit integers may be treated as string values and calculations performed by positive integer conversion to exploit a subtle effect in the storage of integers that allows for much larger numbers to be held in SP-AMS integer variables, such as when strings converted to unsigned integers are not handled the same way internally as 16-bit signed integers. This is one example of a method to allow 32-bit unsigned arithmetic on channel data rates within SP-AMS.
[0009] According to one embodiment, a method may include measuring, by a monitoring agent, a data rate of a set of channels for communication by a remote computer. The method may also include calculating, by the monitoring agent, an average data rate for the set of channels. The method may further include determining, by the monitoring agent, whether any channel of the set of channels is below a threshold amount in reference to the calculated average data rate. The method may also include generating, by the monitoring agent, an alert for a data channel when the data channel is determined to be below the calculated average data rate by the threshold amount.
[0010] According to another embodiment, a computer program product may include a non-transitory computer readable medium. The medium may include code to perform the step of measuring a data rate of a set of channels for communication by a remote computer. The medium may also include code to perform the step of calculating an average data rate for the set of channels. The medium may further include code to perform the step of determining whether any channel of the set of channels is below a threshold amount below the calculated average data rate. The medium may also include code to perform the step of generating an alert for a data channel when the data channel is determined to be below the calculated average data rate by the threshold amount.
[0011] According to yet another embodiment, an apparatus may include a memory and a processor coupled to the memory. The processor may be configured to execute the step of measuring a data rate of a set of channels for communication by a remote computer. The processor may also be configured to perform the step of calculating an average data rate for the set of channels. The processor may further be configured to perform the step of determining, by the monitoring agent, whether any channel of the set of channels is below a threshold amount in reference to the calculated average data rate. The processor may also be configured to perform the step of generating an alert for a data channel when the data channel is determined to be below the calculated average data rate by the threshold amount.
[0012] The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter that form the subject of the claims of the invention. It should be appreciated by those skilled in the art that the conception and specific embodiment disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims. The novel features that are believed to be characteristic of the invention, both as to its organization and method of operation, together with further objects and advantages will be better understood from the following description when considered in connection with the accompanying figures. It is to be expressly understood, however, that each of the figures is provided for the purpose of illustration and description only and is not intended as a definition of the limits of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] For a more complete understanding of the disclosed system and methods, reference is now made to the following descriptions taken in conjunction with the accompanying drawings.
[0014] FIG. 1 is a flow chart illustrating a method of monitoring data channel data rates according to one embodiment of the disclosure.
[0015] FIG. 2 is a call diagram illustrating agentless monitoring of data channel data rates according to one embodiment of the disclosure,
[0016] FIG. 3 is a flow chart illustrating monitoring data channel data rates with recursion according to one embodiment.
[0017] FIG. 4 is a block diagram illustrating a computer network according to one embodiment of the disclosure.
[0018] FIG. 5 is a block diagram illustrating a computer system according to one embodiment of the disclosure.
DETAILED DESCRIPTION
[0019] FIG. 1 is a flow chart illustrating a method of monitoring data channel data rates according to one embodiment of the disclosure. A method 100 begins at block 102 with measuring a data rate of each channel of a set of channels on a remote computer. For example, a monitoring agent may initiate a communications session to a remote computer and execute script commands to obtain the data rates of a set of channels on the remote computer. At block 104 , an average data rate may be calculated for the set of channels. Then, at block 106 , it is determined whether any channel of the set of channels is below a threshold amount below the calculated average. For example, if the calculated average for the set of channels is 1.0 Mb/s and the threshold is 500 kb/s, then any channel with a data rate below 500 kb/s may be flagged for an alert. At block 108 , an alert is generated for any channel flagged at block 106 . The alert may include, for example, a text message or an email to one or more administrators.
[0020] FIG. 2 is a call diagram illustrating agentless monitoring of data channel data rates according to one embodiment of the disclosure. A monitoring agent 204 may execute on a client 202 . The client 202 may host a number of monitors, such as by executing each monitor in a hosted environment. The monitor 204 may initiate a communication session with a server 206 at call 212 . At call 214 , scripted commands are transmitted to the server 206 . One set of example scripted commands for measuring data rates is illustrated in script 214 A. The scripted commands may be selected from sets of scripted commands programmed into the monitor and set to execute at specific times or specific intervals based, at least in part, on the computer name or computer type of the server 206 . At call 216 , the server 206 executes the scripted commands. The scripted commands may be executed, for example, through a simulated user on the server 206 . Executing through a simulated user allows the scripted commands to be executed on the server 206 without any additional software loaded on the server 206 . At call 218 , results from the scripted commands are transmitted from the server 206 to the monitor 204 . One set of example results is illustrated in results 218 A. The monitor 204 then calculates an average and compares the channels to the average for determining whether to generate an alert for a data channel at call 220 .
[0021] FIG. 3 is a flow chart illustrating monitoring data channel data rates with recursion according to one embodiment. A method 300 begins at block 302 with executing periodic channel input/output (I/O) rate commands on the remote computer to monitor a set of channels. At block 304 , SP-AMS receives the results of the rate commands at block 302 and saves a copy of all channel names and sends the channel names to SOMA with an AC Event Report. Then, at block 306 , SOMA presents the channel list to SP-AMS as an ME Event Report. At block 308 , SP-AMS recursively builds an average data rate for the set of channels by passing one less channel to SOMA until the channel name list is exhausted. At block 310 , SOMA receives the channel list and presents it to SP-AMS as an ME Event Report. Then, at block 312 , SP-AMS recursively compares each channel to the average I/O rate and sends a reduced set to SOMA until the list is exhausted. At block 314 , an alert is generated if a degraded channel is found, indicated by an I/O rate below the average by at least a threshold amount.
[0022] FIG. 4 illustrates one embodiment of a system 400 for an information system, including a system for agentless monitoring of data channels. The system 400 may include a server 402 , a data storage device 406 , a network 408 , and a user interface device 410 . In a further embodiment, the system 400 may include a storage controller 404 , or storage server configured to manage data communications between the data storage device 406 and the server 402 or other components in communication with the network 408 . In an alternative embodiment, the storage controller 404 may be coupled to the network 408 .
[0023] In one embodiment, the user interface device 410 is referred to broadly and is intended to encompass a suitable processor-based device such as a desktop computer, a laptop computer, a personal digital assistant (PDA) or tablet computer, a smartphone, or other mobile communication device having access to the network 408 . In a further embodiment, the user interface device 410 may access the Internet or other wide area or local area network to access a web application or web service hosted by the server 402 and may provide a user interface for specifying the threshold for alerts or viewing I/O rates for data channels.
[0024] The network 408 may facilitate communications of data between the server 402 and the user interface device 410 . The network 408 may include any type of communications network including, but not limited to, a direct PC-to-PC connection, a local area network (LAN), a wide area network (WAN), a modem-to-modem connection, the Internet, a combination of the above, or any other communications network now known or later developed within the networking arts which permits two or more computers to communicate.
[0025] FIG. 5 illustrates a computer system 500 adapted according to certain embodiments of the server 402 and/or the user interface device 410 . The central processing unit (“CPU”) 502 is coupled to the system bus 504 . The CPU 502 may be a general purpose CPU or microprocessor, graphics processing unit (“GPU”), and/or microcontroller. The present embodiments are not restricted by the architecture of the CPU 502 so long as the CPU 502 , whether directly or indirectly, supports the operations as described herein. The CPU 502 may execute the various logical instructions according to the present embodiments.
[0026] The computer system 500 may also include random access memory (RAM) 508 , which may be synchronous RAM (SRAM), dynamic RAM (DRAM), synchronous dynamic RAM (SDRAM), or the like. The computer system 500 may utilize RAM 508 to store the various data structures used by a software application. The computer system 500 may also include read only memory (ROM) 506 which may he PROM, EPROM, EEPROM, optical storage, or the like. The ROM may store configuration information for booting the computer system 500 . The RAM 508 and the ROM 506 hold user and system data, and both the RAM 508 and the ROM 506 may be randomly accessed.
[0027] The computer system 500 may also include an input/output (I/O) adapter 510 , a communications adapter 514 , a user interface adapter 516 , and a display adapter 522 . The I/O adapter 510 and/or the user interface adapter 516 may, in certain embodiments, enable a user to interact with the computer system 500 . In a further embodiment, the display adapter 522 may display a graphical user interface (GUI) associated with a software or web-based application on a display device 524 , such as a monitor or touch screen.
[0028] The I/O adapter 510 may couple one or more storage devices 512 , such as one or more of a hard drive, a solid state storage device, a flash drive, a compact disc (CD) drive, a floppy disk drive, and a tape drive, to the computer system 500 . According to one embodiment, the data storage 512 may be a separate server coupled to the computer system 500 through a network connection to the I/O adapter 510 . The communications adapter 514 may be adapted to couple the computer system 500 to the network 408 , which may be one or more of a LAN, WAN, and/or the Internet. The user interface adapter 516 couples user input devices, such as a keyboard 520 , a pointing device 518 , and/or a touch screen (not shown) to the computer system 500 . The keyboard 520 may be an on-screen keyboard displayed on a touch panel. The display adapter 522 may be driven by the CPU 502 to control the display on the display device 524 . Any of the devices 502 - 522 may be physical and/or logical.
[0029] The applications of the present disclosure are not limited to the architecture of computer system 500 . Rather the computer system 500 is provided as an example of one type of computing device that may be adapted to perform the functions of the server 402 and/or the user interface device 410 . For example, any suitable processor-based device may be utilized including, without limitation, personal data assistants (PDAs), tablet computers, smartphones, computer game consoles, and multi-processor servers. Moreover, the systems and methods of the present disclosure may be implemented on application specific integrated circuits (ASIC), very large scale integrated (VLSI) circuits, or other circuitry. In fact, persons of ordinary skill in the art may utilize any number of suitable structures capable of executing logical operations according to the described embodiments. For example, the computer system 600 may be virtualized for access by multiple users and/or applications.
[0030] If implemented in firmware and/or software, the functions described above may be stored as one or more instructions or code on a computer-readable medium. Examples include non-transitory computer-readable media encoded with a data structure and computer-readable media encoded with a computer program. Computer-readable media includes physical computer storage media. A storage medium may be any available medium that can be accessed by a computer. By way of example, and not limitation, such computer-readable media can comprise RAM, ROM, EEPROM, CD-ROM or other optical disk storage, magnetic disk storage or other magnetic storage devices, or any other medium that can be used to store desired program code in the form of instructions or data structures and that can be accessed by a computer. Disk and disc includes compact discs (CD), laser discs, optical discs, digital versatile discs (DVD), floppy disks and blu-ray discs. Generally, disks reproduce data magnetically, and discs reproduce data optically. Combinations of the above should also be included within the scope of computer-readable media.
[0031] In addition to storage on computer readable medium, instructions and/or data may be provided as signals on transmission media included in a communication apparatus. For example, a communication apparatus may include a transceiver having signals indicative of instructions and data. The instructions and data. are configured to cause one or more processors to implement the functions outlined in the claims.
[0032] Although the present disclosure and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the disclosure as defined by the appended claims. Moreover, the scope of the present application is not intended to be limited to the particular embodiments of the process, machine, manufacture, composition of matter, means, methods and steps described in the specification. As one of ordinary skill in the art will readily appreciate from the present invention, disclosure, machines, manufacture, compositions of matter, means, methods, or steps, presently existing or later to be developed that perform substantially the same function or achieve substantially the same result as the corresponding embodiments described herein may be utilized according to the present disclosure. Accordingly, the appended claims are intended to include within their scope such processes, machines, manufacture, compositions of matter, means, methods, or steps.
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Data channels of a computer system may be remotely monitored to detect data channel degradation. A monitoring agent on a client may execute script commands on the remote computer system to monitor input/output (I/O) rates of a set of channels. The monitoring agent may compute an average data rate of the data channels and compare the I/O rate of each channel to the average. When the rate of a channel falls below the average by at least a threshold amount, an alert may be generated to indicate to an administrator a possible failure with the data channel.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of provisional patent application Ser. No. 61/353,994, filed with the USPTO on Jun. 11, 2010, which is herein incorporated by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable.
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISK
[0003] Not applicable.
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] The present invention generally relates to the treatment of articulated joint injuries and maladies, whether pre- or post-operative or degenerative in nature, and more specifically to systems/devices that facilitate joint recovery by applying constant microclimate cooling or heating and optionally compression to an affected joint in a secure, comfortable and reliable manner, even during repeated joint flexure or movement.
[0006] 2. Background
[0007] As is already known in the art, the knee is the most injury-prone joint of the body and, at the same time, is frequently affected by arthroses since it can easily become mechanically unstable and bears the full weight of the body. Muscular imbalance often causes pains in the anterior kneecap. In persons who practice sedentary professions, the ischioscural musculature is for the most part contracted, drawing the articular capsule rearward, increasing contact pressure in an undesirable manner. Sporting injuries of the knee joint frequently result when the lower leg is twisted while placing weight on the joint—often resulting in lesions of the knee and associated local pain. The complexity of the joint renders exact diagnosis and treatment difficult, often contributing to later degenerative processes.
[0008] As is also known, other articulating joints evidence similar problems. Some of the more common articulating joints and maladies are discussed in the next few paragraphs.
[0009] Ankles are quite complex, being comprised of both the subtalar joint and the ‘true’ ankle joint (itself comprised of the tibia, which forms the medial portion of the ankle; the fibula, which forms the lateral portion of the ankle; and the talus, underneath)—all bearing full body weight loads and being prone to stress and potential injury under torsional loads.
[0010] While shoulder joints do not bear the constant heavy loads borne by either knees or ankles, they sustain motion in many axes and are required to bear high dynamic loads. The two main bones of the shoulder are the humerus and the scapula (shoulder blade). The shoulder joint cavity is cushioned by articular cartilage covering the head of the humerus and face of the glenoid. The scapula extends up and around the shoulder joint at the rear to form a roof called the acromion, and around the shoulder joint at the front to form the coracoid process. The end of the scapula (the glenoid) meets the head of the humerus to form a glenohumeral cavity that acts as a flexible ball-and-socket joint. The joint is stabilized by a ring of fibrous cartilage (the labrum) that surrounds the glenoid. Ligaments and tendons join the bones to surrounding muscles, stabilizing the joint. For instance, four short muscles originate on the scapula and pass around the shoulder where their tendons fuse together to form the rotator cuff. These components of the shoulder, along with the muscles of the upper body, work together to manage the stress experienced by the shoulder through flexure, extension, lifting and throwing. Nature's design of this joint underscores an essential point relating to products seeking to bring thermal and/or pressure treatment to articulated joints: the design of a successful treatment product must contemplate both necessary joint range of motion (both extent and angle) as well as the musculature in the affected region.
[0011] Even the elbow joint is more complex than most realize and imposes special considerations for treatment. This joint is essentially a ‘hinge’ joint; comprised of the humerus, ulna and radius. The positioning and interaction of these bones allows for a small amount of rotation as well as hinging. Joint stability is principally provided by the ulnar collateral ligament on the medial side of the elbow. The lateral side of the joint suffers the most common afflictions, sometimes going by the name ‘tennis elbow.’
[0012] The wrist is formed where the two bones of the lower arm—the radius and the ulna—meet at the hand. It provides passage to the two major nerves of the hand (the median and ulnar nerves) which run the length of the arm to transmit electrical impulses to and from the brain to create movement and sensation.
[0013] One of the more common afflictions of the wrist is Carpal Tunnel Syndrome, a pinching of the median nerve within the wrist—frequently a result of highly repetitive and recurring motion. The carpal tunnel is a bony canal within the palm side aspect of the wrist that allows for the passage of the median nerve to the hand. Pinching or compression of this nerve by the transverse carpal ligament sets into motion a progressively crippling disorder which eventually results in wrist pain, numbness and tingling in the hand, pain consisting of a “pins and needles” feeling at night, and weakness in the grip. The wrist is also subject to cartilage damage (much like the knee), which is often repaired with arthroscopic surgery.
[0014] All of these joints can suffer damage from high dynamic loading, overloading in/across the wrong motions/axes, and through repeated repetitive motions commonly develop tendon, muscle and joint related—and even degenerative—problems that can be mitigated by using a suitable articulated joint treatment system. When traumatized, these joints frequently swell and may create further trauma by involving local muscles or tendons.
[0015] While the body has additional articulating joints (e.g. the neck), each of which may require different overall system design changes to optimize therapeutic outcome, to one skilled in the art it is apparent that a well designed treatment system ‘approach’ will include variations or parameters that enable the treatment of other articulated body joints that are not discussed herein.
[0016] Arthroscopic surgery, often used to repair joint/cartilage problems, has become quite common; indeed, arthroscopic knee surgery has become the most commonly performed orthopaedic procedure in the United States. While this surgery can be quite effective in repairing many kinds of joint, cartilage or tendon damage, it typically has limited utility on degenerative joint conditions.
[0017] In addition to degenerative conditions catalyzed by injury, osteoarthritis has become one of the most common joint diseases known to man and afflicts millions of people to a clinically significant degree in the United States alone. While degenerative pathologies vary by person, the principal symptoms suffered by osteoarthritis patients are pain in and around the affected joint and a lessening of joint mobility. Largely because arthroscopic procedures generally deliver limited long-term value in treating degenerative joint conditions (and, in part, because some patients do not favor surgery), osteoarthritis centers have sprung into being to help patients improve affected joint mobility and manage pain. The incidence of this disease generally increases with the age of the patient.
[0018] As is already known, diverse treatment protocols and devices have been developed to treat different articulated joint (and associated tendon/musculature) problems. Such treatment protocols may include either cooling or heating the affected area in conjunction with different means of either immobilizing the joint or specifically enabling and managing flexure through range of motion and strength building exercises, whether by brace, prosthetic device or flexible wraps. Some of the associated devices apply gentle pressure—others do not—using carefully shaped bandages or inflated structures. Yet other treatment includes the use of anti-inflammatory agents (such as aspirin) or the intra-articular injection of various materials including corticosteroids or cartilage powder(s).
[0019] Cooling treatment is commonly used for acute injuries, especially where swelling is or may become present—providing both short-term pain relief and a reduction of swelling by reducing blood flow to the injured area.
[0020] For instance, the R.I.C.E. method is commonly used—RICE stands for “Rest, Ice, Compression and Elevation”—where ice or ‘frozen gel’ packs are used to relieve pain, limit swelling and protect the injured tissues, promoting faster healing. Unfortunately, the RICE method has historically relied upon the use of either ice or ‘frozen gel’ to achieve localized cooling, both of which can cause profound skin and/or tissue damage if left in contact with the body for more than about 20 minutes (proper use of this method cycles cooling packs on and off the affected area). This can be problematic in both medical settings (where staff responsibilities may preclude cycling packs on/off at the necessary intervals) and especially at home—where both inadequate training regarding the risks of thermal over-exposure exacerbated by the body's natural tendency towards adaptation (wherein the body becomes less sensitive to temperature sensations) cause the patient to believe the pack doesn't yet need to be removed/cycled. The incidence of RICE method accidents is high enough that numerous class action lawsuits are being developed around failures of this technique.
[0021] Various approaches/equipment have been devised to provide such localized cooling—ranging from a frozen bag of peas held in place by hand to using various cooling packs such as those described in U.S. Pat. Nos. 4,628,932 and 6,470,705 and others. Some embodiments include an outer layer that helps buffer the cold so the user can more comfortably hold the pack against the affected area; others integrate layers to absorb attendant bodily fluids and/or condensate from the cooling bags (which are quite cold). Yet other embodiments include various attachment means, including straps in different configurations so the cooling pack can be held against the knee without being manually held in place or means to lash or wrap the cooling bag or container to the joint.
[0022] A common problem amongst such devices is their inability to readily conform to the affected joint (in the case of the patents noted above, the knee joint)—especially during motion. It becomes nearly impossible to use such cooling to reduce swelling while simultaneously operating the joint through range of motion or repetitive exercises.
[0023] When the attachment means is lashing or wrapping the cooling pack against the injured joint, joint movement commonly causes the lashing to unravel and/or become looser, potentially aggravating the injury and causing additional pain. While wrapping the joint more tightly can mitigate the risks of loosening, joint pain and potential swelling often rises with increased wrapping tension. As well, properly adjusting the cooling pack to the affected joint can be difficult; adjustments may require the joint to be completely unwrapped and then re-wrapped. These problems are exacerbated by the need to cycle cooling packs off the joint every 20 minutes or so in order to prevent tissue damage associated with over cooling.
[0024] U.S. Pat. No. 4,585,003 seeks to remedy these problems by using die-cut flexible materials to more conveniently attach cooling bags—but this approach often creates other problems associated with frequent use because the material may not breath, can irritate the skin (sometimes causing rashes) and accommodates bacterial infestations which can transfer to (and affect) the user's skin. These hygiene problems make it unwise to use a given wrap with more than a single patient. Moreover, most such devices do not allow external access to the ice/gel packs for ready removal or replacement.
[0025] U.S. Pat. Nos. 5,728,057 and 5,728,058 develop a flexible web which is designed to accommodate bending of the user's knee joint, and which integrate discrete thermal elements into the web to apply either modest heating or cooling to an injured joint. These wraps are meant to be disposable—so hygiene problems are generally eliminated—and the design helps to address the challenges of wrap ‘bunching’ or other undesired movement during repeated knee flexure. Because of how the thermal elements are incorporated into the design, however, only limited heating or cooling can be applied to the joint, sharply limiting therapeutic value. Long-term thermal treatment can become quite expensive since these webs are designed to support only one-time use. Unintended device movement—and movement of thermal elements away from the intended region(s)—is also a problem with other articulated joints.
[0026] Similar problems pertain to devices designed to deliver heat, typically by means of disposable heating packs. Disposable packs based upon iron oxidation, such as described in U.S. Pat. Nos. 4,366,804 and 4,649,895 and 5,046,479 are known. However, most such devices are often bulky, cannot maintain a consistent and controllable temperature, have difficulty staying in place during use and/or cannot be easily incorporated into wraps that conform to the body's contours. Such devices are inconvenient to use on a regular or extended basis because the thermal energy may not be immediately available when needed or released in a controllable manner. Some such devices include risks of topical burns—analogous to the skin/tissue damage associated with ice/gel packs, though caused by heat rather than cold—especially due to the non-linear heat release characteristics of iron oxide heating packs. U.S. Pat. No. 6,048,326 describes a wrap that mitigates some of these conformity and positioning problems, but without addressing the non-linear heat release tendencies.
[0027] Various devices have been proposed to address longer-term heating or cooling non-linearity or to create a more consistent localized temperature—some in conjunction with compression. U.S. Pat. No. 5,314,455 sets forth a cuff with a watertight cavity shaped to envelope only the anterior and sides of the knee. This device has therapeutic limits—it does not cover all sections of the knee for which cooling is typically specified—and uses a gravity fed approach to fill the cuff The patient must hold a container above the cuff until it is sufficiently filled and later—once the fluid temperature has changed and the fluid needs to be refreshed—must siphon the contained fluid into a container so the process can be repeated. This process is, at best, frustrating, and may require external assistance. As well, such cuffs limit joint flexure and effectively immobilize the patient.
[0028] US Patent Application US 2005/0033390 A1 describes a thermal compression system incorporating a (thermal) fluid input and output line with an external pump that circulates the heating/cooling fluid. This system helps mitigate the challenges of replacing thermal packs on a frequent and repetitive basis and solves some of the problems unaddressed in U.S. Pat. No. 5,314,455, but still requires significant patient or external professional interaction and may significantly limit patient mobility and/or joint flexure. It is unclear whether sensors or safety systems exist to limit thermal fluid temperatures to a regime safe for long-term skin/tissue exposure.
[0029] Various commercial devices have been developed, as the need for decent treatment devices is so keen. The “Moji” knee, for instance, offers many of the features described in the patents above: frozen gel, a moisture wicking fabric layer, and an elastic wrap which applies tension to help keep the system in place. This design still suffers critical flaws: it must still be removed after 15-20 minutes, (as it is too cold for long-term skin contact), has limited capacity for pressure adjustment, and somewhat limits knee joint flexure.
[0030] What is needed is an articulated joint treatment solution that provides:
a constant, consistent and safe microclimate temperature—one chosen by a treatment professional to optimize therapeutic/recovery outcome—in order to achieve therapeutic benefits without any associated risks of adverse events such as skin/tissue damage through over exposure or long-term use; usage without requiring proximal connection (such as power cords or tubing used to convey either gas or liquid) to ancillary systems, which may substantially limit patient mobility; a shape/fit that delivers thermal treatment where it is physically needed to enhance joint recovery and comfort; for joint flexure using one or more ‘active hinges’ to interconnect and register the multiple wraps/pieces in a way that enables full range of motion, repetitive motion and strength building exercises without causing the treatment system to move, bunch, create additional patient discomfort or to relocate the thermal treatment away from the specific affected regions needing this treatment; a skin contact surface that either inhibits bacterial and/or fungal growth which lends itself to cleaning/sterilization; a skin contact surface or surfaces that minimize patient skin discomfort and/or allergic reactions; an adjustable fit, so it can be used on patients of different size and/or so device tension can be optimized to patient comfort and/or the chosen recovery regimen; sufficient durability to be used in more than one treatment session, whether by the patient or a treatment center (that may use the device amongst several patients); a design comprised only of materials that are safe for use with skin and tissue so that a broken or compromised device doesn't pose additional danger(s) to the wearer. In the case of a system containing fluid(s), for instance (as discussed below), the fluid(s) should be non-toxic, non-caustic and dielectric (to eliminate shock risks if used in conjunction with powered sub-systems); an optional capacity to temporarily immobilize the articulated joint treatment system as needed (to position the joint precisely as chosen by a treatment professional while still delivering the benefits of constant-temperature treatment) so the beneficial effects of long-term constant temperature microclimate modification can be delivered while the joint is immobilized. The angle of such immobilization may be either adjustable or non-adjustable to suit therapeutic needs; and an optional capacity to apply pressure, via integrated means (such as one or more pressurized bladders), to apply pressure to a specific treatment area or areas. To be of greatest utility, said pressure(s) should be adjustable and capable of being sustained for long periods of time. Such pressurized bladders may be a permanent feature of the invention's assembly, or may be installed into pockets or other attachment means.
[0042] Unfortunately, as noted herein, previous efforts to create articulated joint treatment devices that modify wearer microclimate suffer from profound disadvantages including: significant risk of skin/tissue damage from prolonged exposure to heat or cold, hygienic risks that may exacerbate joint recovery in post-operative scenarios, overly restrictive joint range of motion, severely restricted patient mobility, the tendency to bunch up or “move” thermal treatment cells away from the intended location(s) during joint flexure and exercise, sub-optimal microclimate temperature and thermal consistency (including the need to cycle thermal packs on/off the joint or failure to sustain the localized temperature within an optimal temperature range), or requiring proximal connection to ancillary systems—whether to enable recirculation, power (such as for thermo-electric modules) or other purposes.
[0043] While ice, gels and iron oxides—the most common cooling and heating technologies respectively—have been around for generations, constant cooling devices (whether set for single or multiple stable transitions) have not. A constant cooling device could work to keep the operational temperature at (or approximately at) a preset or given temperature. In cooling, for instance, such a device could be elevated well above said ice and or gel associated temperatures, providing all the benefits of cold therapy without the associated risks, such as, frostbite, histamine and aqueous production.
[0044] As is known in the art, thermo-electric modules—with suitable feedback sensors or controls (whether external or integral to the module)—are capable of presenting a stable constant temperature microclimate but suffer additional problems such as: high cost, physical inflexibility, difficulty to incorporate into shapes/wraps etc needed to conform to a joint, and the need to provide electricity to power the modules (requiring attachment to ancillary systems and/or creating additional reliability and/or safety risks).
[0045] As is also known in the art, there are a wide range of Phase Change Materials (PCMs), that is, substances with a high heat of fusion, which, melting and solidifying at a certain temperature, are capable of storing and releasing large amounts of energy. Thermal energy is absorbed or released when the material changes from solid to liquid, making PCMs a latent heat storage material.
[0046] As is also known, while PCM latent heat storage can be achieved through all forms of chemical transition: (solid-solid, solid-liquid, solid-gas and liquid-gas phase change) the only phase change of practical use in most applications is the solid-liquid change. Liquid-gas phase changes are not practical for use as thermal storage due to the large volumes or high pressures required to store the materials when in their gas phase. Liquid-gas transitions do have a higher heat of transformation than solid-liquid transitions. Solid-solid phase changes are typically very slow and have a rather low heat of transformation.
[0047] Initially, solid-liquid PCMs behave like sensible heat storage (SHS) materials; their temperature rises as they absorb heat. Unlike conventional SHS, however, when PCMs reach the temperature at which they change phase (their melting temperature) they absorb large amounts of thermal energy at an almost constant temperature. The PCM absorbs heat without a significant rise in temperature until all the material is transformed to the liquid phase. When the ambient temperature around a liquid material falls, the PCM solidifies, releasing its stored latent heat. These properties make PCMs suited to providing either articulated joint therapeutic system heating or cooling, provided the PCM temperature(s) is/are properly chosen.
[0048] The best-known phase change material is water—which can exist as either liquid or ice at 32° F. (0° C.) at normal pressures. Certain properties of water/ice, however, render it of little use (or useless) in given applications, including: the phase temperature cannot be modified (ice is too cold to be used for long in most biological applications as applying ice to tissue quickly results in severe vasoconstriction and vastly reduced capillary blood flow), the water to ice transition results in a volumetric expansion of ˜9%—making it a challenge to use in mechanical applications, and ice exhibits little mechanical “give” in the fully frozen state. While this expansion factor may not be relevant in some joint treatment applications, the overly cold temperature is.
[0049] Other PCMs can be either organic or inorganic, can be chemically stable or unstable, can be caustic or non-caustic, flammable/inflammable, etc. In short, like any other substances, PCM chemical properties vary as a function of the specific substance. PCMs are typically characterized by their Heat of Fusion (measured in kJ/kg), the amount of energy required to melt one kilogram of the material, and the Duration Index [measured in Joules/(cubic centimeter*degrees Centigrade)], which provides a basis of comparison of how long a PCM will remain at a constant temperature during its phase change.
[0050] Common PCMs include paraffins (alkanes), salt hydrates, eutectic compounds, fatty acids and esters (including animal fats) and others. Individual PCMs will suggest themselves over others depending on the user's specific requirements. Some transition sharply (at a given temperature), whereas others (especially with impurities) do so over a several degree temperature range with reduced heat capacity. Others lose the capacity to transition sharply after a certain number of uses (eutectics often degrade after a few thousand cycles, rendering them of little use in many applications). Some PCMs are highly flammable; some are not. In general, however, PCMs can be useful as thermal energy storage media provided their other chemical properties are consistent with a given application.
[0051] The disclosed system is an articulated joint treatment constant or phased temperature microclimate control system that can be fine-tuned at the time of manufacture to specific treatment/recovery applications, ambient temperature ranges and therapeutic regimens, and is capable of meeting either specific microclimate temperatures and/or cooling/heating periods. It does this while concurrently providing an adjustable fit and pressure to the joint, imparting protective force impact protection to the wearer, and while enabling either superior range-of-motion or fixed-position therapeutic treatment.
BRIEF SUMMARY OF THE INVENTION
[0052] The present invention comprises a system and/or method that have one or more of the following features and/or steps, which alone or in any combination may comprise patentable subject matter.
[0053] According to one embodiment of the present invention, an articulated joint treatment system which creates a localized impact absorbing microclimate managed environment comprising one or more conforming wraps, these wraps being held in alignment or registration to each other via tangs, registration marks or other visible features used in combination with ties, straps or more solid mechanical connection; each wrap having one or a plurality of cells of one or more sizes and shapes wherein each of the one or plurality of cells is comprised of a momentarily deformable high modulus material containing cooling or heating thermal material, wherein the materials may be different from cell to cell.
[0054] In another embodiment of the present invention, the shape of the one or plurality of thermal material containment cells may be adjusted to be relatively flat on one face (which is worn against the treated area) with the opposing face being allowed to bulge outwards to contain a high volume of the cooling or warming material, in this manner creating a comfortable surface against the wearer's body while still incorporating long thermal treatment periods.
[0055] Another embodiment of the present invention may yet further comprise one or more sections which are capable of applying pressure to select portions of the wearer's body, said pressure being independently adjustable by section (chosen, for instance, by the cognizant healthcare professional or athletic trainer) and sustainable for extended periods of time.
[0056] In yet another embodiment of the present invention, said pressure-applying capacity may be configured as either a permanent feature of the system or one that is temporarily installed.
[0057] Yet still another embodiment of the present invention may further comprise an articulated joint treatment system wherein mechanical limiting structures, such as rigid or semi-rigid features are used in conjunction with holding pockets slits or other attachment structures known within the art to fix or immobilize the joint at a chosen angle.
[0058] A preferred embodiment will incorporate a constant or phased constant temperature microclimate control system to create a stable thermal environment, such as can be achieved by use of an appropriate PCM, which can be fine-tuned at time of manufacture.
BRIEF DESCRIPTION OF THE DRAWINGS
[0059] FIGS. 1-4 depict multiple embodiments and configurations of treatment systems of the present invention.
[0060] FIG. 5 depicts one embodiment of tendon treatment within the scope of the present invention.
[0061] FIG. 6 depicts one embodiment of a hexagonal cell configuration of the present invention, wherein one face of the cells—which is worn against the patient—is adjusted to be relatively flat, while the opposing face is allowed to bulge outwards to contain a high volume of thermal treatment material.
[0062] FIG. 7 depicts one embodiment of joint immobilization within the scope of the present invention.
[0063] FIGS. 8-9 depict an embodiment and configuration having an integrated capacity to apply pressure that is within the scope of the present invention.
[0064] FIG. 10 depicts one embodiment and configuration within the scope of the present invention of a feature that can be installed into the articulated joint treatment system to apply pressure to select areas of the wearer.
DETAILED DESCRIPTION OF THE INVENTION
[0065] Although the following detailed description contains many specifics for the purposes of illustration, anyone of ordinary skill in the art will appreciate that many variations and alterations to the following details are within the scope of the invention. Accordingly, the following preferred embodiments of the invention are set forth without any loss of generality to, and without imposing limitations upon, the claimed invention.
[0066] The invention is a ‘thermal management system’ comprised of one or several wraps, each manufactured to specific predetermined sizes/shapes for given articulated joint therapy applications. For any given case a wrap may be endothermic or exothermic (relative to nominal body temperature) with precise temperature(s) chosen at the time of manufacture to optimize therapeutic outcome. While this ‘thermal management system’ may be comprised of one or more pieces, one preferred embodiment uses from one to six pieces to treat an articulated joint—each installed to provide specific thermal management characteristics to and around the joint. This preferred embodiment includes one or multiple features on each piece/wrap to align or register the pieces to each other, so that when donned, the pieces maintain the best aspect/fit as determined by either the wearer or therapeutic provider. These alignment/registration features form an ‘active hinge’ between the pieces (holding wrap-to-wrap alignment as set when the system is first donned, ensuring that thermal treatment is optimally applied) enabling joint flexure, and may be manifest as a manufactured feature of one or more of the wrap pieces (whether the feature attaches directly or is held in place using various attachments) and/or may optionally consist of carefully designed ‘straps’ to interconnect the wrap pieces in a controlled manner. Such straps may be comprised of any suitable material/dimension that affords proper strength, stiffness, physical robustness, stretchiness (or lack thereof) and capability of being attached to the wrap(s).
[0067] Referring to the drawings now in detail, reference is first made to FIGS. 1-4 , wherein an articulated joint treatment system for knees is shown, generally designated by the numeral 20 .
[0068] One embodiment of the “active knee” system 20 may comprise an upper wrap 21 and a lower wrap 22 that are registered via tang 23 which forms an “active hinge”, which is itself connected to lower wrap 22 via attachment strap 24 . Note the upper wrap 21 has two wings pointing downward, which, when wrapped on the knee, direct thermal therapy to tears of the menisci and/or ligament damage, giving the wearer significant pain relief.
[0069] Each wrap is itself comprised of multiple layers, which may include: flexible, resilient, impact-resistant layers of tri-polymer plastic, TPU, or other urethane or polymer films, or other such materials exhibiting superior physical ‘memory’, strength and workability, formed into either one or a plurality of impact resistant cells/pockets of one or many shapes and thicknesses, themselves designed and specifically placed to balance the characteristics of physical flexibility and fluidity of movement, comfort, volumetric capacity, force impact protection performance, anti-microbial performance, durability and cleanability; cooling or warming material; and (optionally) other layers such as Veltex® display loop or other hook and loop attaching system and/or materials, enabling the use of various anchor attachment straps or other mechanical mounting and holding provisions.
[0070] Straps 24 and 25 (or like equivalent structures) are suitable for use in conjunction with attachment materials (such as the open loop configuration already described), such straps being comprised of stretchable and/or non-stretchable materials in sizes/shapes to enable proper fit and tension adjustment and to best enable comfort for the wearer.
[0071] FIG. 3 depicts lower wrap 22 being “turned out” to show the inside surface, which (in this embodiment) is formed into hygienic thermal containment cells 26 . FIG. 4 shows the active knee system 20 installed on a knee.
[0072] Reference is made to FIG. 5 , which depicts additional wrap embodiments of the present invention that can be used in conjunction with articulated joint treatment systems 20 of the present invention. Such embodiments, as depicted at 50 and 51 , are typically placed to treat specific muscles or tendons that may not be fully covered by a given joint wrap treatment system. Embodiments 50 and 51 are comprised of multiple material layers and include thermal material containment cells as described above herein, but also include mounting straps 52 terminated in tie down (or “D”) rings 53 which allow the straps 52 to be used on limbs of different sizes. Straps 52 are bonded to containment cells 26 via thermal sealing, RF sealing or other means to create a high-strength, low profile connection points that will not irritate the wearer's skin. Critical placement of these wraps (relative to other wraps pieces of an articulated joint treatment system) is accomplished by using a short (generally inflexible) strap such as that depicted as attachment strap 24 above to specifically register embodiments 50 or 51 or the like relative to other wraps.
[0073] FIG. 6 depicts a cutaway view of contiguous thermal containment cells 26 , herein shaped as hexagons of equal size. By controlling the bonding tension between the conjoined upper layer of display loop (or other material) and the layers of high modulus plastic, it is possible to force the containment cell face opposite the display loop into a relatively flat aspect—which is placed against the wearer's skin—while the layer conjoined with display loop bulges outwards to contain relatively high volumes of thermal PCM material. This feature is critical to enhancing wearer comfort, as containment cells are normally fully symmetric and can, when tightly filled, create uncomfortable “bulges” against the wearer when the PCM is charged. Relatively greater cell containment capacity translates to greater thermal treatment durations. Surrounding individual cells with thin peripheral transition spaces enables wrap flexibility so the wrap can conform to the wearer's limb/joint and will not hinder joint flexure.
[0074] Reference is made to FIG. 7 , wherein another embodiment of the invention adds one or more mechanical limiting structures such as rigid features to the articulated joint treatment system 20 (in this case, to either side of the knee) to temporarily hold the articulated joint in a specific aspect/position. In this example, rigid feature 39 is inserted into and held in alignment by one or more retaining structures such as pockets 27 which may be a part of upper wrap 21 and lower wrap 22 . A series of such pockets 27 (or slits) may be built into wraps 21 and 22 to facilitate specific rigid feature 39 positioning, and/or rigid feature 39 may include an adjustable center pivot 28 that may be set by the treatment professional. Additional straps, such as attachment strap 24 , can be used to further stabilize rigid feature 39 . One or more retaining structures such as pockets 27 are preferably stitched to their respective wrap, but the scope of the present invention includes one or more retaining structures including but not limited to stitching, hook and loop fasteners, rivets, slits, and the like.
[0075] One material particularly well suited as the rigid feature 39 of this application is polyethylene terephthalate (also known commercially as PET, PETE or PET-P), a thermoplastic polymer that can be formed into nearly any shape. Another well-suited material is Delrin®, a DuPont thermoplastic polymer. In a preferred embodiment, such a material is formed into a rod/shape whose dimensions make it possible to firmly ‘capture’ or hold this feature by two of the permanent pocket 27 , slits, or other end attachment means. In yet another preferred embodiment, Velcro® or another display hook and loop compatible material is permanently affixed to the rod/shape (which may be held between or in the pockets 27 ), so when it touches the one or more articulated joint treatment wraps 21 and 22 (e.g. between the pockets) it provides further attachment strength, and providing a firm fixed position. By optionally using rods/shapes of different length in conjunction with different fixation elements on the wraps (including the use of threading on the rod and adjustment via secondary structures which are held in place on the treatment structure) the immobilized position/angle of the joint can be modified.
[0076] Reference is made to FIGS. 8-9 , wherein yet another embodiment of a system 30 of the invention incorporates the ability to apply pressure to select portions of the wearer's limb. Lower wrap 32 is similar to lower wrap 22 except it incorporates sealed pressure bladders/cells 37 at either end of the wrap (positioning is representative and not restrictive). In FIG. 8 a complete pressure bladder 37 is shown in full aspect, consisting of a sealed cell with a valve 38 . In this embodiment, when system 30 is donned, the wings of upper wrap 31 and the containment cells 36 are preferably placed directly against the body and lower wrap 32 is placed over these wings (being registered by the active hinge formed by tang 33 [not shown but same as tang 23 in FIG. 2 ] and attachment strap 34 ) and is held in place by strap 35 (such as with strap 25 shown in FIGS. 1 and 4 ). Valves 38 are used to inflate pressure cells 37 which develop pressure against the body. Individual pressure cells 37 can be pressurized with either liquid or gas and can be independently inflated (to different chosen pressures). The invention allows for incorporation of one or a plurality of pressure cells/bladders 37 that are used to apply pressure in a precise manner. Pressure cells 37 can be permanently integrated into a wrap's construction or may be temporarily accommodated by the articulated joint treatment system.
[0077] Reference is made to FIG. 10 , depicting a single air pressure bladder 40 , an embodiment of the present invention, with application for temporary inclusion in the articulated joint treatment system. Bladder 40 is comprised of the same high modulus materials used in constructing bladder(s) 37 and uses the same/equivalent valves 41 as those depicted in FIGS. 8-9 at valve 38 . In a preferred embodiment, inclusion of sealed features 42 (flattened sections, which are exemplary but not restrictive of such shaping features) in the plastic layers provide specific shape to the bladder when pressurized. Such sealing features 42 are used both to reinforce bladder strength (note features around valve 41 , for instance) and to precisely shape where/how pressure is applied to the wearer.
[0078] In one embodiment, provisions for temporarily including such a pressure bladder 40 into the articulated joint treatment system are made by inserting the bladder(s) 40 into bladder pocket(s) on the wrap's outer cloth or display loop layer (the bladder pocket is preferably stitched to this layer wrap, but the scope of the present invention includes all fixation means known within the art including but not limited to stitching, hook and loop fasteners, rivets, and the like) or by placing this bladder 40 between or under wrap surfaces (giving the treatment professional an opportunity to apply both pressure and thermal treatment in a precise way). Such a structure is capable of holding substantial—and sustained—pressure, with the pressure level and placement chosen by the treatment professional.
[0079] In a preferred embodiment, pressure valves 38 or 41 are incorporated into air pressure bladders 37 or 40 so they can be sealed to one of the high modulus layers comprising the wraps/bladders. A preferred embodiment uses a polyurethane “Schrader-like” or “Presta-like” valve featuring a flattened base held between layers of the high modulus urethane plastic. In this embodiment, a layer of TPU is permanently bonded to the valve base via RF welding, creating a reliable leak-free bond. In a preferred embodiment, the Schrader-like valve can be inflated or deflated via a handheld squeezable pressure bulb, facilitating easy adjustment of the pressure level.
[0080] In a preferred embodiment of the invention, the cooling or warming material is an alcohol based gel mixture directly confronting or encapsulating an electronic cooling or warming module, such as a miniature Peltier module, which holds the gel at a constant temperature. In another preferred embodiment, the cooling or warming material is a PCM incorporating a single phase transition point. In yet another embodiment, with appropriate design or formulation, the cooling or warming material is a PCM offering two to ten specifically chosen stable temperature transition points, and in yet another embodiment a single transition temperature which cannot be achieved by commonly available PCMs. In this way an articulated joint treatment system can create a specific microclimate phasing which, itself, depends on both ambient and wearer conditions. In still another preferred embodiment, the system's one or more wraps are comprised of a specifically chosen PCM or system of PCMs (with one or more stable temperature phase points) contained in a plurality of cells, said cells being confronted by a contained layer of gel which is worn directly against the body. In this way the gel can achieve the exact microclimate temperature(s) of the PCM(s), while providing a soft interfacing layer to the wearer. Preferably the cell-contained PCM is formulated or selected to yield phase transition points to within ±1° F. to ±10° F. of a targeted transition temperature. Other properties of specific PCMs that will enhance utility in an articulated joint treatment system featured in other embodiments include: (1) the capacity to undergo any number of thermal cycles without notable degradation, (2) the capacity to provide a relatively constant temperature microclimate for a long duration, (3) the chemical property of not being harmful or caustic to skin or organs and (4) third-party registration of such safety [such as an FDA 510(k)] and (5) dielectric properties that render the PCM non-conducting (enhancing user safety if the invention is used around electronics or electrical equipment). One such family of PCMs is HTFEXOTHERM® manufactured by HTFx Inc.
[0081] When using a somewhat or relatively viscous PCM such as HTFEXOTHERM®, whether in the somewhat hardened charged state or even in the fully discharged liquid state, the PCM material contributes directly to the wrap's ability to dissipate or dampen incident force impact energy, helping to protect the wearer from incident blunt force trauma. In preferred embodiments, these protective characteristics are dramatically amplified by containing the PCM in one or a plurality of cells that are built from physically malleable materials such as tri-polymer films or in a plurality of such cells designed to release or transfer PCM fluid from cell to cell when one or more cells experiences the high hydroscopic pressure caused by a force impact. This quality can be obtained by varying cell shape, size and placement, and by selecting one or more material sealing technologies—such as thermal impulse sealing and RF sealing—and by including one or a plurality of channels of one or many widths between cells (whether these channels are always open or some are forced open only by a high impact force) to adjust the strength and reactivity of the cell walls. This approach can be used quite effectively to create a system of small scale “baffles” from cell to cell, making it possible to disburse and dampen force impact shock waves across a plurality of cells and to create a system responsive to both high and low speed force impacts. Such baffling can be crafted to keep the articulated joint treatment system from applying greater than therapeutic levels of pressure to a wearer if the system is misused or improperly installed. These macroscopic qualities are maintained even when an incident blow has enough force to damage one or more cells. Absent a force impact, the PCM will remain relatively static in the plurality of cells. While such incident impact forces are unlikely in most articulated joint therapeutic settings, this design feature will protect the wearer who exercises using external equipment or suffers an unintended accident. Such baffling will also facilitate use of thermal management structures in association with joint immobilization or “air casts” by reducing the likelihood that a multi-cell structure will impose overly high, localized pressures.
[0082] Different embodiments will use different combinations of film material and number of layers, shape (including the use of one or many different wrap shapes simultaneously), size (including the use of one or many sizes simultaneously), placement of cells, size and shape of cells (including an intermixing of suitable and different cell sealing technologies to form effective systems of force dispersal, pressure applying, thermal treatment and dampening which can be incorporated into the articulating joint treatment system).
[0083] For instance, in a preferred embodiment, the plurality of impact resistant cells/pockets of one or many shapes and thicknesses are formed into hexagons, each hexagonal cell containing PCM material, such as containment cells 26 and 36 depicted in FIGS. 1-6 and FIGS. 8-9 , respectively. In yet another preferred embodiment these hexagonal containment cells allow liquid or semi-liquid PCM to flow between cells when subjected to a given amount of pressure or flexing of the wrap. The hexagonal shape is particularly effective at balancing flexibility and fluidity of motion (necessary for comfort) with PCM capacity—enabling wraps that are capable of comfortably cooling/warming the affected joint for an extended duration.
[0084] Regarding the protective or microclimate utility or overall performance of the articulated joint treatment system, it is possible to either loosely or tightly couple each cooling or heating wrap around the wearer's articulated joint with specific fit/placement and tension adjusted for each wearer and to separately align multiple wraps with respect to each other in a preferred relation/fit using the one or many active hinge feature(s) formed by tang 23 and attachment strap 24 or tang 33 and attachment strap 34 , respectively. This is particularly important when the wearer is participating in an ‘active’ exercise, range of motion or joint flexure regimen, to minimize the tendency of the one or more wraps to bunch up or move elsewhere on the wearer's limb (when referenced to the affected joint)—and to continue to deliver optimum thermal performance even during exercise.
[0085] In yet another variation of the immobilizing articulated joint treatment system, a device resembling any kind of air cast can be differently constructed to provide thermal treatment benefits by having one or more of its air bladders replaced by one or more thermal or thermal/pressure-applying wraps of suitable size and shape, the wraps being comprised of one or a plurality of cooling/heating cells containing suitable PCM material, or a combination of one or a plurality of thermal/pressure-applying cells such that the cast provides joint immobilization while the one or more wraps provides directed heating/cooling and/or pressure.
[0086] A number of embodiments of articulated joint treatment devices are detailed within this document, which also contains images of certain embodiments that have been reduced to practice. Other objects of the present invention will become apparent to those skilled in this art, including variations applicable to all other articulated body joints. As it will be realized, the invention is capable of other different embodiments and its several details are capable of modification in various, obvious aspects all without departing from the invention. The principles and concepts disclosed herein may easily and readily be applied to systems covering other joint and/or non-joint body surfaces and all such embodiment are within the scope of the present invention. Accordingly, all drawings, descriptions, embodiments, and specifically depicted examples will be regarded as only illustrative in nature and not as restrictive.
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A treatment for articulated joint injuries and maladies, whether pre- or post-operative or degenerative in nature, and more specifically to systems and/or devices that facilitate joint recovery by applying constant microclimate cooling/heating and optional pressure to an affected joint in a secure, comfortable and reliable manner, even during repeated joint flexure or movement.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. application Ser. No. 12/031,939, filed on 15 Feb. 2008 and entitled “Method for Producing an HTSC Strip,” which claims priority under 35 U.S.C. §119 to Application No. DE 102007007567.9, filed on 15 Feb. 2007 and entitled “Method for Producing an HTSC Strip.” The disclosures of each of the above applications are hereby incorporated by reference in their entireties.
FIELD OF THE INVENTION
[0002] The invention relates to a method for producing a high temperature superconductor (HTSC) from a strip which has an upper side precursor layer, wherein the strip is drawn across a support for continuous sintering of the strip within a furnace in the presence of a fed-in reaction gas.
BACKGROUND OF THE INVENTION
[0003] In a conventional process for preparing a multi-layer superconductor article, a reactor (e.g., a tube furnace) includes a housing having an upper wall with passages (e.g., slots or nozzles) that are in fluid communication with gas mixture sources (e.g., oxygen, water, and one or more inert gases (e.g., nitrogen, argon, helium, krypton, xenon). A substrate, which is wound around reels, moves through reactor in a predetermined direction.
[0004] As a substrate enters the reactor, it passes through a various regions within the reactor, during which time the gas mixture is directed downward, toward substrate. A film containing a precursor (e.g., a superconductor precursor film containing barium fluoride and/or additional materials, such as CuO and/or Y 2 O 3 ) is present on the surface of substrate, moving through the regions of the reactor. The precursor is exposed to the gas mixture, reacting therewith. Spent reaction gas is drawn-off by a pump that directs the spent gas through a through a porous material positioned adjacent the passages (the slots or nozzles) in the upper wall.
[0005] In the conventional system using the above process, fresh and used reaction gases are mixed without control. This, in turn, leads to impairment of quality of the HTSC layer and/or long retention times of the strip in the furnace. Thus, it would be desirable to develop an HTSC formation method that controlled to level of mixing between the fresh and used reaction gases.
OBJECTS AND SUMMARY OF THE INVENTION
[0006] One object of the invention is to provide a method of forming a strip-shaped HTSC of constant high quality. Another object of the invention is to provide a reactor/furnace for performing a method of this kind. The above and still further objects, features, and advantages of the present invention will become apparent upon consideration of the following descriptions and descriptive figures of specific embodiments thereof, wherein like reference numerals in the various figures are utilized to designate like components. While these descriptions go into specific details of the invention, it should be understood that variations may and do exist and would be apparent to those skilled in the art based on the descriptions herein.
[0007] In accordance with the invention, a strip having a precursor layer is drawn across a porous support through which fresh reaction gas is continuously fed. The continuous feeding forms a laminar flow of the fresh reaction gas above the porous support and along the sides of the strip. A vortex zone forms above the strip in the flow shadow of the strip. In the boundary region between the vortex zone and the regions of laminar flow adjacent/lateral to the vortex zone, a continuous exchange of gas takes place between the vortex zone and the laminar flow. As a result, the vortex zone is always sufficiently enriched with fresh reaction gas. In this manner, the vortices ensure good mixing of fresh and used reaction gas. Thus, provision is made for the precursor layer to be uniformly and sufficiently subjected to a flow of reaction gas during the sintering.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 illustrates a cross sectional view of a furnace in accordance with an embodiment of the invention.
[0009] FIG. 2 illustrates the fluid flow pattern within the furnace of FIG. 1 , showing the substrate support oriented in a lowered position.
[0010] FIG. 3 illustrates the fluid flow pattern within the furnace of FIG. 1 , showing the substrate support oriented in a mid-height position.
[0011] FIG. 4 illustrates the fluid flow pattern within the furnace of FIG. 1 , showing the substrate support oriented in a raised position.
DETAILED DESCRIPTION OF THE INVENTION
[0012] FIG. 1 is a cross-sectional view of a system in accordance with an embodiment of the invention. As illustrated, the system includes a furnace 1 with a furnace space defined by a furnace inner wall 1 . 1 . Within the furnace space is a porous support 2 such as a porous plate. The support 2 is adapted to be raised and lowered within the furnace space. Both of the side/outer edges of the support 2 are generally flush with the furnace inner wall 1 . 1 . A substrate or strip 3 having on its upper side a precursor layer may be positioned onto the support 2 . For example, the strip 3 may be drawn across the support 2 orthogonally to the cross-section plane (e.g., it may be drawn from left to right across the support from the perspective of FIG. 1 ). The furnace 1 further includes at least one exhaust opening 4 formed in the furnace inner wall 1 . 1 . The exhaust opening may be centrally located above the strip 1 . The exhaust opening 4 is in fluid communication with the furnace space, and, as such, is configured to remove reaction gas from the furnace space.
[0013] Referring to FIGS. 2-4 , in operation, reaction gas is fed into the furnace 1 at a point below the support 2 . The air travels toward the lower surface of the support 2 , passing through its pores and around the strip 3 with an HTSC precursor layer disposed on the upper surface of the support. This feeding creates a substantially laminar flow 6 towards the exhaust opening 4 , above the support 2 and proximate the sides of the strip 3 . A vortex zone 5 of an approximately onion-shaped cross-section is formed above the strip 3 within its flow shadow.
[0014] Thus, the continuous feeding of fresh reaction gas forms a laminar flow 6 above the porous support and along the sides of the strip 3 . The vortex zone 5 forms above the strip 3 in the flow shadow of the strip. In the boundary region between the vortex zone 5 and the regions of laminar flow 6 adjacent/lateral to the vortex zone, a continuous exchange of gas takes place between the vortex zone and the laminar flow. As a result, the vortex zone 5 is always sufficiently enriched with fresh reaction gas. In this manner, the vortices ensure good mixing of fresh and used reaction gas.
[0015] The support 2 may further be adapted to raise and lower to predetermined positions within the furnace space. As best seen in FIGS. 2-4 , the support 2 may begin in a first position ( FIG. 2 ) and be raised to a second position ( FIG. 3 ) and/or a third position ( FIG. 4 ). Conversely, the support 2 may be lowered from the third position to either the first or second positions. In this manner, the distance between the strip 3 and the exhaust opening 4 can be varied by raising and lowering the support 2 . The height at which the support may be positioned is not particularly limited.
[0016] With a constant volume flow of the reaction gas, the size and shape of the vortex zone 5 (and thus the flow velocity in the vicinity of the precursor layer and the degree of gas exchange between the vortex zone and the region of laminar flow 6 ) can be adjusted.
[0017] Since part of the reaction gas fed into the porous support 2 does not partake in an exchange with the vortex zone 5 , it is preferred to conduct the reaction gas in a circuit, feeding it into the support several times (e.g., the gas may be intermittently fed into the furnace and through the support). Used reaction gas is removed from the circuit and replaced by fresh reaction gas.
[0018] Before being fed into the support 2 , the reaction gas may be heated to a predetermined temperature, e.g., to at least to about the sintering temperature. By way example, when the gas has a temperature slightly above the sintering temperature, the gas will heat the strip 3 to the sintering temperature.
[0019] Similarly, at least a portion of the support 2 may be heated to a predetermined temperature. By way of example, the region of the support 2 facing the entry side of the strip 3 into the furnace 1 may be heated. Heating the support 2 serves to heat the strip 3 rapidly to the sintering temperature.
[0020] A plurality of strips 3 may be drawn through the furnace in parallel and preferably spaced from each other. The spacing between the strips 3 preferably should be dimensioned so that a vortex zone 5 is formed above each strip. In this way, a plurality of strips 3 may be sintered simultaneously, with each strip being sufficiently and uniformly subjected to a flow of reaction gas.
[0021] Friction between the support 2 and the strip 3 may be reduced by directing gas of sufficient pressure between the support and the strip. In other words, the volume flow or the pressure of the gas fed into the support 2 can be adjusted so that reaction gas also emerges between the strip 3 and the support 2 , thereby reducing the friction occurring between the support 2 and the strip 3 . The strip 3 can then be drawn across the support 2 more easily, and less abraded matter is formed. This helps to inhibit blockage of the pores of the support, since fine abraded matter would be fed together with the circulating gas into the support 2 and block the pores thereof, at least after some time.
[0022] Preferably, the furnace 1 has at least one suction or vacuum means disposed above the support 2 for conducting-away reaction gas. The suction means, e.g., an exhaust mechanism, may extend parallel to the direction of drawing-through the strip 3 . It is particularly preferred to draw-off the reaction gas above the strip or strips 3 . This causes the cross-section of the vortex zone to become generally onion-shaped. The size of the vortex zone 5 , the flow conditions within the vortex zone, and the gas exchange between the vortex zone and the laminar flow can be adjusted by the position and the shape of the exhaust openings 4 .
[0023] With exhaust openings 4 disposed to be parallel to the direction of drawing-through, an average concentration of fresh reaction gas that is substantially constant along the direction of drawing-through is obtained in the vortex zone 5 .
[0024] The flow of the reaction gas may be controlled particularly well when the exhaust openings 4 are slits that extend parallel to the direction of drawing-through, and/or when each strip drawn through the furnace is provided with its own row of exhaust openings disposed in parallel with the direction of drawing-through.
[0025] Thus, to perform the above-described method, a sintering furnace 1 is suitable that comprises a porous support 2 as a rest for a strip with an HTSC precursor layer, and at least one inlet and at least one outlet for a reaction gas. The support 2 communicates with the inlet for the reaction gas. Consequently, the reaction gas flows into the support 2 and/or around the sides of the support, ultimately flowing around the strip 3 as described above.
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The invention relates to a method for producing a high temperature superconductor (HTSC) from a strip including an upper side precursor layer and which, for continuous sintering of the precursor layer within a furnace in the presence of a fed-in reaction gas, is drawn across a support. A furnace for performing the method is also described.
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FIELD OF THE INVENTION
[0001] The present invention relates to the field of image processing. More specifically, the present invention relates to autofocus.
BACKGROUND OF THE INVENTION
[0002] An autofocus optical system uses a sensor, a control system and a motor to focus fully automatic or on a manually selected point or area. An electronic rangefinder has a display instead of the motor, and the adjustment of the optical system has to be done manually until indication. The methods are named depending on the sensor used such as active, passive and hybrid. Many types of autofocus implementations exist.
SUMMARY OF THE INVENTION
[0003] A hierarchical method of achieving auto focus using depth from defocus is described herein. The depth from defocus technique is performed hierarchically in the resolution that is determined to be optimal at each step. Where higher resolution gives the better accuracy but requires more computational costs, the optimal resolution is estimated based on the target accuracy and the possible max blur amount at each step, which determines the amount of the computation and the number of pixels in the focus area. The proposed multi-resolution depth-from-defocus-based autofocus enables the reduction in the required resource, which is beneficial in the system where resource is limited.
[0004] In one aspect, a method of autofocusing programmed in a memory of a device comprises determining an optimal resolution based on estimating a maximum iteration number and a blur size fitting matching area, performing depth from defocus for the optimal resolution and repeating depth from defocus until autofocus at the optimal resolution is achieved. The method further comprises acquiring content. The content comprises a first image and a second image. The first image is acquired at a first lens position and the second image is acquired at a second lens position. The method further comprises implementing hierarchical motion estimation targeting the optimal resolution. The method further comprises determining if the content is in focus, if the content is in focus, then the method ends and if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result. The method further comprises determining a new optimal resolution. The method further comprises determining if the new optimal resolution equals the previous optimal resolution, if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content and if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus. The optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution. The device is selected from the group consisting of a personal computer, a laptop computer, a computer workstation, a server, a mainframe computer, a handheld computer, a personal digital assistant, a cellular/mobile telephone, a smart appliance, a gaming console, a digital camera, a digital camcorder, a camera phone, a smart phone, a portable music player, a tablet computer, a mobile device, a video player, a video disc writer/player, a television, and a home entertainment system.
[0005] In another aspect, a method of autofocusing programmed in a memory of a device comprises acquiring content, determining a blur size and a maximum iteration number based on a current lens position, determining an optimal resolution, implementing hierarchical motion estimation targeting the optimal resolution, implementing depth from defocus in the optimal resolution and determining if the content is in focus. The content comprises a first image and a second image. The first image is acquired at a first lens position and the second image is acquired at a second lens position. The method further comprises if the content is in focus, then the method ends and if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result. The method further comprises determining a new optimal resolution. The method further comprises determining if the new optimal resolution equals the previous optimal resolution, if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content and if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus. The optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution. The device is selected from the group consisting of a personal computer, a laptop computer, a computer workstation, a server, a mainframe computer, a handheld computer, a personal digital assistant, a cellular/mobile telephone, a smart appliance, a gaming console, a digital camera, a digital camcorder, a camera phone, a smart phone, a portable music player, a tablet computer, a mobile device, a video player, a video disc writer/player, a television, and a home entertainment system.
[0006] In another aspect, an apparatus comprises an image acquisition component for acquiring a plurality of images, a memory for storing an application, the application for: determining a blur size and a maximum iteration number based on a current lens position, determining an optimal resolution, implementing hierarchical motion estimation targeting the optimal resolution, implementing depth from defocus in the optimal resolution and determining if an image of the plurality of images is in focus and a processing component coupled to the memory, the processing component configured for processing the application. A first image of the plurality of images is acquired at a first lens position and the second image of the plurality of images is acquired at a second lens position. The application further comprises if the content is in focus, then the method ends and if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result. The application further comprises determining a new optimal resolution. The application further comprises determining if the new optimal resolution equals the previous optimal resolution, if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content and if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus. The optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 illustrates an example of a step edge when the blur size is zero.
[0008] FIG. 2 illustrates an example of a blurred step edge.
[0009] FIG. 3 illustrates an example of a picture matching process according to some embodiments.
[0010] FIG. 4 shows the matching curves generated for the step edge for different displacement of the matching area in horizontal direction according to some embodiments.
[0011] FIG. 5 shows a subset of FIG. 4 , where the matching area has the step edge within the matching area when the image is in focus according to some embodiments.
[0012] FIG. 6 shows a higher resolution-based DFD result is able to be better than a lower resolution-based DFD according to some embodiments.
[0013] FIG. 7 shows an example of relationships among the blur size, iteration curve, affordable matching area (width and height), and number of Depth of Fields (DOFs) from the focus position for different resolutions according to some embodiments.
[0014] FIG. 8 illustrates a flowchart of a method of multi-resolution depth-from-defocus-based autofocus according to some embodiments.
[0015] FIG. 9 illustrates a block diagram of an exemplary computing device configured to implement the autofocus method according to some embodiments.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0016] Certain terminology is used throughout the application which is described herein. Blur size is the total number of pixels in one direction (horizontal or vertical) that are altered due to Point Spread Function (PSF) of the optics. Iteration number is the number of the process P A used for the convergence, which represents the amount of blur difference between the two images. Matching area is the area that is used for process E. Matching curve is a plot of the iteration number in vertical axis with depth position in the horizontal axis. Iteration curve is the same as the matching curve. Depth-From-Defocus (DFD) is the process to estimate the depth based on a procedures such as the one shown in FIG. 3 . Depth Of Field is DOF.
[0017] High accuracy in depth-from-defocus-based (DFD-based) autofocus results are able to be achieved under typical embedded system restrictions such as processor and hardware resource limitations. The following characteristics are able to be exploited using the DFD-based autofocus under such resource restrictions by a multi-resolution approach: processing DFD on a higher resolution is able to yield the better result, and containing blur within a matching area for DFD process is able to yield the better result.
[0018] There are some applications that conduct depth-from-defocus-based autofocus. An embedded system such as a personal digital camcorder or digital still camera are such examples.
[0019] In depth from defocus, it is important to know all or a majority of the blur (blurred edge, dot or texture) for the higher accuracy of estimated depth.
[0020] Although the blur-size or PSF size is able to be defined in several ways, it is able to be defined as the total number of pixels in one direction (horizontal or vertical) that are altered due to PSF of the optics.
[0021] To better illustrate, a step edge scene is used as an example. For example, when the image is in focus, the blur size is zero. FIG. 1 illustrates a case when the blur size is zero.
[0022] FIG. 2 illustrates an example of a blur size in a blurred step edge. In FIG. 2 , the blur size is 24.
[0023] Furthermore, the blur-size is usually linearly proportional to the number of depths of field that exist between the object position and the lens focus position.
[0024] Also, the depth of the target object is able to be estimated based on the blur difference in more than one image that is captured with a different defocus level. The blur difference is able to be represented by the number of iterations in a picture matching process such as the process in FIG. 3 .
[0025] Supposing image1 and image2 in FIG. 3 have different amounts of blur from one optic system, and image2 is sharper. The amount of the blur difference between the two images is able to be computed. The P A process is able to be defined as a blur function that models the optic system well, which could be a simple 3×3 convolution kernel. Then, process E is defined to be an error generation function between the two images, which is able to be a simple Sum of Absolute Differences (SAD) function that works on a certain area of two images. By repeating the loop shown in FIG. 3 until the previous error generated by process E becomes smaller than the newly generated error (or current error), the number of this repetition is able to be used to represent the blur difference between the two images. In some embodiments, registration of two images (such as motion compensation) is performed beforehand.
[0026] Having all or a major part of the blur within a matching area or the blur difference estimation between the two images is important in order to have accurate depth estimation. FIG. 4 shows the matching curves generated for the step edge for different displacement of the matching area in horizontal direction. FIG. 5 shows a subset of the FIG. 4 , where the matching area has the step edge within the matching area when the image is in focus. The matching curve becomes very noisy when there is no edge within the matching area.
[0027] The more the edge of the step edge scene deviates from the center of the matching area, the more the iteration curve deviates from the ideal curve. This is mainly because the iteration curve is impacted when the part of the blur edge is out of the matching area.
[0028] Since a higher resolution image contains more information, and the DFD process is able to yield better accuracy when performed at a higher resolution.
[0029] FIG. 6 shows a higher resolution-based DFD result is able to be better than a lower resolution-based DFD. Where a ¼ resolution-based DFD result is able to identify the true focus position of the target object, a ⅛ based resolution is not able to identify the true focus position.
[0030] It is important to contain all or the majority of blur within a matching area in order to obtain accurate depth estimation or blur difference estimation results. Also, the DFD process is implemented in higher resolution in some embodiments. However, often in embedded optic systems such as digital cameras or camcorders, there is a limitation of processing and hardware resources including: accelerator, bandwidth, and memory, which limits the size of matching area and amount of computational intensity. Also, depending on the optical systems, the blur size is able to be very large. FIG. 7 shows an example of relationships among the blur size, iteration curve, affordable matching area (width and height), and number of Depth of Fields (DOFs) from the focus position for different resolutions. Furthermore, performing a motion estimation on a higher resolution is often able to become too expensive in terms of computational cost.
[0031] The affordable matching area size is 60×45 (width, height) pixels in a certain embedded digital camera system, and the blur size and the iteration curve for 3 different resolutions (⅛, ¼, and ½) are as shown in FIG. 7 . Also, the system is only able to afford up to around 64, 16, and 4 iteration numbers for ⅛, ¼, and ½ resolution respectively (assuming that the one iteration in ¼ resolution takes about 4 times more than in ⅛ resolution and one iteration in ½ resolution takes about 4 times more than in ¼ resolution) iteration number for one resolution. In this environment, the objective is to achieve the final autofocus accuracy that is equivalent to that of ½ resolution DFD.
[0032] For example, the camera system has the total range of around 300 DOFs such as shown in FIG. 7 . If autofocus were to start from a nearest lens position that the camera is able to focus, the most extreme case will be the case when the target object is at infinity. In such case, the blur size will be expected to be around 250, 125, and 62.5 for ½, ¼, and ⅛ resolution respectively. At this position, the DFD process at only ⅛ resolution seems feasible because the blur size is too big for matching area (60×45) for ¼ and ½ resolution. However, DFD process in ⅛ resolution will not give us the accuracy equivalent to DFD process in ½ resolution.
[0033] The idea is to use the multi-resolution approach (low to high) to reduce the motion estimation cycle in DFD-based autofocus by starting motion estimation with full search range at the lower resolution (or the highest resolution allowed both in terms of computational and memory cost). DFD-based autofocus is repeated within the “optimal” resolution until autofocus is achieved with the desired accuracy. The information of the blur size or possible max blur size at a given lens position is used in order to determine the “optimal” resolution for performing the DFD process. In some embodiments, the “optimal” resolution is the one that satisfies some or all of the following criteria: the highest resolution where the possible blur size fits in the matching area, the highest resolution where the DFD process with the possible biggest iteration number is affordable in terms of computational cost and to estimate the possible max blur size based on the DFD result at a lower resolution.
[0034] Multi-resolution approach (low to high) in motion estimation, which is often called hierarchical motion estimation, is a technique to utilize. The idea is that if one were to find a motion vector at, for example, ½ resolution for M×N matching area with +−S in both horizontal and vertical direction, if this were done in a straightforward way, error calculation such as SAD calculation for M×N is computed for (S+S+1)̂2 positions. However, simply doing motion vector search in a lower resolution such as ¼ resolution, SAD calculation of M/2×N/2 for (S/2+S/2+1)̂2 positions and the refinement search are performed. The refinement search in this case often includes SAD calculation of M×N area for (1+1+1)̂2 points. Therefore, the multi-resolution technique is able to be used in DFD-based autofocus. The target resolution is able to be the “optimal” resolution determined as described herein, and the lower resolution for this hierarchical motion estimation is able to be determined by the computational cost restriction.
[0035] To determine the “optimal” resolution for DFD process: in order to find out the possible max blur size one is able to think of the extreme scenario and find out the corresponding blur size using a pre-generated data such as the one in shown in the FIG. 7 . For example, if the current lens position is in the near-side half range of the entire focus-able DOF range, the object at infinity will be the extreme case, and if the lens position is in the farther half of the entire focus-able DOF range, the closest object will be the extreme case. Then, depending on the obtained blur size, the resolution is chosen when the affordable matching area is big enough. This approach will guarantee that the matching area size will be big enough if the target object is located at the center of the matching area. One could also think of determining the optimal DFD resolution based on some sort of statistical information as well. How to find out the possible biggest iteration number is very similar to the method described above. The same method is able to be used except that the iteration number is used instead of the blur size based on pre-generated iteration curve such as the one shown in the FIG. 7 . In order to estimate the possible maximum blur size, the iteration number relationships among different resolutions is known or determined. For example, in a DFD process where blur difference between a pair of images is expressed in terms of difference in special variance, the iteration number is proportional to the resolution. For example, iteration A in ⅛ resolution will likely to yield 4 A in ¼ resolution. When estimating a possible max iteration in a higher resolution based on a lower resolution DFD result, adding a room for error (such as 4 A+e in the example) is able to be useful.
[0036] FIG. 8 illustrates a flowchart of a method of multi-resolution depth-from-defocus-based autofocus according to some embodiments. In the step 800 , two images are captured at different lens positions. In the step 802 , the possible maximum blur size and the possible maximum iteration number are determined based on the current lens position and the depth intervals of the two images taken in the step 802 . In the step 804 , an optimal resolution is determined. In the step 806 , motion estimation targeting the optimal resolution is implemented. In some embodiments, the motion estimation in the step 806 is hierarchical motion estimation targeting the optimal resolution. In the step 808 , DFD in optimal resolution is implemented. In the step 810 , it is determined if the image is in focus or out of focus. If the image is in focus, the process ends. If the image is out of focus, the possible maximum blur size and possible maximum iteration number is determined based on the DFD result and the depth intervals of the two images taken in the step 802 , in the step 812 . In the step 814 , the optimal resolution is determined. In the step 816 , it is determined if the new optimal resolution equals the previous optimal resolution. If the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth in the step 818 , and the process returns to the step 800 . If the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented in the step 820 , and the process returns to the step 808 . In some embodiments, the order of the steps is modified. In some embodiments, more or fewer steps are implemented.
[0037] FIG. 9 illustrates a block diagram of an exemplary computing device 900 configured to implement the autofocus method according to some embodiments. The computing device 900 is able to be used to acquire, store, compute, process, communicate and/or display information such as images and videos. In general, a hardware structure suitable for implementing the computing device 900 includes a network interface 902 , a memory 904 , a processor 906 , I/O device(s) 908 , a bus 910 and a storage device 912 . The choice of processor is not critical as long as a suitable processor with sufficient speed is chosen. The memory 904 is able to be any conventional computer memory known in the art. The storage device 912 is able to include a hard drive, CDROM, CDRW, DVD, DVDRW, flash memory card or any other storage device. The computing device 900 is able to include one or more network interfaces 902 . An example of a network interface includes a network card connected to an Ethernet or other type of LAN. The I/O device(s) 908 are able to include one or more of the following: keyboard, mouse, monitor, display, printer, modem, touchscreen, button interface and other devices. Autofocus application(s) 930 used to perform the autofocus method are likely to be stored in the storage device 912 and memory 904 and processed as applications are typically processed. More or less components shown in FIG. 9 are able to be included in the computing device 900 . In some embodiments, autofocus hardware 920 is included. Although the computing device 900 in FIG. 9 includes applications 930 and hardware 920 for the autofocus, the autofocus method is able to be implemented on a computing device in hardware, firmware, software or any combination thereof. For example, in some embodiments, the autofocus applications 930 are programmed in a memory and executed using a processor. In another example, in some embodiments, the autofocus hardware 920 is programmed hardware logic including gates specifically designed to implement the autofocus method.
[0038] In some embodiments, the autofocus application(s) 930 include several applications and/or modules. In some embodiments, modules include one or more sub-modules as well. In some embodiments, fewer or additional modules are able to be included.
[0039] Examples of suitable computing devices include a personal computer, a laptop computer, a computer workstation, a server, a mainframe computer, a handheld computer, a personal digital assistant, a cellular/mobile telephone, a smart appliance, a gaming console, a digital camera, a digital camcorder, a camera phone, a smart phone, a portable music player, a tablet computer, a mobile device, a video player, a video disc writer/player (e.g., DVD writer/player, Blu-ray® writer/player), a television, a home entertainment system or any other suitable computing device.
[0040] To utilize the multi-resolution depth-from-defocus-based autofocus method, a user acquires a video/image such as on a digital camcorder, and before or while the content is acquired, the autofocus method automatically focuses on the data. The autofocus method occurs automatically without user involvement.
[0041] In operation, the multi-resolution depth-from-defocus-based autofocus enables achieving a DFD-based autofocus accuracy of a desired resolution at lower computational cost. Additionally, the multi-resolution depth-from-defocus-based autofocus overcomes the real world restriction of the size limit for the matching area that can be implemented in a system (given a certain restriction on the number of pixels in a matching area, working in the lower resolution enables capturing a bigger blur size than in a higher resolution).
Some Embodiments of Multi-Resolution Depth-from-Defocus-Based Autofocus
[0000]
1. A method of autofocusing programmed in a memory of a device comprising:
a. determining an optimal resolution based on estimating a maximum iteration number and a blur size fitting matching area; b. performing depth from defocus for the optimal resolution; and c. repeating depth from defocus until autofocus at the optimal resolution is achieved.
2. The method of clause 1 further comprising acquiring content.
3. The method of clause 2 wherein the content comprises a first image and a second image.
4. The method of clause 3 wherein the first image is acquired at a first lens position and the second image is acquired at a second lens position.
5. The method of clause 1 further comprising implementing hierarchical motion estimation targeting the optimal resolution.
6. The method of clause 2 further comprising:
a. determining if the content is in focus; b. if the content is in focus, then the method ends; and c. if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result.
7. The method of clause 6 further comprising determining a new optimal resolution.
8. The method of clause 7 further comprising:
a. determining if the new optimal resolution equals the previous optimal resolution; b. if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content; and c. if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus.
9. The method of clause 1 wherein the optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution.
10. The method of clause 1 wherein the device is selected from the group consisting of a personal computer, a laptop computer, a computer workstation, a server, a mainframe computer, a handheld computer, a personal digital assistant, a cellular/mobile telephone, a smart appliance, a gaming console, a digital camera, a digital camcorder, a camera phone, a smart phone, a portable music player, a tablet computer, a mobile device, a video player, a video disc writer/player, a television, and a home entertainment system.
11. A method of autofocusing programmed in a memory of a device comprising:
a. acquiring content; b. determining a blur size and a maximum iteration number based on a current lens position; c. determining an optimal resolution; d. implementing hierarchical motion estimation targeting the optimal resolution; e. implementing depth from defocus in the optimal resolution; and f. determining if the content is in focus.
12. The method of clause 11 wherein the content comprises a first image and a second image.
13. The method of clause 12 wherein the first image is acquired at a first lens position and the second image is acquired at a second lens position.
14. The method of clause 11 further comprising:
a. if the content is in focus, then the method ends; and b. if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result.
15. The method of clause 14 further comprising determining a new optimal resolution.
16. The method of clause 15 further comprising:
a. determining if the new optimal resolution equals the previous optimal resolution; b. if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content; and c. if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus.
17. The method of clause 11 wherein the optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution.
18. The method of clause 11 wherein the device is selected from the group consisting of a personal computer, a laptop computer, a computer workstation, a server, a mainframe computer, a handheld computer, a personal digital assistant, a cellular/mobile telephone, a smart appliance, a gaming console, a digital camera, a digital camcorder, a camera phone, a smart phone, a portable music player, a tablet computer, a mobile device, a video player, a video disc writer/player, a television, and a home entertainment system.
19. An apparatus comprising:
a. an image acquisition component for acquiring a plurality of images; b. a memory for storing an application, the application for:
i. determining a blur size and a maximum iteration number based on a current lens position; ii. determining an optimal resolution; iii. implementing hierarchical motion estimation targeting the optimal resolution; iv. implementing depth from defocus in the optimal resolution; and v. determining if an image of the plurality of images is in focus; and
c. a processing component coupled to the memory, the processing component configured for processing the application.
20. The apparatus of clause 19 wherein a first image of the plurality of images is acquired at a first lens position and the second image of the plurality of images is acquired at a second lens position.
21. The apparatus of clause 19 wherein the application further comprises:
a. if the content is in focus, then the method ends; and b. if the content is out of focus, then the blur size and the possible maximum iteration number is determined based on the depth from defocus result.
22. The apparatus of clause 21 wherein the application further comprises determining a new optimal resolution.
23. The apparatus of clause 22 wherein the application further comprises:
a. determining if the new optimal resolution equals the previous optimal resolution; b. if the new optimal resolution equals the previous optimal resolution, the lens is moved to the estimated depth and the method returns to acquiring content; and c. if the new optimal resolution does not equal the previous optimal resolution, the refinement motion estimation is implemented and the method returns to implementing depth from defocus.
24. The apparatus of clause 19 wherein the optimal resolution comprises some or all of the following criteria: a highest resolution where a possible blur size fits in a matching area, the highest resolution where a depth from defocus process with a possible biggest iteration number is affordable in terms of computational cost and to estimate the possible maximum blur size based on the depth from defocus result at lower resolution.
[0099] The present invention has been described in terms of specific embodiments incorporating details to facilitate the understanding of principles of construction and operation of the invention. Such reference herein to specific embodiments and details thereof is not intended to limit the scope of the claims appended hereto. It will be readily apparent to one skilled in the art that other various modifications may be made in the embodiment chosen for illustration without departing from the spirit and scope of the invention as defined by the claims.
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A hierarchical method of achieving auto focus using depth from defocus is described herein. The depth from defocus technique is performed hierarchically in the resolution that is determined to be optimal at each step. Where higher resolution gives the better accuracy but requires more computational costs, the optimal resolution is estimated based on the target accuracy and the possible max blur amount at each step, which determines the amount of the computation and the number of pixels in the focus area. The proposed multi-resolution depth-from-defocus-based autofocus enables the reduction in the required resource, which is beneficial in the system where resource is limited.
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PRIORITY
[0001] This application claims foreign priority of the German application DE 10260242.5 filed on Dec. 20, 2002.
TECHNICAL FIELD OF THE INVENTION
[0002] The invention relates to circuit modules for motor vehicles, having a housing accommodating a motor vehicle circuit and having a contact wire brought out of said housing, said contact wire being connected to said motor vehicle circuit.
[0003] The invention further relates to an arrangement for contacting the contact wire.
BACKGROUND OF THE INVENTION
[0004] A circuit module of this kind is known from DE 199 07 949 A1. The known circuit module is a motor vehicle control unit comprising a metal base plate on which a ceramic carrier is disposed. On the base plate there is additionally a flexible circuit board surrounding the ceramic carrier on all sides. The flexible circuit board is wire-bonded to the electronic circuit disposed on the ceramic carrier. On the circuit board there is disposed a sealing ring running round the carrier and surmounted by a housing lid covering the circuit board. In the assembled state, the housing lid is riveted onto the continuous sealing ring, thereby pressing it onto the flexible circuit board. As the flexible circuit board and the sealing ring completely surround the carrier, the carrier is made oil-tight, the circuit disposed on the carrier being contactable using conductor paths implemented in the flexible circuit board.
[0005] The known circuit module is particularly suitable for incorporating an electronic circuit into the engine or transmission of a motor vehicle. For in addition to being able to operate over a wide temperature range of −40° C. to 150° C., it also provides a high degree of vibration resistance.
[0006] One disadvantage of the known circuit module is the high cost of the flexible circuit board, as this circuit board is generally manufactured from expensive polyimide. Material with this composition is generally known, for example, under the trade name KAPTON.
SUMMARY OF THE INVENTION
[0007] Based on this prior art, the object of the invention is to create a circuit module for accommodating circuits in the automobile field which can be less expensively manufactured compared to the prior art. The object of the invention is additionally to specify an arrangement for contacting the circuit modules.
[0008] This object can be achieved by a circuit module for motor vehicles, comprising a housing accommodating a motor vehicle circuit and comprising a contact wire brought out of said housing, said contact wire being connected to the motor vehicle circuit, wherein the contact wire is brought out of the housing through a housing wall surface enclosing the contact wire and that the contact wire passes through an elastomeric seal which seals the wall surface against oil and splash water.
[0009] The seal can be made of a polyimide-based material or an epoxy-resin-based material. The seal can be positively locked in the wall surface of the housing. The contact wire can be positively locked in the seal. The seal may cover an opening in the wall surface and surmounts a sealing ring running around the opening. The seal may be implemented in a compression element which can be pressed into the wall of the housing. The seal can be implemented as a male connector containing a plurality of contact wires.
[0010] The object can also be achieved by a circuit module for motor vehicles, comprising a housing accommodating a motor vehicle circuit and comprising a contact wire brought out of said housing, said contact wire being connected to the motor vehicle circuit, wherein the contact wire is enclosed by a glass seal disposed in a compression element which can be inserted in the wall surface of the housing.
[0011] The object can also be achieved by an arrangement for contacting contact wires of an automobile circuit module, comprising connecting leads and contact pins, wherein the connecting leads comprise conductors reinforced by extruded ribbons and are connected to the contact pins.
[0012] The object can furthermore be achieved by a method of manufacturing a circuit module, comprising the steps of:
[0013] providing a module housing having a base plate;
[0014] providing at least one opening in said base plate;
[0015] placing an electronic circuit inside said housing on said base plate,
[0016] providing a sealing element which includes a connector for providing electrical connection,
[0017] sealing said opening with a seal element, and
[0018] connecting said connector with said circuit.
[0019] The seal can be surrounded by a compression element and can be manufactured of a polyimide-based material, an epoxy-resin-based material, or of glass. The opening may receive a seal with a single connector or multiple connectors separated from each other through the seal. The method may further comprise the steps of:
[0020] providing a connecting lead, wherein the connecting lead comprise at least one conductor reinforced by extruded ribbons, and
[0021] connecting the conductor with said connector to establish an electrical connection with the electronic circuit.
[0022] In the circuit module, the contact wires are not brought out of the housing in a flexible circuit board having an extended surface area as in the prior art. Instead the contact wire is brought out through an opening formed in the wall surface of the housing, said opening being made tight using a seal made of a duroplastic or elastomeric material. An expensive flexible circuit board is not therefore required for the circuit module. The very expensive material required for the seal is concentrated more on the sealing area where it ensures the tightness of the openings in the wall surface. It is therefore likely that devices constructed in this way for accommodating motor vehicle circuits can be manufactured at lower cost compared to the prior art.
[0023] In a preferred embodiment, the contact wire is positively locked in the duroplastic or elastomeric seal. The duroplastic or elastomeric seal can also be positively locked in the opening. These measures ensure that the contact wires are fixed in position with respect to the housing.
[0024] In a further preferred embodiment, the opening in the housing is sealed by a cover made of a duroplastic or elastomeric material surmounting a sealing ring disposed on the wall surface. A large number of contact wires can be brought out through said cover. Covers implemented in this way can be manufactured separately from the rest of the housing. The cover with the contact wires can then be mounted on the openings provided for the purpose and fixed in position when the motor vehicle circuit is assembled.
[0025] In a further preferred embodiment, the contact wire and the seal are implemented in a compression element which can be pressed into a cutout in the wall of the housing. Press-fit connections of this kind have the advantage that no additional fixing means are required. For this embodiment, fused glass can also be used for sealing the contact wires.
[0026] At final assembly, the contact wires are preferably brought into contact with connecting leads having conductor paths embedded in extruded ribbons. Leads of this kind have low mass, thereby reducing the vibration loading of the contact wires.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The invention will now be explained with reference to the accompanying drawings:
[0028] [0028]FIG. 1 shows a cross-sectional view of a circuit module for motor vehicles;
[0029] [0029]FIG. 2 shows the circuit module from FIG. 1 viewed from below;
[0030] [0030]FIG. 3 is an enlarged cross-section showing the penetration of the contact pin through the wall of the circuit module from FIG. 1;
[0031] [0031]FIG. 4 shows a cross-section through another embodiment of the penetration of the contact pin through the wall of the circuit module; and
[0032] [0032]FIG. 5 shows a cross-section through another modified embodiment of the penetration of the contact pin through the wall of the circuit module.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] [0033]FIG. 1 shows a cross-section through a circuit module 1 accommodating, for example, a circuit for controlling a motor vehicle engine or transmission. The circuit is disposed on a carrier 2 located on a base plate 3 . The base plate 3 is surmounted by a cover 4 which seals the carrier 2 against oil and splash water. In the base plate 3 there are provided openings 5 and 6 through which the contact pins 7 are brought out. The contact pins 7 are connected via bond wires 8 to the circuit implemented on the carrier 2 . The openings 5 and 6 are sealed by seals 9 and 10 , respectively, which will be described in detail below.
[0034] [0034]FIG. 2 shows a view of an underside 11 of the circuit module 1 . Whereas the openings 5 are bores of circular cross-section, the opening 6 is implemented as a slot and the seal 10 is in the form of a male connector comprising a plurality of adjacently disposed contact pins 7 .
[0035] [0035]FIG. 3 shows a cross-section through the opening 5 of the circuit module 1 from FIG. 1. The opening 5 is made tight by means of the seal 9 which is positively locked in the opening 5 via lugs 12 . In addition, the contact pin 7 has a collar 13 by means of which the contact pin 7 is anchored in the seal 9 . Instead of the lug 12 and collar 13 , there can also be provided recesses in the base plate 3 and the contact pin 7 through which the contact pin 7 is positively locked in the seal 9 and the seal 9 positively locked in the opening 5 . In addition, it is also possible to friction-lock the contact pin 7 in the seal 9 .
[0036] During manufacture of the circuit module 1 , the contact pins 7 are bonded or cast into the base plate 3 .
[0037] [0037]FIG. 4 shows a modified embodiment in the form of a seal 10 implemented as a male connector. The seal 10 extends inside the circuit module 1 over the opening 6 in the base plate 3 . The seal 10 holds the contact pin 7 via recesses 14 on the contact pin 7 , thereby positively locking the contact pins 7 in the seal 10 . Friction locking is also possible between the contact pin 7 and the seal 10 .
[0038] The seal 10 additionally overlies a sealing ring 15 running round the opening 6 and is suitably fastened to the base plate 3 . For example, the seal 10 can be latched to the base plate 3 . A particularly secure connection between the seal 10 and the base plate 3 is obtained if the seal 10 is riveted to the base plate 3 . To prevent the sealing ring 15 from being pressed out, a stop 16 is implemented on the seal 10 .
[0039] The seals 10 are preferably produced by injection molding, the contact pins 7 being cast into the seal 10 during this process. The seals 10 are then only mounted on the openings 6 during final assembly.
[0040] [0040]FIG. 5 shows another embodiment of a seal 17 which holds the contact pin 7 in a compression element 18 . Said compression element 18 is a so-called self-clinch plug which is pressed into the base plate 3 in such a way that the material of the base plate 3 flows into recesses 19 under a cutting collar 20 . This therefore produces a positive fit between the compression element 18 and the base plate 3 . The compression element 18 can be implemented as a single plug with a single contact pin 7 or as a male connector with a plurality of contact pins 7 .
[0041] The seals 17 are preferably produced by injection molding, the contact pins 7 being cast into the seal 10 during this process. The seals 10 are then only mounted on the openings 6 during final assembly.
[0042] [0042]FIG. 5 additionally shows a preferred embodiment of a connecting lead 21 which has conductors 23 embedded in extruded ribbons 22 . A connecting lead 21 of this kind has a low mass so that the vibration loading of the contact pins 7 is much lower than when using conventional leadframes.
[0043] Duroplastics or elastomers are envisioned as materials for the seals 9 , 10 and 17 . In particular, polyimide- or epoxy-resin-based materials should be used. As the plastic is limited to just the area of the seals 9 , 10 and 17 , only a small amount of material is used for the seals 9 , 10 and 17 . The seals 9 , 10 and 17 can therefore be inexpensively manufactured.
[0044] In a modified embodiment of the seal 17 , glass into which the contact pins 7 are sealed is used for this purpose.
[0045] In particular the seals 10 and the compression element 18 with the seal 17 can be manufactured separately from the circuit module 1 . During manufacture of the circuit module 1 , the seal 10 implemented as a male connector and the compression element 18 provided with the seal 17 are then mounted on the base plate 3 .
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A circuit module for the automobile field has contact wires ( 7 ) which are brought out through a wall ( 3 ) of the housing and which are made tight by a seal ( 9 ) made of a duroplastic or elastomeric material.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] NA
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention is in the field of travel accessories including luggage and travel carriers and pertains more particularly to a travel carrier with interchangeable elongate sections for carrying elongate utilities and accessories when traveling by air or ground.
[0004] 2. Discussion of the State of the Art
[0005] In the field of travel, there are a variety of luggage carriers and the like adapted to contain items that a traveler needs at least at the travel destination. The most common type of luggage is the suitcase adapted to contain a traveler's cloths, shoes, and other items that the user is not personally carrying during travel.
[0006] In air travel for example people check bags into the airline luggage transport service connected with the flight the traveler is taking. These bags are typically suitcase style rectangular bags or carriers that have wheels and an extendible handle that allows travelers to pull the carrier on wheels using the extendible handle as a lever similar to maneuvering a two-wheeled hand truck. These typical carrier bags or cases may vary in size and capacity to very small cases that can be carried such as on a flight to much larger cases that have to be separately transported.
[0007] One limitation to the typical travel case is that it is only designed to carry typical travel items like clothing, shoes, and general necessities one requires at a travel destination. Carry on bags that are small enough to travel with the traveler include smaller back packs, handled carry bags, brief cases, and the like. These are also limited in what they can carry for a traveler.
[0008] There are, of course, current carriers for elongate items like snow boards and skis, and these are typically too large to be taken on-board as hand luggage, and must be checked as baggage. One problem many travelers have with such luggage is that these carriers are very clumsy to handle when standing in line or maneuvering through crowded airport terminals.
[0009] Many travelers take flights or other means of mass transportation to vacation sites where they ski, snowboard, fish, wake board, surf, and other activities.
[0010] What is clearly needed is a carrier that is configurable to stow elongate items that are otherwise awkward to carry in a manner that protects the items from exposure to elements and shock, that allows a traveler to maneuver and carry the item in an efficient and non-obtrusive way, and that may be left to stand upright on a floor with a very small footprint, to avoid the problems of maneuverability in lines, and that may also be moved along in this upright position.
SUMMARY OF THE INVENTION
[0011] The problem stated above is that typical travel cases for elongate items like snowboards or skis are designed to be carried with the long axis horizontal, and this makes maneuverability in lines and crowds quite difficult. Such carriers cannot be stood on a floor with the long axis upward in a stable manner, and will not stand unsupported in this aspect.
[0012] The inventors therefore considered functional elements of a travel case, looking for elements that exhibit the potential to provide a way to enclose and protect elongate items such as skis or a snowboard for example, but in a manner that would not be inconvenient to maneuver.
[0013] The present inventor realized in an inventive moment that if a travel case could be designed that would facilitate enclosure and protection of an elongate item while still having room for the accessories associated with the item, a significant convenience might result for the traveler. The inventor therefore constructed a unique travel carrier for stowing elongate utility items and accessories that allowed convenient and efficient maneuvering and space utilization while offering covered protection for the items stowed. A significant convenience results, with no impediment to maneuvering of the carrier or with space utilization of the carrier.
[0014] Accordingly, in one embodiment of the present invention a travel carrier comprising a first region having a rigid floor and walls extending to a height defining a volume of a size to accommodate at least a pair of boots, a closable opening into the first region for depositing and removing items to be carried, a second, elongate region extending upward from the first region of a length and cross-sectional area at least sufficient for holding one or more elongate items, a closable opening into the second region for depositing and removing items to be carried, and two or more wheels along one edge of the floor of the first region and supports along an opposite edge of the floor of the first region, such that the travel carrier, resting on the wheels and supports, is stably supported in an upright aspect with the elongate second region extending upward and positioned within the footprint of the floor of the first region, and wherein the carrier may be tipped onto the wheels to be pulled along a floor by a person holding the second region.
[0015] In one embodiment the first region is rectangular and the second elongate region is tubular. In one embodiment the travel carrier further includes an adapter in the form of a rigid square tube into which the second elongate region is seated. In this embodiment the first region is rectangular and the second elongate region is a semi-rigid rectangular sleeve.
[0016] In another embodiment the travel carrier further includes an adapter in the form of a rigid rectangular sleeve into which the end of an elongate item enclosed by the second elongate region is seated. In one embodiment the wheels are castor wheels and a handle is strategically located on the second elongate region to enable maneuvering of the carrier on the wheels. In one embodiment another handle is provided on the travel carrier and is located on one wall of the first region.
[0017] In one embodiment the first region and second elongate region are covered with a heavy material or, with the exception of the rigid floor of the first region, fabricated of a heavy material. In a variation of this embodiment the heavy material may be completely separated into two parts along a zippered edge with a zipper for adjoining the two parts with one part remaining integral to the first region and the other part remaining integral to the second elongate region when unzipped and separated.
[0018] In one embodiment including an adapter, the first region supports attachment and removal of different adapters associated with different elongate regions. In a variation of this embodiment, one second elongate region attachable to the first region by an associated adapter is adapted to house one or more skis and poles, the first region adapted to house ski boots and accessories. In another variation of the embodiment, one second elongate region attachable to the first region by an associated adapter is adapted to house a snowboard, the first region adapted to house snowboard boots and accessories.
[0019] In one embodiment supporting the use of heavy material separable into two parts by a zipper, the zippered edge defines an opening into the first region when unzipped. In one embodiment wherein the second elongate enclosure is a semi-rigid rectangular sleeve the second elongate region includes a vertical zippered edge with a zipper defining a vertically disposed opening into the region. In one embodiment wherein the second elongate region is tubular, the closeable opening of the second elongate region is a lid attached by zipper to the body of the region.
[0020] According to another aspect of the invention, a method is provided for configuring a travel carrier to enclose a different elongate item or items and accessories than an elongate item or items and accessories it is currently configured to enclose, the carrier having a first region and a second elongate region disposed within the footprint of the first region, the regions associated together through an adapter, and a closable opening separate to each region comprising the steps (a) detaching the second elongate region of the travel carrier from the first region of the travel carrier, (b) removing the adapter from the first region of the travel carrier, (c) installing a different adapter to first region of the travel carrier, and (d) attaching a different elongate region to the first region with the aid of the adapter of step (c).
[0021] In one aspect of the method the travel carrier is covered with or fabricated from a heavy material and in step (a) detachment is by unzipping the second region from the first region along a zippered edge in the material. In this aspect in step (d), attachment is by zipping the elongate region to the first region after first orientating the elongate region to the first region orientation aided by the adapter. In one aspect in step (d), the adapter orientates and seats the elongate region relative to the first region. In another aspect, in step (d), the adapter is adapted to accept an end of an elongate item being enclosed by the elongate region.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0022] FIG. 1 is a perspective view of a travel carrier with an elongate section according to an embodiment of the present invention.
[0023] FIG. 2 is a side-elevation view of the carrier of FIG. 1 in a luggage line.
[0024] FIG. 3 is a perspective view of a travel carrier with an elongate section according to another embodiment of the present invention.
[0025] FIG. 4 is a side-elevation view of the carrier of FIG. 3 in a luggage line.
[0026] FIG. 5 is an overhead view into the carrier of FIG. 1 .
[0027] FIG. 6 is an overhead view into the carrier of FIG. 2 .
DETAILED DESCRIPTION
[0028] The inventor provides a travel carrier for completely enclosing elongate items that otherwise are awkward to carry such as a pair of skis or a snowboard and associated accessories like boots, gloves and the like. The carrier may be checked onto a flight as luggage or as a carryon bag and is adapted to be handled in a fashion similar to wheeled suitcases typically used in flight travel. The invention shall be described in detail using the various embodiments presented below.
[0029] FIG. 1 is a perspective view of a travel carrier 100 with an elongate enclosure according to an embodiment of the present invention. Travel carrier 100 includes a primary base enclosure 101 and a secondary elongate enclosure 103 . Base enclosure 101 may be a rectangular structure having a floor and walls 102 . In one embodiment the base enclosure is a square enclosure. In another embodiment the base enclosure may assume another geometric form such as a three-sided enclosure or one that has more than four sides. In still another embodiment, the enclosure may be annular having a floor and a peripheral wall.
[0030] In this example, primary enclosure 101 has a rigid floor 110 . Floor 110 may be manufactured of a polymer, fiber board, or some other rigid material. A pair of castor wheels 105 is provided and installed on the lower surface of floor 110 to provide a wheeled base that enables carrier 100 to be pulled or pushed and rolled along on the wheels in a fashion similar to wheeled suitcases popular in airline travel.
[0031] Secondary enclosure 103 is linear in form and is an elongate tube in this example. Enclosure 103 may be manufactured of polymer, fiberboard, heavy cardboard, or some other rigid or semi-rigid material. Enclosure 103 may be attached to primary enclosure 101 such that it is supported in vertical extension above the base of the carrier. The terms primary and secondary used to reference the enclosures serves only to distinguish the enclosures from one another in general description. Primary enclosure 101 is primary only in that it serves as a base for supporting secondary enclosure 103 .
[0032] A heavy material 106 such as canvas or some other durable material may be provided to completely cover travel carrier 100 including primary enclosure 101 and secondary enclosure 103 . Material 106 may be glued onto primary and secondary enclosures or it may be stretched over the enclosures. Walls 102 of base enclosure 101 may include a covering of canvas or other heavy material 106 sewn over or glued onto a heavy cardboard, polymer, or fiber board backing thus giving a semi rigid quality to walls 102 of enclosure 101 . In another embodiment, walls 102 are made of the heavy material without backing and take form when the carrier is assembled and packed.
[0033] Elongate secondary enclosure 103 has a closeable end cap 104 that attaches to the enclosure body 103 by a zipper 111 . Other methods may be used to close off the free end of enclosure 103 such as snap, tie, or buckle without departing from the spirit and scope of the present invention. End cap 104 includes a handle 108 sewn onto or otherwise affixed to the top surface of end cap 104 . Handle 108 may be a polymer handle or a handle made from some other rigid or resilient material. Handle 108 enables a user to pull or push travel carrier 100 on wheels 105 by tilting the carrier from an upright position onto wheels 105 and maneuvering it as desired. Another handle 109 is provided in this example on a wall ( 102 ) of carrier 100 to illustrate that it may also be manipulated as other luggage types by carrying it in a horizontal position.
[0034] Material 106 may be separable along a zippered edge demarked by a zipper 107 . In one embodiment, unzipping zipper 107 provides an opening into and therefore access to primary enclosure 101 . Unzipping zipper 107 completely may separate the material 106 stretched over base enclosure 101 and elongate enclosure 103 . Material 106 may be firmly attached to both enclosures 101 and 103 in certain specific regions so that unzipping the material does not displace the material from the respective enclosures that the material covers. In one embodiment industrial adhesive may be used to attach the material to the structure of the base enclosure and that of the tube enclosure as well.
[0035] Travel carrier 100 has at least one material pocket illustrated herein by a zipper 112 marking the opening of the pocket. Pockets may be present in multiple locations on carrier 100 and may be used to stow gloves, hats, and other items. Travel carrier 100 may be provided in different forms or versions that are adapted to accommodate specific items that would otherwise be awkward to carry during travel such as airline travel, for example. The defining component in different versions of carrier 100 is an elongate enclosure though the exact physical forms of elongate enclosures from carrier to carrier may differ according to the physical properties of the item that the enclosure is adapted for. In this example, carrier 100 is adapted to enclose a ski or a pair of skis and poles enclosed within elongate enclosure 103 and ski boots, bindings and perhaps other accessories associated with skiing in primary enclosure 101 .
[0036] The design of travel carrier 100 is such that it may be stood upright when not being maneuvered on wheels 105 . Base enclosure 101 provides a stable anchor for elongate enclosure 103 preventing tipping over. As such, a user may easily maneuver carrier 100 among other baggage typically handled without any problems related to convenience of movement or with space utilization. Travel carrier 100 may in some cases fit onto a luggage rack horizontally and may be set upright in line or when it is not being maneuvered without inconvenience.
[0037] FIG. 2 is a side-elevation view of carrier 100 of FIG. 1 in a luggage line 200 . Some elements illustrated in FIG. 2 are also illustrated and described relative to FIG. 1 above. Those elements which are again illustrated in this example may or may not have an element number illustrated in this example since they have already been introduced with element numbers and described above. Those elements that are again illustrated here with the element numbers from FIG. 1 shall not be reintroduced. Travel carrier 100 is illustrated in position between a suitcase 205 and a suitcase 206 in luggage line 200 . Carrier 100 supports an elongate item or items in a vertical position taking up the least amount of footprint (floor space) possible. Bags 205 and 206 represent typical check-in bags at the airport the bags having wheels, stand-offs feet and an extension handle. Carrier 100 has wheels and a pair of standoff feet 203 . A broken outline of a boot 202 is illustrated in this example to show that a pair of boots is contained within base enclosure 101 . It is noted herein that the width of base enclosure 101 need not exceed that of a typical travel suitcase in order to accommodate boots and other accessories that may be included with the elongate item being carried.
[0038] An adapter 201 is provided within base enclosure 101 and is adapted to be secured to the floor and walls of the enclosure. Adapter 201 is illustrated herein with a broken outline. In an embodiment where elongate enclosure 103 is a tube, adapter 201 may be a rectangular tube or an annular tube structure. In either case, the inside diameter of the adapter may be held just larger than the outside diameter of secondary enclosure 103 so that the enclosure can be fitted into the adapter for support. In one embodiment no fastening is required in order to support enclosure 103 in a vertical position. Assembly in this embodiment consists of seating the elongate enclosure tube into the adapter tube.
[0039] After elongate enclosure 103 is seated into the adapter on base enclosure 101 , the heavy material coverings previously described may be zipped together to hold the carrier together. In some other embodiments fastening hardware may be provided to secure the elongate enclosure to the adapter on the base enclosure. Adapter 201 may be secured to the floor and back wall of the primary enclosure by screws and brackets or by other fastening hardware.
[0040] In one embodiment enclosure 101 remains open with respect to having a hinged lid or a top piece and is not covered until the heavy material covering the carrier is zipped together thus forming a material top or cover. The material flap with a zippered edge may be a part of the elongate enclosure and when the enclosure is properly connected to the base enclosure, the material sections may be zipped together forming the top of the base enclosure and physically supporting and retaining the elongate enclosure from becoming displaced. An interior space or pocket 204 is illustrated herein as a space that may be accessed through a zippered opening such as through zipper 112 described further above with respect to FIG. 1 .
[0041] In one embodiment of the invention primary enclosure 101 may be utilized to carry items without having a secondary enclosure attached. In this case a material top having a zipper edge may be provided to close off the enclosure on top. Also in this embodiment an extensible handle (not illustrated) may be provided on the primary enclosure so that it may be maneuvered in the manner of a typical airline bag having wheels and an extensible handle.
[0042] In a preferred embodiment, the secondary enclosure or region as it may be referred to is disposed vertically and remains within the footprint of the primary enclosure the carrier enabled to stand upright without tipping. In one embodiment a counterweight may be provided in the primary enclosure to ensure a more stable upright position. However, it is not required to practice the invention as the items stowed in the primary enclosure are of sufficient weight to provide good stability for an upright elongate item like a snowboard or a pair of skis, both of which are relatively light in weight.
[0043] FIG. 3 is a perspective view of a travel carrier 300 with an elongate section 303 according to another embodiment of the present invention. Travel carrier 300 is adapted to carry an elongate item like carrier 100 described further above. However in this case the secondary enclosure illustrated herein as enclosure 303 is formed differently according to the physical characteristics of the item it is designed to enclose.
[0044] Secondary enclosure 303 may be attached or affixed to primary enclosure 101 with slight modification of base enclosure 101 such as replacing the adapter ( 201 ) described with respect to FIG. 2 above with another adapter of a different form. Primary enclosure 101 includes wheels 105 and may include stand-off feet 203 not illustrated in this view but described and illustrated further above.
[0045] Secondary enclosure 303 may be a semi-rigid enclosure. In this example, enclosure 303 is rectangular having a rigid or semi-rigid back wall (not visible in this view) and rigid or semi-rigid side walls such as wall 308 (visible in this view). Enclosure 303 may also include a rigid or semi-rigid top or end wall that is rigid enough to support handle 302 . The walls of elongate enclosure 303 may be heavy cardboard, fiberboard, polymer, or some other rigid to semi-rigid material. These support structures may be backing that forms the basic shape of the enclosure over which a heavy material 306 may be sewn, stretched over, or glued.
[0046] Elongate enclosure 303 has a front wall 310 , which may be made from material 306 . A zippered edge demarked by a zipper 301 is provided and disposed vertically along the length of enclosure 303 roughly centered on front wall 310 to provide access to the contents of the enclosure. Enclosure 303 may be designed to contain a snowboard, for example. Zipper 301 is provided to open or to close the opening in this example but other fastening hardware may be used instead such as snaps, hooks, buckles or the like.
[0047] In one embodiment of the present invention, elongate enclosure 303 and elongate enclosure 103 of FIG. 1 above are interchangeable with respect to primary enclosure 101 . In this embodiment a user may configure the travel carrier as carrier 100 or as carrier 300 by installing the appropriate elongate enclosure. It is noted herein that any adapter associated to either secondary enclosure may be required to accommodate the elongate enclosure in an installed position relative to the base enclosure. In one embodiment zippered edge (zipper 301 ) is provided along side wall 308 instead of at the center axis of wall 310 . In this case, the contents may be placed into or removed from enclosure 303 from the side of the enclosure instead of from the front.
[0048] In one embodiment enclosure 303 is a flexible non-reinforced material like canvas material 306 or perhaps cordura used as a material in flight bags because of its durability. In this case the enclosure takes vertical form after the contents are enclosed therein. The contents, in this case, a snowboard, may be fitted partially into an adapter attached to the back wall of base enclosure 101 in order to ensure a vertical predisposition of the otherwise flaccid elongate enclosure when it is zipped up over the snowboard. In the case of a semi-rigid enclosure the adapter may still be used to anchor the snowboard so that a vertical presentation is secured.
[0049] FIG. 4 is a side-elevation view of carrier of FIG. 3 in a luggage line 400 . Luggage line 400 includes travel carrier 300 a travel case 405 and a travel case 406 for reference. Carrier 300 includes base enclosure 101 with wheels ( 105 ) stand-off feet 203 . Elongate enclosure 300 includes a rigid or semi-rigid back wall 309 and rigid to semi-rigid sidewalls 308 . A snowboard boot 402 is illustrated by a broken outline within base enclosure 101 . An adapter 401 is provided within base enclosure 101 (illustrated by broken outline). Adapter 401 may be a rectangular sleeve or tubing that is secured to the back wall and to the floor of enclosure 101 by screw and bracket, or by other hardware.
[0050] Adapter 401 may be manufactured of a durable polymer or other durable material and may be adapted to accept one end of a snowboard or other elongate item so that the item may be partly secured for carrying. The heavy material of elongate enclosure 303 may be zipped onto base enclosure 101 around the periphery of the enclosure after stowing boots ( 402 ) and other accessories if so desired into the base enclosure. The enclosure may then be stretched or otherwise positioned over the inserted snowboard and zipped into place protecting, enclosing and helping to retain the snowboard in position to be carried. Handle 302 may be used to push or pull carrier 300 along on the castor wheels. When at rest the carrier may remain upright with contents enclosed. An interior space 304 represents a pocket within which additional accessories may be stowed like sunglasses, sun screen, or other like items.
[0051] Referring now back to FIG. 3 items may be retrieved from base enclosure 101 by unzipping zipper 107 and reaching into the enclosure and removing the items. This action will not dislodge or upset any contents (snowboard) stored within enclosure 303 because the snowboard is actually retained by the adapter attached to the base enclosure as will be seen in more detail below.
[0052] FIG. 5 is an overhead view into base enclosure 101 of FIG. 1 . FIG. 6 is an overhead view into base enclosure 101 of FIG. 3 . Referring now to FIG. 5 , base enclosure 101 includes tube fixture 201 in the form of a rectangle. Adapter 201 may be secured to the rigid floor and/or to the back wall of the enclosure using provided brackets 502 . Tube end 103 representing the tubular elongate enclosure of FIG. 1 is illustrated for reference herein as being inserted into adapter 201 . The contents of tubing enclosure 103 may pass into the adapter and may be stopped only by the floor of the base enclosure. In one embodiment thumbscrews or other hardware may be provided to help secure tubing 103 into adapter 201 such that it does not become displaced. Interior space 501 is available for storage of accessories like boots, gloves, and other items.
[0053] Referring now to FIG. 6 , enclosure 101 is configured with adapter 401 instead of adapter 201 . In this example adapter 401 is secured to the floor of enclosure 101 via tabs and screws 601 . Other fastening hardware may be used in place of tabs and screws. Adapter 401 is a rigid rectangular tube that presents an oblong profile having a minor inside wall-to-wall diameter and a major inside wall-to-wall diameter. The inside sleeve dimensioning of adapter 401 is just larger than the outer dimensions of the end of a snowboard so that the snowboard may be secured into a vertical presentation by the adapter.
[0054] Referring momentarily back to FIG. 4 , adapter 401 may extend the entire depth of enclosure 101 thus providing sufficient sleeve length to hold the snowboard upright in a secure manner. In one embodiment adapter 401 may be modified to accept the end of another elongate item like a surfboard, for example. The end of a surfboard may have a tail fin protruding off of the bottom end of the board. A cutout slot may be provided through the accessible wall of adapter 401 to accommodate a fin of a surfboard. Similarly, other modifications can be made to accommodate other end configurations of an elongate item.
[0055] The elongate enclosures are interchangeable to a single base enclosure so that a user may pre-configure the carrier to transport a specific utility and accessories. Other possible items that may be accommodated in this way include fishing poles and tackle, surfboards, and other utilities that are too long for conventional travel cases. The carrier of the invention may be conveniently checked into an airport luggage transport service as a checked bag, or it may in some cases be carried on board.
[0056] It will be apparent to one with skill in the art that the travel carrier of the invention may be provided using some or all of the mentioned features and components without departing from the spirit and scope of the present invention. It will also be apparent to the skilled artisan that the embodiments described above are exemplary of inventions that may have far greater scope than any of the singular descriptions. There may be many alterations made in the descriptions without departing from the spirit and scope of the present invention.
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A travel carrier has a first region having a rigid floor and walls extending to a height defining a volume of a size to accommodate at least a pair of boots, a closable opening into the first region for depositing and removing items to be carried, a second, elongate region extending upward from the first region of a length and cross-sectional area at least sufficient for holding one or more elongate items, a closable opening into the second region for depositing and removing items to be carried, and two or more wheels along one edge of the floor of the first region and supports along an opposite edge of the floor of the first region, such that the travel carrier, resting on the wheels and supports, is stably supported in an upright aspect with the elongate second region extending upward and positioned within the footprint of the floor of the first region, and wherein the carrier may be tipped onto the wheels to be pulled along a floor by a person holding the second region.
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TECHNICAL FIELD
The present invention relates generally to relief valves, and more particularly to a quiet relief valve which includes both spring and air biasing means.
BACKGROUND ART
Spring loaded relief valves are well known in the art. While such valves are generally reliable and fail-safe in nature, it is not convenient to provide such valves with external means to open the valve in order to exercise and/or test the valve. While an air or other form of pressure-biased valve can be readily provided with external actuating means, such a valve will not remain operational as a relief valve in the event of a loss of biasing pressure.
Because of the inherent problems associated with the prior art relief valves, it has become desirable to develop a valve which is operable as a relief valve independent of pressure or other external biasing forces, which is fail-safe, and which can be opened by external means for exercising and testing the valve.
SUMMARY OF THE INVENTION
The present invention solves the aforementioned problems associated with the prior art as well as other problems by providing a relief valve which is biased by both spring and air pressure means, and wherein the air biasing means includes means for applying air pressure to the valve opposite to the biasing direction and against the spring biasing means to open the valve for exercising and testing purposes. In the event of a loss of air pressure, the spring biasing means is still effective to bias the valve into the closed condition. The relief valve includes a housing, inlet means, outlet means, a valve element, and a biasing assembly which normally biases the valve element closed with a predetermined closing force such that the valve element will open a flow path from the inlet means to the outlet means when the closing force is exceeded by an oppositely directed pressure force. The biasing force is applied to the stem member to which it is attached by means of an air cylinder formed integrally with the valve body, and by a plurality of spring members acting between the valve body and the stem. The air cylinder is divided into an upper and a lower chamber by a piston member operatively attached to the valve stem, and air inlet ports are provided to the two chambers for supplying biasing pressure to the valve to bias the valve closed in combination with the spring biasing means, and for supplying an opening pressure to the valve, against the spring biasing force. If air pressure is lost the valve will remain biased closed by the spring force, however, it can be appreciated that the valve will relieve at a lower pressure than if it were biased closed by both spring and air pressure.
In accordance with the invention, the valve also includes a "quiet" element surrounding the valve element to reduce the noise level when the valve is relieving excess pressure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view of a relief valve constructed in accordance with the invention.
FIG. 2 is a plan view of one of the disks of the quiet valve element incorporated in the invention.
FIG. 3 is an elevation view of the disk of FIG. 2.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings where the illustrations are for the purpose of describing the preferred embodiment of the invention and are not intended to limit the invention hereto, FIG. 1 illustrates a safety relief valve 10 comprising a body assembly 2, a valve assembly 14 received with the body assembly 12, and a biasing assembly 16 also received with the body assembly.
The body assembly 12 comprises a lower section 18, an intermediate section 20 attached to the lower section, and an upper section 22 attached to the intermediate section.
The lower section 18 of the body assembly 12 includes an inlet portion 24, which can be a separate piece welded or otherwise attached to the lower end of the lower section 18, an outlet portion 26, and a valve element receiving portion 28. The upper end of the lower section 18 includes spaced, outwardly directed radial lugs 30 through which the intermediate section 20 and the lower section 18 are maintained together vertically, and a plurality of flange sections 32 (only one of which is shown) which receive bolts locking the sections together as will be hereinafter described.
The intermediate section 20 of the body assembly 12 comprises a cast body including an upper, upwardly opening cup-like portion 34; a lower, downwardly opening cup-like portion 36; and a plurality of webs 38 which connect the upper and lower cup-like portions. The lower, cup-like portion 36 includes spaced, radially inwardly directed lugs 40, which are interengageable with the lugs 30 on the lower section 18 when the lower and intermediate sections are brought together and turned relative to one another so that the lugs coincide. The intermediate section 20 also includes a plurality of flange sections 42 (only one of which is shown), which are aligned with the flange sections 32 when the lugs 30,40 are interengaged, so that bolts 44 received through the flange sections 42 and threaded into the flange sections 32 will lock the lower and intermediate sections together.
The upper cup-like portion 34 of the intermediate section 20 includes an outwardly directed radial lip or flange 46 which has a plurality of splines 47 formed on the outer end thereof for attachment to the upper section 22 as will be hereinafter described. A first air inlet port 48 is formed in the side wall 50 of the cup-like portion 34 adjacent the flange 46. A second air inlet port 52 is also formed in the side wall 50 adjacent the lower edge thereof. A vent port 51 is formed through the side of the lower cup-like portion 36 of the intermediate section 20.
The upper section 22 of the body assembly 12 is an inverted bowl-shaped member having an outwardly extending flange 54 formed at the lower end thereof, and having a central bore 56 formed in the bore 58 thereof. A plurality of splines 59 are formed on the outer edge of flange 54 and are alignable with the splines 47 formed in the flange 46. A ring clamp 61, having a plurality of internal splines formed therein can be placed over the flanges 46 and 54 as shown, to clamp the upper section 22 and the intermediate section 20 together, while positively preventing relative rotation therebetween. Prior to assembling the upper and intermediate sections, an air chamber wall member 62 is inserted, as shown, between the upper and intermediate sections, and is retained by the ring clamp 61.
The valve assembly 14 comprises a valve stem 64 slidingly received within a bearing 66 retained in the lower cup-like portion 36 of the intermediate section 20 between a shoulder 67 formed therein and a retaining ring 68, and a valve element assembly 70 threadably attached to the valve stem 64 adjacent the lower end thereof.
The valve element assembly 70 comprises a seal member 72 threadably attached to the valve stem 64, and a valve member 74 which is attached to the seal member by pins 75. A plurality of resilient seal elements 76 separated by spacers 77 are received over a reduced diameter portion of the seal member 72, and are retained axially between a shoulder 78 formed on the seal member, and a ring 80 which is threaded onto the seal member.
The seal elements 76 slidingly engage the inside diameter of a cylindrical insert 82 which is threaded into the lower section 18 of the body assembly 12. The insert 82 is preferably of hardened steel to define a durable wearing surface for the seal elements 76.
The valve member 74 includes a relatively large diameter portion 84, and a relatively smaller diameter portion 86. The outer diameter of the smaller diameter portion 86 fits within a counterbore 88 formed in the bottom portion of the seal member 72, and the lower end 90 of the valve stem 64 is received within a counterbore 92 formed in the top portion of the valve member 74. The pins 75 are received through the annular walls defined between the respective outer diameters and counterbores of the valve member 74 and the seal member 72.
The inlet portion 24 of the lower section 18 of the body assembly 12 extends upwardly into an outlet chamber 94 formed within the outlet portion 26 of the valve, and has a valve seat 96 formed at the upper end thereof where an inlet passage 98 formed through the inlet portion 24 opens into the outlet chamber 94. The bottom surface of the valve member 74 has an annular sealing face 100 formed thereon which contacts the valve seat 96 when the valve is in the closed position, as shown in FIG. 1.
A so-called "quiet" valve element 102 is received within the outlet chamber 94 in surrounding relationship with the valve member 74. The quiet element essentially comprises a plurality of annular rings 104 stacked between the bottom face of the insert 82 and a lower ring 106 which is received against a shoulder 108 formed on the inlet portion 24. The stack of rings 104 is received between stepped upper and lower washers 109 and 110 which interfit with complementary stepped portions formed on the insert 82 and the lower ring 106, and is retained by threading the insert 82 into the lower section 18 of the body assembly 12 to clamp the stack between the insert 82 and the inlet portion 24.
A "quiet" valve element such as the stack of rings 104 is well known in the art, and one of several known types can be used, however, in the preferred embodiment illustrated in FIG. 2, each of the rings comprises an annular plate having a plurality of spaced apart wall segments 112 upstanding from the plate surface and arranged in concentric rings with the wall segments alternating. When the stack of rings 104 is formed as shown in FIG. 1, fluid passing through the valve flows from the center outwardly into chamber 94 and must follow a circuitous path around the wall segments 112 as indicated by the arrows on FIG. 2. In this manner the "quiet" valve element acts as a muffler to reduce the noise level of the flow of fluid through the valve.
The biasing assembly 16 comprises an air biasing assembly 114 and a spring biasing assembly 116, both operatively acting on the valve stem 64 to bias the valve into its closed position, as shown in FIG. 1.
The air biasing assembly 114 comprises a piston 118 having a hub portion 119 received over a reduced diameter portion 120 of the valve stem 64, and a seal element 121 received in an annular groove formed in the outer diameter of the piston 118 and acting against the inside diameter of the upper cup-like portion 34 of the intermediate section 20. The hub 119 extends through an aperture formed in the wall member 62 and is sealed by an O-ring 123. The piston 118 divides the volume within the upper cup-like portion 34 and bounded by the wall member 62 into an upper chamber 122 and a lower chamber 124. The air inlet port 48 opens into the upper chamber 122, and the air inlet port 52 opens into the lower chamber 124. The piston 118 is received on the valve stem 64 against a shoulder defined by the intersection of the reduced diameter portion 120 and the main body of the stem 64, and is retained thereon by a washer 126 and a nut 128 threaded onto the end of the stem 64.
The spring biasing assembly 116 comprises a spring element 130 acting between the upper section 22 of the body assembly 12 and the valve stem 64. In the embodiment illustrated in FIG. 1, the spring element 130 comprises a plurality of spring washers 132 stacked together in pairs and positioned between a thrust washer 134 received on the upper end of the hub portion 119 of the piston 118 and a cylindrical sleeve 136 received through the central bore 56 in the bore 58 of the upper section 22 and retained by a cover plate 138 which bears against the sleeve. The cover plate 138 is retained relative to the upper section 22 by bolts 140 received through the cover plate and threaded into the bore 58. The biasing force of the spring element 130 can be controlled by the extent to which the bolts 140 are threaded into the upper section 22.
OPERATION
In operation, the spring biasing assembly 116 is adjusted by means of the bolts 140 to obtain a predetermined spring force biasing the valve member 74 into its closed position. Air pressure is then introduced into the upper chamber 122 through the air inlet port 48 to act on the upper surface of the piston 118 to add an additional biasing force to the valve member 74. Thus, the total force holding the valve closed is the combined spring force plus the pressure force applied by the piston 118.
When the valve is to be tested or exercised, air pressure is introduced into the lower chamber 124 through the air inlet port 52 to act on the underside of the piston 118 to apply an opening force, against the biasing force, to the valve member 74. Depending on the conditions under which the valve is to be tested or exercised, air pressure can continue to be applied to the air inlet port 48, in which case both the spring and air pressure biasing forces must be overcome to open the valve. Alternatively, air to air inlet port 48 can be discontinued, in which case only the spring biasing force must be overcome.
When the biasing force is overcome, either by an overpressure condition during normal operation, or during testing or exercising, the valve member 74 will lift off the valve seat 96, opening a flow path from the inlet passage 98, through the "quiet" valve element 102 into the outlet chamber 94, and out through an outlet passage 142 formed in the outlet portion 26, the "quiet" element acting to minimize the noise level of the escaping fluid. When the valve member 74 opens, the vent port 51 prevents a build-up of pressure above the valve member.
If there should be a loss of air pressure, resulting in the loss of the pressure biasing force, the valve will remain operational, but will relieve at a lower pressure represented by the spring biasing force only.
Certain modifications and improvements will occur to those skilled in the art upon reading the foregoing description. It will be understood that all such improvements and modifications have been deleted herein for the sake of conciseness and readability but are properly within the scope of the following claims.
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A relief valve (10) having both spring biasing means (116) and air pressure biasing means (114). The spring biasing means (116) includes a plurality of spring washers (132) acting between the valve body (12) and a valve member (74). The air biasing means (116) includes an air cylinder defined by an intermediate portion (20) of the valve body (12), and a piston (118) disposed within the cylinder and acting on the valve member (74). An air inlet port (48) is provided above the piston (118) to permit the area above the piston (118) to be pressurized to add to the biasing force of the spring biasing means (116), and an air inlet port (52) is provided below the piston (118) to permit the area below the piston (118) to be pressurized to open the valve manually for testing and exercising. A "quiet" element (102) surrounds the valve member (74) to reduce the sound level of the fluid flowing through the valve when the valve opens.
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FIELD OF THE INVENTION
[0001] The invention relates to extracting compounds from plant material and to formulations including compounds extracted from plant material, especially but not exclusively, spray formulations for controlling pests.
BACKGROUND OF THE INVENTION
[0002] Many compounds produced by plants can be used as pesticides, food additives, pharmaceuticals, cosmetics, cleaning and disinfecting agents and the like.
[0003] Compounds may be extracted from plant material by steam distillation, a process that typically involves applying steam to plant material to release volatile compounds from the plant material into steam and then condensing the steam to harvest the released volatile compounds. Alternatively, volatile compounds may be released by boiling plant material in water to release the compounds into steam and then condensing steam. Typically the extracted compounds are in the form of an oil that is insoluble in water formed by condensation. The oil is separated from water by a simple decanting process.
[0004] Solvent extraction is another process for extracting compounds from plants. This process typically involves immersing plant material in a solvent for a period of time and under conditions suitable for compounds to be extracted from the plant material into the solvent, and then physically separating the solvent from the plant material. The extracted compounds may then be separated from the solvent by evaporating the solvent in a heating step to provide a residue comprising extracted compounds. Alcohols, particularly methanol and ethanol, hydrocarbons, particularly hexane, ketones, particularly acetone, halogenated hydrocarbons, and ethers are typically used as solvents in these processes.
[0005] The step of heating plant material and/or solvent is a key feature of both the steam distillation and solvent extraction processes. Given that the desired activities of many plant compounds are destroyed or otherwise inactivated by heat (for example, a plant compound, polygodial is transformed at elevated temperatures into less active or inactive isomers; it may also react with other compounds at elevated temperatures), a limitation applies to the efficacy of these processes for extracting compounds from plant materials.
[0006] Solvents having a low boiling point, such as fluorocarbons are useful for extraction of compounds from plant material with minimal heating. However, these solvents are not environmentally friendly. Indeed some of the most effective fluorocarbon solvents for extraction of compounds from plant material, the hydrochlorofluorocarbons, are covered by ozone protection legislation that prescribes a well advanced phase-out schedule. Other hydrofluorocarbons are powerful greenhouse gases. Further they are less suitable for use as a solvent as they generally have a poor solvency power. Fluoroethers are too expensive to use as a solvent in a commercial application.
[0007] Derwent Abstract Accession Number 92-30466/37, Class B04, JP04210642-A (KAO CORP) 31 Jul. 1992 is directed to providing an extract that can be used in the treatment of cerebrovascular dementia and senile dementia including Alzheimers disease. According to the methods therein, the exact is obtained by extracting Hypercium erectum with a water or aqueous polar solvent such as glycerin, polyethylene glycol, hydrophilic surfactants and alcohols in water.
[0008] Derwent Abstract Accession Number 93-348326/44, Class B04.D21 JP 05255046-A (KAO CORP) 5 Oct. 1993 is directed to providing an extract that promotes growth of hair. According to the methods therein, the extract is obtained by extracting Gittiferae hyderiaceae with a variety of solvents.
[0009] GB 350,897 (Standard Oil Development Company) 15 Jun. 1931 is directed to fortifying or supplementing the insecticidal power of petroleum white oil with a plant extract having insecticidal properties. According to the methods therein, a plant extract is added to petroleum white oil, or otherwise a plant material is extracted in petroleum white oil.
[0010] Diemunsch A. M and Mathis C. (1983), Expo-Congr. Int. Technol. Pharm., 3 rd , vol. 2 pp 233-240. “Effects of aqueous glycol plant extracts on properties of aerosol foams” Publisher: Assoc. Pharm Galenique Ind., Chatenay-Malabry, Fr. (CAPLUS Abstract 1985: 600744) is directed to an aerosol foam including a propellant and liquid phase containing a surfactant, water and an aqueous glycol extract of a plant at 3-10% concentration. Propylene glycol, PEG 400 or diethylene glycol were used to extract plants such as Calendula, Hamamelis, ivy or mallow. According to the disclosure, the plant extracts improved the stability of foams, draining, collapse and the size or areoles.
[0011] Caron dos Anjos, Amaury (1967), Tribuna Farmaceutica, vo. 35(3/4), pp 53-62; 1968 36(1/4), pp 9-23; 1969 34(1), pp 49-59; 37(2), pp 135-9. “Use of surface-active (surfactant) substances in extraction processes” (CAPLUS abstract 1971:425300) is directed to liquid extraction of ipecac samples using non ionic and anionic surfactants.
[0012] DE 4205783 C1 (CASSELLA AG) 22 Jul. 1993 is directed to extracting compounds using an aqueous solvent.
[0013] Choi Maggie P. K. et al., (January 2003) J. Chrom. vol 983 pp 153-162 “Pressurized liquid extraction of active ingredients (ginsenosides) from medicinal plants using non-ionic surfactants” is directed to determining the effectiveness of employing an aqueous solution containing a common non-ionic surfactant (Triton X-100) as the extracting medium in pressurized liquid extraction (PLE) and ultrasonic-assisted extraction by comparing with conventional extraction solvents such as water and methanol as a function of experimental parameters such as temperature, pressure and concentration of the surfactant.
[0014] Huie C. W. (200) Anal Bioanal Chem vol. 373, pp 23-30. “A review of modern sample-preparation techniques for the extraction and analysis of medicinal plants” is a review of developments and applications of sample-preparation techniques for the extraction, clean-up and concentration of analytes from plants including solid-phase microextraction, supercritical-fluid extraction, pressurized-liquid extraction, microwave assisted extraction, solid phase extraction and surfactant mediate extraction.
[0015] WO2001/15534A1 (Australian Native Foods Resource Development Pty Ltd) 8 Mar. 2001 is directed to an insecticidal extract of Tasmannia stipitata. The extract is obtained by solvent extraction.
[0016] WO 01/07135 (Pisacane) 1 Feb. 2001 is directed to extracting materials from plants using solvents derivable from plants and especially terpenes and plant oils comprising terpenes such as rosemary oil and lavender oil, to obtain an insecticide. According to WO 01/07135, terpene-based solvents are required to extract a compound that, according to WO 01/07135, is a mixture of terpenes.
[0017] FR 2448 856 (SAPHYR SARL) 12 Sep. 1980 is directed to solvent extraction of compounds from plants.
[0018] There is a need for improved processes for extracting compounds that have useful activities from plant material.
SUMMARY OF THE INVENTION
[0019] In one aspect there is provided a method for extracting a compound from a plant material including:
[0020] providing an extractant including a fatty acid ester
contacting the extractant with a plant material to extract a compound from the plant material.
[0022] In another aspect there is provided a method for producing a spray formulation including:
[0023] providing an extractant including a non sulfonated triacyl glycerol and/or fatty acid ester
[0024] contacting the extractant with a plant material to form an extract of pestidicidal compounds from the plant material
[0025] optionally adding a pesticidally active oil to the formed extract, to produce a spray formulation.
[0026] In another aspect there is provided a spray formulation produced by the above described method.
[0027] In another aspect there is provided a method for producing a food additive or ingredient from a plant material including:
[0028] providing an extractant including a triacyl glycerol and/or fatty acid ester
[0029] contacting the extractant with a plant material to produce a food additive or ingredient from the plant material.
[0030] In another aspect there is provided a method for producing a pharmaceutical compound from a plant material including:
[0031] providing an extractant including a fatty acid ester
[0032] contacting the extractant with a plant material to produce a pharmaceutical compound from the plant material.
[0033] In another aspect there is provided a method for producing a cosmetic compound from a plant material including;
[0034] providing an extractant including a fatty acid ester
[0035] contacting the extractant with a plant material to produce a cosmetic compound from the plant material.
[0036] In another aspect there is provided a method for producing a reagent for use in a cleaning or disinfecting agent from a plant material including:
[0037] providing an extractant including a triacyl glycerol and/or fatty acid ester
[0038] contacting the extractant with a plant material to produce a reagent for use in a cleaning or disinfecting agent from a plant material.
DETAILED DESCRIPTION OF THE INVENTION
[0039] It has been surprisingly found that fatty acid esters can be used as an extractant, or in other words, a solvent, to extract a variety of useful compounds from plant material, especially plant material obtained from Australian native plant species.
[0040] Further it has been found that fatty acid esters provide a much higher solvency power to the extractant than would otherwise be provided by a triglyceride—containing oil or other oil. Accordingly, one key advantage of the method is that it provides for an improved selectivity for extraction of a compound of interest from a plant material.
[0041] Advantageously, it is possible to adjust the polarity of the extractant, and so select certain molecules for extraction from plant material in preference to others, by selecting particular types of fatty acid esters for use in the extractant.
[0042] Another key advantage of a higher solvency power is that an extract containing a high concentrate of a desired plant compound can be obtained. This is particularly important for those applications where downstream processing to provide for example a pesticide, food additive, pharmaceutical in cosmetic, tends to result in an undesirable dilution of compound in a plant extract.
[0043] Accordingly, in one aspect there is provided a method for extracting a compound from a plant material including:
[0044] providing an extractant including a fatty acid ester
[0045] contacting the extractant with a plant material to extract a compound from the plant material.
[0046] Typically the fatty acid ester is an ester selected from a group consisting of methyl, ethyl, propyl and butyl esters, although other fatty acid esters are within the scope of the invention. Further examples of fatty acid esters include pentyl, hexyl, heptyl, octyl, nonyl, decyl, undecyl and dodecyl esters.
[0047] It will be understood that the fatty acid ester for use in the extractant may be derived by any process for derivation of a fatty acid ester known to the skilled worker. For example, the fatty acid ester could be obtained by chemical synthesis from a precursor molecule, such as an alkyl. Alternatively, the fatty acid ester could be obtained by an enzymatic catalysis of pre-cursor molecules, such as occurs in the cleavage of fatty acyl chains from glycerol with lipase.
[0048] Another way of deriving the fatty acid ester for use in the extractant is by esterification of a triglyceride. For example, a triglyceride—containing oil, such as a vegetable or animal oil may be reacted with an alcohol such as methanol or ethanol in the presence of an alkaline catalyst to produce a mixture of fatty acids and glycerol. For example, canola oil is rich in oleic acid, generally containing greater than 60% and often 80% by weight oleic acid. This oleic acid, together with other fatty acids such as linolenic acid is present in canola in the form of triglycerides. When the oil is reacted with ethanol in the presence of an alkaline catalyst at about 50° C., a mixture of glycerol and fatty acid esters is formed. The glycerol is then removed, leaving a mixture rich in the ethyl ester of oleic acid.
[0049] Examples of fatty acid esters that may be obtained by esterification of vegetable oils include oleic acid, methyl ester; oleic acid, ethyl ester, and octadecanoic acid, butyl ester.
[0050] Examples of animal oils that could be used to derive fatty acid esters for use in the extractant include tallow, lard, wool grease, fish oils.
[0051] Examples of vegetable oils that could be used to derive fatty acid esters for use in extractant include soyabean, sunflower, safflower, canola, cotton, coconut, castor, corn, linseed, peanut palm, hemp, rice bran, tung, jojoba and olive oil.
[0052] The extractant may further include one or more of a polar oil, a non polar oil, and a surfactant. These are particularly useful for modifying the selectivity of the extractant for extraction of compounds in plant material.
[0053] Examples of polar oils include oils that contain one or more of triglycerides, terpenes and various oxygen containing compounds from terpenes such as alcohols, eg tepineol, ketones and camphors, limxonene and pinenes. Rosemary oil and lavender oil are examples of plant oils that contain terpenes. Other examples include tea tree, eucalyptus, orange, lemon, pine and cypress. Polar oils maybe useful in the extractant for extraction of polar compounds from plant material.
[0054] Examples of non polar oils include mineral oils, such as paraffin, white oil and the like. These may have a carbon chain length in the range of C12 to C28. Other examples of non polar oils include petroleum oils. Non polar oils may be useful in the extractant for extraction of non poplar compounds from plant material.
[0055] Typically, the polar and non polar oils are miscible with the fatty acid ester in the extractant.
[0056] Typically the surfactant is a non ionic surfactant, although other surfactants may be used. Non ionic surfactants are preferred especially where the extract is to be used in a stray formulation. Examples of non ionic surfactants include polyethylene glycol dioleate; 9-octadecanoic acid monoester with 1,2-propanediol; ethoxylated sorbitan trioleate; polyethylene glycol, monococonut ester; polyethylene glycol, monooleate; diethylene gycol, monooleate; glycerol monooleate, propylene glycol monooleate.
[0057] Typically, the extractant contains about 20 to 90% by weight of fatty acid esters and may contain 2-30% by weight of surfactant. One example is an extractant that contains 15% surfactant, 35% fatty acid esters and 50% non polar oil. Other examples of surfactants are those having components in the following ranges: 5-30% surfactant; 20-95% fatty acid esters; and 0-60% non polar oil.
[0058] The extractant may further include a solvent for solubilising certain molecules in the plant material, otherwise known as a second solvent. Examples of these solvents include ethanol, acetone, glycerol and hexane. These may comprise from about 5% to 50% by weight of the extractant.
[0059] Depending on the type of fatty acid ester and other components of the extractant, the plant material and the intended use of the compounds to be extracted from the plant material, the above ranges can be broader.
[0060] The method can be applied to a wide variety of plants including the following Autralian native plants:
[0061] Plants of the genus Callitris, in particular Callitris glaucophylla and Callitris endlicheri
[0062] Plants of the genus Tasmannia, in particular Tasmannia stipitata and Tasmannia lanceolata
[0063] Plants of the genus Leptospermum, in particular Leptospermum polygalifolium, Leptospermum petersonii, Leptosermum grandiflorum, Leptospermum neglectum, Leptospermum speciosum, Leptospermun brevipes, Leptospemum oreophiilum and Leptospermum gregarium.
[0064] Plants of the genus Prostanthera, in particular Prostanthera incisa and Prostanthera rotundifolia
[0065] Plants of the genus Rhodamnia, in particular Rhodamnia whiteana and Rhodamnia argentea
[0066] Plants of the genus Eremophila, in particular Eremophila mitchelii
[0067] Plants of the genus Melaleuca, in partcular Melaleuca uncinta, Melaleuca stypheloides, Melaleuca quinquenervia and Melaleuca altenifolia
[0068] Plants of the genus Phebalium, in particular Phebalium squameum and Phebalium dentatum
[0069] Plants of the genus Eucalyptus, in paricular Eucalyptus melanophloia and Ezcalyptus cloeziana
[0070] Plants of the genus Acacia, in particular Acacia howittii
[0071] Other plants including Cryptocaria cunninghamii, Austromyrtus dulcis, Backhousia citriodora and Backhousia anisata (also known as Anetholea anisata ) Pesticidally active compounds can, for example, also be extracted from the following plants not native to Australia;
[0072]
Polygoman hydropiper
[0073] Azadirachta indica (neem)
[0074] Chrysanthemum cinerariaefolium (pyrethrum)
[0075]
Ginkgo biloba
[0076] Nicotiana tabacum (tobacco)
[0077]
Derris elliptica
[0078]
Melia azadirachta
[0079]
Warburgia stuhlmannii
[0080]
Warburgia ugandensis
[0081]
Cannella winterana
[0082]
Drimys winteri
[0083]
Ailanthus altissima
[0084]
Glycosmis species
[0085]
Anabasis aphylia
[0086]
Ryania speciosa
[0087] The plant material may include the whole or any part of a plant, including leaves, flowers, trunks, butts and roots.
[0088] Typically the plant material is pre-treated so that it is in an appropriate physical form to facilitate the extraction of the compounds. Typically this includes treating the plant material to increase the surface area of the plant material, so that contact between the plant material and the extractant is increased. Commonly, some form of comminution process is used to reduce the particle size of the plant material. A particle size with a maximum dimension of 1-3 mm is normally adequate to achieve a good yield.
[0089] In some cases, the moisture content of the plant material is also reduced prior to contacting the plant material with the solvent. The reduction in moisture content should be carried out in a manner which minimises the loss of any volatile compounds desired to be extracted from the plant material, and minimises the destruction or inactivation of compounds desired to be extracted from the plant material.
[0090] Typically, the plant material is contacted with the solvent by passing the solvent past the plant material, or immersing the plant material in the solvent.
[0091] The extraction process may for example be cared out by the following procedure:
1. The solvent is placed in a vessel, preferably a vessel equipped with a high shear mixer. Where high shear agitation is used, it may not be necessary to reduce the particle size of the plant material prior to contacting the plant material with the solvent as this may occur during the mixing of the plant material and solvent. 2. Agitation of the solvent is commenced and the plant material is added progressively. 3. Optionally, if the compounds of interest are not heat sensitive, the mixture may be heated to enhance extraction rate and yield. 4. Agitation is continued until the plant material is dispersed and the extraction process is proceeding. Alternatively, agitation can be continued throughout the extraction process. 5. When a suitable amount of compounds have been extracted, the mixture is removed from the vessel and filtered or centrifuged to separate the solvent containing the extracted compounds from the plant material. 6. Additional extract may be obtained by subjecting the residue of plant material to pressure. 7. Beneficiation processes may be performed on the solvent containing the extracted compounds as necessary. For example, additional filtration steps can be performed, any moisture present in the solvent can be removed and/or the solvent can be passed through charcoal or activated clay to remove any colouring matter. Beneficiation can also involve the addition of other compounds, such as quinic, ascorbic or citric acid, to improve the stability of, and enhance the efficacy of, the extracted compounds, or the addition of antioxidants such as tocopherols to further enhance stability and product shelf life.
[0099] The above process can, for example, be used to extract the compound citral from leaves of Backhousia citriodora (lemon myrtle) which have been air dried and milled to a particle size of 2 mm, using a solvent consisting of a mixture of an esterified vegetable oil, a non polar oil and non-ionic surfactants. Citral is known to possess useful fungicidal properties.
[0100] In an alternative extraction process, the plant material may be contacted with the solvent by placing the plant material in contact with the solvent, and leaving the plant material in contact with the solvent for a few days (for example 2 to 4 days) to several weeks typically at room temperature. The amount of time the plant material is left in contact with the solvent will vary depending upon the particle size of the plant material, the temperature, the solvency power of the solvent and the desired yield of the extracted compounds.
[0101] The method is typically carried out at room temperatures (for example at about 10° C. to about 30° C.). However, if the compounds to be extracted are not heat sensitive, the methods can be carried out at higher temperatures.
[0102] Depending on the plant species, a variety of compounds can be extracted from plant material, including those that can be used as a pesticide, for example, an insecticide, termiticide, fungicide, bactericide etc. Examples of pesticidally active compounds that can be extracted from plant material using the method include, for example, citral, polygodial, anethole, azadirachtin, citronellal, alpha and beta pinene, caryophyllene, gualol, linalool pyrethrum, quinine, terpineol and vanillia.
[0103] An extract including pesticidal compounds obtained by the above described process may be added to a carrier or excipient to provide a pesticidal composition. A pesticidally active oil is a preferred excipient. A pesticidally active oil is an oil that repels or kills or otherwise affects pests, especially arthropod pests that cause damage to plants and/or transfer microorganisms that cause fungal or bacterial diseases to plants, and/or repels kills or otherwise adversely affects microorganisms that cause fungal or bacterial disease in plants. Paraffinic oils are an example of a pesticidally active oil.
[0104] The invention is particularly useful for providing a spray formulation. A spray formulation has a high quantity of a pesticidally active oil, and is typically sprayed onto a plant surface as an emulsion with water. Spray formulations typically comprise about 80% to 90% by weight of one or more pesticidally active oil(s) and about 2% to 20% by weight of one or more surfactant(s). The spray formulation may also contain a small amount, for example up to about 10% by weight of other components.
[0105] Thus, in another aspect there is provided a method for producing a spray formulation including:
[0106] providing an extractant including a non sulfonated triacyl glycerol and/or fatty acid ester
[0107] contacting the extractant with a plant material to form an extract of pestidicidal compounds from the plant material
[0108] optionally adding a pesticidally active oil to the formed extract, to produce a spray formulation.
[0109] In one particularly preferred embodiment, the extractant includes a pesticidally active oil. This is advantageous, because it avoids the dilution of the extracted compound that would otherwise occur when an extract is added to a pesticidally active oil to produce a spray formulation.
[0110] According to the method, a surfactant as described above may be added to the extractant before extraction of pesticidal compounds from plant material. Alternatively, the surfactant may be added after extraction of the pesticidal compounds.
[0111] Further, a polar and/or non polar oil and other solvents as described above may be added to the extractant before extraction, or they may be added after extraction.
[0112] In another aspect there is provided a spray formulation produced by the above described method. The spray formulation may contain by weight, 10% surfactants and 90% C16-C20 paraffinic oil. The oil may be applied to plants as a 1-2% emulsion in water.
[0113] The method of the invention also has utility in providing compounds with application as a pharmaceutical, a food additive, such as a colouring or flavouring agent, a cosmetic or fragrance or surface cleaning agent.
[0114] Thus, in another aspect there is provided a method for producing a food additive or ingredient from a plant material including:
[0115] providing an extractant including a triacyl glycerol and/or fatty acid ester
[0116] contacting the extractant with a plant material to produce a food additive or ingredient from the plant material.
[0117] As an example, the fruit of paprika contains a strongly coloured oleoresin. According to the invention, dried, milled paprika fruit can be contacted with an extractant of 20% esterified fatty acids and 80% sunflower oil. The extract obtained can be used as flavouring in foods and as a colorant in cosmetic preparations.
[0118] In another aspect there is provided a method for producing a pharmaceutical compound from a plant material including:
[0119] providing an extractant including a fatty, acid ester
[0120] contacting the extractant with a plant material to produce a pharmaceutical compound from the plant material.
[0121] As an example, the leaves of the plant Mebaleuca alternifolia, referred to as “tea tree” contain compounds used in pharmaceutical preparations. These compounds can be extracted by contacting the leaves of Melaleuca alternifolia with fatty acid esters and the extract obtained formulated into creams and lotions for topical application.
[0122] In another aspect there is provided a method for producing a cosmetic compound from a plant material including:
[0123] providing an extractant including a fatty acid ester
[0124] contacting the extractant with a plant material to produce a cosmetic compound from the plant material.
[0125] For example, the seeds of species of plants of the genus Echium are known to contain a fatty acid known as stearidonic acid. Stearidonic acid has use both as a nutritional supplement and has been shown to have anti-wrinkle properties when applied topically. The crushed seed of the plant Echium plantagieum can be contacted with fatty acid esters to extract a mixture of fatty acids including stearidonic acid. The extract obtained can be used as a nutitional supplement or formulated into creams and lotions for topical application.
[0126] In another aspect there is provided a method for producing a reagent for use in a cleaning or disinfecting agent from a plant material including:
[0127] providing an extractant including a triacyl glycerol and/or fatty acid ester
[0128] contacting the extractant with a plant material to produce a reagent for use in a cleaning or disinfecting agent from a plant material.
[0129] The invention is described below by reference to certain non-limiting examples. It will be appreciated by persons skilled in the art that numeous variations and/or modifications may be made to the invention as described in the examples without departing from the spirit or scope of the invention as broadly described. The following examples are, therefore, to be considered in all respects as illustrative and not restrictive.
EXAMPLES
Example 1
[0130] The following table shows a comparison between insecticidal efficacy of a solvent containing compounds extracted from plant material prepared by the method of the present invention using the product Hasten™ as the solvent (Victorian Chemicals Pty Ltd, 37-49 Appleton St, Richmond VIC 3121 Australia), versus a comparable extract produced using the solvent dimethyl sulphoxide. Hasten™ comprises ethylated canola oil blended with non-ionic surfactants. Dimethyl sulphoxide is a solvent which may be used in conventional solvent extractions of plant materials and is regarded as a powerful solvent.
[0131] In each case, dried leaves of Tasmannia stipitata from the same bulk sample were used. The same extraction process was carried out for each solvent. The solvent was placed in a vessel equipped with a high shear mixer. Agitation of the solvent was commenced and the plant material added progressively. Agitation was continued until the plant material was dispersed in the solvent. Agitation was then stopped and the mixture allowed to stand at room temperature for 24 hours. The plant material was then separated from the solvent by filtration.
[0132] The solvent containing the compounds extracted from the plant material was mixed with water at the percentage by volume listed in the table below (CONC %), and the mixture sprayed on a surface containing Two Spotted Mites and the mortality, feeding and egglaying of the mites was observed. The results are reported in the table below.
MEAN TWO SPOTTED MITE (TSM) MORTALITY PRODUCT CONC (%)* 24 h (%) COMMENTS Tasmannia Formed emulsion stipitata 0.5 62.7 No TSM eggs, no feeding extracted with esterfied 1.0 98.4 TSM convulsing vegetable oil and 2.0 100 Some phytoxicity surfactants 4.0 100 High phytoxicity 8.0 100 High phytoxicity Tasmannia Formed clear solution stipitata 0.5 3.9 Normal TSM feeding and extracted with egglaying dimethyl 1.0 2.8 Some TSM eggs, sulphoxide convulsing 2.0 66.2 No TSM eggs, no feeding 4.0 92.9 TSM convulsing, some phytoxicity 8.0 100 Phytoxicity *CONC (%) refers to the percentage by volume of the total extract (i.e. the compounds extracted from the plant material and the solvent) dispersed in water.
[0133] This example demonstrates that the solvent containing the extracted compounds produced by the method of the present invention had pesticidal activity against Two Spotted Mites.
Example 2
[0134] The method for extracting compounds from plant material described in Example 1 was repeated using the leaves of Tasmannia stipitata and the product “Hasten” as the solvent, to produce a solvent containing compounds extracted from the leaves of Tasmannia stipitata. The solvent containing the extracted compounds was in the form of a dilute dark green solution. The solvent containing the extracted compounds was combined 50% w/w with a C24 paraffinic spray oil to produce a clear, greenish coloured formulation. This formulation can be used as a spray formulation.
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The invention relates to extracting compounds from plant material and to formulations including compounds extracted from plant material, especially but not exclusively, spray formulations for controlling pests.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to U.S. Provisional Patent Application No. 61/984,655 filed Apr. 25, 2014 and entitled “WEAPON WITH REDIRECTED LIGHTING BEAM,” the respective disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention is directed to a lighting device for a firearm that uses a mirror to redirect the light beam along the side or top of the firearm and preferably parallel to the longitudinal axis of the firearm's barrel.
BACKGROUND OF THE INVENTION
As used herein, “light source” means any source of light, such as a laser or flashlight. “Laser” means any form of laser light source that projects a beam of laser light suitable for weapon alignment or sighting purposes.
It is known to utilize a light beam, such as a beam from a laser, as a sighting aid for weapons, particularly guns. A laser beam is preferred because it has comparatively high intensity, can be focused into a narrow beam with a small divergence angle so it produces a small, bright spot on a target. When the light beam and gun bore are properly aligned, the bullet (or other projectile) will hit on or very close to the location of the spot produced by the laser on the target.
It is, however, difficult to mount lasers to small guns, particularly small revolvers, that can be concealed in a pocket or purse. The problem is that the laser and associated mechanisms are too large for the gun. Consequently, they interfere with the operation of the gun and/or make the gun more difficult to conceal.
The disclosures of the following references that are not inconsistent with this disclosure are incorporated herein by reference: U.S. Pat. No. 8,127,485 entitled “GUN WITH MOUNTED SIGHTING DEVICE” to Moore et al., U.S. Pat. No. 8,312,665 entitled “SIDE-MOUNTED LIGHTING DEVICE” to Moore et al. and U.S. patent application Ser. No. 13/707,312 entitled “SIGHTING DEVICE REPLICATING SHOTGUN PATTERN SPREAD” to Moore et al.
SUMMARY OF THE INVENTION
Embodiments of the present invention are mountable on a gun, particularly a small revolver, without interfering with the operation of the gun or affecting the ability to conceal the gun. Disclosed is a laser (or other light source) that is disposed in a grip of the gun. In the embodiments shown, the laser module is mounted at an angle of 0°-45° from the vertical axis and is not positioned so that it is in line with the longitudinal axis of the gun barrel. A mirror is positioned adjacent the end of the laser module that emits light, and the mirror redirects the light, preferably parallel to the longitudinal axis of the gun barrel to enable a user to sight the gun.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded view of a lighting device according to aspects of the invention showing how the device fits onto part of the gun grip.
FIG. 2 is a rear, perspective, partially-exploded view of a gun with the lighting device of FIG. 1 not yet assembled on the gun.
FIG. 3 is a rear view of a gun including a lighting device in accordance with FIGS. 1 and 2 .
FIG. 4 is a bottom view of the gun according to FIG. 3 .
FIG. 5 is a front view of the gun according to FIG. 3 .
FIG. 6 is a left-side, perspective view of a gun according to FIG. 3 .
FIG. 7 is a left-side view of a gun according to FIG. 3 .
FIG. 8 is a right-side, perspective view of a gun according to FIG. 3 .
FIG. 9 is a right-side view of a gun according to FIG. 3 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Turning now to the Figures where the purpose is to describe preferred embodiments of the invention and not limit same, FIG. 1 is an exploded view of a first section 100 of a grip according to aspects of the invention. First section, or grip portion, 100 is preferably made of plastic, metal or a combination thereof and most preferably of injection-molded plastic, and has a main body portion 100 A.
In this embodiment, a housing 12 includes a cavity 12 B, and is integrally formed as part of first section 100 (although it could be connected to first section 100 in any suitable manner). The cavity 12 B of housing 12 is dimensioned to receive laser module 14 . In this embodiment module 14 has a first end 14 A through which laser light is emitted.
A module nose ball 16 fits over laser module 14 and allows the module 14 to pivot so its position can be adjusted, thereby adjusting the direction of the light beam emitted from end 14 A. Housing 12 has an outer wall with two openings 12 A, each of which receive a set screw 18 (or other suitable device) that can be tightened or loosened in an opening 12 A to alter the position of laser module 14 in housing 12 . As shown, the openings 12 A and corresponding set screws 18 are positioned 90° apart and are in a axial alignment approximately perpendicular to the longitudinal axis of laser module 14 when module 14 is positioned in cavity 12 B of housing 12 .
Before laser module 14 is positioned in housing 12 , module nose ball 16 , a biasing spring 20 , and a spring bias insert 22 are positioned on module 14 . The combination of spring 20 and spring bias insert 22 bias the laser module 14 towards the two set screws 18 . In this manner, as one or more of set screws 18 is loosened the laser module 14 will move in the direction of that set screw(s). Spring 20 may also provide a negative electrical contact for laser module 14 .
A mirror 24 fits into a slot 26 integrally formed as part of first section 100 . In the embodiment shown, mirror 24 is stationary, but it could be adjustable to adjust, or help adjust, the travel of the light beam emitted from first end 14 A. In the embodiment shown, mirror 24 deflects the travel of light emitted from end 14 A of laser module 14 so that the light preferably travels along the side or top of a gun, preferably parallel to the axis of the gun barrel, to properly sight a target. Light reflected from the mirror 26 passes through a lens 28 . Lens 28 fits onto first section 100 and is transparent, colored, or translucent, and could be a diffraction lens. For example, lens 28 may alter the laser light existing the internal laser module, such as to create a pattern of light, such as a cross hair, vertical beam, horizontal beam, circular pattern of light beams, or circular pattern of light beams with a light beam in the center of the circumference of the circular pattern.
A back cover 30 is positioned onto first section 100 to retain mirror 24 , laser module 14 , laser module nose ball, spring 20 and spring bias insert 22 in place and protect them. Cover 30 can be attached to first section main body 100 A in any suitable fashion but is preferably snap fit into place by projections 32 being received in openings 34 . Alternatively, screws could be passed through openings 34 and projections 32 could be threaded or contain screw bosses to retain the screws.
A button, or switch, 40 is preferably a momentary switch that is pressure activated by a user squeezing it. Most preferably a user must apply at least 2, at least 3, or at least 5, pounds of force to activate switch 40 because in that manner a user would not accidentally activate the switch 40 simply by grasping the grip. Alternatively, another type of switch may be used and the switch may be at any suitable location. A PCB 44 is positioned in the back of switch 40 . When switch 40 is activated, PCB 44 is moved and it connects the power source 60 to the laser module 14 to emit light from end 14 A.
Switch 40 and PCB 44 fit into slot 42 of main body 100 A, and there is a corresponding slot (shown in FIG. 2 ) on second section 200 , so that when sections 100 and 200 are connected through the gun handle frame 502 , they hold the switch 40 and PCB 44 in place.
A button press tab 46 is retained in slot 48 . The power source 60 comprises three 3V photo cell batteries 62 , although any suitable power source (preferably a light and portable 3V source) can be used. The power source (batteries 62 ) in this embodiment are retained in a tube 64 that is preferably cylindrical with a cavity 66 and a mounting board 68 that communicates with PCB 44 when switch 40 is activated.
An insulation sleeve 70 is positioned in cavity 66 and batteries 62 are positioned inside the sleeve 70 . Contact board 68 is positioned on frame 74 of main body 100 A and is preferably retained in place by screws 76 being positioned through openings 68 A and threaded into openings 74 A. Insulation sleeve 70 is positioned in cavity 66 and batteries 62 are placed inside sleeve 70 . Then spring 72 is placed inside of cavity 66 to bias batteries 62 towards board 68 , and a cap 76 is placed on the end of battery tube 64 , preferably by threading it onto the end of tube 64 , or by any other suitable attachment method.
FIG. 2 shows an exploded view of a grip according to the invention prior to it being mounted to the handle frame 502 of a revolver 500 . In this figure first section 100 is fully assembled. Handle frame 502 has an opening 504 through which portions of first section 100 and second section 200 are pressed together and/or are connected.
Sections 100 and 200 are pressed against the respective sides of handle frame 502 . Screw boss 202 aligns with opening 80 , sleeve 204 aligns with slot 42 to retain switch 40 , and flange 206 aligns with and presses against flange 41 to create a seal between first section 100 and second section 200 . A fastener 120 is passed through opening 80 and threadingly received in screw boss 202 to retain first section 100 and second section 200 in place, although any suitable attachment mechanism may be used. When attached, the cap 76 of battery tube 64 aligns with an opening 210 in second section 200 , which can best be seen in FIGS. 6 and 7 . In this manner, the battery tube 64 can be easily accessed to remove and replace batteries 62 , although any suitable method of battery removal and replacement may be utilized.
In the embodiment shown, the laser module 14 and first section 100 are on the right-hand side of the gun 500 . Alternatively, they could be on the left-hand side with first section 100 and second section 200 replaced with respective sections that have the same structures, but reversed.
FIG. 3 is a rear view of device 10 . Gun 500 is a revolver with a barrel 506 , a cylinder 508 for holding bullets (not shown), an optional back plate 510 (not shown in all figures) that retains the bullets in the cylinder, a trigger guard 512 , a trigger 514 , a hammer 516 and a mechanical front site 518 .
As shown in FIGS. 3-9 , the housing 12 and lens 28 are positioned completely behind the trigger guard 512 , trigger 14 and cylinder 508 so as to not interfere with the operation of the gun 500 . In this embodiment lens 28 is positioned entirely above cylinder 508 so that the light emitted from lens 28 will not be blocked or partially blocked by the cylinder. The housing 12 only extends outward to approximately a position directly even with the outward edge of the cylinder, or by no more than 1/32″, 1/16″, ⅛″ or ¼″ beyond that position. Also, the lens 28 is entirely preferably about 1/32″, 1/16″, ⅛″, or ¼″ above the cylinder.
Having thus described some embodiments of the invention, other variations and embodiments that do not depart from the spirit of the invention will become apparent to those skilled in the art. The scope of the present invention is thus not limited to any particular embodiment, but is instead set forth in the appended claims and the legal equivalents thereof. Unless expressly stated in the written description or claims, the steps of any method recited in the claims may be performed in any order capable of yielding the desired result.
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A lighting device for a gun, which is preferably a small revolver having a total length of less than 6″, is positioned in a grip (or handle portion) of the gun and includes a mirror to redirect the light beam along the side or top of the gun and preferably parallel to the axis of the gun barrel.
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BACKGROUND OF THE INVENTION
The present invention comprises an apparatus for applying a liquid coating to a workpiece, particularly an irregularly shaped workpiece. Although the apparatus could be used to apply many different types of coatings, e.g. paints, rust resistant coatings, oils, etc., it is particularly useful where the coating is something such as paint. While the apparatus could apply such a coating to any irregularly shaped workpiece, it is particularly useful for applying such coatings to elongate workpieces, and even more specifically, to workpieces such as joists or trusses or other elongated structural members, which are comprised of a number of interconnected components such as struts and beams, with open spaces therebetween. With such structures, it is difficult to completely coat all sides of the numerous components which make up the elongate members, and particularly to ensure that the coating gets into all the crevices, recesses and the like formed in and between those components, in a quick, preferably automated, operation.
Dip tanks might appear to be an obvious way of painting such complex, irregular structures. However, they are undesirable because more environmentally friendly, water-based paints do not work well in dip-type applications, and thus organic-based paints must be used. Organic-based paints, especially in dip tanks having openings large enough to introduce a workpiece such as a joist or truss, pose an environmental problem, since undesirably large volumes of hazardous organics can evaporate into the surrounding environment. Accordingly, workers must wear protective clothing, and the area must be ventilated. Even then, undesirable amounts of organic vapors are often released into the atmosphere. Additionally, dipped type structures tend to leave paint drippings in the surrounding locations to the dip tanks, on trucks being loaded with the workpieces, etc.
SUMMARY OF THE INVENTION
Apparatus according to the present invention for applying a liquid coating to a workpiece, particularly an irregularly shaped workpiece, comprises a housing defining a coating chamber having an inlet and an exit. A conveyor system or the like conveys the workpiece into the inlet, through the coating chamber, and out the exit. A manifold comprising a plurality of sprayheads are mounted in the coating chamber, in generally surrounding relationship to the workpiece. These spray heads are preferably arranged at various angles with respect to the workpiece for spraying the liquid coating toward the workpiece from a number of different directions. This is one of the features of the invention which helps to ensure that all sides and crevices of the components of the irregularly shaped workpiece are coated.
A plenum structure is connected to the housing and defines a plenum chamber communicating with the coating chamber. A vacuum system, usually associated with the plenum chamber, draws a vacuum thereon and on the coating chamber. This vacuum not only further helps to ensure dispersion of the coating around the various sides of the parts of the workpiece, but also prevents the coating from flowing freely out into the working environment through the inlet and exit of the coating chamber.
A means, e.g. a blower system, adjacent the exit of the coating chamber blows pressurized gas, e.g. air, into the coating chamber toward the workpiece. This helps to remove excess coating from the workpiece as it exits the coating chamber and creates a turbulence in the coating chamber which further helps to ensure coating of all sides of the components of the workpiece.
The blower system also helps to ensure such complete coating in another way, again most especially when combined with the vacuum. Specifically, when high pressure air is blown against one side of a component of the workpiece, e.g. a strut of a truss, a low pressure area is created on the opposite side, so that the coating is literally sucked around the component into the low pressure area e.g., from the one side to the other.
In preferred embodiments, the coating is delivered by suitable piping or the like from the discharge end of a respective pump, collected through a drain in the coating chamber, and delivered back to a closed chamber communicating with the intake of that pump. This helps to minimize the volume of coating potentially exposed to the working environment at any given time, and thus to minimize harmful emissions.
Furthermore, baffle-like structures associated with the plenum chamber tend to minimize the amount of coating which will eventually reach the vacuum pump, and thus be discharged to the atmosphere.
Various objects, features, and advantages of the invention will be made apparent by the following detailed description, the drawings, and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevational view of an apparatus according to the present invention, viewed from the exit end of the coating chamber, with certain parts broken away to show interior structure.
FIG. 2 is an enlarged, detailed cross-sectional view taken on the line 2--2 of FIG. 1.
FIG. 3 is a view taken on the line 3--3 of FIG. 2.
FIG. 4 is a view taken along the line 4--4 of FIG. 2.
FIG. 5 is a view taken along the line 5--5 of FIG. 2.
DETAILED DESCRIPTION
Referring now to the drawings, there is shown an apparatus according to the present invention for applying paint to elongate joists, such as that indicated in phantom at 10. The exemplary joist 10 includes a pair of parallel angle irons 12 interconnected by angularly disposed struts 14. To fully coat the joist 10 with paint, the paint must be applied to all sides of each of the angle irons 12 and struts 14, including the surfaces of such defining, for example, the crevices between the angle irons 12 and between the juncture of the angle irons 12 and struts 14.
The apparatus for so applying the paint includes a rectangular housing 16 defining a coating chamber 18 and having a generally rectangular inlet 20 and an aligned exit 22 in respective opposite walls of the housing 16. The housing 16 is supported on the floor of the work area by a base structure 24.
Preferably, the conveyor system of the apparatus includes two point contact slat-type conveyors: an inlet conveyor 26, whose upper surface is aligned with housing inlet 20, and an exit conveyor 28, whose upper surface is aligned with exit opening 22. Because the distance between the opposed ends of the conveyors 26 and 28, and therefore the distance between the openings 20 and 22, is less than the length of the workpiece 10 to be treated, and because the workpiece 10 is rigid, the workpiece 10 need not be directly contacted or supported within the chamber 18. Thus, all surfaces of the section of the workpiece 10 within the chamber 18 are exposed for potential coating by paint, in a manner to be described more fully below.
The paint to be applied to the workpiece 10 is contained in a reservoir or tank 30 located near the housing 16. A stirrer 32 may be provided within the reservoir or tank 30 and rotated by a motor 34. A paint pump 36 e.g. an air operated diaphragm pump, is mounted on or near the tank 30. Standard air processing equipment, i.e. a filter-regulator-lubricator assemblage 37, is associated with pump 30. A line 38 is connected to the intake side of pump 36, passing through a filter 40 and a valve 42 and communicating thence with the bottom of tank 30.
The discharge side of pump 36 discharges into another line 44 connected to a pipe 46 which passes through a wall of housing 16 and communicates with a rectangular circuit of piping 48. The shape of the rectangle defined by circuit 48 is similar to and aligned with, but slightly larger than, those of the inlet and exit 20 and 22. Thus, the circuit 48 surrounds the workpiece 10, and the workpiece 10, in turn, passes through the rectangle defined by circuit 48 as it is conveyed through the coating chamber 18.
Circuit 48 carries and communicates with a plurality of sprayheads 50, all of which are directed generally inwardly, i.e. toward the locus of the workpiece 10, but preferably at various angles, so as to spray paint toward the workpiece 10 from a number of different directions.
Housing 16 has a drain 52 in the bottom thereof which is connected via a line 54 and a valve 56 with the bottom of tank 30. Thus, the paint is recycled in a nearly closed circuit, and is exposed to the atmosphere only in small amounts, i.e. only such amounts as are present in the coating chamber 18, at any given time.
The varying angles of the sprayheads 50 help to ensure coating of all surfaces of workpiece 10, and the nearly closed circuit in which the paint is recycled helps to minimize the emission of potentially hazardous materials to the working environment. Both of these ends are further enhanced by another sub system of the apparatus.
Specifically, a plenum structure is "connected to" the housing 16 (which, for present purposes, may be construed to include structures in which the housing and plenum structure form one continuous body). The plenum structure defines a plenum chamber communicating with the coating chamber 18. In the embodiment shown, the plenum structure comprises several sections. A central section 58 extends directly upwardly from the top of the housing 16. This section 58 is the part of the plenum structure which directly communicates with the coating chamber 18, and it so communicates with and extends from that chamber 18 in a direction transverse to the path of movement of the workpiece 10.
The plenum structure further comprises a blind lateral section 60 which extends from section 58 in a lateral direction transverse to both the path of movement of workpiece 10 and the vertical orientation of section 58. Another lateral plenum section 62 extends from the opposite side of section 58 from section 60. Section 62, in turn, communicates with a cylindrical, vertically oriented section 64, the lower end of which, in turn, communicates with the suction side of a vacuum pump 66.
Pump 66 draws a vacuum on the entire plenum chamber defined by the interiors of the hollow sections 58-64 and hence the coating chamber 18, which vacuum, among other things, helps to prevent the coating from escaping directly into the working environment through the inlet 20 and the exit 22.
A baffle 68, which is generally horizontal, but inclined slightly, extends into the portion of the plenum chamber defined by section 58 directly above the coating chamber 18. Thus, coating or gasses therefrom being evacuated by pump 66 are forced to follow a tortuous path upwardly from the coating chamber 18, then to the right (as viewed in FIG. 1) into plenum section 60, then to the left through the upper part of section 58 and through section 62, and finally downwardly through section 64. Baffle 68 also provides a surface on which particles of paint may impinge and fall back down into chamber 18 where they may be collected by the paint recycling system described above. Mounted within plenum section 64 is an auger-shaped structure 70 which provides additional surfaces on which paint may disengage and be separated from the gasses (air) being evacuated, so that there is little, if any, paint in the air which is exhausted to atmosphere by pump 66.
A compressor 72 compresses air and discharges it, e.g. at about 10 psi, into a line 74 which leads toward the exit 22 of the coating chamber 18 and there, via a manifold 75, branches into four lines 74a-74d. Each of these lines 74a-74d communicates with a respective elongate pipe or "air knife" 76a-76d, each of which has a number of openings 78 e.g. slots, holes, etc. spaced along its length. The pipes 76a-76d are disposed just outwardly of the exit 22, and each of the pipes parallels a respective edge of the exit 22, and also overlaps that edge, so that its openings 78 open into the chamber 18. It will thus be seen that the air or other compressed gas flowing through the air knives 76a-76d serve to generate four converging sheet or planes of compressed air blowing across the workpiece. Thus, virtually any surface of the workpiece which faces the exit 22 from virtually any angle will be subjected to the high pressure air flow from one of the sheets or planes of air.
The compressed air thus blown into the chamber 18 at the truss 10 removes excess paint from the truss 10 as it exits chamber 10. The compressed air also creates a turbulence in the coating chamber 18 which further assists in ensuring complete coating of all surfaces of the joist 10, and the vacuum drawn by pump 66 may further augment this. In addition, this compressed air is directed toward the joist 10, as indicated by the arrows A, and, again augmented by the presence of a vacuum, creates low pressure areas on the opposite sides of angle irons 12 and struts 14 from those against which the air is blowing. These low pressure areas tend to literally suck paint thereinto, thereby further ensuring complete coating.
As shown in FIG. 1, one of the tubes 76a (air knife) is movably mounted on an arm 80 pivoted to plenum section 58 so that it can be moved toward or away from the other tubes 76b-d to adjust for different sizes of workpiece. To accommodate this movement, line 74a, as shown, is flexible.
It will thus be seen that the apparatus of the present invention utilizes three methods to ensure complete coating of workpieces, particularly irregularly shaped workpieces such as joists. First of all, the apparatus provides direct application of paint or similar coating from the paint manifold comprised of circuit 48 and associated spray heads 50 onto the surface of the workpiece. Secondly, since the paint or coating is subjected to the turbulent flow of the air knives or compressed air being blown into the chamber across the workpiece, coating of otherwise hard to reach surfaces is enhanced. Lastly, since voids, recesses and the like formed at interconnection of the components of the workpiece on the leeward side of the workpiece are subjected to a low pressure area caused by the impinging air blown into the coating chamber 18 and across the workpiece via the air knives, the surfaces which define those voids, recess etc. are subjected to paint or coating which is literally sucked into the low pressure area. Thus, the apparatus effectively coats all surfaces on the workpiece.
Numerous modifications of the embodiments described above are within the skill of the art and the scope of the invention, the latter being limited only by the claims which follow.
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Apparatus for applying a liquid coating to an irregularly shaped workpiece comprises a housing defining a coating chamber having an inlet and an exit. A conveyor system is adapted to convey the workpiece into the inlet, through the coating chamber, and out the exit. A plurality of sprayheads are mounted in the coating chamber, in generally surrounding relation to the workpiece, and arranged at various angles with respect to the workpiece, for spraying the liquid coating toward the workpiece. A plenum structure is connected to the housing and defines a plenum chamber communicating with the coating chamber. A vacuum system is associated with the plenum chamber for drawing a vacuum thereon. A blower system adjacent the exit of the coating chamber blows air into the coating chamber toward the workpiece.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. Ser. No. 12/846,103 filed Jul. 29, 2010, which is a continuation of U.S. Ser. No. 11/923,339 filed Oct. 24, 2007, issued as U.S. Pat. No. 7,789,858, which is a continuation of International Application No. PCT/CH2006/000221, filed 24 Apr. 2006, which claims the benefit of priority from Swiss Application No. 724/05, filed 25 Apr. 2005, the subject matter of both are hereby incorporated by reference in their entirety.
BACKGROUND
[0002] The present invention relates to devices for injecting, infusing, administering, delivering or dispensing substances, and to methods of making and using such devices. More particularly, the invention relates to a device for administering a fluid product, in particular a device for administering a fluid product at a continuous delivery rate.
[0003] For various diseases, such as for example diabetes, it can be necessary to continuously administer a particular amount of a fluid medicine to a patient. Various systems for this purpose are known, which enable the medicine to be supplied continuously over an extended period of time. The period of time of administration, the amount of the product administered within the period of time, the repetition rate of a number of consecutive administrations and possible extra deliveries can usually be set in such systems. Administering devices are known which can be connected to an external product container for a fluid medicine and, as soon as said container is empty, can be connected to the next container. Accordingly, such administering systems can be reused. Furthermore, implantable devices are also known which can be inserted into a patient's body tissue and are coupled to an external product container by means of a connector. Various possibilities exist for driving such systems, such as for example using gravity, various drive systems in the form of mechanical springs or hydraulic drives. In order to regulate the flow rate, the flow amount from the product container for the fluid medicine is usually limited at the outlet. Simple valves, clamps or programmable electronic devices can be used for this.
[0004] U.S. Pat. No. 5,788,673 discloses an infusion system in which a drive unit is combined with a conventional syringe. The syringe includes a product container that accommodates the fluid product, and a drive piston rod by which a product stopper within the product container can be advanced. The fluid product can be discharged from the syringe through an outlet opposite the product stopper. At the opening, the syringe also includes a valve for regulating the fluid flow. The drive unit comprises a chamber for a liquid medium, a second chamber which communicates with the first chamber, a piston and a valve system. A spring force can be exerted on the piston that conveys the liquid medium from the first chamber to the second chamber and back. The valve system controls the movement of the piston in the forward or backward direction and thus the discharge of the fluid product from the syringe.
[0005] The known systems for administering fluid medicines are generally designed to be reused. They therefore exhibit a complex construction comprising a large number of components and are therefore costly to manufacture. Furthermore, the patient or an assistant has to learn how to change the administering device from an empty product container to a new, full product container. If handled incorrectly, it is for example possible for an incorrect dosage to be administered to a patient.
SUMMARY
[0006] The present invention to provides a device for administering a fluid medicine, which is easy to handle, can be initiated in a few operating steps, ensures reliable functioning and ensures a continuous discharge at a constant medicine rate.
[0007] In addition, according to the invention, an administering device for continuously administering a fluid medicine, which is suitable for being used once, is provided.
[0008] The administering device of the present invention, according to certain embodiments, is configured to administer a fluid product, primarily a therapeutic medicine such as for example insulin. However, the administering device may also be used for administering other fluid products, which are to be administered into a body tissue. The administering device comprises a product container which accommodates the product to be administered and comprises an opening for discharging the product from the product container at its front, distal end, and a product stopper at its rear, proximal end. A typical ampoule, such as is used for injection syringes or pens for quickly administering small dosages and/or injection shots, may be used as the product container. The product stopper may be moved relative to the product container and seals the proximal end of the container in a fluid-proof seal.
[0009] According to various embodiments, the administering device also comprises a fluid reservoir for a drive fluid and a drive means that acts on the fluid reservoir. The drive fluid may be a non-compressible liquid. At least one of the fluid reservoir and the product container should be a non-compressible chamber; and in some implementations, the fluid reservoir and the product container are each formed by a non-compressible chamber. A non-compressible chamber may include solid, stable walls in a suitable geometric shape. The fluid reservoir includes a drive stopper, which transfers the action of the drive means onto the drive fluid within the fluid reservoir and charges the fluid reservoir with pressure. Various systems, including known systems, can be used as the drive means, such as for example mechanical springs, hydraulic drives or gas drives. A mechanical spring, for example a mechanical pressure spring, may be used as the drive means in the present invention.
[0010] A pressure chamber may be connected to the product stopper of the product container, according to some implementations. The pressure chamber may be formed by one or more walls of the product container, the product stopper and a closed end of the container. The closed end of the pressure chamber may be formed by a casing wall, such as by means of a seal. Accordingly, the pressure chamber may be at least partially or completely arranged within the product container. According to certain embodiments, the product container may be subdivided by the product stopper into a chamber for the product and the pressure chamber. A fluid connection is provided between the fluid reservoir and the pressure chamber, and the drive fluid may be conveyed out of the fluid reservoir, through the fluid connection, into the pressure chamber.
[0011] In accordance with the present invention, the drive means acts on the fluid reservoir in such a way that the pressure chamber is charged with pressure via the fluid connection, said pressure acting on the product stopper and thus discharging the product from the product container. Although for certain embodiments, a casing of the device forms a compartment for a product container, which is or can be accommodated in it, the casing, in other embodiments, may accommodate one or more or all of the components of the administering device in order to directly form the product container.
[0012] According to one embodiment of the present invention, the fluid connection exhibits a first, resting state in which it is closed, i.e. in which no drive fluid can flow from the fluid reservoir to the pressure chamber. A connecting means is provided in the administering device and moves the fluid connection from the first, closed, resting state to a second, open, administering state in which the fluid connection is open to the drive fluid. The connecting means therefore serves to connect the fluid reservoir containing the drive fluid to the pressure chamber connected to the product stopper of the product container. If, in the second, open state, the drive means then acts on the fluid reservoir or drive stopper of the fluid reservoir, the drive fluid is conveyed through the fluid connection.
[0013] According to certain embodiments, the drive means is biased in the administering device in the resting state, i.e. the drive means constantly acts on the fluid reservoir or drive stopper. The drive means may be held in the biased position by a holding and/or securing device. The holding device may include known locking systems in which, for example, the drive stopper of the drive means is held in place by a movable latch or stopper, for example, which may be removed or released by a push button or slider in order to release the locking system. In another embodiment, the holding device may be formed by the seal of the fluid connection, for example by means of the sealing membrane. The bias on the drive means may then be released by opening the fluid connection. In alternative embodiments, the drive means may only be tensed when the fluid connection is opened or after the fluid connection has been opened.
[0014] According to one embodiment, a casing is provided which accommodates the product container, the fluid reservoir, the pressure chamber and the fluid connection. In some implementations, a pre-assembled unit may be provided that includes the casing, the fluid reservoir, the pressure chamber and the fluid connection, and comprises a compartment into which the product container can be inserted when necessary, for example shortly before the required administration. Accordingly, in order to use the administering device in accordance with the invention, only the product container need be inserted into the casing compartment. When the product container is inserted into the casing, the connecting means may be activated, such that the fluid connection is moved from the resting state to the administrating state. If the drive means is already biased within the casing, the drive means may be triggered with the aid of the product container and the pressure chamber consequently charged with pressure. The pressure force begins to act on the drive stopper in such a way that the stopper is shifted relative to the fluid reservoir, and drive fluid flows from the fluid reservoir into the pressure chamber, wherein a pressure is built up in the pressure chamber which acts on the product stopper, and the fluid product is therefore discharged through the opening in the product container.
[0015] According to certain embodiments, the fluid connection comprises a sealing membrane for sealing it. The fluid connection may be moved from the closed state to the open state by penetrating the sealing membrane, and connecting means then exhibits a flow cross-section through which product can flow. For example, a tube-like hollow element, such as a hollow needle, conduit, capillary, or passage may serve as a connecting means and penetrate and/or pierce the sealing membrane of the fluid connection. Accordingly, the connecting means can form a part of the fluid connection. It is for example possible on the one hand for the fluid connection to be formed by a narrow capillary which feeds from the fluid reservoir, is conveyed within the casing towards the product container compartment, and is sealed with the sealing membrane at the end, which feeds into the compartment, and on the other for the fluid connection to be formed from the hollow needle of the connecting element. The pressure in the pressure chamber may be defined by dimensioning the fluid connection. The pressure in the pressure chamber is dependent on the size of the outlet area and/or the diameter of the fluid connection and on the length of the capillary. It is independent of the pressure of the drive element on the fluid reservoir or drive stopper. This implementation enables pressure fluctuations in the drive means to be equalized. In some implementations, the fluid connection may have a diameter of about 0.5 to about 3 mm. It is also possible to arrange the fluid connection within the casing in a looping, spiralling, meandering or labyrinthine manner. This enables the fluid connection path between the fluid space and the pressure chamber to be lengthened and the pressure in the pressure chamber to be regulated by selecting a particular fluid connection length.
[0016] In a particular embodiment, the connecting means forms a partial section of the fluid connection in the state in which the fluid reservoir is connected to the product reservoir. In another embodiment, the connecting means alone forms the fluid connection in the connected state. Alternatively, the hollow element, which penetrates the sealing membrane, may form the fluid connection. For example, the sealing membrane may form a wall of the fluid reservoir thus allowing the hollow element to form a fluid connection with the fluid in the reservoir once the hollow element penetrates the membrane.
[0017] The administering device of the present invention may be configured to be a single-use device. A user inserts the product container into the casing comprising the other components of the device, which in some embodiments, connects the pressure chamber to the fluid reservoir. Inserting may also simultaneously trigger administration. No further hand operations are necessary in order to initiate the device or regulate the administering amount. Once administration is complete, i.e. as soon as the product container is empty, the connection to the patient can be interrupted and the whole administering apparatus disposed of.
[0018] In alternative embodiments, the administering device may be reusable. If, for example, the drive means is only tensed or charged when the product container is inserted or after the product container has been inserted or by inserting the product container, the administering device may be repeatedly charged and used by again inserting a product container. The drive means can also be biased before a new product container is inserted.
[0019] According to some implementations, the connecting means is activated by the product stopper when the product container is inserted into the casing. As described, this can move the fluid connection from a closed state to an open state. It is, however, also simultaneously possible to form the connecting means in such a way that the product stopper within the product container is shifted in the distal direction of the product container when the container is inserted into the casing. The connecting means may advance the product stopper by a distance which allows the product container to be vented. This only requires a small movement by the product stopper within the product container, which may remove possible air pockets within the product container through the front opening of the product container, and the administering device may be directly connected to an administering conduit, which leads to the patient. The frictional force to overcome the snug fit of the product stopper in the product container is preferably greater than the force required to move the fluid connection from the closed state to the open state, i.e. to pierce the sealing membrane. When the product container is inserted, the membrane is then pierced first and the fluid connection between the fluid reservoir and the pressure chamber thus opened, and then the product stopper is distally shifted by a venting distance. The pressure building up in the pressure chamber immediately begins to advance the product stopper and thus administer the product.
[0020] In accordance with another aspect of the invention, a method is claimed, according to which, in a device for administering, and in some instances, for continuously administering, a fluid product, inserting a product container triggers the administration and/or a venting process for venting a product container.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 depicts a first embodiment of an administering apparatus in accordance with the present invention, in a resting state;
[0022] FIG. 2 depicts the administering device according to FIG. 1 , in an administering state;
[0023] FIG. 3 depicts the administering device during administration; and
[0024] FIG. 4 depicts a second embodiment of an administering device in accordance with the present invention.
DETAILED DESCRIPTION
[0025] FIG. 1 shows a first embodiment of an administering device in accordance with the present invention. The administering device comprises a casing ( 1 ) in which a product container in the form of an ampoule ( 2 ), a fluid reservoir ( 3 ), a drive means in the form of a spring ( 4 ), a fluid connection ( 5 ) and a connecting means ( 6 ) are accommodated. Water may be used as the drive fluid, the physical parameters of which are well known. However, it is also possible to use other fluids that differ in viscosity. The ampoule ( 2 ) is filled with the fluid product ( 7 ). Ampoule ( 2 ) comprises an opening ( 8 ) at its front, distal end and a product stopper ( 9 ) at its rear, proximal end. In FIG. 1 , the ampoule ( 2 ) has not yet been completely inserted into the casing ( 1 ) and the administering device is in its resting state.
[0026] In the embodiment in accordance with FIGS. 1 to 3 , the ampoule ( 2 ) and the fluid reservoir ( 3 ) together with the spring ( 4 ) are arranged next to each other, offset in parallel, within the casing. The fluid connection ( 5 ) forms a transverse connection within the casing ( 1 ). This arrangement enables the overall length of the administering device to be kept small. The fluid connection ( 5 ) is spread over the area of the casing ( 1 ) in a number of loops (not shown).
[0027] The connecting means ( 6 ) is provided within the casing ( 1 ) as a movable element. The connecting means ( 6 ) can be moved along the longitudinal axis of the ampoule and is arranged between the ampoule ( 2 ) and the fluid connection ( 5 ) and comprises a hollow needle ( 10 ). The fluid connection ( 5 ) is permanently connected to the fluid reservoir ( 3 ) at one end and sealed by a sealing membrane ( 13 ) at the other end. The hollow needle ( 10 ) of the connecting element ( 6 ) is arranged opposite the sealing membrane ( 13 ) at an axially small distance. In addition, the connecting means ( 6 ) is provided centrally relative to the product stopper ( 9 ).
[0028] The system consisting of the spring ( 4 ), the fluid reservoir ( 3 ), the fluid connection ( 5 ) and the sealing membrane ( 13 ) forms a sealed fluid system in the resting state. In this embodiment, the spring ( 4 ) is already biased within the system. Even in the resting state, it therefore exerts a pressure on the fluid reservoir comprising the drive fluid. The sealing membrane ( 13 ) is therefore embodied such that it withstands this pressure.
[0029] In FIG. 2 , the ampoule ( 2 ) has been completely inserted into the casing ( 1 ) of the administering device. When the ampoule ( 2 ) is completely inserted into the casing ( 1 ), the product stopper ( 9 ) comes to rest on the connecting means ( 6 ). If the ampoule ( 2 ) is inserted further, the product stopper ( 9 ) initially presses the connecting element ( 6 ) towards the sealing membrane ( 13 ) until the hollow needle ( 10 ) pierces the membrane and the connecting element ( 6 ) abuts a shift stopper ( 14 ), which may be formed by the casing or may be affixed to the casing. The connecting means ( 6 ) cannot then be shifted further in the direction of the longitudinal axis of the ampoule, relative to the casing. The ampoule ( 2 ) can, however, still be inserted further in the insertion direction, into the casing ( 1 ), wherein the product stopper ( 9 ), which abuts the connecting means ( 6 ), is shifted relative to the wall of the ampoule ( 2 ). This shift path of the product stopper ( 9 ) reduces the volume within the ampoule ( 2 ) for the fluid product, and the ampoule is vented and/or a small amount of the fluid product is discharged from the ampoule ( 2 ) through the opening ( 8 ). A small shift path of a few millimetres is sufficient for the venting process. The ampoule ( 2 ) is inserted into the casing ( 1 ) until it also abuts a shift stopper ( 14 ) within the casing, wherein the circumference of the proximal end of the ampoule ( 2 ) abuts a seal ( 11 ). In order to secure the ampoule ( 2 ) within the casing ( 1 ), a latching or locking mechanism can advantageously be provided.
[0030] The administering device is then in an administering state in which a fluid connection ( 5 ) is provided by piercing the sealing membrane ( 13 ) in the open state.
[0031] FIG. 3 shows the administering device in the administering state, after a certain product amount has been administered. The pressure chamber ( 12 ), which is formed by the wall of the ampoule ( 2 ), the product stopper ( 9 ), the connecting means ( 6 ) and the seal ( 11 ), can be seen in FIG. 3 . Since the spring ( 4 ) is mounted, already biased, within the casing, opening the fluid connection ( 5 ) causes the drive fluid to flow from the fluid reservoir ( 3 ), through the fluid connection ( 5 ) through the hollow needle ( 10 ), into the pressure chamber ( 12 ). The flow amount through the fluid connection ( 5 ) depends on the diameter and length of the fluid connection ( 5 ). The pressure exerted on the product stopper ( 9 ) is therefore independent of variants in the pressure of the drive element, i.e. the spring ( 4 ). The discharge rate of the administering device can be defined by selecting the diameter and length of the fluid connection ( 5 ) and then remains constant throughout the administration of the fluid product ( 7 ) from the ampoule ( 2 ).
[0032] As soon as the product stopper ( 9 ) has reached the front, distal end of the ampoule ( 2 ), the ampoule is completely empty and the administering device can be disposed of.
[0033] FIG. 4 shows another embodiment of the present invention, in which the ampoule ( 2 ), the fluid reservoir ( 3 ) and the drive spring ( 4 ) are arranged along the same axis within the casing ( 1 ). In this embodiment, the administering device exhibits a slim, elongated shape. Its mode of operation corresponds to the functioning of the embodiment from FIGS. 1 to 3 .
[0034] In this second example embodiment, the connecting means ( 6 ), i.e. its hollow needle ( 10 ), alone forms the entire fluid connection ( 5 ) between the fluid reservoir ( 3 ) and the pressure chamber on the proximal side of the product stopper ( 9 ).
[0035] Embodiments of the present invention, including preferred embodiments, have been presented for the purpose of illustration and description. They are not intended to be exhaustive or to limit the invention to the precise forms and steps disclosed. The embodiments were chosen and described to provide the best illustration of the principles of the invention and the practical application thereof, and to enable one of ordinary skill in the art to utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated. All such modifications and variations are within the scope of the invention as determined by the appended claims when interpreted in accordance with the breadth they are fairly, legally, and equitably entitled.
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An administering device for a fluid product includes a product receptacle that accommodates the product to be administered, a fluid reservoir for a driving fluid, a driving means, a product chamber, and a fluid connection. The product receptacle includes an opening at a forward end and a product stopper at a rear end. The driving means acts upon the fluid reservoir, the pressure chamber adjoins the product stopper while the fluid connection is located between the fluid reservoir and the pressure chamber, and the driving means acts upon the fluid reservoir in such a way that the pressure chamber is impinged upon by pressure which affects the product stopper and the product is discharged from the product receptacle.
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CROSS REFERENCES TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 62/326,481, filed 22 Apr. 2016.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable.
REFERENCE TO SEQUENTIAL LISTING, ETC.
[0003] Not applicable.
BACKGROUND OF THE INVENTION
Field of Invention
[0004] The present invention relates to hinges and, in particular, to a device and method for restoring function and operation to malfunctioning or inoperable hinges by using stretchable resilient material. At least in one embodiment, for example, the present invention relates to the repair (i.e. restoration of function and operation) of hinges in vehicles. [The words/phrases “repair” and “restoration of function and operation” are herein used interchangeably.]
Description of the Related Art
[0005] Many hinges are made as a part of a larger compartment and cannot be replaced without replacing the entire compartment.
[0006] Many hinges today are made of non-durable materials and break after repeated use. For example, some hinges are made with holes through hard plastic, making the hinge leaves, and a metal rod as a hinge pin. The plastic has a tendency to break with repeated use. In addition, in order to be self-closing, many hinges have a second mechanism such as a torsion spring.
[0007] There are many automotive parts made of plastic that open and close via a hinge. Sometimes the hinge can be removed separately from the compartment while other times the hinge is part of the compartment. Many times these hinges are not reliable over time. Standard practice is to remove and replace the hinge or replace the entire compartment housing the hinge. In either case, the cost of labor and parts to repair or replace those hinges or the compartment which incorporates the hinge is expensive.
[0008] In one embodiment, my device and method could be used to restore function and operation to a malfunctioning, inoperable, partially broken hinge pin spring and/or partially broken hinge interlocking leaf or leaves on a variety of vehicles. For example, in one embodiment my device and method can be used to restore function and operation to a malfunctioning, inoperable, partially broken hinge pin spring and/or partially broken hinge interlocking leaf or leaves on a Mercedes Benz SL, years 2003-2012, R230 body style [hereinafter Mercedes Benz SL], right and/or left rear edge cover trim panel (passenger side/driver side) [hereinafter trim panel].
[0009] The Mercedes Benz SL, as well as other vehicles, has a trim panel that has a non-movable portion [hereinafter panel] and a hinged portion [hereinafter flap]. The flap is designed to open when the convertible hard-top is up and close when the convertible hard top is stored in the trunk.
[0010] When the panel hinge leaf/leaves or spring used to close the hinged door is partially broken or inoperable, the conventional way of restoring function and operation to the malfunctioning, inoperable, partially broken hinge pin spring and/or partially broken hinge interlocking leaf or leaves of the trim panel is to remove and replace the entire trim panel, because the hinge leaves are incorporated as part of the panel and not sold as a separate part.
[0011] In one embodiment, the invention restores function and operation to a malfunctioning, inoperable, partially broken hinge pin spring and/or partially broken hinge interlocking leaf or leaves of the Mercedes Benz SL as well as other vehicles.
[0012] In one embodiment, the invention restores the function and operation of the Mercedes Benz SL trim panel without removing or replacing any parts that comprise the trim panel.
[0013] It should be understood that the detailed description and specific examples, while indicating exemplary embodiments of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention
SUMMARY OF THE INVENTION
[0014] It is the primary objective of an embodiment of this present invention to restore function and operation of all types of hinges by attaching stretchable resilient material to the hinge without the necessity of replacing the hinge or, in the case where a hinge is incorporated as a part within a unit or compartment, without the necessity of replacing the unit or compartment in order to replace the hinge.
[0015] An embodiment of the present invention results in hinges becoming self-closing, regardless of whether the hinges were previously self-closing.
[0016] It is an objective of an embodiment of this invention to increase the life of hinges at a minimal cost.
[0017] It is an objective of an embodiment of this invention to serve as an alternative to removing inoperable or malfunctioning hinges.
[0018] It is an objective of an embodiment of this invention to serve as an alternative to removing units, compartments or the like, in order to replace or repair an inoperable or malfunctioning hinge.
[0019] An embodiment of this invention attaches in any manner resilient material to a malfunctioning or inoperable hinge, making the hinge fully operational and making the hinge self-closing, whether or not the hinge was previously self-closing.
[0020] An embodiment of this present invention utilizes self-adhesive resilient material.
[0021] An embodiment of this invention uses self-adhesive double-sided tape applied to one side of the resilient material.
[0022] An embodiment of this invention makes the resilient material self-adhesive by coating one side of the resilient material with a bonding solution or adhesive, or by using brackets, screws, rivets or channels to attach the resilient material.
[0023] An embodiment of this invention uses self-adhesive resilient material adapted to be stretched in the direction of its width, i.e. the direction that is perpendicular to the interlocking hinge pin leaf/leaves. By adhering the resilient material to a malfunctioning or inoperable hinge, one embodiment of this invention makes the hinge fully operational and makes the hinge self-closing, whether or not the hinge was self-closing prior to
[0024] In one embodiment of this invention the amount of tension is dependent upon the particular amount of tension necessary to effect closure.
[0025] In one embodiment of this invention, as one skilled in the art knows, the pounds of force resistance and thickness and dimensions of the resilient material are dependent on the particular size and specification of the hinge leafs and hinge plates.
[0026] In one embodiment of this invention, one of more components as described herein may be provided as a repair kit.
[0027] Various materials may be used in addition to those components described herein to enhance functionality of the invention.
[0028] In another embodiment, my device and method could be used to restore function and operation of a non-operable, partially broken hinge pin spring on doors and closures.
[0029] Referring to the device in FIG. 1 and FIG. 2 , as well as the mirror images of FIG. 1 and FIG. 2 (not shown), and the method of repair, one embodiment of this invention, repairs the function and operation of the Mercedes Benz SL trim panel without removing or replacing any parts that comprise the trim panel.
[0030] The above summary of the present invention is not intended to describe each embodiment or every implementation of the present invention. One or more features of each of the embodiments may be modified and still perform the same functionality or additional functionality without departing from the scope of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Many aspects of the present embodiments can be better understood with reference to the following drawings. The components in the drawing are not necessarily drawn to scale, the emphasis instead being placed upon illustrating the principles of the present embodiments. It is to be understood that the drawings are to be used for the purposes of illustration only and not as a definition of the limits of the preferred embodiments. Various modifications of the illustrative embodiments, as well as additional embodiments of the invention, will be apparent to persons skilled in the art upon reference to this description.
[0032] In the preferred embodiment of this invention:
[0033] FIG. 1 is a top view of the face of the cut to size and shape flexible resilient material that does not adhere or attach to any portion of the hinge that is being repaired.
[0034] FIG. 2 is the bottom view of the face of the cut to size and shape flexible resilient material with the double sided tape adhered to the cut to size and shape flexible resilient material and is later adhered to the hinge that is being repaired.
[0035] Referring to FIG. 2 , sections A and C show the face of the cut flexible resilient material specific locations where the double sided tape is applied to the flexible resilient material. Referring to FIG. 2 , sections A and C of the flexible resilient material will adhere to a hinge that is to be repaired.
[0036] Referring to FIG. 2 , section A depicts one side of the double sided tape attached to a section of the flexible resilient material. When the hinge is being repaired, Section A will attach parallel to the hinge's interlocking hinge pin leaves without attaching to the interlocking hinge pin leaves.
[0037] Referring to FIG. 2 , B depicts the middle section of the flexible resilient material where no double sided tape is applied.
[0038] Referring to FIG. 2 , sections C show where additional double sided tape is attached to the flexible resilient material. When the function and operation of a hinge is being restored, sections C will attach parallel to but without adhering to the interlocking hinge pin leaves.
[0039] Referring to FIG. 1 and FIG. 2 , mirror images of FIG. 1 and FIG. 2 (not shown) may be used as appropriate.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0040] The following description of certain exemplary embodiments is exemplary in nature and is not intended to limit the invention, its application, or uses. The components in the drawings are not necessarily drawn to scale.
[0041] Referring to FIG. 1 , this invention is made by cutting a sheet of flexible resilient material to a specific size and shape as determined by measuring the hinge to be repaired as follows:
[0042] The length of the flexible resilient material is best determined by measuring the inoperable hinge's length and shape parallel to the interlocking hinge pin leaves.
[0043] The width of the flexible resilient material is best determined by measuring the entire width of the inoperable hinge perpendicular to the hinge pin leaves and subtracting the measured distance of the interlocking hinge pin leaves.
[0044] The width of the flexible resilient material will be shorter than the entire width of the hinge. It is best that the flexible material is shorter in width than the hinge's width so that when flexible resilient material is stretched and adhered to the hinge being repaired, the flexible resilient material applies enough pressure over the interlocking hinge pin leaves to hold the interlocking hinge pin leaves together and make the hinge self-closing.
[0045] FIG. 1 shows the top side of the cut to size and shape flexible resilient material. FIG. 1 , the top side, does not adhere or attach to any portion of the hinge or anything else.
[0046] FIG. 2 is the opposite side of FIG. 1 . FIG. 2 is the cut to size and shape flexible resilient material with the double sided tape adhered to sections A and C. FIG. 2 side of the invention will attach to the inoperable hinge, making the inoperable hinge operable.
[0047] There are many methods for attaching the flexible resilient material to the partially broken or inoperable hinge. Methods include, but are not limited to: double sided tape, adhesive products, mechanical methods, screws, rivets, brackets, tracks, etc. The lengths and widths of adhesives, such as double sided tape, may be varied depending on the need.
[0048] In the preferred embodiment the flexible resilient material is attached to the inoperable hinge by using double sided tape, which has peelable liners protecting the tape.
[0049] FIG. 2 , sections A and C show specific locations where the double sided tape is positioned. The double sided tape in this preferred embodiment cover the surfaces of sections A and C.
[0050] FIG. 2 , section A shows the location where one side of the double sided tape is attached to the flexible resilient material. Peel the liner from one side of the double sided tape exposing the adhesive of one side of the double sided tape. Attach the adhesive side of the double sided tape to section A, of FIG. 2 . The double sided tape in the preferred embodiment covers the surface of section A. When the hinge repair is complete, section A will be parallel to the inoperable hinge's interlocking hinge pin leaves.
[0051] FIG. 2 , section B shows a middle section of the flexible resilient material. Tape is not applied to Section B.
[0052] FIG. 2 , sections C show the location where double sided tape is attached to sections C of the flexible resilient material. Peel the liner from one side of the double sided tape exposing the adhesive of one side of the double sided tape. Attach the adhesive side of the double sided tape to sections C, of FIG. 2 . When the hinge repair is complete, sections C will be parallel to the hinge's interlocking hinge pin leaves.
[0053] The next step is to attach the flexible resilient material to the inoperable hinge.
[0054] Remove the protective peelable liner from the double sided tape, exposing the adhesive portion of the double side tape from the double sided tape shown in FIG. 2 , section A.
[0055] Adhere the flexible resilient material to the inoperable hinge perpendicular to the inoperable hinge's interlocking hinge pin.
[0056] Remove the protective peelable liner from the double sided tape, exposing the adhesive portion of the double side tape from the double sided tape shown in FIG. 2 , sections C. Stretch the resilient material over and parallel to the interlocking hinge pin leaves and, while stretched, adhere the flexible resilient material as shown in FIG. 2 , sections C, to the other entire length of the hinge without attaching it to the interlocking hinge pin leaves.
[0057] In one embodiment, FIG. 1 and FIG. 2 device and method restore the function and operation of the Mercedes Benz SL passenger side trim panel without removing or replacing any parts that comprise the trim panel.
[0058] In one embodiment, the mirror images of FIG. 1 and FIG. 2 (not shown) device and method restore the function and operation of the Mercedes Benz SL driver side trim panel without removing or replacing any parts that comprise the trim panel.
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A device and method that relate to restoring function and operation to a malfunctioning or inoperable hinges by attaching a flexible resilient material to the malfunctioning or inoperable hinge when the function and/or operation of a partially broken hinge pin spring and/or the function and/or operation of a partially broken hinge interlocking leaf or leaves cause the hinge to malfunction when the hinge is used to connect an out-swinging closure to a fixed structure.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 14/050,768, filed Oct. 10, 2013, and entitled “METHOD FOR ENSURING MEDIA STREAM SECURITY IN IP MULTIMEDIA SUB-SYSTEM,” which issued as U.S. Pat. No. 9,167,422 on Oct. 20, 2015, which is a continuation of U.S. patent application Ser. No. 11/774,271, filed Jul. 6, 2007, and entitled “METHOD FOR ENSURING MEDIA STREAM SECURITY IN IP MULTIMEDIA SUB-SYSTEM,” which issued as U.S. Pat. No. 8,582,766 on Nov. 12, 2013, which is a continuation of PCT/CN2005/002429, filed Dec. 31, 2005, and entitled “A METHOD FOR ENSURING THE SAFETY OF THE MEDIA-FLOW IN IP MULTIMEDIA SUB-SYSTEM,” and which published as WO/2006/072212 on Jul. 13, 2006, and which claims priority to CN 200510000097.7, filed Jan. 7, 2005. The entire contents of each of the foregoing applications are expressly incorporated herein by reference in their entireties.
FIELD OF THE INVENTION
The present invention relates to the media stream security technologies in communication networks, and in particular, to a method for ensuring media stream security in an IP Multimedia Subsystem (IMS) network.
BACKGROUND OF THE INVENTION
As a core session control layer in the fixed and mobile networks, the IMS has become a main topic in the art. Many specifications related to the IMS have been defined in the Third Generation Partnership Project (3GPP) and Telecommunications and Internet Converged Services and Protocols for Advanced Networking (TISPAN) standards, which concerns network architecture, interface, protocol, etc. Particularly, security is an important consideration in the 3GPP and TISPAN. In the current specifications, the IMS network is split into an access domain and a network domain in view of the security, and security specifications are defined for the access domain and the network domain respectively. FIG. 1 shows a security model for the IMS network, in which interfaces requiring the security are defined. Although having been described in detail in the specifications, these interfaces are defined only in terms of the control plane of the IMS network, i.e. how to ensure the security of the session protocols in the IMS network, instead of how to ensure the security of the media plane in the IMS network. In fact, the security of the media plane is also very important. Otherwise, media streams may be tampered or eavesdropped during the conversation of the subscribers, which results in degradation of the quality of service for the subscribers or leakage of confidential information.
Usually, an approach for protecting the media streams in the IMS network comprises: a Real-time Transfer Protocol (RTP) proxy is introduced into the architecture of the IMS network; keys are shared between User Equipment (UE) and the RTP proxy through the Generic Bootstrapping Architecture (GBA, which is also a generic authentication and key assignment model defined in the 3GPP specifications); confidentiality and integrity of the media streams are secured between the UE and the RTP proxy through the shared keys, achieving the security of the media streams in the access domain; and the security of the media streams in the network domain may be achieved in two ways: the first one is that no protection is provided between the RTP proxies, if the network is trustable or secure in the network domain; and the other one is that the media streams between the RTP proxies are protected through the IP_Security (IPSec) Encapsulating Security Payload (ESP) protocol under the security mechanism in the 3GPP IMS network domain.
FIG. 2 shows an architecture of the GBA model and FIG. 3 illustrates an application of the GBA model to key assignment for the media streams. In the application, the Session Initiation Protocol (SIP) server (such as Proxy Call Session Control Function (P-CSCF) defined in the 3GPP IMS network) and the RTP proxy are taken as a whole, i.e. a Network Application Function (NAF) entity in the GBA. The SIP server acquires from the Bootstrapping Server Function (BSF) a key shared between the NAF and an SIP client The key shared between the NAF and an SIP client is stored in the BSF. The SIP server then sends the key to the RTP proxy via Is interface. Thus, the key for media stream security is shared between the. SIP client and the RTP proxy.
In the GBA model, both the NAF and the BSF are logical function entities. All Application Servers (ASs) and even the Call Session Control Function (CSCF) entity may be used as an NAF to acquire a key shared with the UE in the GBA processes. Likewise, the BSF may be implemented by any device, such as a CSCF entity, a Home Subscriber Server (HSS), an Authentication, Authorization and Accounting (AAA) server, and a web portal, etc.
SUMMARY OF THE INVENTION
Embodiments of the invention provide a method for enhancing end-to-end media stream security in an IMS network, thereby solving the problem that the security and the quality of service for an end-to-end media stream are impaired as a result of many times of encryption and decryption required for the media stream.
The embodiments of the invention provide the following technical solutions.
A method for ensuring media stream security in an IP Multimedia Subsystem network, including the following steps:
assigning, by a first network device of a first User Equipment; UE, an end-to-end media stream security key for the first UE, and transmitting the end-to-end media stream security key to a second network device of a second UE; encrypting the end-to-end media stream security key using a first session key shared with the first UE, and transmitting the encrypted end-to-end media stream security key to the first UE via a first session message; encrypting the end-to-end media stream security key using a second session key shared with the second UE, and transmitting the encrypted end-to-end media stream security key to the second UE via a second session message; encrypting or decrypting a media stream, by at least one of the first UE or the second UE, using the end-to-end media stream security key.
Optionally,
the first UE is a calling UE, the second UE is a called UE; or the first UE is a called UE, the second UE is a calling UE.
The first network device may be a Service-Call Session Control Function, S-CSCF, of the first UE, the end-to-end media stream security key is transmitted by the first network device to a Proxy-Call Session Control Function, P-CSCF, of the first UE, and is encrypted and transmitted to the first UE by the P-CSCF of the first UE, the second network device may be an S-CSCF of the second UE, the end-to-end media stream security key is transmitted by the second network device to a P-CSCF of the second UE, and is encrypted and transmitted to the second UE by the P-CSCF of the second UE.
Alternatively, the first network device may be an Application Sewer, AS, of the first UE, the end-to-end media stream security key is encrypted and transmitted to the first UE by the AS of the first UE, the second network device may be an AS of the second UE, the end-to-end media stream security key is encrypted and transmitted to the second UE by the AS of the second UE.
The method may also include: specifying a media stream security capability between the first UE and the second UE by the first network device or the second network device according to security capabilities provided by the first UE and the second UE.
The method may also include: transmitting the assigned end-to-end media stream security key by the first network device or the second network device to a listening device listening to the encrypted media stream by decrypting the media stream using the end-to-end media stream security key.
The media stream security key is transmitted between the first network device and the second network device, in plain text in a session message in a network domain, or through a security mechanism in the IMS network domain.
The end-to-end media stream security key may be a cipher key or an integrity key.
Another embodiment of the invention provides a system for ensuring media stream security in an IP Multimedia Subsystem network, including: a first network device of a first User Equipment, hereinafter referred to as UE, for assigning an end-to-end media stream security key for the first UE, transmitting the media stream security key to a second network device of a second UE, encrypting the end-to-end media stream security key using a first session key shared with the first UE, and transmitting the encrypted end-to-end media stream security key to the first UE via a first session message; and a second network device of the second UE, for encrypting the end-to-end media stream security key using a second session key shared with the second UE, and transmitting the encrypted end-to-end media stream security key to the second UE via a second session message.
Yet another embodiment of the invention provides a system for ensuring media stream security in an IP Multimedia Subsystem network, including: a first network device of a first User Equipment, hereinafter referred to as UE, for assigning an end-to-end media stream security key for the first UE, and transmitting the media stream security key to a second network device of a second UE; a third network device of the first UE, for encrypting the end-to-end media stream security key using a first session key shared with the first UE, and transmitting the encrypted end-to-end media stream security key to the first UE via a first session message; and a fourth network device of the second UE, for encrypting the end-to-end media stream security key using a second session key shared with the second UE, and transmitting the encrypted end-to-end media stream security key to the second UE via a second session message.
In the method according to an embodiment of the invention, the media stream security key is assigned for the calling UE and the called UE by an application server acting as a network device, or a network device such as a CSCF, etc. The media stream needs to be encrypted or decrypted only once by the calling UE or called UE during the transmission of the media stream. Therefore, there is no substantial affect on the performance of the IMS network device, and the quality of service for the media stream can be ensured easily. In terms of security, a key becomes invalid upon completion of the session because the key is assigned dynamically during each session. In this way, a very high security may be ensured.
Because the security capabilities of the calling UE and the called UE may be negotiated in an interactive way while negotiating the media stream security key, an end-to-end security association may be established dynamically between the calling UE and the called UE.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram illustrating an IMS network security model in the related art;
FIG. 2 is a schematic diagram illustrating a GBA model in the related art;
FIG. 3 illustrates an application of the GBA in media stream security;
FIGS. 4 and 5 are flow charts illustrating embodiments of the invention.
DETAILED DESCRIPTION OF THE EMBODIMENTS
In FIG. 1 , the Call Session Control Function (CSCF) entities defined in the IMS network are operable to implement functions such as controlling, routing, etc. during call and session. Proxy-Call Session Control Function (P-CSCF), Service-Call Session Control Function (S-CSCF) and Interrogating-Call Session Control Function (I-CSCF) are distinguished from one another for the purpose of implementing different functions. Particularly, the Proxy-Call Session Control Function (P-CSCF) is used for access of a User Equipment (UE), all UEs access the network via the P-CSCF; the Service-Call Session Control Function (S-CSCF) provides the core functions, such as session controlling, routing, etc.; and the Interrogating-Call Session Control Function (I-CSCF) is used for selection of S-CSCF and intercommunications among different operators or the networks at different regions, as well as network shielding function and the like. For example, the I-CSCF may be used as the only egress for different operators. The Application Server (AS) in the IMS network provides services for users, for example, various applications such as call waiting, conference, instant message, etc. Different applications may be located in different ASs. The S-CSCF entity is responsible for forwarding a session request from a user to different ASs, depending on different services info.
In an embodiment of the invention, to reduce the times of encryption and decryption on the media stream during transmission, a security association is established directly between the Session Initiation Protocol (SIP) client, i.e. the calling UE, and the called UE, such that the media stream is protected through a direct encryption and decryption between the calling UE and the called UE, thus achieving the end-to-end media stream security.
An end-to-end media stream security key may be negotiated in two ways. The first one is that the end-to-end media stream security key is assigned by a CSCF entity. The second one is that the end-to-end media stream security key is assigned by an Application Server (AS). The end-to-end media stream security key is a Cipher Key (CK) or an Integrity Key (IK).
Referring to FIG. 4 , the end-to-end media stream security is implemented in the first way as follows.
Block 1 : during the process of establishing a session, an S-CSCF among the CSCF entities with which the calling UE or the called UE is registered determines whether the media streams for this session need to be protected, according to subscription information of the UE, or an instruction from the AS regarding protection of the media stream in a session message. If protection is necessary, the S-CSCF assigns the end-to-end media security key according to the protection way specified in the subscription information. If the specified protection way is by encryption, an end-to-end Cipher Key (CK) is assigned. If the specified protection way is by integrity protection, an end-to-end Integrity Key (IK) is assigned.
Block 2 : after assigning the end-to-end media stream security key, the S-CSCF of the calling UE or the called UE transmits the end-to-end media stream security key to an S-CSCF of the opposite UE in a session message of the network domain. The S-CSCF of the calling UE transmits the end-to-end media stream security key to the P-CSCF of the calling UE by using a session message, and the S-CSCF of the called UE transmits the end-to-end media stream security key to the P-CSCF of the called UE by using a session message.
If it is assumed to be trustable or secure in the network domain, the end-to-end media stream security key may be transmitted in plain text (i.e. the key is not protected by encryption at all). Practically, the end-to-end media stream security key may be transmitted through the security mechanism in the IMS network domain.
Block 3 : the P-CSCF to which the calling UE or the called UE accesses encrypts the end-to-end media stream security key using a cipher key shared between the calling UE or called UE and the P-CSCF, the cipher key is obtained by the UE through negotiation during the process of registering Authentication and Key Agreement (AKA).
Block 4 : the P-CSCF to which the calling UE access transmits the encrypted media stream security key to the calling UE in cipher text by using a session message, and the P-CSCF to which the called UE access transmits the encrypted media stream security key to the called UE in cipher text by using a session message, so as to ensure that the end-to-end media stream security key is transmitted securely in the insecure access-side network. Either of the calling UE or called UE obtains the end-to-end media stream security key between the calling UE and called UE by decrypting the encrypted media stream security key using the session key (i.e., the cipher key) shared with the P-CSCF.
Block 5 : media stream messages are transmitted between the calling UE and the called UE after being encrypted or integrity-protected using the end-to-end media stream security key according to the Security Association (SA) negotiated during the process of establishing the session, thus achieving the end-to-end media stream security.
If only the media stream from the calling UE to the called UE needs to be protected, the calling UE encrypts or integrity-protects the media stream using the end-to-end media stream security key before sending the media stream to the called UE, while the called UE authenticates and decrypts the received media stream using the end-to-end media stream security key, and does not encrypt the media stream to be sent. If only the media stream from the called UE to the calling UE needs to be protected, the process is similar as the above. If both the media streams sent by the calling UE and the called UE need to be protected, both of the two parties encrypt or integrity-protect the media streams using the end-to-end media stream security key before sending the media streams, and decrypt the received media streams using the end-to-end media stream security key.
Referring to FIG. 5 , the end-to-end media stream security is implemented in the second way as follows.
Before initiating a session, each of the calling UE and called UE negotiates a security key to be shared between each of the calling UE and the called UE and Network Application Function (NAF) during the process of registering and authenticating AKA, in combination with the GBA procedures. When initiating or responding to a session request subsequently, the calling UE or the called UE carries a Bootstrapping procedure Transaction identifier (B-TID) in a session message or during interaction with the NAF (alternatively, an application layer security key may be negotiated between the UE and NAF in another way, the detailed description of which is not limited to the above).
Block 10 : during the process of establishing a session, an Application Server (AS) of the calling UE or the called UE determines whether the media streams for this session need to be protected, according to a requirement of the service or the subscription information of the user. If the protection is needed, the AS assigns the end-to-end media security key according to the protection way specified in the subscription information or the requirement of the service. If the specified protection way is by encryption, the end-to-end Cipher Key (CK) is assigned. If the specified protection way is by integrity protection, the end-to-end Integrity Key (IK) is assigned.
Block 11 : the AS assigning the end-to-end media stream security key encrypts the end-to-end media stream security key through the security mechanism in the network domain and transmits the encrypted media stream security key by using a session message to an AS of the opposite UE.
If the network domain is assumed to be trustable, the key may be transmitted in plain text in the network domain.
Block 12 : the AS of the calling UE requests an application layer security key shared between the NAF and the calling UE from the Bootstrapping Server Function (BSF) according to the Bootstrapping procedure Transaction identifier (B-TID) carried in the session message from the calling UE, the AS of the called UE requests an application layer security key shared between the NAF and the called UE from the Bootstrapping Server Function (BSF) according to the Bootstrapping procedure Transaction identifier (B-TID) carried in the session message from the called UE.
The application layer security key may also be stored in a Home Subscriber Server (HSS). In this case, the AS of either of the calling UE or the called UE acquires the key from the HSS according to the B-TID carried in the session message from the UE (practically, the application layer key may be assigned between the AS and the UE in other ways).
Block 13 : the AS of the calling UE or the called UE encrypts media stream security key using the application layer security key shared with the UE, respectively, and transmits the encrypted media stream security key to the calling UE or the called UE via a session message, respectively.
Block 14 : the calling UE or called UE obtains the end-to-end media stream security key between the calling UE and called UE by decrypting the encrypted media stream security key using the application layer key shared with the AS.
Block 15 : media stream messages are transmitted between the calling UE and the called UE after being encrypted or integrity-protected using the end-to-end media stream security key according to the Security Association (SA) negotiated during the process of establishing the session, thus achieving the end-to-end media stream security.
If only the media stream from the calling UE to the called UE needs to be protected, the calling UE encrypts or integrity-protects the media stream using the end-to-end media stream security key before sending the media stream to the called UE, while the called UE authenticates and decrypts the received media stream using the end-to-end media stream security key and does not encrypt the media stream to be sent. If only the media stream from the called UE to the calling UE needs to be protected, the process is similar as the above. If both the media streams sent by the calling UE and the called UE need to be protected, both of the two parties encrypt or integrity-protect the media streams using the end-to-end media stream security key before sending the media streams, and decrypt the received media stream using the end-to-end media stream security key.
In block 12 , the application layer security key shared between an Application Server (AS) and a User Equipment (UE) may be acquired in another way in related art.
For the format of a media stream message after being encrypted or integrity-protected, reference may be made to the definition of the format of RTP message in the Draft “Security RTP” of the IETF. Such a message format is substantially the similar as the format of RTP message, and defines information such as message to be encrypted, message to be authenticated, and locations of the encryption and authentication information in message, etc.
While negotiating the end-to-end media stream security key during the process of establishing a session, the security capabilities of the calling UE and the called UE may be negotiated in an interactive way, for example, information such as the supported algorithm for encryption or integrity protection, etc. The procedure and mechanism are similar to those described in the RFC 3329 Security Mechanism Agreement for the Session Initiation Protocol (SIP). While determining whether the media stream needs to be protected and assigning a security key, the AS or S-CSCF may specify the media stream capability between the calling UE and the called UE according to the security capabilities submitted by the calling UE and the called UE, thus establishing an end-to-end security association between the calling UE and the called UE.
The media stream is encrypted on an end-to-end basis during transmission. However, the end-to-end media stream security key is assigned by the AS or S-CSCF, thus, when the encrypted media stream transmitted needs to be listened to, the AS or S-CSCF may route the session, passing through a listening device, to the called UE while assigning the end-to-end media stream security key, so that the media stream of user is relayed to the listening device. The AS or S-CSCF send the Cipher Key (CK) to the listening device during the process of exchanging session messages with the listening device, so that the listening device may listen to the encrypted media stream by decrypting the media stream.
It is apparent to those skilled in the art that various modifications and variations may be made to the invention without departing from the spirit and scope of the invention. Therefore, such modifications and variations are intended to be encompassed in the invention provided that they fall into the scope of the invention as defined by the appended claims and their equivalents.
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A method for ensuring media stream security in an IP Multimedia Subsystem network is disclosed. The method includes: assigning an end-to-end media stream security key for a calling User Equipment (UE) or a called UE, by a network device with which the calling UE or the called UE is registered, respectively, and transmitting the media stream security key to a network device with which the opposite end is registered; encrypting the end-to-end media stream security key using a session key shared with the calling UE or the called UE respectively, and transmitting the encrypted end-to-end media stream security key to the calling UE or the called UE, respectively, via a session message; encrypting or decrypting a media stream, by the calling UE or the called UE, respectively, using the end-to-end media stream security key.
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FIELD OF INVENTION
[0001] This invention relates to a method and system for amplifying auditory sounds. In particular, the present invention relates to an amplifier method and system for use in a classroom, a conference room or an office room.
BACKGROUND OF INVENTION
[0002] During a teaching session in a classroom the background noise may, firstly, prevent some of the participating students in hearing the voice of the teacher, since the signal to noise ratio in the classroom is low, and thereby reducing the possibility of learning. Consequently, the background noise may, secondly, cause the teacher to increase vocal amplitude thereby straining the teacher's vocal chord.
[0003] American patent no.: U.S. Pat. No. 5,818,328; discloses an area audio amplification system, which provides an improved signal to noise ratio and which is not susceptible to interference from frequency modulated signals. The system comprises a speech processor processing the audio signal to adjust signal level and response. In order to achieve this, the system comprises a low pass filter and de-emphasis network for limiting audio response to speech frequencies. The corner frequency of this network is 5 kHz. However, the system provides a time constant amplification of the audio signal, and therefore the background noise as such is not considered relative to the auditory sound, which primarily was attempted to communicate.
[0004] Further, American patent application no.: US 2003 0144847; discloses a sound masking system for masking out noise generated in large working environments. The system comprises a plurality of flat panel sound generators emitting highly effective and spatially uniform masking sounds within various zones. Hence the system provides masking of distracting noises in the working environment. Thus the system, as such, does not provide amplification of speeches, rather, oppositely reduces the noise relating to vocal communication.
SUMMARY OF THE INVENTION
[0005] An object of the present invention is to provide a method and system for amplifying auditory sounds as a function of background noise. In particular, an object of the present invention is to augment speech in noisy conditions.
[0006] A further object of the present invention is to provide a method and system for filtering selected parts of selected sound and compensate the consequence of the filtering by increasing gain of amplification, thus preserving the overall sound pressure level (SPL).
[0007] A particular advantage of the present invention is the provision of a controllable amplifier ensuring that desired sounds are amplified to increase speech intelligibility.
[0008] The above objects and advantage together with numerous other objects, advantages and features, which will become evident from below detailed description, are obtained according to a first aspect of the present invention by a system for amplifying a sound in an auditory environment and comprising a microphone for transforming said sound to an electric sound signal; a band-pass filtering means connecting to said microphone, receiving said sound signal, and outputting a filtered sound signal; and an amplifier receiving said filtered sound signal, amplifying said filtered sound signal, and outputting a filtered and amplified sound signal to a loudspeaker; and wherein said amplifier has an amplification gain being a function of bandwidth of said band-pass filtering means.
[0009] The term “auditory environment” is in this context to be construed as a definition of an environment defined by reverberation, background noise i.e. noise floor, and sounds to be amplified. That is, the auditory environment is determined by the physical properties of, for example, a classroom; by number of sound generating elements in said classroom; and finally by the sound to be amplified.
[0010] The system according to the first aspect of the present invention may provide amplification of an auditory signal in accordance with the lower and upper cutoff frequencies of the filtering means. Hence when the bandwidth of the auditory signal is limited, the noise disturbing frequencies are eliminated and consequently not amplified. In addition, the amplifier gain is advantageously controlled so as to increase gain as bandwidth is narrowed. This ensures that even though the auditory sound may loose speech power in the filtered auditory signal this is compensated by increasing gain of the filtered auditory signal.
[0011] The term “cutoff frequency” is in this context to be construed as a frequency at which the amplification of the amplifier is reduced by 3 dB. Further, the term bandwidth is in this context to be construed as a frequency span defined between a lower cutoff frequency and an upper cutoff frequency.
[0012] The above objects, advantages and features together with numerous other objects, advantages and features, which will become evident from below detailed description, are obtained according to a second aspect of the present invention by a system for amplifying a sound in an auditory environment and comprising a microphone for transforming said sound to an electric sound signal; a band-pass filtering means connecting to said microphone, receiving said sound signal, and outputting a filtered sound signal; and an amplifier receiving said filtered sound signal, amplifying said filtered sound signal, and outputting a filtered and amplified sound signal to a loudspeaker; and wherein said band-pass filtering means comprises a passive first filter having a first bandwidth and first gain, an active second filter having a second bandwidth and a second gain larger than said first gain, and an active third filter having a third bandwidth and a third gain larger than said second gain.
[0013] The system according to the second aspect of the present invention provides means for advantageously controlling amplification and bandwidth of the overall system. The utilization of active filters establishes a simple approach.
[0014] The above objects, advantages and features together with numerous other objects, advantages and features, which will become evident from below detailed description, are obtained according to a third aspect of the present invention by a system for amplifying a sound in an auditory environment and comprising a microphone for transforming said sound to an electric sound signal; an band-pass filtering means connecting to said microphone, receiving said sound signal, amplifying said filtered sound signal, and outputting a filtered and amplified sound signal to a loudspeaker; and wherein said band-pass filtering means comprising a plurality of active filters each having an amplification gain associated with frequency bandwidth.
[0015] The band-pass filtering means according to the first, second and third aspect of the present invention may comprise switching means for switching between a plurality of filters having associated lower and upper cutoff frequencies. Thus by operating the switching means a user may select a filter bandwidth and amplification gain required for obtaining a sufficient signal to noise ratio. Alternatively, the system may comprise a switch controller, which based on the noise floor of the auditory signal switches between the plurality of filters.
[0016] The switching means according to the first, second and third aspect of the present invention may further simultaneously switch between a plurality of gains of said amplifier having each gain associated with a specific filter of said plurality of filters. Hence by switching between the plurality of filters, or rather switching between different lower and upper cutoff frequencies, the gain of the amplifier is appropriately simultaneous changed.
[0017] The plurality of filters according to the first, second and third aspect of the present invention may comprise a first filter having a lower cutoff frequency in the range between 20 and 100 Hz, such as 70 Hz, and an upper cutoff frequency in the range between 9 and 20 kHz, such as 12 kHz. This reproduces the auditory sound of a talker, such as a teacher, including relevant harmonics below 100 Hz and above 8 kHz. The first filter may comprise an associated first gain of the amplifier. The first filter may be established by the amplifiers gain frequency response, or may be established by passive elements inserted before and/or after the amplifier.
[0018] The plurality of filters may further comprise a second filter having a lower cutoff frequency in the range between 100 and 400 Hz, such as 300 Hz, and an upper cutoff frequency in the range between 3 and 9 kHz, such as 5 kHz. This bandwidth represents 95% of speech intelligibility with upward masking and with a minimum of boundary reflections. The second filter may comprise an associated second gain being larger than the first gain. Hence the gain is increased thereby compensating for cutting away the lower frequency part of the speech so as to preserve speech intelligibility.
[0019] The plurality of filters may further comprise a third filter having a lower cutoff frequency in the range between of 400 and 800 Hz, such as 600 Hz, and an upper cutoff frequency in the range between 3 and 9 kHz, such as 5 kHz. This bandwidth further focuses the amplification to frequencies essential to speech, which is centered at 2 kHz and reduces amplification for unwanted background noise. The third filter may comprise an associated third gain larger than the second gain. Hence the gain is further increased relative to the second gain thereby compensating for the loss of speech power due to the narrowing of the bandwidth. In fact, the system converts speech power from the lower frequencies to higher frequencies.
[0020] The system according to the first aspect of the present invention may further comprise an active filtering means comprising said first, second and third filters, and said amplifier. By incorporating the amplifier into the bandwidth filtering means a simple construction is achieved.
[0021] The above object and advantage together with numerous other objects, advantages and features, which will become evident from below detailed description, are obtained according to a fourth aspect of the present invention by a method for amplifying auditory sounds, and comprising receiving a sound signal from a microphone; band pass filtering said sound signal and outputting a filtered sound signal by means of a band-pass filter; amplifying said filtered sound signal as a function of bandwidth of said band pass filter and outputting a filtered and amplified sound signal to a loudspeaker.
[0022] The method according to the second aspect of the present invention may further comprise switching between a plurality of filters and between a plurality gains associated with each of said filters.
[0023] The method according to the second aspect of the present invention may incorporate any features of the system according to the first aspect of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] The above, as well as additional objects, features and advantages of the present invention, will be better understood through the following illustrative and non-limiting detailed description of preferred embodiments of the present invention, with reference to the appended drawing, wherein:
[0025] FIG. 1 , shows a overview of the system according to the preferred embodiment of the present invention;
[0026] FIG. 2 , shows a graph of the frequency responses of the system according to the preferred embodiment of the present invention; and
[0027] FIGS. 3 a through 3 c , show a first, second and third embodiment of the system according to the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0028] In the following description of the various embodiments, reference is made to the accompanying figures, which show by way of illustration how the invention may be practiced. It is to be understood that other embodiments may be utilized and structural and functional modifications may be made without departing from the scope of the present invention.
[0029] FIG. 1 , shows a classroom designated in entirety by reference numeral 100 . In the classroom 100 a teacher 102 speaks to an audience of students 104 . The teacher 102 carries a microphone around the neck or attached on a collar of a coat or shirt. The microphone converts the sound from the teacher 102 to an electric auditory signal. The classroom 100 comprises signal processing element receiving the electric auditory signal and performing a filtering and amplification of the auditory signal. In one embodiment of the present invention the signal processing system is implemented a wireless transmitter transmitting the auditory signal to a wireless receiver 106 , and in a second embodiment of the present invention the signal processing system is implemented in the receiver 106 .
[0030] Following filtering and amplification of the auditory signal, which will be described in detail with reference to FIGS. 3 a through 3 c , the receiver 106 communicates the filtered and amplified auditory signal to a plurality of loudspeakers 108 , 110 , 112 and 114 . The filtered and amplified auditory signal may be communicated to the loudspeakers through a wired or wireless connection known to a person skilled in the art.
[0031] The signal processing system may be controlled by the teacher 102 by operating a switch or may be controlled by a switch controller, shown in FIGS. 3 a through 3 c as reference numeral 316 , so as to adjust the bandwidth of the auditory signal to be amplified. FIG. 2 shows the asymptotic frequency responses 202 , 204 , 206 of the signal processing system in three different switching positions.
[0032] The signal processing system is designed to augment speech signals in noisy conditions. Depending on the noise floor, i.e. noise base in the frequency spectrum, the teacher 102 may select a ‘low’ position providing the frequency response 202 . This selection yields a full speech bandwidth from 70 Hz up to 12 kHz covering all necessary harmonics. By including the lower frequencies in the amplification the reproduced signal has more fidelity components.
[0033] If the noise floor is moderate the teacher 102 may select a ‘medium’ position providing frequency response 204 . This selection yields a lower cutoff frequency of approximately 300 Hz (0 dB at 200 Hz) and an upper cutoff frequency of approximately 5 kHz (−6 dB at 7 kHz). Since the frequencies below 300 Hz and above 5 kHz only contribute little to the overall speech intelligibility, and furthermore since the lower frequencies may mask higher frequencies within the bandwidth of the speech, the speech is in fact more understandable.
[0034] If the noise floor is very high the teacher 102 may select a ‘high’ position providing frequency response 206 . This selection yields a lower cutoff frequency of approximately 600 Hz (0 dB at approximately 300 Hz) and an upper cutoff frequency of approximately 5 kHz (−6 dB at 7 kHz). Hence the frequency response 206 of the ‘high’ position is shifted upward in frequencies relative to the frequency response 204 of the ‘low’ position.
[0035] Similarly, the switch controller operates the switch between the ‘low’, ‘medium’ and ‘high’ positions. The switch controller receives a part of the auditory signal and evaluates whether the auditory signal contains ambient noise beyond predetermined thresholds. Hence if the switch controller evaluates a higher ambient noise level the switch controller switches to a higher level, namely ‘medium’ or ‘high’.
[0036] FIG. 3 a shows a first embodiment of the signal processing system according to the present invention designated in entirety by reference numeral 300 . The system 300 comprises an input 302 connecting to a microphone worn by a person making a presentation, such as the teacher 102 . The microphone converts the sound of the person to an electric signal. The electric signal is communicated from the input 302 to a switching unit 304 enabling switching between a range of filtering and amplification modes of the system 300 .
[0037] The system 300 further comprises a filter block 306 comprising a plurality of individual filters, such as filter 308 , each having a specific bandwidth. Each filter of the filter block 306 is selected through the switching unit 304 and provides a filtration of the electric signal thereby generating a filtered electric signal. The filtered electric signal is forwarded from the filter block 306 to an amplifier block 310 comprising a plurality of individual amplifiers, such as 312 , for each filter in the filter block 306 .
[0038] The amplifier in the amplifier block 310 amplifies the filtered electric signal according to the bandwidth of the filter so as to compensate for the losses of in the speech power caused by the removal of lower frequencies in the electric signal. Following amplification of the filtered electric signal the amplified electric signal is forwarded to a loudspeaker unit 314 converting the amplified electric signal to sound.
[0039] The switching operation may be performed manually by the person using the microphone or sound technician, or may be performed by a switch controller 316 . The switch controller 316 identifies a noise floor in the electric signal, and when the noise floor exceeds a predetermined threshold the switch controller 316 switches the switch 304 accordingly. The switch controller 316 may receive an estimate of the noise floor from a separate noise detector or may integrate a noise detector.
[0040] FIG. 3 b shows a second embodiment of a system according to the present invention, which system is designated in entirety by reference numeral 320 . Like components in the first and second embodiment of the present invention are referred to by like reference numerals.
[0041] The system 320 comprises an input 302 forwarding an electric signal from the microphone (not shown) of the system 320 . The electric signal is forwarded from the input 302 to a switching unit 322 for switching between a range of filtering and amplification modes. The switching unit 322 is directly coupled to simultaneously switch triggering a number generator 326 , by for example switching a ‘high level’ to different inputs. The number generator 326 thus generates a number ‘X’ in accordance with the switching operation of the switching unit 322 , which number matches the selection of the bandwidth, or rather the selection of the filter.
[0042] The number ‘X’ generated by the number generator 326 is forwarded to an amplifier block 328 , which accordingly selects an appropriate gain function for amplifying the filtered electric signal received from the filter block 306 . The amplified signal is as before forwarded to a loudspeaker unit 314 .
[0043] FIG. 3 c shows a third embodiment of a system according to the present invention, which system is designated in entirety by reference numeral 350 . Like components in the first, second and third embodiments of the present invention are referred to by like reference numerals.
[0044] The system 350 comprises an input 302 receiving an electric signal from a microphone. The electric signal is forwarded from the input 302 to a switch 352 operable to switch between a plurality filtering and amplification modes. The switch 352 connects an active filter block 354 comprising one or more active filters 356 , 358 360 . The number of active filters in the active filter block 354 determines the number of gain frequencies responses.
[0045] The filtered and amplified electric signal is forwarded from the operating active filter 356 , 358 , or 360 to a loudspeaker unit 314 .
[0046] Common for the first, second and third embodiments of the systems 300 , 320 , 350 of the present invention is the frequency response of the gain function is determined so as to compensate for the removal of the lower frequency ranges by increasing the gain in the remaining frequency gain bandwidth. The compensation is determined in accordance with amount of speech power removed from the gain frequency response by increasing the lower cutoff frequency, and is effected by providing an increase in speech power in the remaining gain frequency response by increasing the gain substantially corresponding to the lost speech power. Further, the compensation additionally may advantageously incorporate the human frequency response curve to ensure that the lost speech power is compensated appropriately according to human hearing perception.
[0047] Further, common to the first and second embodiments of the systems 300 and 320 one of the filters in the filter blocks 306 may, in an alternative embodiment, be bypassed thus providing a frequency response determined by the amplifier blocks 310 and 328 . Similarly, in the third embodiment of the system 350 one of the active filters 356 , 358 , 360 may, in an alternative embodiment, be substituted by a single amplifier 362 , which consequently determines the overall frequency response in one of the switch positions.
[0048] Furthermore, common to the first, second and third embodiments of the systems 300 , 320 , 350 the preferred frequency response is a first frequency response having a lower cutoff frequency of 70 Hz and an upper cutoff frequency of 12 kHz together with a base level gain, a second frequency response having a lower cutoff frequency of approximately 300 Hz and an upper cutoff frequency of approximately 5 kHz together with a maximum gain 2.5 dB above the base level gain, and a third frequency response having a lower cutoff frequency of approximately 600 Hz and an upper cutoff frequency of approximately 5 kHz together with a maximum gain 6 dB above the base level gain. Obviously, the cutoff frequencies and gain may be adjusted accordingly to accomplish any desired effect.
[0049] Finally, common to the first, second and third embodiments of the systems 300 , 320 , 350 the systems may be implemented in analogue or digital circuit technology as will be known to persons skilled in the art.
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This invention relates to a system for amplifying a sound in an auditory environment. The system comprises a microphone for transforming said sound to an electric sound signal; a band-pass filtering means connecting to said microphone and outputting a filtered sound signal; and an amplifier amplifying said filtered sound signal and outputting a filtered and amplified sound signal to a loudspeaker. The band-pass filtering means comprises a passive first filter having a first bandwidth and first gain, an active second filter having a second bandwidth and a second gain larger than said first gain, and an active third filter having a third bandwidth and a third gain larger than said second gain.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a continuation of U.S. patent application Ser. No. 12/660,260 for Load Line Connection Spillage Container filed Feb. 23, 2010 which is a continuation of U.S. patent application Ser. No. 12/259,577 for Load Line Connection Spillage Container filed on Oct. 28, 2008 now U.S. Pat. No. 7,673,658.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates generally to containment of oil, waste, and chemical spills, and more particularly, to a container for containing spillage at a load line connection. As used herein, the terms “load line connection spillage container,” “load line spillage container,” and “load line container” refer, interchangeably, to applicants' invention.
[0004] 2. Discussion
[0005] Environmental concerns require containment of oil, waste, and other chemical spills from pipelines, storage tanks, tanker trucks, and railroad tankers. Pollution occurring when liquids are transferred between storage tanks and tanker vehicles through transfer lines is a continuing concern. Although transfer lines occasionally fail, leakage more typically occurs where the line from the tanker truck or railroad tanker attaches to the storage tank unloading line. The transfer lines are normally equipped with quick connect fittings, but spillage can occur during connection and disconnection of the transfer lines.
[0006] U.S. Pat. No. 5,313,991 is directed to an oil and waste line connection spillage containment apparatus (also referred to herein as a “load line container”) constructed from non-corrosive and rustproof materials. A substantially cylindrical container has two openings for receiving oil and waste loading and unloading lines therein. The lines are connected within the container. A circular cover encloses the container and is fastened and unfastened from the container using a pair of L-shaped members. Any oil and waste spilled from the connection is removed from the container when the lines are disconnected. In the alternative, a removal line with an auxiliary valve is used to withdraw the oil and waste from the container through the loading line. When the unloading line is removed from the opening in the container, a vented plug is inserted into the opening.
[0007] U.S. Pat. No. 5,647,412 is also directed to an apparatus for containing oil and waste spillage at a line connection. A load line container has opposed sidewall openings which receive loading and unloading lines, respectively, which are coupled within the container. Any spillage from the ends of the lines and the line connection is retained within the container. A lid closes the top end of the container when the unloading line is removed from the apparatus. With the unloading line removed from the container and the lid closed, an extension member attached to the lid covers the sidewall opening that is used for receiving the unloading line within the container.
[0008] Load line containers according to U.S. Pat. No. 5,647,412 made from fiberglass, medium density polyethylene, and high density polyethylene have been marketed in the United States and abroad. These load line containers have capacities, i.e., the maximum volume of spillage to be contained, of up to 35 gallons. The weight of the apparatus itself is nominal, but the combined weight of transfer lines and steel couplings associated with the unloading line and transfer lines is significant. In addition, the oil and waste spillage contained within the apparatus can weigh up to about 250 pounds. Finally, the apparatus is typically deployed in remote locations requiring a rugged product able to withstand rough treatment. In the past, steel collars, steel plates, and steel saddles have been used to strengthen the load line containers. It would be highly desirable to have a load line container which is sufficiently rugged for oil field application without the necessity of reinforcing steel collars, plates, and saddles.
[0009] What is needed is an injection molded load line container having a structure which is inherently strong and rugged, thereby eliminated the need for reinforcing steel collars, plates, and saddles.
SUMMARY OF THE INVENTION
[0010] An injection-molded load line connection spillage container for catching and retaining liquid spilled during transfers of liquids between storage tank and tankers provides an injection-molded reservoir and an injection-molded cover attached to the reservoir by hinges. Reinforcing ribs molded into the reservoir provide the strength and ruggedness required for oil field applications. Gussets molded into the reservoir hinge brackets ensure repeated stresses produced by energetic opening of the cover does not result in failure of the hinge brackets. An optional load line mounting assembly permits secure mounting of the load line container directly onto the load line. An optional cleanout assembly provides a valved suction line for removing retained spillage, and an optional sampling assembly provides a valved sample line for sampling the liquid being transferred. An optional main line valve contained within the load line container provides secure control of transfer between the storage tank and the tankers. An optional flow meter assembly, either in-line or clamped to the exterior of a transfer line, permits measurement of the volume of liquid transferred.
[0011] An object of the invention is to provide a rugged corrosion-resistant and wear-resistant container for collecting spillages at load line connections.
[0012] Another object of the invention is to provide a load line connection spillage container with a built-in cleanout assembly for removing captured liquids from the container.
[0013] Another object of the invention is to provide a load line connection spillage container which can endure the wear and tear associated with oil field operations.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a front view of a load line connection spillage container, including a reservoir and a reservoir cover, according to the present invention.
[0015] FIG. 2 is a side view of the load line connection spillage container shown in FIG. 1 .
[0016] FIG. 3 is a side view, with the reservoir cover open, of the load line connection spillage container shown in FIGS. 1 and 2 .
[0017] FIG. 4 is a front view, with cover and load line mounting assembly removed, of the reservoir of the load line connection spillage container shown in FIGS. 1-3 .
[0018] FIG. 5 is another view, with cover and load line mounting assembly removed, of the reservoir of the load line connection spillage container shown in FIGS. 1-3 .
[0019] FIG. 6 is a bottom view of the reservoir of the load line connection spillage container shown in FIGS. 1-6 .
[0020] FIG. 7 is a view of the load line connection spillage container shown in FIGS. 1-3 with a load line mounting assembly and an optional clean-out assembly. The load line connection spillage container in FIG. 7 is shown with the reservoir cover partially cut away.
[0021] FIG. 8 is an enlarged detail of the load line mounting assembly and the clean-out assembly shown in FIG. 7 .
[0022] FIG. 9 is a rear view of the load line connection spillage container shown in FIGS. 1-3 and FIG. 7 with an optional bottom drain assembly.
[0023] FIG. 10 is a view of the load line connection spillage container according to the present invention, together with the optional bottom drain assembly.
[0024] FIG. 11 is another view of the load line connection spillage container shown in FIG. 10 without the optional bottom drain.
[0025] FIG. 12 is a view of another load line connection spillage container according to the present invention.
[0026] FIG. 13 is a view, with the hinged reservoir cover partially cut away, of the load line connection spillage container according to the present invention in conjunction with optional enclosed main valve, optional cleanout assembly, and optional sampling assembly.
DETAILED DESCRIPTION OF THE INVENTION
[0027] In the following description of the invention, like numerals and characters designate like elements throughout the figures of the drawings.
[0028] Referring generally to FIGS. 1-3 , a load line container 20 has a reservoir cover 22 (also referred to herein as a cover) attached to a reservoir 24 by hinges 26 . Typically, the load line container 20 is mounted on a load line (not shown) from a storage tank (not shown). Another line (not shown) extends from a removal source such as a tank truck (not shown) for connection to the loading line within the load line container 20 . Thus the load line container 20 provides a point of connection between the loading line (from the storage tank) and the unloading line (from the tank truck). It will be understood by one skilled in the art that, while the present invention is described in the context of transfer of liquid from a storage tank to a removal source such as a tank truck, liquids are also routinely transferred from tank trucks to storage tanks. Thus, whereas the term “loading line” is used herein, for ease of illustration, to indicate the line attached to the storage tank and the term “unloading line” is used, for ease of illustration, to indicate the line attached to a tank truck or other removal source (e.g., a rail car), both “loading lines” and “unloading lines” are liquid transfer lines facilitating flow either to or from a storage facility.
[0029] Still referring to FIGS. 1-3 , the reservoir cover 22 is generally circular with a central dome portion 28 and a lip 30 . A handle 32 adjacent the lip 30 is generally centered over a downwardly projecting arcuate member 34 . The downwardly projecting arcuate member 34 and the handle 32 are generally diametrically opposed to the hinges 26 . A recess 36 in the lip 30 has a bore 38 therein for receiving a lock (not shown).
[0030] Referring now to FIG. 3 , a pair of reservoir cover hinge members 40 extend outwardly from the lip 30 opposite the handle 32 and the downwardly projecting arcuate member 34 . The reservoir cover hinge members 40 and the pair of hinges 26 are shown more clearly in FIG. 10 and FIG. 12 . Hinge pins 42 are disposed through bores 44 (not shown) in the cover hinge members 40 . In FIGS. 10 and 12 , the hinge pins 42 are threaded bolts with self-locking nuts. As will be discussed more fully below, the self-locking nuts prevent access to the load line container 20 by unauthorized personnel.
[0031] Referring now to FIGS. 4-6 in conjunction with FIGS. 1-3 , the reservoir 24 of the load line connection container 20 has an integrally molded bottom 46 and upstanding side walls 48 defining an open upper end portion 50 . The open upper end portion 50 has a front upstanding wall portion 52 , a rear upstanding wall portion 54 , a left upstanding wall portion 56 , and a right upstanding wall portion 58 . A transfer line channel 60 located in the front upstanding wall portion 52 is sized to receive a transfer line (not shown). A load line throughway 62 located in the rear upstanding wall portion 54 provides a location for attachment of a load line mounting assembly 100 (See FIGS. 7-8 ). The upper end portion 50 of the reservoir 24 terminates in an integrally molded J-shaped lip 64 having a sidewall portion 66 and a rollover portion 68 . Lip gussets 70 spaced about the circumference of the open upper end portion 50 between the sidewall portion 66 and the rollover portion 68 strengthen the integrally molded J-shaped lip 64 and the open upper end portion 50 of the reservoir 24 .
[0032] Referring now to FIGS. 4-6 , the front channel 60 is positioned opposite the load line throughway 62 located in the rear upstanding wall portion 54 . Integrally molded internal reinforcing ribs 72 in the rear portion 54 of the upstanding wall 48 strengthen the rear upstanding wall portion 54 at the point of attachment of the load line connection spillage container 20 to the load line. Integrally molded external reinforcing ribs 74 extend downwardly along the exterior 76 of the rear upstanding wall portion 54 of the reservoir 24 and continue across the exterior 78 of the bottom 46 of the reservoir 24 (See FIG. 6 ). Bores 80 spaced around the load line throughway 62 are used to attach the load line mounting assembly 100 shown in FIGS. 7-8 .
[0033] Still referring to FIGS. 4-6 , an integrally molded lock bracket 82 projecting outwardly from the J-shaped lip 64 has a bore 84 for receiving a lock (not shown). The lock bracket 82 mates with the recess 36 in the container cover 22 so the bore 38 aligns with the bore 84 in the lock bracket 82 to receive the lock (not shown).
[0034] Still referring to FIGS. 4-6 in conjunction with FIG. 2 , the integrally molded J-shaped lip 64 extends from one side of the rear upstanding wall portion 54 along the top of the right upstanding wall portion 58 , then around the transfer line channel 60 in the front upstanding wall portion 52 , and along the top of the left upstanding wall portion 56 to the other side of the rear upstanding wall portion 54 . When the reservoir cover 22 is closed on the reservoir 24 , as shown in FIG. 2 , the cover lip 30 extends downwardly around the upper end portion 50 of the reservoir 24 and the downwardly extending member 34 of the reservoir cover 22 rests against the J-shaped lip 64 along the transfer line channel 60 in the reservoir 24 , thereby closing off the transfer line channel 60 . Thus the cover 22 , in the closed position, prevents accumulation of water, snow, and debris within the reservoir 24 . The cover 22 also prevents small animals from gaining access to the reservoir 24 . Yet the reservoir 24 is vented to avoid buildup of chemical vapors.
[0035] Referring now to FIG. 4 , the reservoir 24 is sized based on the volume of spillage to be contained. Likewise, the load line throughway 60 is sized to accommodate the pipe size of the loading line. For large volumes of spillage, the load line connection spillage container 20 can optionally be supported by the ground (with or without a concrete slab) or by a stand used to align the load line throughway 60 with the load line. When so deployed, the bores 80 are unnecessary.
[0036] Referring now to FIGS. 5-6 , integrally molded reservoir hinge brackets 86 project rearwardly from the top portion 88 of the rear upstanding wall portion 54 of the reservoir 24 . Each hinge bracket 86 has a pin bore 90 for receiving a hinge pin 42 (See FIG. 3 ). Integrally molded gussets 92 reinforce and strengthen the hinge brackets 86 . As shown in FIG. 3 (enlarged detail), the reservoir cover hinge members 40 enclose the hinge brackets 86 . When the reservoir cover 22 is in the open position, as shown in FIG. 3 , the extent to which the reservoir cover 22 will open is limited, by contact of the reservoir cover hinge members 40 with the bottom sides 94 of the hinge brackets 86 , to an angle 96 greater than 90 degrees. The integrally molded gussets 92 provide additional strength to what might otherwise be a failure point as the cover is moved from the closed position, as shown in FIGS. 1-2 , to the open position illustrated in FIG. 3 .
[0037] Referring now to FIGS. 7-8 , a load line mounting assembly 100 is shown. The load line mounting assembly 100 consists of a length of pipe 102 threaded on each end 104 , 106 and a flange 108 located between the ends 104 , 106 . Flange bores 110 in the flange bores 108 mate with the throughway bores 80 spaced around the load line throughway 62 located in the rear upstanding wall portion 54 of the reservoir 24 . Fasteners 112 secure the flange 108 to the rear upstanding wall portion 54 . For security, bolts with locking nuts are preferred for the fasteners 112 .
[0038] Still referring to FIGS. 7-8 , an optional cleanout assembly 120 attached to the load line mounting assembly 100 permits evacuation of contents of the reservoir 24 through a transfer line (not shown). A valve 122 connects a suction line 124 to the load line mounting assembly 100 by appropriate pipe fittings 126 through a threaded bore 128 adjacent the threaded end 104 of the length of pipe 102 . The suction line 124 is sized to extend from the valve to just above the bottom 46 of the reservoir 24 . In operation, while the transfer line is in place and a pump is pulling tank contents into the tank truck, the valve 122 is opened and any liquid which has accumulated in the reservoir 24 will be transferred to the tank truck.
[0039] Referring now to FIG. 9 , the load line connection spillage container 20 is shown in conjunction with an optional bottom drain assembly 140 . A valve 142 is connected at one end by appropriate pipe fittings 146 to the bottom 46 of the reservoir 24 . A drain line 144 extends downwardly from the other end of the valve 142 . When the valve 142 is opened, any liquid collected within the reservoir 24 of the load line container 20 drains from the reservoir 24 into an appropriate container (not shown).
[0040] Referring now to FIGS. 7-9 , the advantages of the current invention injection molded load line connection spillage container 20 are apparent. The integrally molded internal reinforcing ribs 72 and the integrally molded external reinforcing ribs 74 permit attachment of the load line connection spillage container 20 to a loading line, using the load line mounting assembly 100 , without use of additional steel collars and saddles.
[0041] Still referring to FIGS. 9-10 , the optional bottom drain assembly 140 permits removal of any liquid which may accumulate in the reservoir 24 . A valve 142 connects a drain line 144 to the reservoir 24 by appropriate piping 146 through a threaded bore 148 in the bottom 46 of the reservoir 24 . As shown in FIG. 10 , the precise location of the threaded bore 148 in the bottom 46 of the reservoir 24 is arbitrary. Any convenient location is within the scope of the present invention.
[0042] Referring again to FIG. 10 in conjunction with FIG. 11 , the load line connection spillage container 20 is shown with an optional saddle 150 which extends from the rear upstanding wall portion 54 downward and across the bottom 46 of the reservoir 24 . Saddle bores 152 align with the bores 80 spaced around the load line throughway 60 , and the saddle 150 is secured by the fasteners 112 used to secure the load line mounting assembly 100 to the rear upstanding wall portion 54 of the reservoir 24 . One threaded end 106 of the pipe length 102 of the load line mounting assembly 100 extends through a cutout 154 in the saddle 150 .
[0043] Referring now to FIG. 12 , the load line connection spillage container 20 is shown with an optional backing plate 160 . The backing plate 160 has backing plate bores 162 which align with the bores 80 spaced around the load line throughway 60 , and the backing plate 160 is secured by the fasteners 112 used to secure the load line mounting assembly 100 to the rear upstanding wall portion 54 of the reservoir 24 . One threaded end 106 of the pipe length 102 of the load line mounting assembly 100 extends through a cutout 164 in the backing plate 160 .
[0044] It will be understood by one skilled in the art that the saddle 150 and the backing plate 160 are primarily cosmetic and not needed to support the weight of the load line connection spillage container 20 and its contents.
[0045] Referring now to FIG. 13 , the load line connection spillage container 20 according to the present invention is shown in conjunction with an optional enclosed main valve, an optional cleanout assembly, and an optional sampling assembly. The load line mounting assembly 100 shown in FIGS. 7-9 is secured to the rear upstanding wall portion 54 of the reservoir 24 . A main valve 170 is connected at one end to the threaded end 104 of the load line mounting assembly 100 by a pipe fitting 172 . A short pipe 174 connects the other end of the main valve 170 to a quick connect fitting 176 . On one side of the short pipe 174 , an optional cleanout assembly 120 (See FIGS. 8-9 ) is connected to the short pipe 174 by a threaded bore 178 (not shown) in the wall of the short pipe 174 . On the other side of the short pipe 174 , an optional sampling assembly 180 is connected to short pipe 174 through a second threaded bore 182 (not shown) in the wall of the short pipe 174 .
[0046] Still referring to FIG. 13 , the sampling assembly 180 includes a valve 184 , a goose-neck sample tap 186 attached to one end of the valve 184 , and a pipe fitting 188 connecting the other end of the valve 184 to the threaded boar 182 in the wall of the short pipe 174 .
[0047] It will be understood by one skilled in the art that load line connection spillage container 20 , when configured as shown in FIG. 13 with the optional main valve 170 , the optional cleanout assembly 120 , and the optional sampling assembly 180 , offers substantial advantages to oil field operators. With the load line connection spillage container locked, access is restricted to the load line, thereby precluding unauthorized persons from draining the storage tank. The cleanout assembly 120 permits easy removal of liquids from the reservoir 24 , and the sampling assembly 180 permits sampling of crude oil or other liquids being transferred from the storage tank to the tank truck.
[0048] The load line connection spillage container 20 can be manufactured from any thermoplastic or thermosetting plastic material suitable for injection molding. The most commonly used thermoplastic materials are polystyrene (low cost but lacking the strength and longevity of other materials), ABS or acrylonitrile butadiene styrene (a ter-polymer or mixture of compounds used for everything from toy parts to electronics housings), polyamide (chemically resistant, heat resistant, tough and flexible), polypropylene (tough and flexible), polyethylene (also tough and flexible), and polyvinyl chloride or PVC (more commonly extruded to make pipes, window frames, or wiring insulation where high proportions of plasticizer are added for flexibility). Plastics reinforced with short fibers can also be injection molded.
[0049] Referring now to FIGS. 12 and 13 , an optional flow meter assembly 200 positioned at a convenient location measures the flow between the storage tank (not shown) and the tank truck (not shown). Many different types and styles of flow meters are well known in the art. In-line flow meters are placed in a transfer line using suitable fittings. New technological breakthroughs have enabled measurement of fluids, including oil and water mixtures, using clamp-on designs. It will be understood by one skilled in the art that the flow meter assembly 200 may be placed either within or without the reservoir 24 .
[0050] The foregoing descriptions of specific embodiments of the present invention have been presented for purposes of illustration and description. They are not intended to be exhaustive or to limit the invention to the precise forms disclosed, and obviously many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and its practical application, to thereby enable others skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
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An injection-molded load line connection spillage container for catching and retaining liquid spilled when liquids are pumped between storage tanks and tankers provides an injection-molded reservoir and an injection-molded cover attached to the reservoir by hinges. Reinforcing ribs molded into the reservoir provide strength and ruggedness without the need for reinforcing steel collars and saddles. Gussets molded into the reservoir hinge brackets ensure repeated stresses produced by energetic opening of the cover does not result in failure of the hinge brackets. An optional load line mounting assembly permits secure mounting of the load line container directly onto the load line. An optional cleanout assembly provides a valved suction line for removing retained spillage, and an optional sampling assembly provides a valved sample line for sampling the liquid being transferred.
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FIELD OF THE INVENTION
The present invention relates to objects defined within an object-oriented computer programming system. More specifically, the present invention relates to a method and apparatus for creating objects within an object-oriented computer programming system.
RELATED ART
The recent proliferation of ever smaller and more capable computing devices has lead to the use of platform-independent programming languages on these smaller devices. Platform-independent programming languages allow the creation of programs that can be compiled to a set of platform-independent codes, which can be executed on a variety of computing devices. Many of these computing devices have interpreters that execute these platform-independent codes. The JAVA™ programming language is an example of a platform-independent programming language and JAVA bytecodes are an example of platform-independent codes.
The terms JAVA, JVM and JAVA VIRTUAL MACHINE are registered trademarks of SUN Microsystems, Inc. of Palo Alto, Calif.
Many platform-independent programming languages, including JAVA, are object-oriented programming languages. An object is typically an instance of a class, which usually has data and methods associated with it. Note that methods are functions that are used to manipulate data.
These objects may also have a meta-class instance associated with them. For instance, the JAVA virtual machine (VM) creates a java.lang.Class instance for each class that is loaded by the VM. The meta-class instance is created in an area of memory called the heap and contains information common to all objects of that class. Information within the meta-class instance includes, but is not limited to, the number of variables associated with each instance of the class and the number of methods associated with the class.
Some drawbacks to creating meta-class instances on the heap are that these objects can take up a large amount of space on the heap and that a program may create many of these objects. This can be a problem for smaller computing devices, which have limited storage space within the heap that can be quickly consumed by the meta-class instances. Also, with many meta-class instances stored within the heap, garbage collection takes more of the computing devices resources, thereby slowing the overall execution of the program.
Under many circumstances, creation of the meta-class instance is not required. As an example, the JAVA specification requires the creation of a meta-class instance only when the java.lang.Object::getClass method is explicitly invoked. Hence, creating the meta-class instance wastes resources under many circumstances.
What is needed is a method and apparatus for eliminating this waste of resources while maintaining the integrity of the platform-independent programming system.
SUMMARY
One embodiment of the present invention provides a system for creating objects in a virtual machine. The system operates by receiving a request to create an object within an object-oriented programming system. Upon receiving the request, if a meta-class instance associated with the object does not already exist, the system creates a structure to represent the meta-class instance in a data space that is not subject to garbage collection. If an explicit instruction to create the meta-class instance is detected, the system creates the meta-class instance within a garbage-collected data space.
In one embodiment of the present invention, the structure is created by directly executing instructions in a native language of a computing device, without having to convert platform-independent instructions into instructions in the native language of the computing device.
In one embodiment of the present invention, the system initializes a variable within the structure with a value. After initializing the variable with a value, the system can change the value of the variable. The system can also invoke an executable method of the object. In this embodiment, the acts of initializing a variable, changing the value of the variable, and invoking an executable method of the object involve executing the native language of the computing device.
In one embodiment of the present invention, the system destroys the structure using the native language of the computing device when the object is no longer needed.
In one embodiment of the present invention, the meta-class instance is created by executing instructions within an interpreted language.
In one embodiment of the present invention, the system initializes a variable within the meta-class instance with a value. After initializing the variable with a value, the system can change the value of the variable. The system can also invoke an executable method of the meta-class instance. In this embodiment, the acts of initializing a variable, changing the value of the variable, and invoking an executable method of the object include converting platform-independent instructions into native language instructions of a computing device.
In one embodiment of the present invention, the system allows the meta-class instance to be deleted by a garbage collector when the meta-class instance is no longer needed.
In one embodiment of the present invention, the meta-class instance includes a java.lang.Class instance.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 illustrates computing device 100 in accordance with an embodiment of the present invention.
FIG. 2 illustrates platform-independent virtual machine 102 in accordance with an embodiment of the present invention.
FIG. 3 is a flowchart illustrating the process of fetching instructions and creating a structure or a meta-class instance in accordance with an embodiment of the present invention.
FIG. 4 is a flowchart illustrating the process of deleting a structure or a meta-class instance in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
The following description is presented to enable any person skilled in the art to make and use the invention, and is provided in the context of a particular application and its requirements. Various modifications to the disclosed embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the present invention. Thus, the present invention is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles and features disclosed herein.
The data structures and code described in this detailed description are typically stored on a computer readable storage medium, which may be any device or medium that can store code and/or data for use by a computer system. This includes, but is not limited to, magnetic and optical storage devices such as disk drives, magnetic tape, CDs (compact discs) and DVDs (digital versatile discs or digital video discs), and computer instruction signals embodied in a transmission medium (with or without a carrier wave upon which the signals are modulated). For example, the transmission medium may include a communications network, such as the Internet.
Computing Device
FIG. 1 illustrates computing device 100 in accordance with an embodiment of the present invention. Computing device 100 may include any type of computer system, including, but not limited to, a computer system based on a microprocessor, a mainframe computer, a digital signal processor, a personal organizer, a device controller, and a computational engine within an appliance.
Included within computing device 100 is platform-independent virtual machine 102 . In one embodiment of the present invention, platform-independent virtual machine 102 is a JAVA VIRTUAL MACHINE. Platform-independent virtual machine 102 includes local storage 104 , executor 110 and garbage-collected heap 112 .
Local storage 104 can include any type of storage that can be coupled to a computer system. This includes, but is not limited to, semiconductor random access memory, read-only memory, magnetic, optical, and magneto-optical storage devices, as well as storage devices based on flash memory and/or battery-backed up memory. Local storage 104 includes program store 106 and data store 108 . Program store 106 stores and provides the instructions that executor 110 uses to perform operations directed by a program. Data store 108 stores data structures for executor 110 . Note that these data structures serve as surrogate meta-class instances for objects within an object-oriented programming system.
Executor 110 performs operations within platform-independent virtual machine 102 as directed by the program code stored in program store 106 . In one embodiment of the present invention, executor 110 is implemented as an interpreter, which interprets the platform-independent code within program store 106 .
In addition to storing objects defined within an object-oriented programming system, garbage-collected heap 112 stores meta-class instances for these objects. Note that these meta-class instances stored within garbage-collected heap 112 are subject to garbage-collection.
Platform-Independent Virtual Machine
FIG. 2 illustrates platform-independent virtual machine 102 in accordance with an embodiment of the present invention. As described above, platform-independent virtual machine 102 includes executor 110 . Executor 110 includes instruction fetcher 202 , structure allocator 204 , and heap allocator 206 .
Instruction fetcher 202 fetches instructions from program store 106 for execution by executor 110 . When executor 110 is implemented as an interpreter, executor 110 determines which of its internal, native-code instructions correspond with the fetched instruction from program store 106 . If the instruction is an instruction to create a new object, executor 110 uses structure allocator 204 to allocate a structure within data store 108 as a surrogate meta-class instance for an object within an object-oriented programming system.
If the instruction is an explicit request to create the meta-class instance, for instance a JAVA call instruction to the object's getClass method, executor 110 uses heap allocator 206 to create the meta-class instance within garbage-collected heap 112 .
Creating Structures and Meta-Class Instances
FIG. 3 is a flowchart illustrating the process of fetching instructions and creating a structure or a meta-class instance in accordance with an embodiment of the present invention. The system starts when instruction fetcher 202 fetches the next instruction from program store 106 (step 302 ). Executor 110 then determines if the instruction is an instruction to create a new object (step 304 ).
If the instruction is an instruction to create a new object at step 304 , structure allocator 204 creates a structure in data store 108 to serve as a surrogate meta-class instance (step 306 ). Executor 110 then initializes the structure within data store 108 (step 308 ). Note that since the structure is a surrogate meta-class instance, the structure is a substitute for the meta-class instance and includes variables, which can be initialized and changed by executing the native language of computing device 100 , and executable methods, which can be invoked by executing the native language of computing device 100 .
If the instruction is not an instruction to create a new object at step 304 , executor 110 determines if the instruction is an explicit instruction to create a meta-class instance (step 306 ).
If the instruction is an explicit instruction to create a meta-class instance at step 306 , heap allocator 206 creates a new meta-class instance in garbage-collected heap 112 (step 310 ). Next, executor 110 initializes the meta-class instance (step 312 ).
If the instruction is not an explicit instruction to create a meta-class instance at step 306 , executor 110 executes the instruction (step 314 ).
After initializing the structure at step 308 , initializing the meta-class instance at step 312 , or executing the instruction at step 314 , executor 110 determines if there are more instructions to execute within program store 106 (step 316 ).
If there are more instructions within program store 106 at step 316 , executor 110 returns to step 302 to continue executing instructions. If there are no more instructions at step 316 , the program terminates.
Deleting Structures and Meta-Class Instances
FIG. 4 is a flowchart illustrating the process of deleting a structure or a meta-class instance in accordance with an embodiment of the present invention. The system starts when executor 110 determines if an object is still required (step 402 ).
If the object is not still required, executor 110 determines if the object is a structure or a meta-class instance (step 404 ). If the object is a structure, executor 110 deletes the structure from data store 108 (step 408 ).
If the object is a meta-class instance within garbage-collected heap 112 , executor 110 deletes the reference to the meta-class instance and leaves the object for the garbage collector to delete (step 406 ).
If the object is still required at step 402 , after the structure is deleted at step 408 , or after leaving the meta-class instance to be deleted by the garbage collector at step 406 , the process terminates.
The foregoing descriptions of embodiments of the present invention have been presented for purposes of illustration and description only. They are not intended to be exhaustive or to limit the present invention to the forms disclosed. Accordingly, many modifications and variations will be apparent to practitioners skilled in the art. Additionally, the above disclosure is not intended to limit the present invention. The scope of the present invention is defined by the appended claims.
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One embodiment of the present invention provides a system for creating objects in a virtual machine. The system operates by receiving a request to create an object within an object-oriented programming system. Upon receiving the request, if a meta-class instance associated with the object does not already exist, the system creates a structure to represent the meta-class instance in a data space that is not subject to garbage collection. If an explicit instruction to create the meta-class instance is detected, the system creates the meta-class instance within a garbage-collected data space.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an optical material which comprises an N-(cyclic) alkyl-substituted maleimide-olefin copolymer, and which is superior in transparency, heat resistance, and surface hardness.
2. Description of the Related Art
Heretofore, optical materials are generally made of glass. Recently, transparent polymer materials have come to be used for optical materials in view of their productivity, light-weight, cost and so forth.
Such polymer materials includes, in particular, polymethyl methacrylate (hereinafter referred to as "PMMA") and polycarbonate (hereinafter referred to as "PC").
PMMA, however, is limited in its use because of its insufficient heat-resistance resulting from its low glass transition temperature (Tg) of about 100° C., although it has superior optical characteristics.
PC, which has a Tg of about 150° C. and has relatively high heat resistance, involves the disadvantage of low surface hardness causing susceptibility to scratching, so that further improvement was desired.
On the other hand, maleimide type copolymers are being studied comprehensively because of its high heat resistance. For example, copolymerization of the aforementioned methyl methacrylate with N-aromatic-substituted maleimide is disclosed in Japanese Patent Publication No. Sho 43-9753, Japanese Laid-Open Patent Applications Nos. Sho 61-141715, Sho 61-171708, and Sho 62-109811; and copolymerization of styrene resins with N-aromatic-substituted maleimide is disclosed in Japanese Laid-Open Patent Applications Nos. Sho 47-6891, Sho 61-76512, and Sho 61-276807. The resins produced by these methods are improved more in heat resistance with the higher content of N-aromatic-substituted maleimide, but thereby causing problems of brittleness, low moldability, discoloration, and so forth, thus being limited in use for optical materials.
After comprehensive study regarding the above problems, it was found that an optical material comprising an N-(cyclic) alkyl-substituted maleimide-olefin type copolymer solves the problems, and the present invention has been accomplished.
SUMMARY OF THE INVENTION
The present invention intends to provide an optical materials which is superior in transparency, heat resistance, and surface hardness.
The present invention provides an optical material, comprising a resin composed of a polymer constituted of 10 to 95 mol %, based on the polymer, of a first structural unit represented by the formula (I), and 90 to 5 mol %, based on the polymer, of a second structural unit represented by the formula (II), and having a weight-average molecular weight of from 1×10 3 to 5×10 6 in polystyrene equivalent: ##STR2## where R 1 is an cyclic alkyl group represented by C m H 2m-1 or a linear or branched alkyl group represented by C n H 2n+1 ; m is an integer of 3 to 8; and n is an integer of 1 to 18;
--CH.sub.2 --CHR.sup.2 -- (II)
where R 2 denotes hydrogen or an alkyl group having 1 to 8 carbons.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The resin constituting the optical materials of the present invention can be derived, for example, from radical copolymerization of an N-(cyclic) alkyl-substituted maleimide with an olefin.
The N-(cyclic) alkyl-substituted maleimide which gives the constitutional unit (I) includes N-methylmaleimide, N-ethylmaleimide, N-n-propylmaleimide, N-isopropylmaleimide, N-n-butylmaleimide, N-isobutylmaleimide, N-s-butylmaleimide, N-t-butylmaleimide, N-n-pentylmaleimide, N-n-hexylmaleimide, N-n-heptylmaleimide, N-n-octylmaleimide, N-laurylmaleimide, N-stearylmaleimide, N-cyclopropylmaleimide, N-cyclobutylmaleimide, N-cyclopentylmaleimide, N-cyclohexylmaleimide, N-cyclooctylmaleimide, and the like. These may be used singly or used combinedly in polymerization.
The olefin which gives the constitutional unit (II) includes ethylene, propylene, 1-butene, 1-hexene, 1-octene, and the like. These may be used singly or combinedly in polymerization. Ethylene is particularly preferred.
The content of the constitutional unit (I) is in the range of from 10 to 95 mol %, preferably from 20 to 90 mol %, more preferably from 25 to 80 mol %, of the whole polymer.
The content of the constitutional unit (II) is in the range of from 5 to 90 mol %, preferably from 10 to 80 mol %, more preferably from 20 to 75 mol %.
An additional vinyl monomer may be copolymerized, if necessary, within the range in which the object of the present invention is achievable. The additional vinyl monomer includes styrene, α-methylstyrene, vinyltoluene, 1,3-butadiene, isoprene, and their halogenated derivatives; methacrylic esters such as methyl methacrylate, ethyl methacrylate, propyl methacrylate, cyclohexyl methacrylate, phenyl methacrylate, and benzyl methacrylate; acrylic esters such as methyl acrylate, ethyl acrylate, butyl acrylate, lauryl acrylate, cyclohexyl acrylate, phenyl acrylate, and benzyl acrylate; vinyl esters such as vinyl acetate, and vinyl benzoate; vinyl ethers such as methyl vinyl ether, ethyl vinyl ether, propyl vinyl ether, and butyl vinyl ether; vinyl chloride, vinylidene chloride, maleic anhydride, N-phenylmaleimide, N-carboxyphenylmaleimide, and acrylonitrile, or a combination of two or more thereof.
The polymerization of these monomers may be conducted by any known polymerization process including bulk polymerization, solution polymerization, suspension polymerization, and emulsion polymerization.
The polymerization initiator includes organic peroxides such as benzoyl peroxide, lauryl peroxide, octanoyl peroxide, acetyl peroxide, di-t-butyl peroxide, t-butylcumyl peroxide, dicumyl peroxide, t-butyl peroxyacetate, and t-butyl peroxybenzoate; and azo type initiators such as 2,2'-azobis(2,4-dimethylvaleronitrile), 2,2'-azobis(2-butyronitrile), 2,2'-azobisisobutylonitrile, dimethyl-2,2'-azobisisobutylate, and 1,1'-azobis (cyclohexane-1-carbonitrile).
The solvent useful in the solution polymerization includes benzene, toluene, xylene, ethylbenzene, cyclohexane, dioxane, tetrahydrofuran, acetone, methyl ethyl ketone, ethyl acetate, dimethylformamide, isopropyl alcohol, butyl alcohol, and the like.
The polymerization temperature is suitably decided depending on the decomposition temperature of the initiator. Generally the temperature is preferably in the range of from 40° to 350° C.
The above resin can also be obtained by imidation of a copolymer of maleic anhydride and an aforementioned olefin by use of a primary amine.
The primary amine includes methylamine, ethylamine, n-propylamine, isopropylamine, n-butylamine, isobutylamine, s-butylamine, t-butylamine, n-pentylamine, n-hexylamine, n-heptylamine, n-octylamine, laurylamine, stearylamine, cyclopropylamine, cyclobutylamine, cyclopentylamine, cyclohexylamine, cyclooctylamine, and the like. These may be used singly or a combination of two or more thereof.
The weight-average molecular weight of the resulting polymer can be measured by gel permeation chromatography (GPC) in styrene equivalent. The molecular weight of the resin of the present invention is in the range of from 1×10 3 to 5×10 6 , preferably from 1×10 4 to 1×10 6 . The polymers having molecular weight of higher than 5×10 6 are poor in moldability, while the polymers having molecular weight of lower than 1×10 3 are brittle.
The resin of the present invention may contain a hindered phenol, a heat stabilizer such as organic phosphate esters, a benzotriazole type UV absorbing agent, a hindered amine type UV stabilizer, a lubricant or the like.
Further, the resin of the present invention may be blended with another compatible resin, if necessary.
The resin of the present invention can be molded by an ordinary molding process including injection molding, extrusion molding, and compression molding
The resulting molded articles are useful for optical parts, for example optical recording mediums such as optical discs, optical cards, optical lenses such as of cameras and videos, automobile lenses such as headlight lenses, and optical fibers, lighting fixtures and so on.
The present invention is described below by reference to examples without limiting the invention thereto in any way.
The optical material composed of the polymer according to the present invention has a Tg value not less than 120° C., preferably not less than 140° C., a light transmittance value not less than 85%, preferably not less than 90%, and a pencil hardness not lower than H.
The Tg of the resulting polymer was measured in nitrogen atmosphere at a temperature elevation rate of 10° C./min. by means of a differential scanning calorimeter, DSC200 (made by Seiko Denshi K.K.).
The decomposition temperature (Td) of the resulting polymer was measured in nitrogen atmosphere at a temperature elevation rate of 40° C./min. by means of TG/DTA200 (made by Seiko Denshi K.K.).
The molecular weight of the resulting polymer was measured by means of GPC (HLC-802A, made by Tosoh Corporation) in polystyrene equivalent.
The light transmittance, the pencil hardness and the rockwell hardness are measured by use of test specimens of the size of 50 mm×25 mm×0.8 mm according to ASTM 1746, JIS K5401, and JIS K7202 respectively.
EXAMPLE 1
179 g (1.0 mole) of N-cyclohexylmaleimide, 0.8 g (5.0×10 -3 mole) of 2,2'-azobisisobutyronitrile (AIBN), and 1 liter of toluene were placed in a 3-liter autoclave equipped with a stirrer, a nitrogen introducing tube, a thermometer, and a degassing tube. The autoclave was purged with nitrogen several times. Ethylene was charged therein to an inner pressure of 50 Kg/cm 2 at 60° C. The mixture was reacted at 60° C. for 10 hours.
The reaction mixture was poured into ethanol to deposit the polymer. The obtained polymer was purified by reprecipitation from toluene-ethanol, and was dried at a reduced pressure at 60° C. for 24 hours. The yield of the polymer was 38 g.
The mole ratio of N-cyclohexylmaleimide units to ethylene units of the resulting polymer was 48/52 according to elemental analysis. The polymer had a weight-average molecular weight (Mw) of 86000, and a Td of 404° C. From this polymer, colorless transparent test specimens were prepared by pressing it at 250° C., and 5 Kg/cm 2 The evaluation results of the polymer are shown in Table 1.
COMPARATIVE EXAMPLES 1 TO 3
Test specimens were prepared from PMMA (ACRYPET made by Mitsubishi Rayon Co., Ltd.), PC (PANLITE made by Teijin Kasei K.K.), and polystyrene (DENKA STYROL made by Denki Kagaku Kogyo K.K.), and were evaluated in the same manner as in Example 1. The results of the evaluation are shown in Table 1.
As clearly understood from the Examples, present invention provides an optical material which is superior in transparency, heat resistance, and surface hardness.
TABLE 1______________________________________ LightPolymer Trans- PencilComposition Tg mittance Hard- Rockwell(mol %) (°C.) (%) ness Hardness______________________________________Example 1 N-cyclohexyl- 170 90 2H 98 maleimide (48) Ethylene (52)Compara- PMMA 105 90 2H 98tiveExample 1Compara- PC 150 88 B 53tiveExample 2Compara- Polystyrene 93 87 F 65tiveExample 3______________________________________
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An optical material, comprising a resin composed of a polymer constituted of 10 of 95 mol %, based on the polymer, of a first structural unit represented by the formula (I) and 90 to 5 mol %, based on the polymer, of a second structural unit represented by the formula (II), and having a weight-average molecular weight of from 1×10 3 to 5×10 6 in polystyrene equivalent: ##STR1## The optical material has a Tg value not less than 120° C., a light transmittance value not less than 85%, and a pencil hardness not lower than H.
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CROSS REFERENCE TO RELATED APPLICATION
This application is the national phase application of International application PCT/JP01/03558, filed Apr. 25, 2001.
TECHNICAL FIELD
The present invention relates to a bone-strengthening agent, a bone-strengthening food, and a bone-strengthening feed composition, which are capable of preventing a decrease in bone density accompanying the onset or progress of osteoporosis.
BACKGROUND ART
In Japan with an aging society, the number of senior persons who have fallen in a bedridden state because of fracture due to osteoporosis, etc., is increasing. Therefore, it is an extremely important task to prevent osteoporosis. With this as a backdrop, a number of remedies have been developed while studies on preventing osteoporosis by means of food ingredients contained in meals and health foods have been increasing. Also, it is important for increasing cost efficiency to strengthen the bone of domestic animals and poultry, thereby maintaining the soundness thereof, as in humans. On the other hand, it is said that pets require more calcium than humans do in order to make their skeletal frames stronger. Therefore, pet foods dedicated to strengthening bone have been demanded.
In contemplating strengthening bone, it is a key point to promote efficient absorption of calcium, which is a main component of bone and is necessary for maintaining bone sound.
Casein phosphopeptide (hereinafter, abbreviated as “CPP”) prepared from proteins in cows' milk has an action of promoting the absorption of calcium and has been practically used as a raw material for a number of foods and feeds. Further, as the invention by which CPP is added to beverages and foods or feeds in order to exhibit the effects of maintaining the bone density and amount of calcium in the bone, reference maybe made to the invention described in JP 10-248525 A. However, this demonstrated no synergism with soybean isoflavone or genistein, one component thereof.
On the other hand, genistein is one of Leguminosae isoflavones and its action of increasing the bone mineral amount has been recently clarified. It has been clarified that genistein has an effect of inhibiting the function of osteoclasts that cause the lysis of bone mineral 10 times as potent as that of daidzein, which is also an isoflavone contained in soybean, etc. (Biol. Pharm. Bull., 22, 805-809, 1999). Further, it is known that genistein directly inhibits the bone resorption by osteoclasts in a culture system using a metaphysial tissue in the femora of old rats (Biochem. Pharmacol., 55: 71-76, 1998) and causes an increase in the amount of DNA, which serves as an index of an increase in bone mineral content and cell growth by osteoblasts (Res. Exp. Med. 197: 101-107, 1997). Furthermore, in 4-weeks old rats, its synergism with zinc on strengthening the bone has been observed (J. Bone Miner. Metab., 18: 77-83, 2000).
An object of the present invention is to provide a novel bone-strengthening agent, a bone-strengthening food composition and a bone-strengthening feed composition that prevent a decrease in bone density in association with the onset or progress of osteoporosis.
The inventors of the present invention have found out that not merely added-up effects but synergistic effects can also be achieved by the combined use of CPP, which is known as promoting the absorption of calcium essentially required for the soundness of bone and thus exerting an effect of strengthening bone, with genistein that directly acts on the bone tissue, inhibits bone resorption, and promotes osteogenesis, thus exerting an effect of strengthening bone. The present invention has been accomplished based on this finding.
SUMMARY OF THE INVENTION
Roughly divided, the present invention includes three types of aspects. That is, a first aspect relates to bone-strengthening agents; a second aspect relates to food compositions for strengthening bone; and a third aspect relates to feed compositions for strengthening bone.
A first aspect of the present invention relates to a bone-strengthening agent characterized by comprising casein phosphopeptide and genistein as active ingredients.
A second aspect of the present invention relates to a bone-strengthening food composition, characterized by comprising casein phosphopeptide and genistein as active ingredients.
A third aspect of the present invention relates to a bone-strengthening feed composition, characterized by comprising casein phosphopeptide and genistein as active ingredients.
Further, in the first to third aspects as described above, the present invention provides those that further contain a mineral in addition to casein phosphopeptide and genistein as active ingredients.
First, for the first aspect, there is provided the bone-strengthening agent described above, characterized by further comprising a mineral as an active ingredient.
Next, for the second aspect, there is provided the bone-strengthening food composition described above, characterized by further comprising a mineral as an active ingredient.
Further, for the third aspect, there is provided the bone-strengthening feed composition described above characterized by further comprising a mineral as an active ingredient.
Furthermore, in the first to third aspects as described above, the present invention provides those in which the above-mentioned mineral is at least one selected from calcium, magnesium and phosphorus.
First, for the first aspect, there is provided the bone-strengthening agent described above and further comprising a mineral, characterized in that the mineral is at least one selected from calcium, magnesium and phosphorus.
Next, for the second aspect, there is provided the bone-strengthening food composition described above and further comprising a mineral, characterized in that the mineral is at least one selected from calcium, magnesium and phosphorus.
Further, for the third aspect, there is provided the bone-strengthening feed composition described above and further comprising a mineral, characterized in that the mineral is at least one selected from calcium, magnesium and phosphorus.
DETAILED DESCRIPTION OF THE INVENTION
As described above, roughly divided, the present invention includes three types of aspects, i.e., the first to third aspects. That is, what belongs to the first aspect relates to bone-strengthening agents as described above; what belongs to the second aspect relates to food compositions for strengthening bone as described above; and what belongs to the third aspect relates to feed compositions for strengthening bone as described above.
The bone-strengthening agent of the present invention as described above, the food composition for strengthening bone of the present invention as described above, and the bone-strengthening feed composition of the present invention as described above, each contains CPP and genistein.
The CPP used in the present invention is casein hydrolysate, which is a phosphopeptide having an activity of solubilizing calcium.
Sources for supplying genistein are not particularly limited and those derived from Leguminosae plants including soybean may be used.
The bone-strengthening agent of the present invention as described above, the food composition for strengthening bone of the present invention as described above, and the bone-strengthening feed composition of the present invention as described above, each further may contain a mineral as an active ingredient.
In this case, as the mineral, at least one selected from three major elements contained in bone, that is, calcium, magnesium and phosphorus, may be used. However, sodium, potassium or other nutritionally indispensable elements such as iron, zinc, copper, chromium, selenium, manganese, and molybdenum may be used without problems.
In the bone-strengthening agent of the present invention as described above, the food composition for strengthening bone of the present invention as described above. and the bone-strengthening feed composition of the present invention as described above, the ratio of CPP to genistein is 500 to 5,000 times, preferably 500 to 1,000 times by weight ratio; the ratio of CPP to calcium is 0.08 times or more by weight ratio, particularly preferably 0.2 to 2 times by weight ratio; the ratio of CPP to magnesium is 0.01 times or more by weight ratio, particularly preferably 0.05 to 1 times by weight ratio; and the ratio of CPP to phosphorus is 0.04 to 4 times by weight ratio.
According to the present invention, the administration of CPP and genistein can significantly increase the contents of bone components in the femora of rats (bone weight, amount of bone calcium, activity of alkaline phosphatase, and amount of DNA).
The effect of it is exerted in both cortical bone (diaphysis) and trabecular bone (metaphysis) regardless of the bone structure of the femora. The simultaneous administration of CPP and genistein exerts an increasing effect stronger than the effects exerted by single administrations of CPP or genistein, in any one of the amount of calcium, the activity of alkaline phosphatase and the amount of DNA in the metaphysial tissue, and this effect is synergistic. In the diaphysial tissue, the simultaneous administration of CPP and genistein brings about a synergistic effect of increasing alkaline phosphatase activity.
The fact that CPP and genistein together have a synergistic effect on the mechanism of controlling the metabolism of bone, as described above, is an effect that cannot be expected from the results of single administrations of CPP or genistein and has an extremely great significance.
And, the effect can be observed not only in young rats but also old rats.
That is, in particular the activity of alkaline phosphatase activity and the amount of DNA in the metaphysial tissue can be synergistically increased by the simultaneous administration of CPP and genistein, as compared with the single administration of CPP or genistein.
This indicates that CPP and genistein together show the effect of increasing the amounts of bone components in senior persons and exerting a preventive effect against a decrease in bone components in the process of physiological senescence.
Therefore, the bone-strengthening agent of the present invention containing CPP and genistein as active ingredients, is useful in that, when in use, it shows the effect of increasing bone components, it can prevent osteoporosis, which is a serious problem to senior persons, and prevent a decrease in bone density in association with the onset or progress of osteoporosis.
And, by using the food composition for strengthening bone of the present invention, containing CPP and genistein as active ingredients, the effects of increasing bone components and preventing osteoporosis or preventing a decrease in bone density in association with the onset or progress of osteoporosis can be obtained concurrently with taking meals and without troubles of taking drugs.
Further, by using the bone-strengthening feed composition of the present invention containing CPP and genistein as active ingredients, strengthening the bone of domestic animals and poultry can be achieved and soundness thereof can be maintained, so that the cost effectiveness can be improved. Also, strengthening the bone of pets can be achieved and thus soundness thereof can be maintained.
Hereinafter, the present invention will be described in detail by examples. However, the present invention should not be considered as being limited thereto.
EXAMPLE 1
1) The materials and methods in Example 1 were as follows.
[Test Animal]
5-weeks old female Wistar rats (Convention) obtained from Japan SLC, Inc. (Hamamatsu, Japan) were used.
[Test Animal Group (Administered Group)]
1. Control group: Basic feed (solid feed for rats, MF, manufactured by Oriental Yeast Co., Ltd.)
2. CPP-administered group: Basic feed+CPP (40 mg/100 g body weight)
3. Genistein-administered group: Basic feed+genistein (50 μg/100 g body weight)
4. CPP+genistein-administered group: Basic feed+CPP (40 mg/100 g body weight)+genistein (50 μg/100 g body weight)
The above-mentioned basic feed contained 57.4% of carbohydrate, 1.15% of calcium, 0.25% of magnesium, and 0.88% of phosphorus.
As the CPP, a solution of CPP-III (casein phosphopeptide content 85%) manufactured by Meiji Seika Kaisha, Ltd., dissolved in distilled water was used. As the genistein, a reagent (manufactured by Sigma Chemical Company in U.S.A.) extracted from soybean and highly purified, dissolved in a 10% ethanol solution was used.
[Feeding and Administration Methods]
Animal groups each consisting of five animals were fed with the basic feed under constant temperature and constant humidity conditions of room temperature 25° C., and 55% humidity. In addition, the control group was administered with 1 ml/100 g body weight of purified distilled water and the other groups were each orally administered with CPP and/or genistein in the above-mentioned amounts once a day for 14 days by using a stomach tube. After 24 hours from the last administration, the rats were sacrificed and the femora were extracted. The extracted femora were used for the measurement of bone components as shown below.
[Measurement of the Dry Weight of a Bone Tissue (Femora) and the Amount of Calcium in the Bone Tissue]
After washing the extracted femora in a cold 0.25 M sucrose solution to remove a soft tissue and drying it in a drier at 100° C. for about 16 hours, the dry weight of the femora was measured. After the measurement, the extracted femora were divided into diaphysis (cortical bone) and metaphysis (trabecular bone) and the amount of calcium in each of them was measured. That is, the obtained diaphysial tissue and metaphysial tissue of the femora were each charged in a test tube, to which was added 3 ml of concentrated nitric acid to decompose them at 120° C. for 24 hours. The solutions were used as sample solutions and the amount of calcium therein was determined by using an atomic absorption spectrophotometer. The amounts of calcium were expressed in terms of mg per 1 g of the dry weight of the bone tissue.
[Measurement of Bone Alkaline Phosphatase Activity]
The diaphysial tissue and metaphysial tissue of the femora obtained as described above were each dipped in 3 ml of a cold 6.5 mM barbital buffer (pH 7.4) and cut into small pieces and homogenized by using a Potter-Elvehjem homogenizer followed by ultrasonic treatment for 60 seconds for crushing. Further, the homogenate was centrifuged for 5 minutes at 600×g and the supernatant fraction was used as a crude enzyme solution.
The activity of bone alkaline phosphatase was measured in accordance with the method of Walter and Schutt (Bergmeyer H. U. (ed.). Methods of Enzymatic Analysis, Vol. 1-2, Academic Press, New York, pp. 856-860, 1974). The enzymatic reaction was initiated by adding 0.05 ml of the above-mentioned crude enzyme solution to 2 ml of 0.1 M diethanolamine hydrochloride buffer (pH 9.8) containing disodium p-nitrophenyiphosphate as a substrate. The reaction was performed by incubation at 37° C. for 30 minutes. The reaction was terminated by adding 10 ml of 0.05N NaOH and the activity was expressed in terms of the amount (μmol) of free p-nitrophenol per 1 minute per the mass (mg) of the enzyme protein used. The concentration of the protein was measured in accordance with the method of Lowry et al. (J. Biol. Chem., 193: 265-273, 1951).
[Measurement of Deoxyribonucleic Acid (DNA) in Bone Tissue]
The diaphysial tissue and metaphysial tissue of the femora thus obtained were each crushed in 4.0 ml of a cold 0.1 N NaOH solution after homogenization of the bone tissue, shaken at 4° C. for 24 hours and extracted. After the alkali extraction, centrifugation treatment was performed at 1,000×g for 5 minutes and the supernatant fraction was used as a sample for the measurement of DNA. The measurement of the amount of DNA was performed in accordance with the method of Ceriotti (J. Biol. Chem., 214: 39-77, 1955). To a test tube containing 2.0 ml of a sample were added 1.0 ml of concentrated hydrochloric acid and 1.0 ml of a 0.04% indole solution and the test tube was shut with an aluminum cap, followed by heating on a boiling water bath for 10 minutes and then quenched on ice to terminate the reaction. Extraction with 4.0 ml of chloroform for 3 to 4 minutes was repeated several times and the amount of DNA was measured on a spectrophotometer (490 nm). The amount of DNA was calculated per wet weight (g) of bone tissue.
[Statistical Treatment Method]
Significant tests of respective measured values were performed by using Student's t-test. Values with a risk factor of 5% or less were taken as significant.
2) Results
[Body Weight]
The body weight after completion of the feeding was 111.4±2.7 g in the control group, 112.2±0.9 g in the CPP-administered group, 123.8±1.2 g in the genistein-administered group, and 119.0±1.9 g in the (CPP+genistein)-administered group. The genistein-administered group (p<0.01) and the (CPP+genistein)-administered group (p<0.05) had significantly higher body weights than that of the control group.
[Dry Weight of Femora]
The results of measurements of the dry weight of femora are shown in Table 1. The dry weight of femora, as compared with that of the control group, increased to 1.09 times in the CPP-administered group, 1.12 times in the genistein-administered group, 1.18 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was additive.
TABLE 1
Dry weight of femora
Administered group
Dry weight of femora (mg)
Control group
204.9 ± 2.60
CPP-administered group
222.5 ± 3.10*
Genistein-administered group
230.4 ± 1.20*
(CPP + genistein)-admninistered group
241.6 ± 1.82* ,#
*p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
[Amount of Calcium in Femora]
The amounts of calcium in femora, which serve as indices of the amounts of bone minerals, are shown in Table 2. The amount of calcium in the diaphysis, as compared with that of the control group, increased to 1.09 times in the CPP-administered group, 1.12 times in the genistein-administered group, and 1.21 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was additive. On the other hand, the amount of calcium in the metaphysis, as compared with that of the control group, increased to 1.04 times in the CPP administered group, 1.07 times in the genistein-administered group, and 1.17 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
TABLE 2
Amount of calcium in femora
Bone calcium(mg/g dry weight)
Administered group
Diaphysis
Metaphysis
Control group
201.6 ± 3.18
190.3 ± 4.89
CPP-administered group
219.2 ± 3.95**
197.1 ± 3.65
Genistein-administered group
225.1 ± 3.23**
204.1 ± 3.56**
(CPP + genistein)-administered
243.5 ± 2.63** ,#
222.3 ± 4.19** ,#
group
*p < 0.05, **p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
[Activity of Femoral Alkaline Phosphatase]
The activity of alkaline phosphatase, which is a marker for the metabolism of bone participating in increasing bone in femora, is shown in Table 3. The activity of femoral alkaline phosphatase in the diaphysis, as compared with that of the control group, increased to 1.02 times in the CPP-administered group, 1.04 times in the genistein-administered group and 1.12 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action of alkaline phosphatase in the (CPP+genistein)-administered group was synergistic. On the other hand, the activity of femoral alkaline phosphatase in the metaphysis, as compared with that of the control group, increased to 1.02 times for the CPP-administered group, 1.04 times in the genistein-administered group and 1.18 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
TABLE 3
Activity of femoral alkaline phosphatase
The activity of alkaline phosphatase
(μmol/min/mg protein)
Administered group
Diaphysis
Metaphysis
Control group
1.737 ± 0.021
1.784 ± 0.017
CPP-administered group
1.779 ± 0.014
1.818 ± 0.013
Genistein-administered group
1.809 ± 0.014*
1.853 ± 0.017**
(CPP + genistein)-administered
1.942 ± 0.017** ,#
2.105 ± 0.017** ,#
group
*p < 0.05, **p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
[Amount of DNA in Femora]
The amounts of DNA, which serves as an index for the proliferation of cells in femora, are shown in Table 4. The amount of DNA in the diaphysis, as compared with that of the control group, increased to 1.05 times in the CPP-administered group, 1.06 times in the genistein-administered group and 1.12 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic. On the other hand, the amount of DNA in the metaphysis, as compared with that of the control group, increased to 1.02 times in the CPP-administered group, 1.09 times in the genistein-administered group and 1.23 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
TABLE 4
Amount of DNA in femora
Amount of DNA
(mg/g wet weight of bone)
Administered group
Diaphysis
Metaphysis
Control group
1.788 ± 0.031
2.653 ± 0.041
CPP-administered group
1.886 ± 0.037
2.701 ± 0.047
Genistein-administered group
1.895 ± 0.013*
2.894 ± 0.034*
(CPP + genistein)-administered
2.002 ± 0.018* ,#
3.276 ± 0.044* ,#
group
*p < 0.05, **p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
EXAMPLE 2
1) The materials and methods in Example 2 were the same as in Example 1 except that 50-weeks old normal female Wistar rats obtained from Japan SLC, Inc. (Hamamatsu, Japan) were used as test animals.
2) Results
[Body Weight]
The body weights of the test animals after completion of the feeding are shown in Table 5. The body weights after completion of the feeding was 228.8±5.9 g in the control group, 227.4±4.4 g in the CPP-administered group, 229.6±7.6 g in the genistein-administered group, and 230.6±7.7 g in the (CPP+genistein)-administered group. The genistein-administered group and the (CPP+genistein)-administered group exceeded the control group, and further, the (CPP+genistein)-administered group exceeded the genistein-administered group. However, none of these groups showed a significant difference to the control group.
TABLE 5
Body weight
Body weight after completion
Administered group
of the feeding (g)
Control group
228.8 ± 5.9
CPP-administered group
227.4 ± 4.4
Genistein-administered group
229.6 ± 7.6
(CPP + genistein)-administered group
230.6 ± 7.7
[Dry Weight of Femora]
The results of measurement of the dry weight of femora are shown in Table 6. The dry weight of femora, as compared with that of the control group, increased to 1.06 times in the CPP-administered group, 1.08 times in the genistein-administered group, 1.10 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action of the (CPP+genistein)-administered group was additive.
TABLE 6
Dry weight of femora
Administered group
Dry weight of femora (mg)
Control group
439.3 ± 6.52
CPP-administered group
464.8 ± 5.68*
Genistein-administered group
475.3 ± 8.35**
(CPP + genistein)-administered group
485.3 ± 8.06** ,#
*p < 0.025, **p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group, that is, as compared with the effect of the case where CPP was administered singly)
[The Amount of Calcium in Femora]
The amounts of calcium in femora, which serve as an index of the amounts of bone minerals, are shown in Table 7. The amount of calcium in the diaphysis, as compared with that of the control group, increased to 1.03 times in the CPP-administered group, 1.07 times in the genistein-administered group and 1.09 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was additive. On the other hand, the amount of calcium in femora in the metaphysis, as compared with that of the control group, increased to 1.08 times in the CPP-administered group, 1.08 times in the genistein-administered group and 1.19 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
TABLE 7
The amount of calcium in femora
Amount of bone calcium
(mg/g dry weight)
Administered group
Diaphysis
Metaphysis
Control group
214.6 ± 4.2
187.2 ± 4.5
CPP-administered group
221.8 ± 3.6
201.6 ± 3.8*
Genistein-administered group
229.2 ± 3.4**
202.1 ± 3.8*
(CPP + genistein)-administered
234.8 ± 3.9***
222.4 ± 3.1*** ,#
group
*p < 0.05, **p < 0.025, ***p < 0.01 (as compared with that of the control)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
[Activity of Femoral Alkaline Phosphatase]
The activity of alkaline phosphatase, which is a marker for the metabolism of bone participating in increasing bone, is shown in Table 8.
According to Table 8, the activity of femoral alkaline phosphatase in the diaphysis, as compared with that of the control group, increased to 1.06 times in the CPP-administered group, 1.12 times in the genistein-administered group and 1.14 times in the (CPP+genistein)-administered group. Among them, the genistein-administered group and the (CPP+genistein)-administered group each showed a significant increase. The increasing action in the (CPP+genistein)-administered group was additive.
On the other hand, the activity of femoral alkaline phosphatase in the metaphysis, as compared with that of the control group, increased to 1.11 times in the CPP-administered group, 1.12 times in the genistein-administered group and 1.28 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
Furthermore, comparison of Table 8 showing the activity of femoral alkaline phosphatase in 50-weeks old rats with Table 3 showing the activity of femoral alkaline phosphatase in 5-weeks old rats indicates that the activity of femoral alkaline phosphatase is considerably decreased by aging.
TABLE 8
Activity of femoral alkaline phosphatase
The activity of alkaline phosphatase
(μmol/min/mg protein)
Administered group
Diaphysis
Metaphysis
Control group
0.581 ± 0.017
0.669 ± 0.023
CPP-administered group
0.616 ± 0.021
0.742 ± 0.020*
Genistein-adiministered group
0.653 ± 0.019**
0.744 ± 0.020*
(CPP + genistein)-administered
0.664 ± 0.021***
0.857 ± 0.024*** ,#
group
p < 0.05, **p < 0.025, ***p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-adininistered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
[Amount of DNA in Femora]
Variations of the amounts of DNA, which serve as an index for the proliferation of cells in femora, are shown in Table 9.
The amount of DNA in the diaphysis, as compared with that of the control group, increased to 1.14 times in the CPP-administered group, 1.14 times in the genistein-administered group and 1.16 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was additive.
On the other hand, the increase in the activity of femoral alkaline phosphatase in the metaphysis, as compared with that of the control group, increased to 1.04 times in the CPP-administered group, 1.05 times in the genistein-administered group and 1.11 times in the (CPP+genistein)-administered group, each showing a significant increase. The increasing action in the (CPP+genistein)-administered group was synergistic.
TABLE 9
Amount of DNA in femora
Amount of DNA
(mg/g wet weight of bone)
Administered group
Diaphysis
Metaphysis
Control group
1.218 ± 0.058
2.695 ± 0.047
CPP-administered group
1.386 ± 0.041*
2.814 ± 0.039
Genistein-adiministered group
1.391 ± 0.043**
2.836 ± 0.041*
(CPP + genistein)-administered
1.410 ± 0.044**
3.004 ± 0.042*** ,#
group
*p < 0.05, **p < 0.025, ***p < 0.01 (as compared with that of the control group)
# p < 0.01 (as compared with that of the CPP-administered group or genistein-administered group, that is, as compared with the effects of the cases where CPP or genistein was administered singly)
As described above, it was observed that oral administration of CPP (40 mg/100 g body weight) and genistein (50 μg/100 g body weight) for two weeks caused a significant increase in bone components (bone weight, amount of bone calcium, activity of alkaline phosphatase, amount of DNA) in the femora of rats.
The effect was exerted in both cortical bone (diaphysis) and trabecular bone (metaphysis) regardless of the bone structure of the femora. Simultaneous oral administration of CPP and genistein exerted an increasing effect stronger than the effects by single administration of CPP or genistein in any one of the amount of calcium, activity of alkaline phosphatase and amount of DNA in the metaphysial tissue, and this effect was synergistic. Furthermore, in the diaphysial tissue, the simultaneous administration of CPP and genistein brought about the effect of synergistic enhancement in the activity of alkaline phosphatase.
As described above, it is an effect unexpected from single administration of CPP or genistein that CPP and genistein together have a synergistic effect on the mechanism of controlling the metabolism of bone, which effect has an extremely great significance.
It has revealed that similar effects exist also in the femora of old rats. That is, although the reactivity of the bone tissues in old rats to single administration of CPP or genistein was at low levels, the simultaneous administration of CPP and genistein demonstrated an additive effect of increasing bone components (amount of bone calcium, activity of alkaline phosphatase, amount of DNA) as compared with the single administration thereof. It has been observed that a complex effect is exerted such that in particular, the amount of bone calcium, the activity of alkaline phosphatase, and the amount of DNA in the metaphysial tissue are synergistically enhanced by the simultaneous administration of CPP and genistein as compared with the single administration of CPP or genistein.
This indicates that CPP and genistein also exert an effect of increasing bone components in senior persons, so that they also exert a preventive effect for a decrease in bone components in the process of physiological senescence.
Industrial Applicability
The bone-strengthening agent of the present invention containing CPP and genistein as active ingredients is useful in that, when in use it shows the effect of increasing bone components, it can prevent osteoporosis, which is now a serious problem to in particular senior persons, and can prevent a decrease in bone density in association with the onset or progress of osteoporosis.
And, by using the food composition for strengthening bone of the present invention containing CPP and genistein as active ingredients, the effect of increasing bone components and the effect of preventing osteoporosis and preventing a decrease in bone density in association with the onset or progress of osteoporosis can be obtained simultaneously with taking meals without troubles in association with taking a medicine.
Furthermore, by using the bone-strengthening feed composition of the present invention containing CPP and genistein as active ingredients, strengthening the bone of domestic animals and poultry and maintaining the soundness thereof can be achieved, so that cost effectiveness can be increased. Also, strengthening the bone of pets can be achieved, so that the soundness thereof can be maintained.
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A novel bone-strengthening agent, a bone-strengthening food composition and a bone-strengthening feed composition which aim at preventing a decrease in bone density in association with the onset or progress of osteoporosis. It is found out that not merely added-up effects but synergistic effects can be achieved by the combined use of CPP, which is known as promoting the absorption of calcium essentially required for the soundness of bone and thus exerting an effect of strengthening bone, with genistein which directly acts on the bone tissue, inhibits bone resorption, and promotes osteogenesis and thus exerts an effect of strengthening bone.
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BACKGROUND OF THE INVENTION
The present invention relates to improved disposable, wet packaged or premoistened paper products, which have superior wet tensile strength at acidic pH and yet which have substantially reduced wet tensile strength at neutral or alkaline pH for ready disposal. These paper products, which are generally used for skin cleansing, are known commercially as towelettes, wet wipes or fem-wipes, and are formed from paper or non-woven fibrous webs which are treated with an improved polymeric binder which gives substantially higher tensile strength compared to prior art binder treated products when stored in an acidic wetting medium and during usage yet which exhibited substantially reduced strength when disposed in neutral or alkaline pH medium. The invention also related to a method of preparing an improved strengthened premoistened paper product through treatment of fibrous web material with an improved polymer binder prepared by the reaction of glyoxal and polyvinyl alcohol prior to drying and then wetting of the treated paper product with an acidic solution.
Current premoistened paper products are prepared by treating paper or fibrous webs, which have been prepared by conventional paper manufacturing processes, with various polymer binders to impart a degree of wet strength to the web when packaged in contact with an acid aqueous medium. These wet tissues or cleansing products are normally stored in sealed packages until used, thus requiring that they maintain their strength during storage and use and yet be readily disposable when flushed in plain water without clogging of typical plumbing and toilet equipment.
Various binders and processes for the manufacture of premoistened paper products have been proposed in the prior art. Thus, for example, U.S. Pat. No. 4,117,187 to James W. Adams discloses a premoistened wipe prepared through use of an acid-insoluble, alkali-soluble polymeric polycarboxylic acid and functional derivative thereof wherein the acid is dissolved in water and enough alkali is added to substantially neutralize all acidic groups prior to application to the fiber web. The binder saturated web is dried and then immersed in a low pH medium to effect an association reaction between the carboxylic group and the cellulose of the web, presumably through hydrogen bonding. These hydrogen bonds provide a reasonably strong linkage in acidic medium and yet will break-up when the wipe is immersed in a sufficiently high pH liquid medium.
Canadian Pat. No. 948,802 to David V. Duchane discloses a non-woven fibric wrapper from rayon fabric formed by conventional wet lay or dry lay processes which is first treated with a cold water soluble polyvinyl alcohol binder, e.g. by spraying, and then oversprayed with a solution of gelling or insolubilizing agent such as borax, to crosslink at least the surface area of the polymer binder before heating to dry to give a water resistant web. Thus Duchane utilizes the complexing reaction between borax and polyvinyl alcohol under heating to give wet strength in an acidic moist environment and yet disposability through dissociation of the polyvinyl alcohol-borax complex upon soaking in excess neutral water. This complexing reaction between borax and polyvinyl alcohol is similar to complexing between boric acid and polyvinyl alcohol as disclosed in R. F. Nickerson in Appl. Polymer Science 15, 111, (1971).
Canadian Pat. No. 1,109,758 to Gerald Miller similarly discloses the use of the reaction of a polyvinyl alcohol binder and boric acid or soluble salts thereof to form complexes having di-diols cross-linkages which are of a gel nature for binding the web. As disclosed in the above mentioned article of R. F. Nickerson, the borate ion is the effective crosslinking agent for the polyvinyl alcohol, and boric acid, at concentrations greater than 0.03 M as in Miller's patent, contributes sufficient amounts of borate ions to provide a gel type complex for binding the web as in the above mentioned Canadian patent of Duchane.
Canadian Pat. No. 1,104,026 to Daniel et al. discloses the use of a dried emulsion of a vinyl acetate-ethylene copolymer binder containing cold water soluble polyvinyl alcohol as a protective colloid with boric acid, which is used to temporarily insolubilize the binder. The polyvinyl acetate or ethylene-vinyl acetate copolymers have no known reaction with boric acid. It is the presence of the polyvinyl alcohol in the emulsion as protective colloid which forms a complex with the boron ions of the boric acid in the same manner as taught in the above patents of Duchane and Miller.
The instant invention has, through the use of a unique glyoxalated polyvinyl alcohol copolymer binder for pre-moistened paper products, achieved a substantially higher wet strength wiper when wetted in acidic medium than that achieved with prior art binders, as shown in comparison examples, and yet which maintains equal or better disposability in neutral pH water.
SUMMARY OF THE INVENTION
A premoistened towelette or wiper type paper product having high wet strength when stored in an acidic pH medium and during usage and lower wet strength when immersed in a neutral or alkaline pH medium for disposal in conventional sewage systems comprising a non-woven fibrous web which is treated with an improved polymeric binder comprising a copolymer of glyoxal and polyvinyl alcohol which maintains high wet strength when stored for sustained periods of time in acidic pH wetting medium conventionally used for external cleansing of the human body and during usage and yet which will readily break-up during flushing. This instant invention also comprises a method of treating non-woven fibrous web, such as cellulosic webs with the improved glyoxalated polyvinyl alcohol copolymer binder and drying prior to wetting in an acidic, e.g boric acid medium.
It is the principal object of this invention to provide a pre-moistened towelette paper product having substantially higher wet strength than prior art towelettes when stored for sustained periods of time in acidic medium and yet which is readily disposed of by flushing in excess neutral pH medium in conventional plumbing and toilet facilities, particularly when used for bathroom or toilet tissue.
It is also an object of this invention to provide an improved binder and a method of use thereof in preparing a pre-moistened towelette paper product of improved wet strength.
These and other objects of this invention will become apparent from the following detailed description of the invention.
DETAILED DESCRIPTION
The paper or non-woven fibrous webs of this invention are of the type commonly used in the art of conventional pre-moistened flushable wipe towelettes, wet wipes, fem-wipes, toilet tissue and the like. The fibrous webs are prepared by conventional paper manufacturing processes and are usually formed of a combination of relatively short cellulosic fibers e.g. 1/16 in.--1/2 in., with longer fibers which provide a degree of increased strength for the web. These fibrous materials lack substantial mechanical strength and require adhesive binders distributed uniformly over the web to impart wet strength to the wipes under conditions of storage and use at low pH and yet which will weaken and disintegrate when flushed in neutral or high pH medium.
In accordance with this invention, the fibrous web or paper is treated with an improved polymeric binder adhesive formed from the reaction of a polyvinyl alcohol with a dialdehyde, glyoxal, or dialdehyde of the general structure ##STR1## wherein R is alkyl, aryl or cycloalkyl, with or without substitution on the group, e.g glutaraldehyde and 2-hydroxyadipaldehyde, etc., with glyoxal being the preferred dialdehyde, for production of a wipe which has substantially higher wet strength than prior art binder treated wipes when stored and used in a low pH medium and yet which maintains disposability, i.e. disintegrates when disposed of in neutral or high pH medium which is at least equivalent to that of prior art wipes.
The improved polymer binder of this invention, which shall hereinafter be described in terms of Applicants' preferred binder, is a copolymer prepared by the reaction of glyoxal, ##STR2## with a hot water soluble polyvinyl alcohol of the form ##STR3## wherein N is the number of repeating structure units to give a glyoxalated polyvinyl alcohol copolymer which can be represented by the following structural formula: ##STR4## wherein m, n, x, m' and n' are integers representing the number of repeating structural units.
The glyoxalated polyvinyl alcohol copolymer of this invention can be applied to the paper or non-woven material in any desired conventional method such as by spraying, immersion, saturation or printing onto the material and then drying by conventional paper drying methods. The web is cut to the desired size, either prior to or after treatment with the binder, and the binder treated webs are then wetted with a low pH medium having a pH which is within acceptable limits for use on the body. The binder treated web can be either prewetted and packaged in a sealed package as in the case of towelettes, or folded and packaged wet in contact with a low pH aqueous medium in a sealed package until used.
The acid medium used in the practice of this invention can be any low pH mineral or organic acid medium conventionally used for cleansing skin at pH of 2.0 to 6.0 and more commonly pH 3.0 to 5.5 depending upon the concentration of acid used, such as boric acid, dilute phosphoric acid, fumaric, oxalic, malic, dilute HCl, etc. Boric acid is preferred since wipes in boric acid exhibit improved resulting wet strength over wipes which have been wetted with other low pH wetting medium. Boric acid in aqueous media containing a concentration of from 1-5% boric acid, and preferrably 4-5% boric acid, have been found to give optimum wet tensile strength when used at levels of about 12% boric acid on a dry weight of acid to dry weight of paper/fibrous web.
The acid wetting medium may also contain other conventional ingredients such as surface active detergent, humectants, bactericides, emulsifiers and scenting or perfuming agents can also be used without detrimental effect upon the unique binder of this invention.
The unique polyvinyl alcohol and glyoxal copolymer binder of this invention is prepared by the condensation reaction of glyoxal and a polyvinyl alcohol in a ratio of from not less than 1:1 to no more than 1:8 by dry weight, with a ratio of 1:1 to 1:4 being preferred. The polyvinyl alcohol used for reaction with glyoxal can be any commercially available polyvinyl alcohol having a degree of hydrolysis ranging from 87 to 99% and viscosities ranging from 4 cps to 70 cps for a 4% solution at 20° C. Polyvinyl alcohols which are hot water soluble with a degree of hydrolysis of 87-89% and a viscosity of 40 cps (4% solution at 20° C.), available for example from Dural Products Limited, Toronto, ONTARIO, CANADA, under the Tradename Covol 9740™, are preferred. The Covol polyvinyl alcohols are available in ranges of hydrolysis of 87-89% (the "97" series in the first two numbers with the last two numbers e.g. "40" being the viscosity in cps. when measured at 4% solid at 20° C.) and 98-99% hydrolysis (the "98" series, with viscosities up to 70 cps.) and have all been found to have utility in preparing the preferred binder of this invention.
The preferred glyoxal-polyvinyl alcohol copolymer binder of this invention has a polyvinyl alcohol to glyoxal ratio of 4:1 on a dry weight basis and is prepared with a hot water soluble polyvinyl alcohol with a degree of hydrolysis of 87-89% and a viscosity of 40 cps. at 20° C. for a 4% aqueous solution. The copolymer is conventionally prepared by the following manufacturing procedure which is outlined as follows:
______________________________________MaterialsReactants % by Weight______________________________________1. Water 69.42. Covol 9740 ™ 6.43. Glyoxal (40% solution) 4.04. Sodium hydroxide (25% solution) 0.25. Water 20.0 100.0______________________________________
Procedure
A. Set condenser for reflux and return if reactor is used.
B. Charge water (1) to reactor. Mix at maximum speed. Heat to 80° C.
C. At 80° C., start adding Covol 9740™ (2) slowly in small portions to the reactor with mixing to help the dispersion in the warm water. It takes about 20-30 minutes for the complete addition of Covol 9740™.
D. Let temperature rise to about 90° C. during and after the addition. Keep at 80°-90° C. with stirring until Covol 9740™ (2) has completely dissolved. This will take about 30-45 minutes time.
E. After Covol (2) has dissolved, the solution is cooled slowly back to 25°-30° C. with stirring.
F. At 25°-30° C., glyoxal 40% (3) is added in slowly with stirring.
G. Stirring is continued for another 5 minutes after the addition of glyoxal (3). Then the pH of the solution is adjusted to 5.5-5.7 with sodium hydroxide solution (4).
H. After the pH is adjusted, the solution is stirred at 25°-30° C. for another 10 minutes.
I. Water (5) is then added and stirred at 25°-30° C. for another 21/2 hours. During this period, Brookfield viscosity is measured every 30 minutes. (LV3/60/25° C.)
J. After the stirring period, the batch is screened through 60 mesh screen and can be drummed off.
The final product should have the following properties:
______________________________________Brookfield viscosity = 380-480 cps (freshly made)(spindle #3 at 60 rpm at 25° C.)Solid content = 8.0 ± 0.5%pH at 25° C. = 5.4- 5.8S.G. at 25° C. = 1.028- 1.032Gardner colour = 1- 2______________________________________
The glyoxalation of polyvinyl alcohol can be carried out at a pH medium ranging from about 1 to 6, while the reaction temperature can vary from about 20° to about 80° C. The reaction time may vary from 20 minutes up to 24 hours until an end point viscosity of the binder solution of from 10 to 1000 cps is reached. The concentration of the final copolymer binder solution can be within the range of 1-10%, depending upon the specific polyvinyl alcohol reactant used.
THE APPLICATION METHOD
Paper to be treated with the binder described in this invention can be made by conventional papermaking processes. The treatment of paper or other non-woven products by this glyoxalated polyvinyl alcohol binder can be made by impregnation, by spraying or by imprinting, depending on the choice of the papermaking companies. Depending on the amount of wet strength required to be imparted onto the paper, the preferable range of resin pick-up level varies from at least 0.5 to 3.0%.
The treated paper is then dried by conventional drying processes. Following drying, the treated paper can then be cut to desired size sheets for the intended use. These sheets can be packaged individually or in numbers, preferably in folded form, in moisture-proof containers. The folded and binder treated sheets can be wetted with boric acid solution prior to being placed into the container, or the appropriate amount of boric acid can be injected into the envelopes containing such folded sheets. Preferably, the boric acid needed should be about 12% based on dry weight of acid to dry weight of paper. The preferred concentration of the boric acid used is a 5% solution. The pH of the wetting solution should be in the acidic range, that is below about 6.
Various resin pick-up levels are used, depending on the strength required. However, any resin pick-up level of greater than 0.5% should be effective. The pH of the wetting liquid varies from about 3.0 to 5.5 depending on the concentration of the boric acid solution used. The concentration of the boric acid used varies from about 2 to 5% although the preferred concentration is a 5% solution. The amount of this wetting liquid can range from 2 to 20% based on the dry weight of acid to dry weight of paper although a 12% is preferred. Within this permissable range of components and reaction conditions, effective binder solution for pre-moistened tissue paper can be produced.
Though the exact mechanism of the function of the unique glyoxalated polyvinyl alcohol polymeric binder of this invention is not known, it is believed that the equilibrium of hemi-acetal formation in acidic medium by the glyoxalated polyvinyl alcohol and the complex formation of this glyoxalated polyvinyl alcohol with acid e.g. boric acid is accountable for maintaining the strength of the binder treated web when it is treated for a prolonged period in aqueous medium containing boric acid. This can be shown graphically as follows: ##STR5##
The above glyoxalated polyvinylalcohol was used to treat paper and heated to cure. The treated paper was soaked in an acid medium comprised of boric acid solution. The boric acid forms an insoluble complex with the glyoxalated polyvinyl alcohol in the acidic medium as shown in the following figures. ##STR6##
The complex prevented the dissolving and disintegration of the polymer network and therefore retained the strength in the acidic medium. However, in the presence of an excess of water, as in the flushability test conditions, the structure decomposes and the system will break down to provide good flushability properties.
The following examples are provided as illustrations of the invention and the preferred embodiments, but are not to be construed as being limiting of the degree of the invention as defined in the appended claims.
EXAMPLE 1
Preparation of Glyoxalated Polyvinyl Alcohol (Glyoxal:Polyvinyl Alcohol=1:1 by dry weight)
The polyvinyl alcohol Covol 9740™ is chosen to be the polyvinyl alcohol used in this example. Covol is a name for grades of polyvinyl alcohols, manufactured by Dural Product Limited. The "97" series has a degree of hydrolysis of 87-89%, while the last two digits in the number after Covol reflects the viscosity of a 4% aqueous solution at 20° C. of the polyvinyl alcohol. Thus Covol 9740™ is a polyvinyl alcohol having a degree of hydrolysis of 87-89% and the viscosity of its 4% aqueous solution is about 40 cps at 20° C. Another grade of Covol is the "98" series. The "98" series polyvinyl alcohols have a degree of hydrolysis of 98-100%. Once again, the last two digits in the number indicate the viscosity of a 4% aqueous solution at 20° C. of the polyvinyl alcohol.
412.5 grams of water were placed in a 3-necked 1 liter flask and stirred. The water was heated to about 80° C. 25 grams of Covol 9740™ were added in slowly with stirring. Stirring was continued after the polyvinyl alcohol was added in. After the Covol has completely dissolved, the solution was cooled to 25°-30° C. Then 62.5 grams of 40% glyoxal solution was added in and stirred for 5 minutes. Then the pH of the solution was adjusted to 3.4 with drops of sulfuric acid. (In other cases, sodium hydroxide solution was used to adjust to higher desired pH.) At this stage, additional water might be added to adjust to the required solid. The solution was held at 25°-30° C. until it reached a Brookfield viscosity of 220 cps (LV 2 spindle, 60 rpm at 25° C). The product has the following properties:
______________________________________Brookfield viscosity = 220 cps(LV2/60/25° C.)Solid content = 10%pH at 25° C. = 3.40______________________________________
EXAMPLE 2
Test of Tensile Strength of Pre-moistened Paper with Glyoxalated Covol 9740™ as made in Example 1
This example showed that glyoxalated polyvinyl alcohol possessed the properties of a binder for the manufacture of pre-moistened paper, i.e., having high initial strength in an acidic wetting medium and the strength drops substantially in neutral water on disposal for flushability. To test this, strips of paper (cut from Whatman Chromatography paper Grade #1 with basis weight of about 80 gm/m 2 ) were saturated in a 4% glyoxalated Covol 9740™ solution (made as Example 1) and then dried at 105° C. oven for one hour. The strips of paper (2.8 gm) were then soaked in an acid solution with pH adjusted to 3.5 for over night before testing.
Half of the strips were then tested as they were while the other half of the strips were soaked in a water bath (300 ml water at pH 7.2) for one hour before testing. The tensile test was carried out using a Thwing-Albert Electro-hydraulic Tensile Tester model #37-4. An average of 8 tests were reported for each test. The results were as follows:
______________________________________Wet Tensile (lb/20 mm width)Binder Acid used Acid Water Drop inSolution in Soaking Soaked Soaked Wet Tensile______________________________________1:1 glyoxal: citric acid 1.39 ± 0.07 0.84 ± 0.09 39.57%Covol boric acid 5.85 ± 0.16 0.80 ± 0.10 86.32%9740 ™ phosphoric 1.70 ± 0.08 0.87 ± 0.06 48.82%(dry wt) acid______________________________________
This showed that the polymer binder gave good strength when wetted in an acidic medium. A drop of about 40 to 86% in wet tensile when soaked in neutral water was an indication of good flushability.
EXAMPLES 3 to 7
Preparation of Glyoxalated Polyvinyl Alcohol of Varying Ratio of Glyoxal to Polyvinyl Alcohol
The following examples demonstrated the preparation of different glyoxalated polyvinyl alcohols using different ratio of glyoxal to polyvinyl alcohol with the same type of polyvinyl alcohol. The amount of glyoxal used in these examples varies from 0 to 50% by dry weight compared to the polyvinyl alcohol, Covol 9740™, used. These glyoxalated Covol 9740™ were prepared in ways similar to Example 1 and are summarized in Table I.
Note that Example 3 has 0% glyoxal added. This means that Example 3 is an 8% Covol 9740™ solution. A solution of polyvinyl alcohol has always been included in series of solutions made and tested under the same conditions. This is for comparison purposes and to show the superiority of our glyoxalated polyvinyl alcohol systems over the corresponding polyvinyl alcohol system when tested under identical conditions.
TABLE I______________________________________Glyoxalated Polyvinyl Alcohols of Different Ratio ofGlyoxal to Covol 9740 ™ Ratio of Properties Glyoxal/Covol 9740 ™ (solid, ViscosityExample (dry weight) @ 25° C.)______________________________________3 0:1 8% 652 cps4 1:1 8% 100 cps5 1:2 8% 271 cps6 1:4 8% 412 cps7 1:8 8% 610 cps______________________________________ NOTE: pH of examples 4 to 7 were adjusted to 5.6 for comparison purposes
EXAMPLES 8 to 12
Preparation of Glyoxalated Polyvinyl Alcohols Using Different Polyvinyl Alcohols
The following examples showed the use of different polyvinyl alcohols in preparation with glyoxal. These glyoxalated polyvinyl alcohols were prepared in manners similar to Example 1 with the exception that the ratio of glyoxal to the polyvinyl alcohol used might be changed. The preparation is summarized in Table II.
TABLE II______________________________________Glyoxalated Polyvinyl Alcohols Using DifferentPolyvinyl Alcohols Ratio of Properties Glyoxal/PVOH (solid, ViscosityExample (dry weight) @ 25° C.)______________________________________ 8 0:1 (Covol 9700) ™ 4% 6 cps 9 1:2 (Covol 9700) ™ 10% 19 cps10 0:1 (Covol 9840) ™ 4% 28 cps11 1:4 (Covol 9840) ™ 8% 171 cps12 1:7 (Covol 9840) ™ 8% 231 cps______________________________________
EXAMPLE 13
Comparison of Tensile Strength of Pre-Moistened Paper Treated with Glyoxalated Polyvinyl Alcohols of Different Ratio of Glyoxal to Covol 9740™ and Their Flushabilities
This example compared the wet tensile performance of various glyoxalated Covol 9740™ including the Covol 9740™ solution alone (as made in Examples 3 to 7) when applied onto paper. The procedure for the preparation of the pre-moistened paper for the test would be described in detail. A new method for observing flushability was also used. In order to demonstrate flushability of the paper, we also tested commercial toilet tissues as references. The flushability of the pre-moistened paper would be demonstrated by comparing with the degree of disintegration of the commercial toilet tissues subjected to the same flushability test.
13-A Test Method
The tissue paper used in the tests was supplied by a commercial paper mill and had the following properties:
______________________________________Thickness (inch) = 0.047 ± 0.002Burst strength (lb/in.sup.2) = 1.52 ± 0.23Dry Tensile (lb/15 mm) = 1.10 ± 0.07Brightness (measured by = 79.9 ± 0.10reflection meter model670 from Photovolt Corp.)Basis weight (gm/m.sup.2) = 25.63______________________________________
The tissue paper was cut into sheets of the size 71/2"×7". The sheets were weighed in an analytical balance before use. The binder solution (diluted to 1%) was sprayed onto the sheets using an air spray gun. It was sprayed in such a way that the binder pick-up was controlled to be the level needed. The paper was then dried for 5 minutes in an 110° C. oven and then conditioned at 22°-25° C. The paper was then re-weighed in the analytical balance to determine the exact pick-up level. Paper sheets with very close resin pick-up levels were grouped and cut into strips of 71/2"×3" with its length parallel to the machine direction of the paper. Each eight of these strips were grouped and rolled and then wetted with 6 ml of the wetting liquid. In all cases in these examples the wetting liquid was 5% boric acid. These wetted strips were sealed in plastic bags for at least over night before testing. The set of paper was then tested as it was by a Thwing-Albert Electro-hydraulic Tensile tester model 37-4. Afterwards, the tested strips were saved for flushability tests.
13-B Flushability Tests
In order to see the flushability performance of the glyoxalated polyvinyl alcohol system, commercial bathroom tissues were tested using the same procedure. The test results were used as references for comparison when the glyoxalated polyvinyl alcohol systems were tested by the same method. The commercial toilet tissues used included:
"Royale"™, manufactured by Facelle Royale Company of Canada.
"New Delsey"™ and "Delsey Boutique"™, by the Kimberly Clark Company of Canada.
"Cottonelle"™, by Scott Paper of Canada.
The procedure of the test was as followed:
A 2.5 gm sample of the toilet tissue was weighed out. The sample was soaked in 700 ml of distilled water in a beaker for 1 minute and then stirred for one, two and three minutes, alternating direction every 15 seconds. The stirring was stopped for 30 seconds between each minute of stirring for observation. The degree of disintegration and de-fibering was observed visually during these 30 second stops and at the end of the third minute of stirring.
The results of the test showed that "New Delsey"™ was the best in disintegration and de-fibering, followed by "Cottonelle"™ and "Royale"™, while "Delsey Boutique"™ was very poor in disintegration and de-fibering. The results are summarized in Table III.
TABLE III______________________________________Flushability Results of Commercial Bathroom Tissues Amount De-Fibered (%) After After AfterBrand 1 Minute 2 Minutes 3 Minutes______________________________________New Delsey ™ 75 100 100Cottonelle ™ 50 100 100Royale ™ 25 75 100Delsey Boutique ™ 2 20 50______________________________________
Using the same method from above, it was found that tissue paper treated with glyoxalated polyvinyl alcohols (Examples 3 to 12) had flushability performance comparable to commercial brands of toilet tissues.
13-C Test Results on Paper Treated with Samples Prepared in Examples 3-7
The series of glyoxalated polyvinyl alcohols using various ratio of glyoxal to Covol 9740™ prepared in Example 3 to Example 7 were tested by the above test method. The results are summarized in Table IV. An average of 8 tests were reported in each test.
TABLE IV______________________________________Wet Tensile Test of Glyoxalated Covol 9740 ™ AgainstCovol 9740 ™Ex- Components Resin Apparentam- Glyoxal:Covol 9740 ™ Pick-Up Wet Tensileple # (dry weight) (%) (lb/3 in width)______________________________________3 0:1 1.09 ± 0.05 1.00 ± 0.094 1:1 1.08 ± 0.05 1.53 ± 0.125 1:2 1.09 ± 0.05 1.82 ± 0.346 1:4 1.09 ± 0.03 2.24 ± 0.367 1:8 1.08 ± 0.03 2.25 ± 0.17______________________________________
These results showed that wet strength of glyoxalated polyvinyl alcohol Examples 4 to 7 are substantially better than polyvinyl alcohol (Example 3). Flushability tests showed that all these glyoxalated Covol 9740™ were just as flushable as the commercial toilet tissue such as "Cottonelle"™ and "Royale"™.
EXAMPLE 14
Comparison of Tensile Performance of Glyoxalated Covol 9700™ Against Covol 9700™ as Made in Examples 8 and 9
Glyoxalated polyvinyl alcohol prepared in Example 9 was tested against Covol 9700™ (Example 8) by a method similar to Example 13. The results are summarized in the following Table V. Once again, an average of 8 tests were reported in each test. Glyoxalated polyvinyl alcohol was again shown to be substantially better than polyvinyl alcohol in wet tensile property.
TABLE V______________________________________Glyoxalated Covol 9700 ™ Against Covol 9700 ™ in TensileStrengthEx- Components Resin Apparentam- Glyoxal:Covol 9700 ™ Pick-Up Wet Tensileple # (dry weight) (%) (lb/3 in width)______________________________________8 0:1 0.71 0.49 ± 0.029 1:2 0.62 0.67 ± 0.19______________________________________
Flushability tests showed that these binders were just as flushable as the commercial toilet tissue, "New Delsey"™.
EXAMPLE 15
Comparison of Tensile Performance of Glyoxalated Covol 9840™ Against Covol 9840™ as Made in Examples 10 to 12
Glyoxalated polyvinyl alcohol prepared in Examples 11 and 12 were tested against Covol 9840™ (as Example 10) by a method similar to Example 13. The results are summarized in Table VI. An average of 8 tests were reported in each test.
This again showed that glyoxalated polyvinyl alcohol is superior to polyvinyl alcohol when different types of polyvinyl alcohol are used. Flushability tests showed that these binders had flushability performance better than the commercial toilet tissue "Delsey Boutique"™ but not as good as "Royale"™.
TABLE VI______________________________________Glyoxalated Covol 9840 ™ Against Covol 9840 ™ inTensile PerformanceEx- Components Resin Apparentam- Glyoxal:Covol 9840 ™ Pick-Up Wet Tensileple # (dry weight) (%) (lb/3 in width)______________________________________10 0:1 1.02 ± 0.01 7.60 ± 0.4111 1:4 1.04 ± 0.02 8.30 ± 0.5512 1:7 1.04 ± 0.02 8.09 ± 0.05______________________________________
EXAMPLE 16
Comparison of Glyoxalated Polyvinyl Alcohol Against Binder Example Used in U.S. Pat. No. 4,117,187
This example illustrated the glyoxalated polyvinyl alcohols against an example used as binder solution for the pre-moistened paper in U.S. Pat. No. 4,117,187 in terms of wet tensile performance when wetted in diluted citric acid and when wetted in water.
The binder example chosen from the patent was Vinac ASB-516™, a vinyl acetate-crotonic acid copolymer obtained from Air Products and Chemical Company. A binder solution of this Vinac ASB-516™ was prepared according to the same procedure as written in Examples 1-4 in the American Can U.S. Pat. No. 4,117,187. According to the procedure, 120 gm of Vinac ASB-516™ was stirred with 1025 gm distilled water containing 55 gm of 10% sodium hydroxide solution. 200 gm of the concentrate was mixed with 800 gm of water and was heated and stirred to completely dissolve the polymer to give a 2% binder solution.
Paper was then saturated with this binder solution and the different glyoxalated polyvinyl alcohol solutions also at 2% binder concentration, dried and tested according to the method similar to Example 2. The results are summarized in Table VII.
TABLE VII__________________________________________________________________________Tensile Performance of Glyoxalated Polyvinyl AlcoholAgainst Vinac ASB-516 ™, an Example of Binder Solutionfrom U.S. Pat. No. 4,117,187 Wet Tensile (lb/20 mm width) DropBinderPolymer Type Acid Soaked Water Soaked in W.T.__________________________________________________________________________Vinac ™Vinylacetate-crotonic 1.19 ± 0.04 0.91 ± 0.10 23.53%ASB-516acid used in Examples1-4 of U.S. Pat. No.4,117,187Glyoxal:Glyoxalated Covol 4.34 ± 0.08 2.30 ± 0.12 47.00%Covol9870 ™ (1:1 dry wt)9870 ™Glyoxal:Glyoxalated Covol 3.51 ± 0.16 1.82 ± 0.12 48.15%Covol9840 ™ (1:1 dry wt)9840 ™Glyoxal:Glyoxalated Covol 1.39 ± 0.07 0.84 ± 0.09 39.57%Covol9740 ™ (1:1 dry wt)9740 ™Glyoxal:Glyoxalated Covol 1.34 ± 0.05 0.91 ± 0.09 31.09%Covol9720 ™ (1:1 dry wt)9720 ™Glyoxal:Glyoxalated Covol 1.48 ± 0.05 0.94 ± 0.07 36.49%Covol9700 ™ (1:1 dry wt)9700 ™__________________________________________________________________________
EXAMPLE 17
Comparison of Glyoxalated Polyvinyl Alcohols Against Binder Claimed in U.S. Pat. No. 4,117,187
In U.S. Pat. No. 4,117,187, Adams claimed styrene-maleic anhydride copolymer to be a binder for pre-moistened wiper (Claim 6). The example here illustrated the comparison of wet tensile performance of glyoxalated polyvinyl alcohols against a styrene-maleic anhydride copolymer when wetted in acid and in water.
A styrene-maleic anhydride copolymer, a copolymer claimed to be a binder for pre-moistened wiper by Adams, was obtained from Polysciences Inc. A binder solution was prepared according to the same method described in Example 1-4 of the American Can U.S. Pat. No. 4,117,187. 20 gm of the copolymer were mixed with 980 gm distilled water, stirred and heated until the copolymer was completed dissolved.
Paper was then separately saturated with this binder solution, and also the glyoxalated polyvinyl alcohol solutions, dried and tested according to the method similar to Example 2. The results are summarized in Table VIII.
TABLE VIII______________________________________Tensile Performance of Glyoxalated PolyvinylAlcohols Against Styrene-Maleic Anhydride Copolymeras Binder Solution Wet Tensile (lb/20 mm width) DropBinder Acid Soaked Water Soaked in W.T.______________________________________Styrene-Maleic 0.53 ± 0.02 0.50 ± 0.03 5.66%Anhydride(Polysciences Inc.)Glyoxal:Covol 4.34 ± 0.20 1.99 ± 0.16 54.35%9870 ™(1:1 dry wt)Glyoxal:Covol 3.34 ± 0.20 1.53 ± 0.07 54.19%9840 ™(1:1 dry wt)______________________________________
EXAMPLE 18
Comparison of Solubility of a Glyoxalated Polyvinyl Alcohol System Against its Corresponding Polyvinyl Alcohol
In order to demonstrate that the glyoxalated polyvinyl alcohol and its corresponding polyvinyl alcohol were different in structure, this example showed the solubility difference of the two systems when soaked in water. The systems used in this test included:
Example 3: an 8% Covol 9740™ solution, and
Example 6: an 8% (1:4 dry wt) glyoxalated Covol 9740™ solution
Films of the two binder solutions were casted separately onto a glass plate using a 3 mil draw down bar. The films were then dried in 110° C. oven for 5 minutes. After drying the films were peeled away from the glass plate. Each of these two dried films was placed separately into a 250 ml jar, each containing 50 ml distilled water. The time taken for the film to drop into the jar and stirred to dissolve completely was recorded.
Results showed that:
______________________________________Film of Time to Dissolve Film______________________________________Example 3 15 secondsExample 6 40 seconds______________________________________
This difference in solubility indicated that the two systems were different in structure in order to give different solubility properties.
EXAMPLE 19
Comparison of Tensile Performance of Glyoxalated Covol 9740™ Against Covol 9740™ Using Different Concentrations of Boric Acid as Wetting Agent
Glyoxalated polyvinyl alcohols prepared in Examples 4 to 7 were tested against polyvinyl alcohol Covol 9740™ (Example 3) by a method similar to Example 13 for tensile performance in different concentrations (2.5% and 1.0%) of boric acid as wetting liquid. The results are summarized as follows in Tables IX and X. An average of 8 tests were reported in each test.
TABLE IX______________________________________Tensile Performance of Glyoxalated Covol 9740 ™ AgainstCovol 9740 ™ in 2.5% Boric Acid as Wetting MediumEx- Components Resinam- Glyoxal:Covol 9740 ™ Pick-Up Apparent W.T.ple # (dry wt) (%) (lb/3 in width)______________________________________3 0:1 0.90 ± 0.01 0.58 ± 0.064 1:1 0.91 ± 0.02 0.71 ± 0.075 1:2 0.94 ± 0.01 1.02 ± 0.176 1:4 0.88 ± 0.07 1.08 ± 0.107 1:8 0.92 ± 0.03 1.01 ± 0.09______________________________________
TABLE X______________________________________Tensile Performance of Glyoxalated Covol 9740 ™ AgainstCovol 9740 ™ in 1.0% Boric Acid as Wetting MediumEx- Components Resinam- Glyoxal:Covol 9740 ™ Pick-Up Apparent W.T.ple # (dry wt) (%) (lb/3 in width)______________________________________3 0:1 1.26 ± 0.03 0.19 ± 0.014 1:1 1.24 ± 0.05 0.22 ± 0.025 1:2 1.28 ± 0.03 0.22 ± 0.016 1:4 1.27 ± 0.05 0.23 ± 0.027 1:8 1.27 ± 0.02 0.20 ± 0.03No -- -- 0.13 ± 0.03binder______________________________________
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A premoistened towelette or wiper type paper product having high wet strength when stored in an acidic pH medium and during usage and lower wet strength when immersed in a neutral or alkaline pH medium for disposal in conventional sewage systems comprising a non-woven fibrous web which is treated with an improved polymeric binder comprising a copolymer of glyoxal and polyvinyl alcohol which maintains high wet strength when stored for sustained periods of time in acidic pH wetting medium conventionally used for external cleansing of the human body and during usage and yet which will readily break-up during flushing. This instant invention also comprises a method of treating non-woven fibrous webs with the improved glyoxalated polyvinyl alcohol copolymer binder and drying prior to wetting in an acidic, e.g. boric acid medium.
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CROSS-REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. Provisional Application No. 61/700,113, filed on Sep. 12, 2012, which is incorporated herein by reference in its entirety.
FIELD OF INVENTION
This invention relates to a device for providing a replica of an existing wall or portion of a wall.
BACKGROUND OF THE INVENTION
The walls of a home are not necessarily true and flat, but may exhibit inconsistencies in trueness, flatness, or both. When it is desired to install cabinets such as kitchen cabinets in a customer's residence, often a considerable time and effort is spent in conforming the rear of a prefabricated cabinet to an existing wall where the cabinet is to be installed. The present device facilitates cabinet and countertop installation by providing a device that simulates an existing wall so that the rear of a cabinet or countertop can be appropriately modified at factory so as to be complementary to the wall portion at the installation site.
SUMMARY OF INVENTION
A frame assembly is provided for simulating the topography of an existing wall portion by providing strategically positioned points of adjustment behind a wallboard panel which permits a fabrication to mimic or replicate imperfections present in an existing wall where a cabinet is to be hung or a countertop installed, thereby minimizing installation time.
The frame assembly includes a metal frame to which is mounted an array of spaced columns. The columns are mounted in a substantially parallel relationship to one another and at spaced intervals from one another.
A plurality of threaded, dish-headed bolts is present in each of the columns. These bolts are threadedly received in the columns and are situated spaced from one another.
Plural weldments extend across the columns, usually at about right angles relative to the columns so as to define a quadrilateral grid with the columns. On one side thereof each weldment is provided with spaced pockets each sized to receive a head portion of one of the dish-headed bolts.
Wood slats are carried by the weldments and a wallboard panel is, in turn, is mounted to the wood slats.
Once the topography of a particular wall is determined by measurement, for example, by laser beam scanning, this topography can be replicated by the frame assembly by adjusting inwardly or outwardly, as required, individual dish-headed bolts so as to conform a wallboard panel carried by the frame to the particular wall.
BRIEF DESCRIPTION OF DRAWINGS
In the drawings,
FIG. 1 is a perspective front view of a frame assembly embodying the present invention;
FIG. 2 is a perspective back view of the frame assembly shown in FIG. 1 ;
FIG. 3 is a detail view showing a preferred relationship between the columns and the weldments in the frame assembly;
FIG. 4 is an enlarged exploded detail view showing a weldment carrying a wood slat about to be mounted to the frame;
FIG. 5 is a front elevational view of a frame assembly embodying the present invention with wood slats and a fragment of a wallboard mounted thereon;
FIG. 6 is a top plan view of the frame assembly shown in FIG. 5 ;
FIG. 7 is a side elevational view of the frame assembly shown in FIG. 5 ;
FIG. 8 shows a pair of frame assemblies embodying the present invention and pivotably joined together at about a right angle; and
FIG. 9 is an enlarged detail view showing a pivotable joint between the frame assemblies of FIG. 8 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIGS. 1 and 2 , frame assembly 10 has peripheral metal frame 12 , an array of spaced columns 14 , and weldments 16 carried by columns 14 . Optional skeleton tube 19 contributes to the rigidity of metal frame 12 . Frame assembly 10 is held in an upright position by horizontal support channels such as channel 18 and support tubes such as support tube 20 . Horizontal support channel 18 and support tube 20 are connected to one another at floor weldment 22 . Support tube 21 is connected to floor weldment 23 and skeleton tube 19 .
FIG. 3 shows a dish-headed bolt, such as dish-headed bolt 24 , received in pocket 26 defined by mounting clip 27 on one side of weldment 16 . Preferably, the dish-headed bolt 24 is a sex bolt or a barrel bolt.
As can best be seen in FIG. 4 , dish-headed bolt 28 terminating at its distal end in a dish 30 is sized to be received in pocket 32 of weldment 34 defined by mounting clip 33 . Wood slat 36 is secured to weldment 34 on the side opposite that equipped with pocket 32 . Dish-headed bolt 28 is threadedly received in column 38 .
Referring to FIGS. 5 , 6 and 7 , frame assembly 40 has outer metal frame 42 and an array of substantially parallel columns 44 mounted therein and spaced from one another. Wood slats 46 are attached to underlying flexible elongated weldments (see FIG. 6 ), carried by columns 44 , by through fasteners, e.g., screws 48 , and the like. Wallboard 50 , in turn, is mounted to wood slats 46 in any convenient manner.
Transverse cross-members 52 can be provided to rigidify frame 40 , if desired.
FIG. 8 shows a pair of frame assemblies 60 and 80 pivotably joined at 95 and arranged to form about a right angle with respect to one another. The included angle between frame assemblies 60 and 80 can be adjusted, however, as desired. Frame assembly 60 has outer frame 62 , an array of substantially parallel columns 64 and spaced weldments 66 carrying wood slats 68 . Likewise, frame assembly 80 has an outer frame 82 , an array of parallel columns 84 , spaced weldments 86 and wood slats 88 attached to weldments 86 .
FIG. 9 shows joint 95 pivotably connecting frames 62 and 82 so that the included angle therebetween can be adjusted. Adjustment is achieved by hinge 92 which comprises hinge brackets or mounts 96 and 98 , as well as hinge pin or tube 100 . Horizontal supports 102 and 104 are received in respective horizontal support securement channels 106 and 108 and are held in place by bolts 110 and 112 .
The frame assembly described hereinabove provides a multi-axis system that can adjust also for a varying angle between a wall and the contiguous floor for plumbers, for a varying angle between contiguous side walls that may not be at a right angle relative to one another, as well as for inward or outward bow of a side wall both vertically and horizontally. These features assist in custom configuration of cabinets in advance of installation in a customer's home and with minimal disruption of the cabinets themselves. Countertop fabrication prior to installation in a customer's home is facilitated as well.
The foregoing description and the drawings illustrate the present invention, but are not to be construed as limiting. Still other variants and arrangements of parts within the spirit and scope of this invention are possible and will readily present themselves to those skilled in the art.
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A frame assembly for simulating topography of an existing wall portion provides points of adjustment behind a wallboard panel mounted to the frame assembly. In this manner imperfections in an existing wall can be replicated to facilitate cabinet or countertop installation.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/246,574, filed Nov. 8, 2000.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to an abrasive composition for polishing magnetic recording disk substrates, and more particularly, to an abrasive composition for polishing magnetic recording disk substrates that allows the obtaining of a magnetic recording disk surface of high accuracy suitable for enabling the flying height of a magnetic head from the disk to be reduced.
[0004] 2. Description of Related Art
[0005] Magnetic recording disks (memory rigid disks) are widely used in the external memories of computers and word processors as means of allowing high-speed access. A typical example of such a magnetic recording disk is one which is produced by preparing a substrate by subjecting an Al alloy substrate to electroless plating of NiP on the surface, surface-polishing the substrate, and thereafter sequentially forming a Cr-alloy underlayer, a Co-alloy magnetic film, and a carbon protective film by sputtering.
[0006] When irregularities or protrusions which are higher than the flying height of a magnetic head remain on the surface of a magnetic recording disk, the magnetic head, which flies over the disk at a predetermined flying height and high speed, may hit such protrusions, causing damage to the head. When a magnetic recording disk substrate has protrusions and polishing scratches, in the case of formation of a Cr-alloy underlayer or a Co-alloy magnetic film on the substrate, protrusions and defects attributed to the polishing scratches arise on the surface of the film, and thus the resulting magnetic recording disk fails to have an even surface of high accuracy. Therefore, in order to produce a magnetic recording disk having a surface of high accuracy, the substrate of the disk must be accurately polished.
[0007] Consequently, there have been proposed many abrasive compositions which remove protrusions, minimize the height of protrusions or rarely form polishing scratches during polishing of magnetic recording disk substrates. For example, although Japanese Unexamined Patent Application, First Publication No. 10-121035 (use of a composition comprising the addition of aluminum nitrate to titania) easily achieves high surface accuracy and abrasion rate as compared with the prior art as a result of using submicron titanium oxide particles for the abrasive particles, it is difficult to achieve the level of surface accuracy required at present due to the effects of hardness of the abrasive particles. In addition, although Japanese Unexamined Patent Application, First Publication No. 11-167715 (use of a composition comprising the addition of aluminum nitrate to colloidal silica) makes it easy to obtain surface accuracy as a result of using fine particles of silicon dioxide having low hardness for the abrasive particles, it was difficult to achieve an abrasion rate that can be used in actual production.
BRIEF SUMMARY OF THE INVENTION
[0008] The quality required of abrasive compositions for polishing aluminum magnetic recording disk substrates that enable high-density magnetic recording is such that a highly accurate disk surface is achieved that allows reduction of the head flying height.
[0009] The object of the present invention is to provide an abrasive composition for polishing magnetic recording disk substrates that lowers the surface roughness of a magnetic recording disk, allows the attaining of high-density recording without the occurrence of protrusions or polishing scratches, and enables polishing to be performed at an economical high speed.
[0010] As a result of conducting extensive research on abrasive compounds for attaining a highly accurate polished surface required by aluminum magnetic recording disks having a low flying height, the inventors of the present invention found that an abrasive composition that uses silicon dioxide for the abrasive material and blends aluminum nitrate, antigelling agent and hydrogen peroxide therein demonstrates superior performance, thereby leading to completion of the present invention. Namely, the present invention is composed of each of the following inventions:
[0011] (1) an abrasive composition for polishing magnetic recording disk substrates comprising: water, silicon dioxide, antigelling agent, aluminum nitrate and hydrogen peroxide;
[0012] (2) an abrasive composition for polishing magnetic recording disk substrates according to (1) above, wherein the silicon dioxide is one or more types selected from colloidal silica, fumed silica and precipitated silica;
[0013] (3) an abrasive composition for polishing magnetic recording disk substrates according to either of (1) or (2) above, wherein the average particle size of secondary particles of the silicon dioxide is 0.03-0.5 μm;
[0014] (4) an abrasive composition for polishing magnetic recording disk substrates according to any of (1) through (3) above, wherein the concentration of silicon dioxide in the composition is 3-30 wt %;
[0015] (5) an abrasive composition for polishing magnetic recording disk substrates according to any of (1) through (4) above, wherein the antigelling agent is one or more types selected from a phosphonic acid compound, phenanthroline and acetylacetone aluminum salt; and,
[0016] (6) an abrasive composition for polishing magnetic recording disk substrates according to (5) above, wherein the phosphonic acid compound is 1-hydroxyethane-1,1-diphosphonic acid.
[0017] According to the present invention, an abrasive composition for polishing magnetic recording disk substrates that is comprised of water, silicon dioxide, antigelling agent, aluminum nitrate and hydrogen peroxide such that, due to the presence of the three ingredients of antigelling agent, aluminum nitrate and hydrogen peroxide, a higher abrasion rate is obtained.
[0018] Although the abrasive composition for polishing of the present invention can be advantageously applied to, for example, a substrate for high-density recording such as a magnetic recording disk for magnetic heads utilizing magnetoresistance (MR) effects (normally having a recording density of 1 Gbit/inch 2 or more), it can also be applied effectively to magnetic recording disks having a lower recording density from the standpoint of improving reliability.
[0019] When disks are polished using the abrasive composition for polishing of the present invention, surface roughness can be reduced significantly and polishing can be performed at a high abrasion rate. A magnetic recording disk using a polished disk is useful as a low flying height rigid disk, and enables high-density recording.
[0020] In particular, a magnetic recording disk using a polished disk has a high degree of usefulness as a high-density recording medium typically represented by media for MR heads (having a recording density of 1 Gbit/inch 2 or more). It is also useful for magnetic recording disks having a lower recording density from the viewpoint of being a highly reliable medium.
DETAILED DESCRIPTION OF THE INVENTION
[0021] There are no particular restrictions on the silicon dioxide contained as abrasive material in the abrasive composition for polishing of the present invention, colloidal silica, fumed silica or precipitated silica may be used, and the average particle size of the secondary particles is preferably 0.03-0.5 μm. The average particle size of the secondary particles refers to the value measured by means of the MICROTRAC UPA 150 (manufactured by Honeywell), which is a laser Doppler frequency analysis type of particle size distribution measuring instrument.
[0022] Although it becomes easier to inhibit fine gelling and aggregation when the size of the secondary particles of the silicon dioxide increases, since the probability of the existence of coarse particles also increases, this can cause the occurrence of polishing scratches. In addition, if the size of the secondary particles decreases, there is increased susceptibility to the above gelling and aggregation, which also causes the occurrence of polishing scratches. Thus, the average particle size of the secondary particles of the silicon dioxide contained as abrasive material in the abrasive composition for polishing of the present invention is preferably 0.03-0.5 μm, and more preferably 0.04-0.2 μm.
[0023] If the concentration of silicon dioxide in the abrasive composition for polishing is less than 3 wt %, the abrasion rate decreases remarkably. In addition, as the concentration of silicon dioxide increases, although abrasion rate also increases, if the concentration exceeds 30 wt %, no further increases in abrasion rate are observed, and gelling occurs easily particularly in the case of colloidal silica. In consideration of economic feasibility, the practical upper limit of the silicon dioxide concentration is 30 wt %. Thus, the concentration of silicon dioxide in the abrasive composition is preferably within the range of 3-30 wt %, and more preferably within the range of 5-15 wt %.
[0024] Although considerable abrasion promotional effects are obtained as a result of using a mixture of the three ingredients of antigelling agent, aluminum nitrate and hydrogen peroxide in the abrasive composition for polishing of the present invention, the amount of antigelling agent added is preferably 0.1-2 wt % and preferably 0.3-1 wt %, the amount of aluminum nitrate added is preferably 1-20 wt % and preferably 2-15 wt %, and the amount of hydrogen peroxide added is preferably 0.2-5 wt % and preferably 0.5-3 wt %.
[0025] If the amount of antigelling agent added is less than 0.1 wt %, abrasion promotional effects are diminished and gelling occurs more easily. In addition, even if the amount of antigelling agent added exceeds 2 wt %, there is no increase in abrasion promotional effects.
[0026] If the amount of aluminum nitrate added is less than 1 wt %, abrasion promotional effects diminish. In addition, gelling tends to occur more easily if the amount of aluminum nitrate added exceeds 20 wt %.
[0027] If the amount of hydrogen peroxide added is less than 0.2 wt %, abrasion promotional effects diminish. In addition, even if the amount of hydrogen peroxide added exceeds 5 wt %, there is no increase in abrasion promotional effects.
[0028] The antigelling agent used in the present invention is preferably one type or a mixture of two or more types selected from a phosphonic acid compound, phenanthroline and acetylacetone aluminum salt. Specific examples of phosphonic acid compounds include 1-hydroxyethane-1,1-diphosphonic acid (C 2 H 6 O 7 P 2 ) and aminotrimethylene phosphonic acid (C 2 H 12 O 9 P 3 N), a specific example of phenanthroline is 1,10-phenanthroline hydrate (C 12 H 8 N 2 H 2 O), and a specific example of an acetylacetone aluminum salt is aluminum complex salt of acetylacetone (Al 2 [CH(COCH 3 ) 3 ]). In particular, 1-hydroxyethane-1,1-diphosphonic acid is the most effective as an abrasion promoter.
[0029] Each of the above ingredient concentrations refer to the concentrations during polishing of a magnetic recording disk substrate. In the case of producing an abrasive composition for polishing and shipping, etc., it is effective to produce an abrasive composition having concentrations greater than those indicated above and then use after diluting to the above concentrations at the time of use.
[0030] Although the abrasive composition for polishing of the present invention is able to demonstrate considerable abrasion promotional effects by mixing the three ingredients of antigelling agent, aluminum nitrate and hydrogen peroxide into silicon dioxide, its mechanism is uncertain. However, it is presumed that the effect of dispersing the antigelling agent has mild physical abrading action, the oxidation effect of the hydrogen peroxide serves to amplify the abrasion promotional effect of the aluminum nitrate making chemical abrading action more effective. By mixing these three ingredients, abrasion rate has been confirmed to be higher than the case of mixing any two ingredients, and the occurrence of polishing scratches and pitting has been confirmed to be inhibited.
[0031] In addition to each of the ingredients described above, additives such as surfactant and preservative can also be added to the abrasive composition for polishing magnetic recording disk substrates of the present invention. However, it is necessary to use caution with respect to the types and amounts of additives added so as not to induce gelling.
[0032] Similar to abrasive compositions for polishing of the prior art, the abrasive composition for polishing of the present invention can be produced by suspending silicon dioxide in water and then adding antigelling agent, aluminum nitrate and hydrogen peroxide, etc.
[0033] Although there are no particular restrictions on the type of magnetic recording rigid disk substrate to which the abrasive composition for polishing of the present invention is applied, when the abrasive composition of the present invention is applied to polishing of aluminum (including aluminum alloy) substrates, and particularly aluminum substrates, for example, subjected to electroless plating of NiP, a polished surface of high quality can be obtained due to synergism between the mild physical abrading action produced by the silicon dioxide, and the chemical abrading action produced by the antigelling agent, aluminum nitrate and hydrogen peroxide.
[0034] The polishing method is performed by sliding a polishing pad typically used for slurry abrasive materials over the magnetic recording disk substrate, and rotating the pad or substrate while feeding slurry between the pad and substrate.
[0035] A magnetic recording disk made from a substrate that has been polished by using the abrasive composition for polishing of the present invention has an extremely low frequency of occurrence of minute defects such as micropits and microscratches, surface roughness (Ra) of about 0.2-0.3 nm, and superior evenness.
EXAMPLES
[0036] Although the following provides a detailed explanation of examples of the present invention, the present invention is not limited to these examples.
Examples 1-13
[0037] Water, antigelling agent, aluminum nitrate and hydrogen peroxide were added to colloidal silica (SYTON HT-50F, manufactured by E.I. du Pont de Nemours and Company) in the proportions shown in Table 2 to prepare various aqueous abrasive compositions for polishing, after which polishing was performed with the polishing machine and under the polishing conditions shown below. Those results are shown in Table 2.
[0038] Furthermore, particle size was measured by means of the MICROTRAC UPA 150 (manufactured by Honeywell), which is a laser Doppler frequency analysis type of particle size distribution measuring instrument. Particle size measured values are shown in Table 1.
Examples 14 and 15
[0039] Precipitated silica (Nippon Silica Industrial Co., Ltd., E-150) and fumed silica (Nippon Aerosil Co., Ltd., AEROSIL 50) were ground using a medium stirring mill and coarse particles were removed by grading to prepare silicon dioxide in which the average particle size of the secondary particles was 0.1 μm. Next, water, antigelling agent, aluminum nitrate and hydrogen peroxide were added in the proportions shown in Table 2 to prepare various aqueous abrasive compositions for polishing followed by polishing with the polishing machine and under the polishing conditions shown below. Those results are shown in Table 2. Furthermore, particle size measured values are shown in Table 1.
[0040] Polishing conditions:
[0041] Substrate employed: 3.5-inch aluminum disk electroless-plated with NiP.
[0042] Polishing machine used and polishing conditions:
[0043] Polishing testing machine: 4-way double-sided polishing machine
[0044] Polishing pad: Suede type (POLITEX DG, Rodel Inc.)
[0045] Lower platen rotating speed: 60 rpm
[0046] Slurry feed rate: 50 ml/min
[0047] Polishing time: 5 min
[0048] Working pressure: 50 g/cm 2
[0049] Evaluation of polishing characteristics:
[0050] Abrasion rate: Calculated from the difference in weight before and after polishing the aluminum disk
[0051] Surface roughness: Measured using Talystep and Talydata 2000 (Rank Taylor Hobson Ltd.)
[0052] The depths of polishing scratches and polishing pits were determined by three-dimensional shape analysis using the P-12 surface analyzer equipped with a stylus (TENCOR).
[0053] The results of evaluating polishing characteristics are shown in Table 2. In Table 2, rating “A” refers to cases in which the depth of a polishing scratch or polishing pit is 5 nm or less, while rating “B” refers to cases in which the depth of a polishing scratch or polishing pit is 5-10 nm. There were no polishing scratches or polishing pits having a depth of more than 10 nm in any of the examples or comparative examples.
Comparative Examples 1 and 2
[0054] Water, antigelling agent, aluminum nitrate and hydrogen peroxide were added to colloidal silica (SYTON HT-50F, manufactured by E.I. du Pont de Nemours and Company) in the proportions shown in Table 2 to prepare an aqueous abrasive composition for polishing followed by polishing in the same manner as the examples. Those results are shown in Table 2.
Comparative Example 3
[0055] Titanium oxide (SUPER TITANIA F-2, Showa Titanium Co. Ltd.) was ground using a medium stirring mill followed by removal of coarse particles by grading to first obtain titanium oxide having an average particle size of 0.3 μm. Next, water and aluminum nitrate were added in the proportions shown in Table 2 to prepare an aqueous abrasive composition for polishing followed by polishing in the same manner as the examples. Those results are shown in Table 2. Furthermore, particle size measured values are shown in Table 1.
TABLE 1 Primary Secondary particle size particle size Product name (μm) (μm) Silicon dioxide (1) SYTON HT-50F 0.05 0.05 (Silica (1)) Silicon dioxide (2) E-150J 0.03 0.1 (Silica (2)) Silicon dioxide (3) AEROSIL 50 0.05 0.1 (Silica (3)) Titanium oxide F-2 0.06 0.3 (titania)
[0056] [0056] TABLE 2 Aluminum Hydrogen Abra- Abrasive Antigelling agent nitrate peroxide sion Surface Amount Amount Amount Amount rate roughness Polish- added added added added (μm/ (Ra) Polishing ing Type wt % Type (wt %) (wt %) (wt %) min) (nm) scratches pits Ex- 1 Silica (1) 2 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 1.0 0.11 0.2 A A ample 2 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 1.0 0.20 0.2 A A 3 Silica (1) 15 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 1.0 0.24 0.2 A A 4 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 1.0 5.0 1.0 0.24 0.2 A A 5 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 2.0 5.0 1.0 0.25 0.2 A A 6 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 2.0 1.0 0.18 0.2 A A 7 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 10.0 1.0 0.23 0.2 A A 8 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 0.1 0.12 0.2 A A 9 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 0.5 0.18 0.2 A A 10 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 2.0 0.22 0.2 A A 11 Silica (1) 6 Aminotrimethylene phosphonic acid 0.3 5.0 1.0 0.20 0.2 A A 12 Silica (1) 6 1,10-phenanthroline monohydrate 0.3 5.0 1.0 0.19 0.2 A A 13 Silica (1) 6 cetylacetone aluminum salt 0.3 5.0 1.0 0.19 0.2 A A 14 Silica (2) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 1.0 0.20 0.2 A A 15 Silica (3) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 5.0 1.0 0.20 0.2 A A Comp. 1 Silica (1) 6 — — 5.0 1.0 0.08 0.4 B A Ex- 2 Silica (1) 6 1-hydroxyethane-1,1-diphosphonic acid 0.3 — 1.0 0.09 0.2 A A ample 3 Titania 6 — — 5.0 — 0.21 0.4 B B
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The present invention provides an abrasive composition for polishing magnetic recording disk substrates that results in a low surface roughness of the magnetic recording disk, allows the attaining of high-density recording without the occurrence of protrusions or polishing scratches, and enables polishing to be performed at an economical speed. The present invention discloses an abrasive composition for polishing magnetic recording disk substrates comprising water, silicon dioxide, antigelling agent, aluminum nitrate and hydrogen peroxide.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to co-pending U.S. Provisional Patent Application Ser. No. 60/972,493 filed on Sep. 14, 2007.
GRANT STATEMENT
Research leading to this invention was federally supported by grant No. FA9550-06-1-0125 from the U.S. Air Force Office of Scientific Research. The U.S. government has certain rights in this invention.
TECHNICAL FIELD
The novel technology relates generally to the materials science, and, more particularly, to a method for producing a toughened ceramic material through the dispersal of a second phase therethrough characterized by a generally spiral architecture.
BACKGROUND
Ceramic materials are typically strong in compression but are generally weak in tension or under torsional forces. Typically, ceramic materials fail in tension and/or under torsion via a crack propagation mechanism. Ceramic materials may be toughened by adding a second phase, such as carbon fibers, to form a composite material. However, the addition of such a second phase may complicate the formation process, adding expense. Further, the operating range of both phases may be very different; for example, carbon fibers may oxidize under high temperature refractory conditions and thus may not be an optimal toughening choice for refractory materials. Thus, there remains a need for a means to toughen refractory ceramic materials. The present novel technology addresses this need.
SUMMARY
The present novel technology relates generally to the toughening of refractory ceramic materials, such as zirconium diboride, and, more particularly, to a method and apparatus for preparing and forming two or more dissimilar materials into an architecture consisting of a first phase characterized by interpenetrating spirals dispersed in a second matrix phase. One object of the present novel technology is to provide an improved composite material system. Related objects and advantages of the present novel technology will be apparent from the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 schematically illustrates a process for making a composite material according to a first embodiment of the present novel technology.
FIG. 2 is a schematic view of two sheets of materials made of respective first and second phases rolled together according to FIG. 1 .
FIG. 3 is a schematic view of the extrusion step of FIG. 1 .
FIG. 4 is an enlarged photographic view of the rolled spiral sheets of FIG. 1 .
FIG. 5 tabularly represents several compositions of the present novel technology.
FIG. 6 schematically illustrates a process for making a composite material having spiral silicon carbide members embedded in a zirconium diboride matrix according to a second embodiment of the present novel technology.
FIG. 7A is a photomicrograph illustrating a first composite composition of the present novel technology fired to 1900 degrees.
FIG. 7B is a photomicrograph illustrating a first composite composition of the present novel technology fired to 2000 degrees.
FIG. 7C is a photomicrograph illustrating a third composite composition of the present novel technology.
FIG. 7D is an enlarged photomicrographic view of the embodiment of FIG. 7C .
FIG. 8A is a first photomicrograph illustrating crack propagation in the composition of FIG. 7A .
FIG. 8B is a second photomicrograph illustrating crack propagation in the composition of FIG. 7A .
FIG. 8C is a third photomicrograph illustrating crack propagation in the composition of FIG. 7A .
FIG. 8D is a fourth photomicrograph illustrating crack propagation in the composition of FIG. 7A .
FIG. 9 is a first graph illustrating the toughness of a composite material having a dispersed spiral phase.
FIG. 10 is a second graph illustrating the toughness of a composite material having a dispersed cylindrical phase.
FIG. 11A is a photomicrograph illustrating a composite material having a dispersed second phase characterized by a spiral architecture.
FIG. 11B is a photomicrograph illustrating a composite material having a dispersed second phase characterized by a first alternate geometric architecture.
FIG. 11C is a photomicrograph illustrating a composite material having a dispersed second phase characterized by a second alternate geometric architecture.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
For the purposes of promoting an understanding of the principles of the novel technology, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the novel technology is thereby intended, such alterations and further modifications in the illustrated device, and such further applications of the principles of the novel technology as illustrated therein being contemplated as would normally occur to one skilled in the art to which the novel technology relates.
As generally illustrated in FIGS. 1-11C , the present novel technology relates to a composite material 10 wherein two or more dissimilar materials or phases 15 , 20 are combined into an architecture consisting of interpenetrating first phase members 15 , each characterized by a predetermined, discrete geometry, such as spirals, dispersed in a second phase matrix 20 . This architecture enables the production of high fracture toughness composite materials 10 combining advantageous properties of two or more dissimilar phases 15 , 20 . In addition to increased fracture toughness, the composite material 10 typically enjoys the enhancement of one or more material properties, tailored through the choice of the individual phases 15 , 20 so combined. For example, both thermal shock resistance and oxidation resistance of zirconium diboride 20 are generally improved by the addition of SiC particles 15 having a spiral geometry to the ZrB 2 matrix 20 . Physical properties of the bulk matrix material 10 such as creep resistance, dielectric behavior, thermal conductivity, electrical conductivity, dielectric constant and the like may also be tailored through the material choice, geometry, and orientation of the added particles of the first phase material 15 having a predetermined geometry or geometries.
The properties of the end composite 10 may be influenced by such factors as the physical properties of their constituent phases 15 , 20 , the relative concentrations of the constituent phases 15 , 20 , the orientation of the dispersed phase(s) 15 in the matrix 20 , and the like. For example, if the dispersed phase members 15 are properly and substantially uniformly oriented, some of the physical properties of the resultant composite material 10 may be made highly anisotropic; alternately, if the dispersed phase members 15 are randomly oriented, the physical properties of the resultant composite material 10 may still be altered while remaining isotropic. The present novel technology achieves these results in fewer steps than previous coextrusion techniques, allowing for such benefits as increased processing efficiency, reduced production costs, accelerated production of components and the like.
In one embodiment, the dispersed first phase material 15 may be prepared from powder polymer blends incorporating ceramic or like precursor materials to be formed into predetermined geometric shapes, such as spirals, spheres, cones, cylinders, ellipsoids, cubes, tetrahedrons, parallelepipeds, pyramids, and the like (see FIGS. 11A-C ). Such geometric architectures are achieved by mixing between about 40 and about 60 volume percent of a first desired powder material 25 with a thermoplastic polymer 30 suitable for extrusion (see FIG. 1 ); the about 40 to about 60 volume percent range is typical, although gratifying results may be achieved with compositions outside this range. While in this example the precursor materials 25 , 30 are powders, each respective precursor 25 , 30 may alternately be introduced in liquid form, granular form, or any convenient form. The ceramic and polymer precursor powders 25 , 30 are typically mixed to yield a substantially homogeneous admixture or blend 35 with the ceramic phase 25 dispersed in a polymer matrix 30 . Once a substantially homogenous blend 35 has been formed, the dispersed-phase precursor material 35 is typically formed 37 into a sheet 40 of the desired thickness 42 . This process is then repeated for a second desired powder material 45 to yield sheets 55 of a second composition 60 (a second desired powder material 45 dispersed in a second thermoplastic resin matrix 50 ) and characterized by a second desired thickness 62 . Typically the second desired composition 60 and the second desired thickness 62 will be different from the respective first desired admixture composition 35 and the first desired thickness 42 ; however, one or both may be the same. These sheets 40 , 55 are then layered one on top of the other (typically with alternating compositions) and rolled up 63 , such as from one edge, until a rolled member 65 of the desired diameter is achieved (see FIG. 2 ). The relative thickness 42 , 62 of these sheets, one to another, defines the final geometry 70 of the resultant spiral 80 , as well as the number of turns the spiral 80 will consist of for a given diameter. This rolled member 65 is then consolidated 67 , typically in a cylindrical die, to form a solid billet or feedrod 85 . The feedrod 85 is then extruded 90 , typically in one step, in order to obtain a component 95 of the desired diameter (see FIGS. 3 and 4 ). The extruded filament 95 can then be incorporated into the final product 10 , be it as short chopped lengths 97 , as continuous lengths of filament 98 , or some combination thereof 99 . The added first phase particles 97 may be made of any convenient size. Typically, the particles are between about 25 μm and about 2 cm in diameter, but may be made larger or smaller if desired.
FIG. 5 illustrates in tabular form a few possible matrix compositions. The listings in FIG. 5 are not exhaustive, but are instead intended to represent a few example compositions. It should be noted that the matrix 20 and dispersed phases 15 may be of the same material, with only the geometry of the dispersed spiral phases 15 being different.
An example of the procedure for producing a typical composite material 10 is detailed below. In this example, illustrated as FIG. 6 , the material 10 is a composite of ZrB 2 and SiC, with SiC spirals 15 dispersed in a ZrB 2 matrix 20 . First, about 54 volume percent ZrB 2 powder 25 was blended with a thermoplastic polymer 30 and a small amount of plasticizer 32 (less than 10 volume percent) using a heated high shear mixer until a first homogeneous blend 35 was formed. This process was repeated using (57 volume percent) SiC powder 45 blended with a thermoplastic resin 50 to yield a second homogeneous blend 60 . The first and second respective powder polymer blends 35 , 60 were then each pressed 37 into respective sheets 40 , 55 , each with a thickness of about 20 mils, using a heated hydraulic press and shims to control the final thickness. Strips 100 , 105 about 3 inches wide by about 8 inches long were then cut from each respective sheet 40 , 55 . The SiC strip 105 was placed atop of the ZrB 2 strip 100 and heated 107 to ˜130° C. on a heated platen. After the material became pliable, the strips 100 , 105 were rolled up 63 from one end to yield a rolled member or rod 65 characterized by the spiral architecture. The rod 65 was then placed in a die of about 0.86 inches in diameter, heated to 130° C., and consolidated 67 into a feedrod 85 using a hydraulic press. Using an extruder, the feedrod 85 was then passed through a heated spinneret 90 reducing the diameter to about 300 microns to yield a filament 98 while maintaining the original geometry of the spiral feedrod 85 . The filament 98 was chopped into 1 mm lengths 97 which were then mixed with additional ZrB 2 powder 20 in order to form a mixture 110 that contained about 30 volume percent SiC. This mixture 110 was hot-pressed in order to form the final ZrB 2 -matrix billet 10 containing 30 volume percent SiC spirals. The amount of second phase material 15 added could vary widely from about 5 to about 95 volume percent. The choice of how much of the first phase material 15 is desired to be added to the second phase matrix 20 to produce a desired and advantageous result would depend on the physical property of properties being manipulated. For mechanical properties, a range of between about 20 and about 40 volume percent would typically be selected. For the manipulation of electrical or thermal properties, a range of between about 5 and about 25 volume percent would typically be appropriate.
FIGS. 7A and 7B are photomicrographs illustrating the dispersed first phase spirals 15 in the second phase matrix 20 . FIGS. 8A-8D are photomicrographs graphically illustrating the crack propagation deflection and attenuation properties of the composite materials 10 . As can be seen, crack propagation is blunted by first phase spiral particles 15 , with the crack either stopped or redirected. FIGS. 9 and 10 graphically illustrate the increase in toughness of the composite material 10 over a test material. Typically, the dispersed first phase 15 is characterized by a spiral architecture, although other geometries (cylinders and the like) may likewise prove advantageous. Likewise, the first and/or second phase 15 , 20 may be ceramic, but may also be metallic, polymeric, vitreous, amorphous or the like.
Crack defection can occur for multiple reasons. Often times in ceramics propagating cracks may be deflected or attenuated by running into to a difference in elastic modulus between two phases; likewise, deflection may occur at the interface between two phases when the interface is weaker than either phase. The tensile stresses generated at the interface between two phases of dissimilar thermal expansions can also draw a crack along the interface as opposed to allowing it to propagate across the interface. Differences in fracture toughness between two phases can also lead to crack deflection as a crack tries to propagate from the low toughness phase into the high toughness phase.
While the novel technology has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only the preferred embodiment has been shown and described and that all changes and modifications that come within the spirit of the novel technology are desired to be protected.
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A toughened composite material, having a first phase defining a matrix and a plurality of typically second phase particles dispersed in the first phase matrix. Each respective particle is characterized by a predetermined geometric architecture, such as a spiral shape. The presence of the geometrically distinct dispersed second phase operates to deflect and attenuate crack propagation.
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RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 60/767,574, filed 09/01/2006, which application is hereby incorporated herein by reference.
BACKGROUND
Water, especially in the western United States and other arid regions, is a valuable resource. Many oil and natural gas production operations generate, in addition to the desired hydrocarbon products, large quantities of waste water, referred to as “produced water”. Produced water is typically contaminated with significant concentrations of chemicals and substances requiring that it be disposed of or treated before it can be reused or discharged to the environment. Produced water includes natural contaminants that come from the subsurface environment, such as hydrocarbons from the oil- or gas-bearing strata and inorganic salts. Produced water may also include man-made contaminants, such as drilling mud, “frac flow back water” that includes spent fracturing fluids including polymers and inorganic cross-linking agents, polymer breaking agents, friction reduction chemicals, and artificial lubricants. These contaminants are injected into the wells as part of the drilling and production processes and recovered as contaminants in the produced water.
Commonly encountered non-natural contaminants in produced water, and their sources, are discussed below.
From high-viscosity fracturing operations—gellants in the form of polymers with hydroxyl groups, such as guar gum or modified guar-based polymers; cross-linking agents including borate-based cross-linkers; non-emulsifiers; and sulfate-based gel breakers in the form of oxidizing agents such as ammonium persulfate.
From drilling fluid treatments—acids and caustics such as soda ash, calcium carbonate, sodium hydroxide and magnesium hydroxide; bactericides; defoamers; emulsifiers; filtrate reducers; shale control inhibitors; deicers including methanol and thinners and dispersants.
From slickwater fracturing operations—viscosity reducing agents such as polymers of acrylamide.
Because of the very wide range of contaminant species as well as the different quality of produced water from different sources, efforts to create a cost effective treatment system that can treat or recycle the spectrum of possible produced water streams have little success. For example, while reverse osmosis is effective in treating many of the expected contaminants in produced water, it is not very effective in removing methanol and it may be fouled by even trace amounts of acrylamide.
As another example, there have been many attempts to reclaim produced water and reuse it as fracturing feed water, commonly referred to as “frac water.” Frac water is a term that refers to water suitable for use in the creation of fracturing (frac) gels which are used in hydraulic fracturing operations. Frac gels are created by combining frac water with a polymer, such as guar gum, and in some applications a cross-linker, typically borate-based, to form a fluid that gels upon hydration of the polymer. Several chemical additives generally will be added to the frac gel to form a treatment fluid specifically designed for the anticipated wellbore, reservoir and operating conditions.
However, some waste water streams are unsuitable for use as frac water in that they require excessive amounts of polymer or more to generate the high-viscosity frac gel. For example, trace amounts of spent friction reducers in the stream inhibit the added polymer from gelling. Because it can be difficult to prevent produced water streams from different sources from being co-mingled, this typically results in all produced water from a well field being made unsuitable for recycling as frac water.
An additional problem occurs when the produced water is also contaminated with methanol and it is desirable to discharge the water to the environment. One way to treat produced water to the extent necessary to discharge the water to the environment, is through filtration techniques such as ultra filtration and reverse osmosis. However, methanol will pass through nearly any available membrane filtration technology.
Yet another problem occurs when the produced water is also contaminated with boron, such as from the use of borate-based cross-linking agents, and it is desirable to discharge the water to the environment. One way to treat produced water with boron is referred to as the HERO® process in which the pH is raised up to at least about 11 prior to treatment with reverse osmosis, resulting in the boron being rejected with the reverse osmosis reject brine. However, raising the pH has several undesirable attributes. First, there is increased scaling within the reverse osmosis system increasing the maintenance costs of the system. Second, the pH must then be reduced before the treated water may be discharged to the environment. Third, the cost of the chemicals to raise the pH coupled with the cost of immediately thereafter lowering the pH and the cost of disposal of the precipitated salts resulting from the lowering of the pH make the HERO process very expensive.
SUMMARY
Systems and methods have been developed for reclaiming water contaminated with the expected range of contaminants typically associated with produced water, including water contaminated with slick water, methanol and boron. The system includes anaerobically digesting the contaminated water, followed by aerating the water to enhance biological digestion. After aeration, the water is separated using a flotation operation that effectively removes the spent friction reducing agents and allows the treated water to be reclaimed and reused as fracturing water, even though it retains levels of contaminants, including boron and methanol, that would prevent its discharge to the environment under existing standards. The treated water may further be treated by removing the methanol via biological digestion in a bioreactor, separating a majority of the contaminants from the water by reverse osmosis and removing the boron that passes through the reverse osmosis system with a boron-removing ion exchange resin.
In part, this disclosure describes a method for generating fracturing water from produced water. The method includes transferring produced water contaminated with slick water, methanol and boron into an anaerobic pond and holding the produced water in the anaerobic pond for at least a first mean residence time. The method further includes transferring anaerobic pond effluent to an aeration pond and aerating the anaerobic pond effluent in the aeration pond for a second mean residence time. After aeration, the method includes transferring aeration pond effluent from the aeration pond to a dissolved air flotation treatment system and floating the aeration pond effluent with the dissolved air flotation treatment system to generate a floated aqueous effluent and a separated solids effluent. The method further includes biologically digesting the floated aqueous effluent in a bioreactor until a desired concentration of methanol is obtained. Then, the bioreactor effluent is transferred from the bioreactor to a reverse osmosis system and contaminants are separated from bioreactor effluent with the reverse osmosis system, wherein the reverse osmosis system passes at least some boron in its permeate. Boron is removed from the reverse osmosis permeate via a boron-selective removal process to obtain a desired level of boron in the reverse osmosis permeate.
In part, this disclosure describes a system for treating water contaminated with methanol and boron. The system includes: an anaerobic digestor that receives the water and holds at least a portion of the water under anaerobic conditions; an aerator that aerates the water; a flotation separator that separates contaminants from the water to produce a reclaimed water stream suitable for use as fracturing water; at least one bioreactor that biologically digests methanol in the water until a desired concentration of methanol is obtained; a boron-selective removal system that removes boron from the water until a desired concentration of boron is obtained; and at least one filtration system that removes contaminants from the water until a desired concentration of contaminants other than boron and methanol is obtained.
In part, this disclosure describes a method for removing contaminants from produced water including boron, methanol and contaminants that inhibit the gelling of fracturing fluid. The method includes anaerobically digesting the produced water containing the contaminants for a first period of time and after anaerobically digesting the produced water, aerating the produced water for a second period of time. After aerating the produced water, the produced water is treated by a dissolved air flotation system and the effluent of the dissolved air flotation system is filtered to generate a filtered water containing concentrations of boron and methanol, but that is suitable for use as a fracturing water in that it does require excessively increased amounts of gellant to create the high-viscosity frac gel. The method further provides for biologically digesting the filtered water, thereby reducing the concentration of methanol in the filtered water and separating contaminants from the filtered water using reverse osmosis, in which the reverse osmosis passes at least some undesirable concentration boron in its permeate. The boron is removed from the reverse osmosis permeate via a boron removing ion exchange resin.
These and various other features as well as advantages will be apparent from a reading of the following detailed description and a review of the associated drawings. Additional features are set forth in the description which follows, and in part will be apparent from the description, or may be learned by practice of the described embodiments. The benefits and features will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
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 further explanation of the invention as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
The following drawing figures, which form a part of this application, are illustrative of embodiments systems and methods described below and are not meant to limit the scope of the invention in any manner, which scope shall be based on the claims appended hereto.
FIG. 1 illustrates an embodiment of a system for treating contaminated water.
DETAILED DESCRIPTION
Unless otherwise indicated, all numbers expressing quantities of ingredients, properties such as molecular weight, concentrations, reaction conditions, temperatures, and so forth used in the specification and claims are to be understood as being modified in all instances by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in the light of the number of reported significant digits and by applying ordinary rounding techniques.
The term “residence time” refers to the average length of time that a fluid or particle spends within a process vessel or in contact with a catalyst. For the purposes of this discussion, the mean residence time of a vessel is defined by dividing the volume of liquid in a vessel (e.g., volume in cubic feet) by the volumetric flow rate of the liquid (e.g., in cubic feet per second).
The term “floating” as used herein refer to treating a liquid with a flotation operation to separate solid or liquid particles from a liquid phase. There are several types of flotation operations that are well known in the art including dissolved-air flotation (DAF), air flotation and vacuum flotation.
Fracturing gel or “frac gel” refers to a high-viscosity gel fluid mix for use in fracturing a subterranean formation. The term “fracturing gel” will be used herein to refer to a fluid having a viscosity greater than about 100 centipoise when injected into the subsurface for the purpose of fracturing the subsurface formations. The term “Fracturing water,” as discussed above, refers to the water to which the gellant is added in order to create the fracturing gel. For the purposes of this disclosure, however, a water is suitable for use as fracturing water if it can be mixed with an economical amount of guar gum, relative to other clean water supplies, to create a frac gel. That is, a water is not suitable for use as fracturing water if it requires significantly more polymer (in order to achieve target properties of the frac gel) than other sources of water readily available. Thus, for the purposes of this disclosure, a water is considered suitable for use as fracturing water only if it can be mixed with an amount of polymer (e.g., guar gum, guar gum derivatives, or other commonly applied gelling agent in the fracturing industry, that will create a frac gel) to create a frac gel having a stable viscosity greater than about 50 centipoise at the injection temperature, and the amount of gelling agent required is no more than about 10% greater than that amount required to create the same viscosity using an equivalently salty water, i.e., distilled water mixed with an equivalent amount of salt content as the purported fracturing water.
Slick water, on the other hand, refers to a relatively low viscosity aqueous fluid used also for fracturing a subterranean formation. The term “slick water” as used herein further refers to low viscosity (i.e., a viscosity less than that used for frac gels) fluid to which friction reduction agents have been added to modify the flow characteristics of the fluid. For example, slick water is often created by adding a small amount of polymer to water in order to change the flow characteristics of the resulting aqueous mixture. Such friction reduction agents include, but are not limited to, polyvinyl polymers, polymethacrylamides, cellulose ethers, polysaccharides, lignosulfonates, and ammonium, alkali metal, and alkaline earth salts thereof. Specific examples of typical water soluble polymers are acrylic acid-acrylamide copolymers, acrylic acid-methacrylamide copolymers, polyacrylamides, partially hydrolyzed polyacrylamides, partially hydrolyzed polymethacrylamides, polyvinyl alcohol, polyvinly acetate, polyalkyleneoxides, carboxycelluloses, carboxyalkylhydroxyethyl celluloses, hydroxyethylcellulose, galactomannans (e.g., guar gum), substituted galactomannans (e.g., hydroxypropyl guar, carboxymethyl hydroxypropyl guar, and carboxymethyl guar), heteropolysaccharides obtained by the fermentation of starch-derived sugar (e.g., xanthan gum), and ammonium and alkali metal salts thereof. Preferred water-soluble polymers include hydroxyethyl cellulose, starch, scleroglucan, galactomannans, and substituted galactomannans. For example, copolymers of acrylamides are disclosed as good friction reduces in U.S. Pat. No. 3,254,719 and U.S. Pat. No. 4,152,274, which disclosures are hereby incorporated herein by reference. An example of an acrylamide-based friction reducer includes that sold under the product name FRW-14 by BJ SERVICES COMPANY. Others are well known in the art.
It should be noted that both fracturing fluids and slick water may include other compounds such as demulsifiers, corrosion inhibitors, friction reducers, clay stabilizers, scale inhibitors, biocides, breaker aids, mutual solvents, alcohols, surfactants, anti-foam agents, defoamers, viscosity stabilizers, iron control agents, diverters, emulsifiers, foamers, oxygen scavengers, pH control agents, and buffers, and the like.
When referring to concentrations of contaminants in water or to water properties such as pH and viscosity, unless otherwise stated the concentration refers to the concentration of a sample properly taken and analyzed according to standard Environmental Protection Agency (EPA) procedures using the appropriate standard test method or, where no approved method is available, commonly accepted methods may be used. For example, for Oil and Grease the test method identified as 1664A is an approved method. In the event two or more accepted methods provide results that indicate two different conditions as described herein, the condition should be considered to have been met (e.g., a condition that must be “above pH of about 7.0” and one accepted method results a pH of 6.5 and another in pH of 7.2, the water should be considered to be within the definition of “about 7.0”).
FIG. 1 illustrates an embodiment of a system for treating contaminated water. The contaminated water may be produced water 120 generated by oil field operations or waste water from some other industrial or residential source. The system 100 is illustrated and discussed below as a continuous flow system. However, in an alternative embodiment some or all of the processes of the system 100 may be operated as batch processes.
In the embodiment shown, the contaminated water is produced water 120 generated from oil, gas or other subsurface extraction operations. In an embodiment, the produced water is contaminated with methanol and boron derived either from natural sources in the subsurface or added as part of the extraction operations.
In an embodiment, the system of FIG. 1 is anticipated to receive produced water having at least about 7,000 milligrams per liter (mg/l) of total dissolved solids (TDS), at least about 10 mg/l of boron, and at least about 500 mg/l methanol, although the system could be used to treat less contaminated water as well. Furthermore, as discussed in greater detail below, the effluent of the system 100 is desired to contain less than about 500 mg/l of TDS, less than about 2 mg/l boron, and less than about 1 mg/l methanol. Preferably, the system 100 can accept any produced water of any quality. In testing, waste water, including produced water with the following ranges of contaminant as provided in Table 1 concentrations, were treated.
TABLE 1
Parameter
Range
TDS @ 180 C., mg/l
up to at least 8830
TSS @ 105 C., mg/l
up to at least 141
Turbidity, NTU
up to at least 239
TOC, mg/l
up to at least 1130
COD, mg/l
up to at least 5750
BOD, mg/l
up to at least 1820
pH
up to at least 7.21
Iron, mg/l
up to at least 0.3
Chloride, mg/l
up to at least 4310
Potassium, mg/l
up to at least 59.2
Calcium, mg/l
up to at least 78.5
Magnesium, mg/l
up to at least 9.1
Sodium, mg/l
up to at least 2750
Sulfate, mg/l
up to at least 26
Carbonate, mg/l
ND as CO 3
Bicarbonate, mg/l
up to at least 459 as HCO 3
Boron, mg/l
up to at least 11.6
Methanol, mg/l
up to at least 610
In an embodiment, the produced water 120 may also be contaminated with slick water and thus may contain friction reducers such as acrylamides. Such contaminants are relevant in that they are hard to remove, foul many treatment operations such as reverse osmosis systems, and inhibit the formation of fracturing gels if the contaminant exists in sufficient concentration in fracturing water.
The system 100 is designed in anticipation that the produced water 120 is likely to contain these contaminants at all times or intermittently.
The system 100 receives the produced water 120 and may temporarily store it, such as in a holding tank, before beginning active treatment. The produced water 120 may be received via truck, pipeline, surface flow or any other suitable method. Produced waters 120 from different sources may also be received and co-mingled immediately or independently treated until the anaerobic treatment stage discussed below. As the system is adapted to treat any type of expected contaminant, this is an advantage over other systems that are tailored to specific water qualities from specific wells or sources.
The produced water 120 may be treated with a gravity separator, such as an API separator as shown, to remove immiscible phases of oil and grease. Gravity separation is well known and any suitable gravity separation system, e.g., API separator design, gunbarrel separator or gravity clarifier, may be used.
The aqueous separator effluent 122 then is transferred to the anaerobic treatment system 104 for anaerobic digestion of contaminants. In an embodiment, an anaerobic pond may be used as the anaerobic treatment system or as part of the anaerobic treatment system 104 . Anaerobic ponds are known in the art and refer to a deep pond that maintains anaerobic conditions at depth, except for a shallow (typically less than about 2 feet) surface zone. In an embodiment, some oxygen may be added to water contained in the anaerobic pond through spray evaporation and ambient contact with air, as long as very little dissolved oxygen is achieved below 2 feet of depth to ensure that the conditions at depth remain anaerobic. In an embodiment, other than mixing incidental to the mixing of the effluent 112 with the contents of the anaerobic treatment system 104 vessel, no additional mixing or aeration is provided by the operators.
The anaerobic treatment system 104 treats the water by anaerobic conversion of organic wastes into carbon dioxide, methane, other gaseous end products, alcohols possibly including methanol, and organic acids. Inorganic wastes may also be anaerobically converted. Some separation will occur in the anaerobic treatment system 104 due to precipitation of converted contaminants as well as via settling. In operation, it was noted that anaerobic digestion served at least two beneficial purposes. First, it typically reduced chemical oxygen demand (COD) by 30% or more and usually by at least 50%. However, it notably did not reduce biological oxygen demand (BOD) by very much. Second, anaerobic digestion reduced the ratio of COD to BOD from the initial value (typically around 3:1) to 2:1 or less.
In an embodiment, the water is treated in the anaerobic treatment system 104 based on residence time. A mean residence time of at least about 50 days has been found to be effective. Larger mean residence times are also effective. In an alternative embodiment, an alternative benchmark or combination of benchmarks may be used to determine if sufficient treatment has occurred, such as a targeted COD reduction relative to the inlet amount (e.g., at least about 15% reduction, or at least about 30% or at least about 50% reduction criteria) or threshold COD to BOD ratio being achieved. A combination benchmark may include a minimum of 50 days residence time and any other benchmark such as COD concentration.
Effluent 124 from the anaerobic treatment system 104 is transferred to an aeration system 106 , which may also be referred to as an aerator 106 . The aeration system 106 actively aerates the water to allow the biological digestion of contaminants in the water over time. In an embodiment, the aeration system 106 treats the water for a mean residence time of at least about 5 days with mean residence times of 5 to 10 days being one treatment target. During treatment, the dissolved oxygen of the system is monitored and the aeration is adjusted to maintain a dissolved oxygen concentration above at least 50% of the solubility limit of oxygen in water at the aeration system 106 temperature, preferable above 75% of the solubility limit and more preferable above 90% of the solubility limit. However, the target dissolved oxygen concentration used may be balanced against the cost of providing the aeration and current throughput needs of the system.
In an embodiment, no supplemental nutrients for bioremediation are added in the aeration treatment step. The amount of aeration may be controlled based on measurement of dissolved oxygen of the water in the aeration system 106 . Aeration may also be controlled based on the effectiveness of the flotation treatment and water quality of the flotation treatment effluent 128 . Submerged combustion heaters, or other heat sources, may be used to raise water temperature as desired, such as in the winter to prevent water freezing if the aerator 106 is an outdoor pond.
In addition to biological digestion, it is believed that some oxidation or other aerobic conversion of some contaminants occurs in the aeration system 106 . In an embodiment, a benchmarks to determine proper aeration may include a minimum residence time at a specific rate of aeration and temperature, a reduction of BOD to below a target threshold (e.g., less than about 1300 mg/l, or more preferably less than about 1000 mg/l), a reduction of sulfate to below 10 mg/l sulfate, a reduction of 50-75% of the input concentration of sulfate in the anaerobic treatment system effluent 124 , and/or a reduction in barium to less than 1 mg/l. However, as mentioned above, sufficient aeration is primarily indicated by the effectiveness of the flotation treatment and water quality of the flotation treatment effluent 128 .
In the aeration system 106 , aerobic digestion of trace metals occurs helping to clarify these compounds and serves many beneficial functions. First, aerobic digestion of trace metals occurs helping to clarify these compounds. This was evidenced by analyses of sludge taken with insufficient aeration and sufficient aeration showing that insufficient aeration resulted in leachable barium (determined by the TCLP analysis) being found in the sludge whereas, under conditions of proper aeration, leachable barium was reduced below the detection limit.
Experimental data suggest that the aeration step does reduce the COD and BOD of the water being treated, but, without being bound to any particular theory, the aeration step also appears to cause a change in the nature of the COD which increases the effectiveness of the flotation system 108 in removing contaminants. This was evidenced by experiments in which insufficiently aerated effluent from the aeration system 106 was transmitted to the flotation system 108 and it was found that the flotation system's ability to coagulate and separate contaminants was drastically reduced. Notably, another effect of insufficient aeration observed during testing was that the resulting COD that was passed by the DAF 108 fouled the bioreactor 112 . Proper aeration eliminated this fouling. Without being limited to a particular theory, it is believed that the COD in produced water contaminated with frac flow back water is at least in part due to long chain acrylamide polymers, fragments of frac gel and other stimulation chemicals, that can be floated out in the DAF, but only after conversion by the digestion operations 104 , 106 .
In an embodiment, an aeration pond is used as the aeration system 106 . Aeration ponds are known in the art. An aeration pond is typically a large, shallow earthen basin provided with some means for actively aerating the water contained in the pond. Types of active aeration using air include sprayers that spray the water into the air and forced air injection via diffusers submerged in the pond attached to floating aerators. Many other aeration means are known in the art; any suitable means for aerating the water may be used.
Aeration system effluent 126 is transferred, with heat as needed for proper operation, to a flotation separator 108 . The flotation separator 108 separates solid particles from the aqueous phase by introducing fine gas bubbles into the aqueous phase. The bubbles attach to the particulate matter and the buoyant force of the combination is great enough cause the particle to rise to the surface and subsequently be skimmed off or otherwise mechanically separated from the aqueous phase.
Flotation separators 108 are well known in the art. In experiments, a dissolved air flotation (DAF) separator was used to float and separate particulates from the aqueous phase, however there is no reason to believe that other flotation separators, such as air flotation or vacuum flotation systems, may not also be effective. In embodiments that utilize a DAF separator, any suitable DAF design, now known or later developed may be utilized. For example, a three vessel DAF in which coagulant is added in the first vessel, the flocculant is added in the second vessel and the third vessel is the actual flotation chamber in which air is added and separation occurs.
Furthermore, any DAF additives may be used as determined to be experimentally suitable in increasing the effectiveness of the DAF separator in removing contaminants. Commercially available coagulants were used to assist the coagulation and increase the performance of the DAF. In an embodiment, Ashland Chargepac 55 with a dose rate between 100 and 200 ppm was used as the coagulant and flocculant polymer was mixed from Ciba Magnafloc 336 and then diluted to a final dose rate of 2 to 7.5 ppm. Preferably, the DAF separator is operated above 35 degrees F. and more preferably at about 55 degrees F. In an embodiment, the DAF separator is operated as necessary to obtain an effluent 128 with an NTU level of less than about 10 NTU.
In the embodiment shown, the aqueous effluent 128 of the flotation separator 108 is further clarified by passing the effluent 128 through a filtration system 110 . Additionally, the effluent 128 may be monitored, such as via a turbidity meter, conductivity sensor or other monitoring device. If the observed level does not meet the desired level of treatment, the effluent 128 may be recycled to an earlier treatment operation. Furthermore, at any point after the aerobic digestion, a biocide may be introduced to eliminate microbes and promote removal of same, such as in the DAF separator 108 or the filtration system 110 or prior to shipment to a frac system.
In the embodiment shown, a sand filter, nominally effective as a 10 micron filter, was used as the filtration system 110 to achieve a turbidity of less than about 5 NTU and preferably less than about 1 NTU. Other filtration designs may also be used. Effluent 128 from the DAF separator 108 may be feed via gravity through the filters 110 to a lift station that transfers water to one or more intermediate surge tanks. In order to achieve the desired level of treatment, one or more separate filters may be utilized in series or in parallel. In an embodiment, each sand filter may be equipped with a sight glass to show the operator how much head is developing in the filter and also with an inline turbidity meter to directly measure filter performance. When the feed water level in the filter reaches the high tank level switch a backwash cycle may be initiated by a programmable logic controller (PLC) that monitors operation of the filters or the system as whole. The back wash cycle may also be triggered manually or based on the readings of the turbidity meter. Back wash water and overflow from the sand filter inlet may be recycled to any prior treatment operation as desired by the operator.
The effluent 130 , 132 of the filtration system 110 is suitable for use as a fracturing water even though in experiments it still contained significant concentrations of COD, total organic carbon (TOC), TDS, and biological oxygen demand (BOD). Its use as a fracturing water was evidenced by the ability to gel sufficiently when combined with polymers to create a high-viscosity fracturing gel. Without being bound to a particular theory, it is believed that trace amounts of the friction reducers from slick water impair the gelling reaction. These friction reducers are also very difficult to remove using either anaerobic or aerobic treatment alone and also difficult to remove without the use of flotation. Indeed, it is believed the combination of anaerobic, aerobic and flotation treatment operations is the most effective way of reclaiming produced water that is unsuitable for use as fracturing water and convert it into water that is suitable for use as a fracturing water.
Typical and target values of contaminant concentrations for fracturing water 130 , 132 obtained from the system 100 are provided below in Table 2.
TABLE 2
Parameter
Range
Target
TDS @ 180 C., mg/l
9,000-16,000
<10,000
TSS @ 105 C., mg/l
0-100
<75
Turbidity, NTU
0-5
<1
TOC, mg/l
400-800
<700
COD, mg/l
1000-3000
<2000
BOD, mg/l
500-1500
<1000
pH
6.5-8
7-7.5
Iron, mg/l
1-10
<5
Chloride, mg/l
5,000-10,000
<6,000
Potassium, mg/l
100-500
<300
Calcium, mg/l
50-250
<150
Magnesium, mg/l
10-100
<25
Sodium, mg/l
2000-5000
<3000
Sulfate, mg/l
40-200
<50
Carbonate, mg/l
0-100
<25
Bicarbonate, mg/l
100-1200
<800
Boron, mg/l
0-20
<15
In the embodiment shown in FIG. 1 , in addition to generating water suitable for reuse as fracturing water, additional treatment operations are provided that treat the produced water to a quality sufficiently clean for discharge to the environment. Thus, the depending on the need for frac water, the system 100 may be operated so that more or less frac water 130 is produced from the produced water 120 stream. Any surplus of unused frac water 130 may then be treated by the remaining portions of the system 100 to a water quality that allows the water to be discharged to the environment.
Treatment of the frac water 130 , 132 to a quality suitable for discharge to the environment requires that the system 100 address methanol and boron concentrations. Methanol is often a contaminant in produced water. In addition, anaerobic digestion may produce methanol from the digestion of guar gels. Testing has shown that in the system shown in FIG. 1 while some methanol reduction (e.g., at the top of the pond) may occur under certain conditions during the anaerobic treatment operation, methanol may be treated significantly during the aeration treatment. However, the aeration system 106 as described can not be depended to sufficiently treat all of the methanol in the produced water. This variability may be due to lack of nutrients, composition of the particular inlet produced water being treated or the ambient weather conditions under which the aeration treatment is being operated.
In the embodiment shown, the system 100 further provides for the effluent 132 of the filtration operation to be transferred to one or more bioreactors 112 , 114 for the biological digestion of the effluent 132 . Biological digestion of the effluent 132 drastically reduces the concentration of the methanol in the water. In an embodiment, the biological digestion of the effluent 132 is performed for a duration sufficient to reduce the methanol to below the target discharge limit or alternatively to a level at which the methanol can no longer be detected.
In the embodiment shown, two stages of biological digestion are performed. First, a bioreactor 112 may be used to perform the majority of the biological digestion. In an embodiment, the bioreactor may be an enclosed vessel, such as a steel tank with internal epoxy coating and standard tank roof with appropriate vents. Coarse bubble diffusers may be mounted on the bottom of the tank with air supplied by compressors. The bioreactor 112 may or may not be heated as needed to maintain a healthy biological environment for digestion. Additionally, nutrients may be added, such as gaseous ammonia for nitrogen and phosphoric acid for phosphorous, as necessary. In an embodiment, a residence time may be chosen so that methanol is completely eliminated or reduced to a desired concentration in the bioreactor 112 . The design and operation of bioreactors are well known in the art and any suitable design may be utilized as part of this operation.
In the embodiment shown, a second, and optional, stage of combined biological digestion and filtration is provided in which the effluent 134 of the bioreactor 112 is transferred to a membrane bioreactor (MBR) 114 as shown. The MBR 114 provides additional biological digestion as well as removing by filtration some contaminants contributing to TOC concentrations in the water 134 . Cleaned water (permeate 136 ) is extracted through the membranes of the MBR 134 . In an embodiment, reject from the MBR 114 may be returned to the bioreactor 112 for additional digestion or to any other prior treatment stage. Any suitable membrane bioreactor design may be utilized, for example a hollow fiber membrane bioreactor such as that sold by ZENON under the trademark ZEEWEED is suitable for use as the MBR 114 .
Permeate 136 of the MBR 114 is transferred to an RO system. In the embodiment shown, a reverse osmosis (RO) system 116 is used to filter the remaining TOC, TDS and other contaminants from the permeate 136 to a level acceptable for discharge, except boron. RO systems 116 are well known in the art and any design, now known or later developed, may be utilized.
Notably, where the pH of the water is not raised, such as for the purposes of precipitating out contaminants, in the prior operations such as is necessary in the HERO process. In an embodiment, there may be some minor reduction of pH in order to maintain the proper conditions within the bioreactor. This, however, does not cause the precipitation of any contaminants, but rather increases the solubility of some contaminants. The pH of the RO permeate 138 will be dictated primarily by the pH of the produced water 120 . Thus, the pH of the RO permeate 138 will generally be much lower than the permeate of the RO in a HERO process. Preferably the RO permeate 138 in the system 100 will be less than about 10.0, still yet less than about 9.0 and even more advantageously less than about 8.0 and greater than about 6.5.
By avoiding lime softening, the production of waste solids by the system 100 is significantly lower in comparison. Other than solids derived from the original contaminants in the produced water feed, the major source of solids generated as a result of the treatment operations is due the use of liquid coagulant in the DAF. This represents a significant cost savings over systems and processes that actively adjust the pH through chemical addition as part of the treatment.
However, because of the pH range at which the RO 116 is operated as described above, boron will not be removed from the water by the RO system 116 in quantities sufficient to meet the desired discharge concentration. In experimental analyses, MBR effluent 136 contained roughly the same concentration of boron as the produced water 120 . The RO system 116 is expected to pass a significant portion of the boron in the stream—a portion that is expected to be beyond the limits necessary to discharge the boron to the environment.
In the system 100 of FIG. 1 , boron is removed from the RO permeate 138 by means of a boron-selective treatment system 118 . In an embodiment, the boron selective treatment system 118 is an ion-exchange resin adapted to optimally remove boron from an otherwise relatively clean aqueous stream. One example of such a resin suitable for use in the systems described herein is that offered by Dow Chemical under the trade name of XUS-43594.00, now alternately referred to under the trade name BSR1, which is marketed as a uniform particle size weak base anion exchange resin for selective boron removal. Other boron-selected resins known in the art include the product MK-51 sold by SYBRON and S-108 sold by PUROLITE. Other systems that are effective for removing boron may also be used, whether now known or later developed. In fact, because the RO permeate 138 is substantially clean except for the boron, any effective boron removal system may be used without worry of fouling or degradation due to other contaminants.
Effluent 140 of the boron-selective treatment system 118 will be of sufficient quality to be discharged to the environment. Exemplified target values of contaminant concentrations for effluent 140 from an embodiment of the system 100 are provided below in Table 3. If, upon testing, the values are outside of the target ranges, the effluent 140 may be recycled to one of the treatment operations until the effluent 140 quality meets the discharge requirements.
TABLE 3
Parameter
Range
TDS
<500
mg/l
TOC
<5
mg/l
Boron
1-2
mg/l
pH
6.5-9.0
Oil &Grease
<10
mg/l
Radium 226
<60
mg/l
Chlorides
<230
mg/l
Various waste streams other than the primary aqueous streams discussed may be disposed in any suitable manner. For example, reject from the RO system 116 may be used as backwash for prior treatment systems, shipped to the oilfield for use as frac water, returned to the treatment flow for reprocessing and further concentration or disposal via injection well. As a further example, in embodiments using an ion-exchange resin for boron removal, the boron-laden regenerate from the ion-exchange regeneration may be blended with RO reject fluid to neutralize the regenerate and injected in the disposal well.
In an embodiment, some or all of the operations of the treatment system may be automated used process controllers, automated transfer pumps, flow control valves, sensors and other equipment as is known in the art.
The fracturing water 130 output of the system 100 may be stored in holding tanks prior to transfer to a fracturing gel production system via pipeline or truck to a wellhead or other location where fracturing chemicals are added to generate fracturing gel. Similarly, the boron-selective treatment system effluent may be discharged to a holding tank for confirmation testing prior to discharge.
Those skilled in the art will recognize that the methods and systems of the present disclosure may be implemented in many manners and as such are not to be limited by the foregoing exemplary embodiments and examples. In other words, functional elements being performed by a single or multiple components, in various combinations. In this regard, any number of the features of the different embodiments described herein may be combined into single or multiple embodiments, and alternate embodiments having fewer than or more than all of the features herein described are possible.
While various embodiments have been described for purposes of this disclosure, various changes and modifications may be made which are well within the scope of the present invention. For example, between one or more of the treatment operations described herein, transfer pumps, surge tanks, control valves, heaters, and other equipment may be provided to assist the efficient operation and maintenance of the system and to provide for various contingencies such as surges, cleaning operations, recycling of flow, bypassing of operations, and low or high ambient temperatures. As a specific example, water being transferred between any two operations may be analyzed and recycled to a previous stage if certain contaminant concentrations are out of a predetermined desired range. Additionally, if the system is operated as a continuous flow system, surge tanks and overflow capacity may be provided at different points within the system to allow for the system throughput to managed as necessary to obtain the proper water quality at each stage of treatment.
Numerous other changes may be made which will readily suggest themselves to those skilled in the art and which are encompassed in the spirit of the invention disclosed and as defined in the appended claims.
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Systems and methods have been developed for reclaiming water contaminated with the expected range of contaminants typically associated with produced water, including water contaminated with slick water, methanol and boron. The system includes anaerobically digesting the contaminated water, followed by aerating the water to enhance biological digestion. After aeration, the water is separated using a flotation operation that effectively removes the spent friction reducing agents and allows the treated water to be reclaimed and reused as fracturing water, even though it retains levels of contaminants, including boron and methanol, that would prevent its discharge to the environment under existing standards. The treated water may further be treated by removing the methanol via biological digestion in a bioreactor, separating a majority of the contaminants from the water by reverse osmosis and removing the boron that passes through the reverse osmosis system with a boron-removing ion exchange resin.
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[0001] This application claims the benefit of European Application No. 05025846.6 filed Nov. 26, 2005. This application is a Divisional of U.S. patent application Ser. No. 11/602,779 filed Nov. 21, 2006, currently pending, entitled “New Polymer Concentrates with Improved Processability”, the contents of which are hereby incorporated by reference in their entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to new polymer concentrates containing (1) one or more polymer additive(s) and (2) one or more polymer(s) which comprise repeating units of ethylene, vinyl acetate and optionally one or more other monomers. The invention also relates to a process for preparing such new polymer concentrates, a process for preparing polymer compounds comprising the new polymer concentrates, the resulting polymer compounds, a process for preparing formed parts thereof and the formed parts.
BACKGROUND OF THE INVENTION
[0003] Mineral hydroxides are an important class of polymer fillers used in particular as flame retardants. Aluminium trihydroxide and magnesium dihydroxide are the major examples of this class of fillers. However, these hydroxides as well as other finely powdered polymer fillers or additives present problems in handling and particularly in compounding into polymers. Ideally, a finer particle size of solid polymer additives should lead to better dispersion in the polymer matrix, and better dispersion equates to more efficient, uniform performance and improved polymer physical properties. Therefore, the solid polymer additives often have particle sizes reduced to less than 10 μm. On the other hand, finer particles are often more difficult to disperse and problems of reagglomeration occur.
[0004] Additionally the general handling of finely powdered polymer additives presents particular problems. One substantial problem of finely powdered polymer additives is dusting. The creation of dust involves loss of raw material, increased clean-up costs, and health concerns for those handling the solids.
[0005] Another problem is bulk density. Finer solids tend to have decreased bulk density and increased packaging size, volume and cost. The fluffy nature and low bulk density of finely powdered polymer additive solids adversely affects additive flow properties, making them more difficult to meter when using continuous compounding equipment, such as twin screw extruders, but also making general handling difficult. More specifically, poor solids mixing homogeneity results in poor performance in general, for example poor physical properties in the final product. Finer solids tend to lead to, for example, poor physical properties in the final product.
[0006] One prior art approach to increasing the mixing homogeneity in the addition of low bulk density solids to polymers involves adding a liquid, such as a plasticizer, to the powder, prior to mixing the powder with the polymer.
[0007] Blending the additive powder into the polymer in the form of a masterbatch concentrate that can be diluted with more polymer to achieve the desired final concentration of powder additive is a further common approach. It decreases dusting during the ultimate polymer processing step. However, it not only adds a costly additional step, but it also does not deal with the problem of poor mixing of a low bulk density additive powder and a polymer in forming the masterbatch concentrate. In fact, the masterbatch sometimes has poorer homogeneity because a higher proportion of incompatible fine powder is added. This method also has a disadvantage for fillers which are used in substantially larger amounts, such as flame retardants, due to the large amount of polymer carrier that is included in the final compound.
[0008] The approach described in U.S. Pat. No. 4,849,134 to solving these problems is cold compaction of the filler. The disadvantage of this method is that compaction (re-)agglomerates the fine particles of the additive. Unless subsequent polymer processing conditions result in complete breakup of the coarse compacted, i.e. agglomerated particles and dispersion into the polymer, any advantage of the fine particles is lost.
[0009] The aim of increasing the bulk density of fine polymer fillers and in particular flame retardants, flame retardant synergists, blends thereof, and other powdered polymer additives has significant value. These additives are included in an amount of about 1% by weight to about 60% by weight, often 10-40% by weight, into a finished polymeric article.
[0010] Certain advantages of a lower bulk density polymer additive upon processing of one polymer, PVC, are referred to in U.S. Pat. No. 3,567,669. This patent discloses a high speed mixing process which requires a temperature of at least 170° F. Under these conditions, the PVC particles have a slightly sintered or glazed surface. Solid additives are absorbed or adsorbed onto the polymer surface.
[0011] U.S. Pat. No. 3,663,674 discloses densification of poly-α-olefins. Such poly-α-olefins are prepared in a dense granular form suitable for moulding or extrusion by the application of sufficient mechanical energy to compress and collapse the porous polymer particles recovered from the polymerisation reactor. Cited advantages of increased bulk density are improved handling characteristics and the lack of a thermal history prior to processing. No mention is made of the effect of the bulk density of powdered additives upon the processability or properties of the polymer. Nor is there any mention of the use of flame retardants or flame retardant synergists.
[0012] Based upon the teachings of the U.S. Pat. No. 3,567,669 and U.S. Pat. No. 3,663,674 it was therefore the object of the present invention to provide new concentrates of polymer additives, in particular fillers and flame-retardants, and polymers which new concentrates possess an enhanced processability, show an improved dispersability of the additive throughout the polymer and eventually result in improved properties of the formed parts prepared by processing polymer compounds containing the new concentrates.
SUMMARY OF THE INVENTION
[0013] The present invention is directed to a concentrate containing
(1) one or more polymer additives and (2) one or more polymers which comprise repeating units of ethylene, vinyl acetate and optionally one or more other monomers,
wherein
(a) the concentrate contains less than 10% by weight of one or more polymers (2), based on the total weight of the polymer additive(s) (1) and the polymer(s) (2), and (b) the concentrate is obtainable by mixing the polymer additive(s) (1) with a solution of the polymer(s) (2) in a solvent and removing the solvent, (c) the mean primary particle size (“d 50 ”) of the polymer additive(s) (1) prior to the mixing with the solution of the polymer(s) (2) is less than 10 μm and (d) the concentrate has a bulk density which is at least 50% greater than that of the polymer additive(s) (1) prior to the mixing with the solution of the polymer(s) (2), wherein such bulk density is measured in accordance with DIN ISO 697 from January 1984.
[0020] The present invention is further directed to a process for preparing the concentrates by mixing the polymer additives (1) with a solution of the polymer(s) (2) and removing the solvent.
[0021] Eventually the present invention is directed to the use of the inventive concentrates for preparing polymer compounds, to a process for preparing polymer compounds comprising the concentrates, a process for preparing formed parts on the basis of such polymer compounds and the formed parts.
BRIEF DESCRIPTION OF DRAWINGS
[0022] For a fuller understanding of the nature and advantages of the present invention, reference should be had to the following detailed description taken in connection with the accompanying drawings, in which:
[0023] FIG. 1 : is a chart of the particle size distributions for Examples 2b to 2f.
DETAILED DESCRIPTION OF THE INVENTION
[0024] The polymer additive(s) (1) used to prepare the inventive concentrates have a finely powdered form. The mean primary particle size (also abbreviated as “d 50 ”) of the polymer additive(s) (1) prior to subjecting the polymer additive(s) (1) to the preparation of the inventive concentrate is less than 10 μm, preferably less than 5 μm, particularly preferred less than 2.5 μm.
[0025] The term “mean primary particle size” (“d 50 ”) means that at least 50% of the polymer additive particles have a particle size less than 10 μm, preferably less than 5 μm, and particularly preferred less than 2 μm, and most preferably 0.5-1.5 μm. This mean primary particle size is typically measured by laser diffraction e.g. by using a Malvern Mastersizer S.
[0026] The polymer additives (1) which may be used to prepare the inventive concentrates may be e.g. fillers, flame-retardants, flame-retardant synergists, pigments or other finely powdered polymer additives or any mixtures thereof. This includes mixtures of different types of polymer additives (1) may be used, e.g. a mixture of a filler and a flame-retardant or a mixture of a filler, a flame-retardant, and a flame-retardant synergist. Such polymer additives (1) are known and commercially available. Usually it is not necessary to further reduce the particle size of the polymer additives (1) available.
[0027] As flame-retardants aluminium trihydroxide (ATH), magnesium hydroxide, antimony trioxide, or mixtures thereof are e.g. suitable.
[0028] As flame-retardant synergists zinc borate, antimony trioxide, sodium antimonate, or mixtures thereof are suitable to additionally enhance the efficiency of the flame-retardant itself.
[0029] Suitable fillers subjected to the preparation of the inventive concentrates include carbon black, graphite, metal powders, talc, clays, mica, wollastonite, silica, calcium carbonate, hydrated minerals, boron-containing compounds, zinc-containing compounds, antimony-containing compounds, and mixtures thereof.
[0030] As pigments which can also be used in the present invention for example iron oxides and titanium dioxide are mentioned.
[0031] The polymer(s) (2) used to prepare the inventive concentrates comprise repeating units of ethylene, vinyl acetate and optionally one or more other monomers. Such polymers are commercially available and are typically produced by radical initiated polymerisation of ethylene, vinyl acetate and optionally one or more other monomers. Some commercial materials may also contain minor amounts of a third monomer such as acrylic acid or esters thereof. Such polymers are described in detail in Ullmann's Encyclopedia of Industrial Chemistry 5 th . Ed. 1993, VCH Verlagsgesellschaft, Vol. 23, page 241 ff and the references cited therein. In particular, these polymers can be prepared in solution, for example in tert. butanol or methanol. Before isolation of the polymer these processes yield a solution of polymer and unreacted monomer in the respective solvent. Such solutions may be also be used in order to prepare the inventive concentrates.
[0032] The polymers (2) used may contain 40 to 90% by weight, preferably 60 to 80% by weight vinyl acetate and 10 to 60% by weight, preferably 20 to 40% by weight ethylene. In said polymers a percentage of the vinyl acetate and/or ethylene may be replaced by one or more further monomers, e.g. 10 to 50% by weight of one or more further monomers, wherein the sum of all monomers in the polymer(s) (2) still has to give 100% by weight
[0033] Further monomer(s) encompass, but are not limited to, alkyl esters of unsaturated mono- or di-carboxylic acids. Fumaric or maleic acid mono- or di-ethyl esters are particularly suitable.
[0034] It is an important feature of the invention that the concentrate contains less than 10% by weight of one or more polymers (2), based on the total weight of the polymer additive(s) (1) and the polymer(s) (2). Preferably the concentrate contains 2 to 10% by weight, particularly preferred 3 to 8% by weight and most preferably 3 to 6% by weight of one or more polymers (2), based on the total weight of the polymer additive(s) (1) and the polymer(s) (2).
[0035] The second object of this invention is a method of preparing such concentrates containing
(1) one or more polymer additives and (2) one or more polymers which comprise repeating units of ethylene, vinyl acetate and optionally one or more other monomers,
comprising
mixing the polymer additive(s) (1) with a solution of the polymer(s) (2) in a solvent, wherein the polymer additive(s) (1) have a mean primary particle size (“d 50 ”) of less than 10 μm prior to the mixing with the solution of the polymer(s) (2), and removing the solvent,
wherein the concentrate has a bulk density which is at least 50% greater than that of the polymer additive(s) (1) prior to the mixing with the solution of the polymer(s) (2).
[0040] The polymer(s) (2) are used in a solution to prepare the inventive concentrates. Solvents which are typically used to prepare the solution of the polymer(s) (2) are organic solvents like e.g. methanol, tert. butanol, toluene or methyl acetate. Typically the solution of the polymer(s) (2) contains 70-99%.b.w of the solvent and 1-30% by weight of the polymer(s), based on the total amount of solvent and polymer(s), preferably 80-98% by weight of the solvent and 2-20% by weight of the polymer(s). Additionally the solution of the polymer(s) may contain from 2-20% by weight, preferably 4-10% by weight of vinylacetate, based on the total amount of solvent, polymer(s) and vinylacetate.
[0041] In the next step the solvent is removed. Typically other volatiles may be also removed together with the solvent.
[0042] To prepare the concentrate of the polymer additive(s) (1), preferably the fillers, flame-retardants, flame-retardant synergists, pigments, other finely powdered polymer additives or any mixtures thereof, and the solution of the polymer(s) (2) different processes can be used, especially in order to get a better redispersibility, higher bulk density, less trapped air, less dusting properties and better flowability compared with the typically fine powder of fillers known as state of the art. The processes which are suitable differ in the amount of solvent in the solution of the polymer(s) (2) that is used and which therefore has to be removed in the second step from the solid granules, pellets or tablets. For each process and the properties of the resulting granules, pellets or tablets the amount of polymer remaining as binder in the granules, pellets or tablets as well as the amount of solvent initially present as moisture for plastizising, dispersing and granulating, each related to the total amount of solids employed, determine the economics of the process as well as the particular method used and the properties of the final granules, pellets or tablets.
[0043] The first process alternative of mixing the solid powder particles of the polymer additive(s) (1) with the solution of the polymer(s) (2) is to disperse the solid powder particles of the polymer additive(s) (1) in the polymer solution by preparing a suspension in a stirred vessel or even with additional deagglomeration forces for the solid powder particles. Processes to be used for dispersing the solid powder particles of the polymer additive (1) can be different types of stirrers (e.g. propeller, horseshoe, helix, tooth wheel), high shear dispersing units (e.g. rotor-stator-mixers batch or continuous, colloid mills, corrundum disk mills), continuous powder dispersing units (e.g. jet pumps, powder draw in with rotor stator systems) or high energy systems such as a jet disperser, ultrasonic systems, roller mills or stirred media mills.
[0044] With these dispersing units the total solids content (this shall mean by definition the sum of the polymer additive(s) (1) and the polymer(s) (2)), is 5-80% by weight, preferably 10-70% by weight and particularly preferred 20-60%, based on the total weight of the solution of the polymer(s) (2) and the polymer additives (1).
[0045] Subsequent to the dispersing step the granules, pellets or tablets have to be formed either in an integrated shaping and drying step such as fluidized bed granulation, spray granulation, vacuum drying in a mixer granulator or in a drying step such as spray drying or vacuum drying with a subsequent granulating step such as roller compaction or tableting.
[0046] Using the second process alternative less amount of solvent is needed: High shear machines for moist powders, pastes or suspensions are used in this case. Typical machines are extruders such as single screw extruders, parallel rotating or counter rotating, twin screw extruders or planetary extruders and kneaders such as co-kneaders or sigma-kneaders as well as other batch or continuous kneaders. With these machines, under high shear conditions, the solid powder particles of the polymer additives (2) can be dispersed in the solution of the polymer(s) (1) and subsequently the mixture can be shaped by an integrated granulation or a further shaping step such as low pressure extrusion with frontal, radial or dome extrusion, pelletizing or granulating from the moist state of product. Such dispersing units work with total solid contents of 5-99% by weight, preferably 50-95% by weight and particularly preferred 55-90% by weight based on the total weight of the solution of the polymer(s) (2) and the polymer additives (1).
[0047] The third and very effective process alternative to obtain granules, which generally employs even less solvent, is growth agglomeration by roll agglomeration or high shear agglomeration or combinations thereof. These processes work by moving the powdered particles of the polymer additive(s) (1) e.g. in a vessel, on a pelletizer plate or in a mixing chamber. The solution of the polymer(s) (2) is then added either at once as a batch, in a flow, as a semibatch or continuously, by spraying either semibatchwise or continuously. Under more or less intensive mixing the powder particles agglomerate by means of fluid bridges and a growth agglomeration results.
[0048] Depending on the particular process which is used for this third alternative a more or less narrow particle size distribution results which can be classified if desired in an integrated or subsequent classifying process. The granulation process itself needs relatively small amounts of the solution of the polymer(s) (2). This third process alternative can be carried out with a total solid content of 20-99% by weight, preferably 50-95% by weight and particularly preferred 60-90% by weight, based on the total weight of the solution of the polymer(s) (2) and the polymer additives (1).
[0049] A very small amount of solvent is possible, when using the affinity of the fine powder of the polymer additives (1) to agglomerate because of its surface forces. The affinity can be intensified and the stability of the resulting granules improved by moistening the solid powder of the polymer additives (1) with a very small amount of polymer solution at the beginning. The subsequent granulating process either can be a growth agglomeration or a dry pressure agglomeration e.g. roller compacting or tableting.
[0050] For most applications of the inventive concentrates in the form of granules the granules are required to be essentially solvent free. How the solvent is removed depends on the form of the moist product after dispersion and/or granulation. Due to the necessity to ensure that no explosion can occur vacuum drying is often used but also convective heat and mass transfer by static or vibrating fluidized bed drying (fluidized bed), spray drying, continuous-flow drying, flash drying or radiation dryers are possible. Depending on the acceptable residual solvent a post drying process (e.g. after a gentle convective drying process to obtain granules of a certain strength) may be necessary. The concentrate may be also subjected to a classifying, if this is deemed helpful.
[0051] Also a spheronising step before or after drying may be helpful, e.g. in order to improve the flow behaviour of the granules, pellets or tablets or to improve the particle size distribution as well as to abrade the rough edges remaining after the granules, pellets or tablets have been formed and dried. Such a step also reduces the dusting of the resulting product.
[0052] The preparation of granules, pellets or tablets and their characterisation is described in an article by M. Müller, Aufbereitungstechnik, 44, (2003), Nr. 2, page 22 ff and in an article by Nold, Löbe and Müller, Interceram, 53, (2004), Nr. 2, page 96 ff.
[0053] It is a decisive feature of the inventive concentrate, of course after the removal of the solvent, that it has a bulk density which is at least 50% greater than the one which the polymer additive(s) (1) have prior to the mixing with the solution of the polymer(s) (2). This means that the present invention allows the preparation of solid concentrates with a high bulk density. Preferably the bulk density of the inventive concentrate is at least 100% greater than the one which the polymer additive(s) (1) have prior to the mixing with the solution of the polymer(s) (2).
[0054] The bulk density is measured in accordance with DIN ISO 697 from January 1984.
[0055] The invention is further directed to the use of the inventive concentrates for preparing polymer compounds and to a process of preparing such polymer compounds containing the concentrates.
[0056] Such process of preparing polymer compounds containing the inventive concentrates comprises mixing the inventive concentrates with one or more polymers (3).
[0057] Such polymers (3) encompass, but not limited to, nitrile rubber (also abbreviated as “NBR”), hydrogenated nitrile rubber (also abbreviated as “HNBR”), polyamides, polycarbonate, polyvinylchloride (“PVC”), AEM and EVM. All such polymers (3) are well-known and either commercially available or may be prepared by a person skilled in the art based on known synthesis or manufacturing processes.
[0058] As used throughout this specification, the term “nitrile rubber” or “NBR” is intended to have a broad meaning and is meant to encompass an elastomer having repeating units derived from at least one conjugated diene, at least one alpha-beta-unsaturated nitrile, and optionally further one or more copolymerizable monomers.
[0059] The conjugated diene may be any known conjugated diene, preferably a C 4 -C 6 conjugated diene. Preferred conjugated dienes are butadiene, isoprene, piperylene, 2,3-dimethyl butadiene and mixtures thereof. Even more preferred C 4 -C 6 conjugated dienes are butadiene, isoprene and mixtures thereof. The most preferred C 4 -C 6 conjugated diene is butadiene.
[0060] The alpha-beta-unsaturated nitrile may be any known alpha-beta-unsaturated nitrile, preferably a C 3 -C 5 alpha-beta-unsaturated nitrile. Preferred C 3 -C 5 alpha-beta-unsaturated nitriles are acrylonitrile, methacrylonitrile, ethacrylonitrile and mixtures thereof. The most preferred C 3 -C 5 alpha-beta-unsaturated nitrile is acrylonitrile.
[0061] Preferably, the copolymer contains in the range of from 40 to 85% by weight of repeating units derived from one or more conjugated dienes, in the range of from 15 to 60 weight percent of repeating units derived from one or more alpha-beta-unsaturated nitriles. More preferably, the copolymer contains in the range of from 55 to 75 weight percent of repeating units derived from one or more conjugated dienes, in the range of from 25 to 40 weight percent of repeating units derived from one or more alpha-beta-unsaturated nitriles.
[0062] Optionally, the copolymer may further contain repeating units derived from one or more copolymerizable monomers, such as unsaturated carboxylic acids, alkyl acrylates and/or styrene. Repeating units derived from one or more copolymerizable monomers will replace either the nitrile or the diene portion of the nitrile rubber and it will be apparent to the skilled in the art that the above mentioned figures will have to be adjusted to result in 100% by weight
[0063] The “hydrogenated nitrile rubber” or “HNBR” means that the residual double bonds (RDB) present in the starting nitrile polymer/NBR are hydrogenated to a certain extent, typically more than 50% of the residual double bonds are hydrogenated, preferably more than 90%, more preferably more than 95% and most preferably more than 99% of the residual double bonds are hydrogenated.
[0064] The term “polyamide” shall encompass homo- or copolymers which contain monomer repeating unit, which are linked by amide groups (—C(═O)—NH—). Examples of such polyamides cover polycaprolactam (nylon 6), polylaurolactam (nylon 12), polyhexamethylenadipate (nylon 6.6), polyhexamethylenazelamide (nylon 6.9), Polyhexamethylensebacamide (nylon 6.10), polyhexamethylenisophthalamide (nylon 6, IP), polyaminoundecansaure (nylon 11), Polytetramethylenadipamide (nylon 4.6) as well as copolymers of caprolactame, hexamethylendiamine and adipic acid (nylon 6.6) and aramides like e.g. polyparaphenylenterephthalamide.
[0065] The term “polycarbonate” shall encompass the group of thermoplastic materials which can be formally considered to be a polyester from carbonic acid and aliphatic or aromatic dihydroxyl moieties. Economically the most important example are the polycarbonate produced from bisphenol A (2,2-(4,4-dihydroxy-diphenyl)-propane) and phosgene, but for particular properties other dihydroxy-diaryl-alkanes as well as other dihydroxy aromatic or aliphatic moieties can be included during the manufacturing process.
[0066] “Polyvinylchloride” or “PVC” shall be assumed to mean those polymers prepared by either suspension, emulsion or bulk polymerisation processes and based formally on the monomeric unit CH 2 —CHCl. Those polymers commercially available can also contain comonomers such as vinyl acetate, vinylidene chloride or acrylonitrile. Additionally, PVC is also available which has been chlorinated after polymerisation and these polymers too are included within the scope of the present invention.
[0067] “Polyacrylates” or “AEM” is used herein to mean the polymers produced by an emulsion (co)polymerisation of, but not limited to, one or more of the following monomers: ethyl acrylate, butyl acrylate, methoxyethyl acrylate, ethoxyethyl acrylate, caprolacton acrylate, 2-chloroethyl vinyl ether, vinyl chloroacetate, p-vinyl benzyl chloride, allyl glycidyl ether, glycidyl methacrylate, acrylic acid and methacrylic acid.
[0068] Eventually the invention concerns the polymer compounds containing the inventive concentrates and one or more polymers (3), a process for preparing such polymer compounds as well as the formed parts manufactured from the polymer compounds.
[0069] The preparation of the polymer compounds is typically achieved by compounding the concentrates of the present invention with one or more polymers (3). This compounding can be done by using for example an internal mixer, a mixing extruder, such as a twin screw extruder or a bus co-kneader.
[0070] The polymer compounds containing the inventive concentrates can be used for preparing formed parts thereof. Such formed parts may be profiles such as sealing profiles or such as window profiles, equipment housings such as for computers and household or industrial electrical equipment, and for functional articles such as hoses and belts.
[0071] Such formed parts can be formed by extrusion, injection moulding or compression moulding techniques and may be vulcanised (crosslinked) after forming to improve the mechanical properties of the finished articles.
[0072] The concentrates obtained by the process of this invention can be described as low dusting during processing and are easy to meter and handle. They maintain the fine particle size, and nevertheless show low dusting. When being used for preparing polymer compounds, they are dispersed in the polymer faster and more efficient than the untreated polymer additive(s) and yield polymer compounds having improved performance due to the more uniform and homogeneous incorporation of the polymer additive(s). Such increase of the compounding speed enhances the commercial attractiveness of the processing.
[0073] Formed parts containing the inventive concentrates are more uniform with respect to density, wall thickness, and more homogeneous compared to formed parts known so far. Physical properties such as flammability test performance and/or impact strength also are enhanced.
[0074] Those skilled in the art would not have expected that increasing the bulk density of the specific polymer additives (1) by transferring them into the inventive concentrates would enhance the processability, achieve better dispersion of the additive throughout the polymer, or enhance the properties of the processed polymer compound.
EXAMPLES
[0075] The concentrates of the present invention can be characterised visually to determine their tendency to form dust. A quantitative indication of the tendency to form dust can be derived from a sieve analysis.
[0076] The bulk density can be measured according to DIN ISO 697 from January 1984.
[0077] The quality of the dispersion of the polymer additives (1), in particular of fillers, in polymers and, in particular, in rubber can be measured by the shear modulus at varying amplitudes as described in A. R. Payne, R. E. Whittacker, Rubber Chem. Technol. 44, 440 (1971).
[0078] In the Examples Mg(OH) 2 was used as polymer additive (1), which has the trade name Magnifin® H10A (Fa. Martinswerk, Germany) and a mean primary particle size (d 50 ) of 0.65-0.95 μm measured by laser diffraction using a MALVERN MASTERSIZER S.
Examples 1a-d
Preparing an Inventive Concentrate in the Form of Fine Granules by Dispersing as a Polymer Additive (1) a Flame Retardant in an Organic Polymer-Solution and Vacuum Drying of the Granules
Example 1a
[0079] In a first example 1a 95 g of the flame retardant Mg(OH) 2 , (Magnifin® H10A, Fa. Martinswerk) was dispersed in 155 g of a solution containing 95 vol.-% of tert. butanol, 5 vol.-% vinyl acetate and 5 g of an ethylene vinyl acetate copolymer itself containing 70% by weight vinyl acetate and 30% by weight ethylene (Levapren®700, Lanxess Deutschland GmbH, Germany). The flame retardant was dispersed by a batch lab disperser (Ultraturrax T18, Fa. IKA, Germany) for 5 minutes resulting in an increase of temperature of 10° C. The resulting suspension had a solid content of 40% by weight. After dispersion, the suspension was dried at 20° C. in a lab extractor hood to yield a thick, solvent containing, paste which was then vacuum dried at 40° C. for 48 h. The resulting fine granules of Mg(OH) 2 contained 5% by weight ethylene vinyl acetate copolymer.
[0080] This procedure was repeated for the following examples all employing Mg(OH) 2 as a filler (Magnifin® H1M, Fa. Martinswerk) and the copolymer used in Example 1a.:
Example 1b
[0081] 90 g of filler, 160 g of a solvent mixture (95 vol. % of tert. butanol and 5 vol. % of vinyl acetate), 10 g of ethylene vinyl acetate copolymer.
Example 1c
[0082] 98 g of filler, 152 g of a solvent mixture (95 vol. % of tert. Butanol and 5 vol. % of vinyl acetate), 2 g of ethylene vinyl acetate copolymer
Example 1d
[0083] 99 g of filler, 151 g of a solvent mixture (95 vol. % of tert. Butanol and 5 vol. % of vinyl acetate), 1 g of ethylene vinyl acetate copolymer
Examples 2a-f
[0084] Preparing an inventive concentrate in the form of coarser granules by agglomerating as a polymer additive a flame retardant with an organic binder solution containing an ethylene vinyl acetate copolymer and vacuum drying of granules.
[0085] In a second example coarse granules were produced by growth agglomeration in an intensive mixer (Eirich-Mixer R02, Fa. Eirich, Hardheim, Germany).
Example 2a
[0086] 1000 g of flame retardant Mg(OH) 2 (Magnifin® H10A, Fa. Martinswerk, Germany) was placed in an “Eirich-Mixer”. The mixing was carried out under a blanket of nitrogen (Level 1 of mixer vessel, 1500 U/min of a pin mixing tool). 350 g of polymer solution containing 85.5% by weight of tert. butanol, 4.5% by weight vinyl acetate and 10% by weight of an ethylene vinyl acetate copolymer, itself containing 70% by weight vinyl acetate and 30% by weight ethylene (Levapren®700, Lanxess Deutschland GmbH) was added in 3:30 min by a flexible tube pump to the dry powder. While the solution was added the granules grew and after a further 5 min of post mixing the granules were modified to a more narrow particle size distribution.
[0087] The granules were then dried at 20° C. in a lab extractor hood for 24 h and finally vacuum dried for 48 h at 40° C.
[0088] The resulting coarse granules contained 3.6% by weight ethylene vinyl acetate copolymer.
[0089] This procedure was repeated for the following examples all employing as a filler Mg(OH) 2 (Magnifin® H1M, Fa. Martinswerk) and the copolymer used in Example 2a:
Example 2b
[0090] 1000 g of filler, 350 g polymer solution with 89.6% by weight tert. butanol, 4.7% by weight vinyl acetate and 5.7% by weight ethylene vinyl acetate copolymer; mixing conditions: mixer vessel level 1, mixing tool 750 U/min
Example 2c
[0091] 1000 g of filler, 350 g polymer solution with 81.4% by weight tert. Butanol, 4.3% by weight vinyl acetate and 14.3% by weight ethylene vinyl acetate copolymer; mixing conditions: mixer vessel level 1, mixing tool 750 U/min
Example 2d
[0092] 1000 g of filler, 350 g polymer solution with 85.5% by weight tert. Butanol, 4.5% by weight vinyl acetate and 10% by weight ethylene vinyl acetate copolymer; mixing conditions: mixer vessel level 1, mixing tool 750 U/min
Example 2e
[0093] 1000 g of filler, 350 g polymer solution with 85.5% by weight tert. Butanol, 4.5% b.w vinyl acetate and 10% by weight ethylene vinyl acetate copolymer; mixing conditions: mixer vessel level 1, mixing tool 1500 U/min
Example 2f
[0094] 1000 g of filler, 350 g polymer solution with 85.5% by weight tert. Butanol, 4.5% by weight vinyl acetate and 10% by weight ethylene vinyl acetate copolymer; mixing conditions: mixer vessel level 1, mixing tool 3000 U/min
[0095] The products from Examples 2b-2e were analysed by sieve analysis (vibrating lab sieve, 100 g, 30% intensity, 10 min) to determine their particle size distribution, but also to determine their fines content which is an objective measure of their dusting characteristic.
[0096] All products had <1 wt.-% fines after drying; they did not dust when shaken.
[0097] The particle size distributions are shown in the following Table 1 and in FIG. 1 .
[0000]
TABLE 1
Example
2b
2c
2d
2e
2f
Sieved Fraction/%
>4
mm
22.2
5..
7.9
16.2
0
2-4
mm
60.8
40.6
49.3
40.4
21.2
1-2
mm
16.1
43.5
36.3
34.1
62.5
0.5-1
mm
0.7
10.2
6.4
8.7
15.3
<0.5
mm
0.1
0.4
0.1
0.6
1.1
[0000]
TABLE 2
Measurement of the bulk density of the granules of Examples 1 and 2 in accordance
with DIN ISO 697 from January 1984.
EVA
bulk density
Trial
Parameters
Sieve fraction*
[% b.w.]
[g/l]
Comparative
No mixing, analysed as
As received
0
300
Example
received
(Magnifin ®
H10A)
Example 2b
Eirich-Mixer, 750 rpm
no Classification after
2
825
Granulation
Example 2c
Eirich-Mixer, 750 rpm
no Classification after
4.8
865
Granulation
Example 2d
Eirich-Mixer, 750 rpm
no Classification after
3.4
855
Granulation
Example 2e
Eirich-Mixer, 1500 rpm
no Classification after
3.4
845
Granulation
Example 2f
Eirich-Mixer, 3000 rpm
no Classification after
3.4
800
Granulation
Example 2b
Eirich-Mixer, 750 rpm
Classifying fraction 2-4 mm
2
685
Example 2c
Eirich-Mixer, 750 rpm
Classifying fraction 2-4 mm
4.8
740
Example 2d
Eirich-Mixer, 750 rpm
Classifying fraction 2-4 mm
3.4
725
Example 2e
Eirich-Mixer, 1500 rpm
Classifying fraction 2-4 mm
3.4
745
Example 2f
Eirich-Mixer, 3000 rpm
Classifying fraction 2-4 mm
3.4
670
Example 1a
Ultra-Turrax T18,
no Classification after
5
485
20.000 rpm
Granulation
Example 1c
Ultra-Turrax T18,
no Classification after
2
480
20.000 rpm
Granulation
*Column “Sieve Fraction”
The entry “no Classification after Granulation” under “Sieve Fraction” means that the product as obtained after granulation was directly subjected to the measurement of the bulk density.
The entry “Classifying fraction 2-4 mm” under “Sieve Fraction” means that the product obtained after granulation was subjected to a classifying at first and the fraction obtained therefrom which had a particle size of 2-4 mm was then subjected to the measurement of the bulk density.
Example 4
Processing the Granules from Examples 1 and 2 in a Polymer on a Two Roll Mill
[0098] The concentrates from Examples 1 and 2, as well as untreated Mg(OH) 2 (comparative example) were mixed with an ethylene vinyl acetate copolymer to produce a visually homogeneous sheet on a laboratory two roll mill. The time taken to produce the apparently homogeneous sheet was recorded.
[0099] The two roll mill (LaboWalz W80T; Vogt Maschinenbau GmbH) used had the following specifications:
[0000] Roll diameter: 80 mm, Roll breadth: 280 mm, Roll speed: front: 16.5 Upm, back: 20 Upm, Friction: 1:1.2, Set temperature: 20° C.
[0100] For each experiment 50 g ethylene vinyl actetate copolymer (Levapren® 700, Lanxess Deutschland GmbH, Germany) was put on the mill and a continuous sheet formed. Thereafter, either the untreated filler (Mg(OH) 2 ) or the inventive concentrate was added as rapidly as possible. For the untreated filler the distance between the rolls (the nip) had to be reduced to 0.5 mm in order to maintain the majority of the powder in the bank of rubber in the nip. For all other experiments the nip was maintained at 0.7 mm.
[0101] The sheets from these experiments were used to measure the shear modulus at varying amplitudes and at a constant frequency of 10 Hz, a temperature of 60° C. using a Rubber Process Analyser (RPA 2000) made by Alpha Technology. The limiting shear modulus at zero amplitude can be seen as a measure of the quality of the dispersion of fillers in a rubber matrix. The results as given in Table 2 below clearly show that the limiting shear modulus at zero amplitude is substantially lower and therefore the dispersion of the filler in the matrix considered better, if the additive is not used untreated but in the form of the inventive concentrates.
[0000]
TABLE 3
Time to visual
Limiting Shear
incorporation
Modulus/kPa
Untreated Filler*
490 s
900
Example 1a
240 s
730
Example 1c
260 s
740
Example 2d
360 s
700
Example 2c
315 s
700
Example 2b
375 s
780
Example 2e
405 s
725
Example 2f
470 s
750
Levapren 700**
.-.
195
*For comparison: Mg(OH) 2 as Magnifin ® H10A, Fa. Martinswerk
**For comparison, Levapren ® 700 (Lanxess Deutschland GmbH, Germany) was solely used.
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New polymer concentrates on the basis of polymer additives, like e.g. fillers and flame-retardants, are provided which have in particular an increased bulk density compared to the polymer additives as such. This increased bulk density leads to a substantial improvement in the processability of such concentrates, their dispersibility during compounding and the properties of the resulting polymer compound. Processing improvements include less dust, faster processing and more homogeneous additive dispersion. The invention also provides a process for preparing such new polymer concentrates, a process for preparing polymer compounds containing the new polymer concentrates, the respective polymer compounds and a process for preparing formed parts thereof. Such formed parts have more uniform properties such as density, wall thickness, and in case of the flame-retardants more homogeneous and consistent flame retardancy.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to gas modules, and more particularly to a gas module which is especially adapted for use in a catheter laboratory.
2. Description of the Related Art
In the field of health care, it is often necessary or advantageous to administer one or more different types of gases to a patient. For instance, oxygen or air is administered to many patients to help them breath normally, and patients undergoing surgery are typically anesthetized using an anesthetic gas, such as nitrous oxide. Frequently, a patient undergoing surgery will receive oxygen and an anesthetic gas concurrently. In addition, during surgery, the surgeon often uses compressed air to remove fluids from internal organs, and a vacuum to extract fluids from the operating area.
In view of the advantageous use of these various gases, it is common to route various types of gases to a common delivery unit, which is often called a gas module. Gas modules include a plurality of outlets which are used to deliver the gases, and the outlets usually include regulating valves which adjust the pressure or flow of the gas being delivered to the patient. A gas module conveniently allows a hospital attendant to select a particular type of gas for administration to a patient, and to regulate the amount of ga delivered to the patient.
In many modern hospitals, a network of gas pipes runs throughout the hospital to deliver the various gases to the rooms in which they are needed. For instance, operating rooms typically receive oxygen, air, compressed air, vacuum, nitrogen, and anesthesia. In operating rooms, it is advantageous that the gas module is moveable, because different surgical operations require different numbers of surgeons to be in different positions within the operating room. Therefore, a gas module which may be located in a convenient location within the operating room prevents the gas module from being an obstruction, while it allows hospital personnel to effectively use the gas module.
While all of these different types of gases may be useful at one time or another in an operating room, all of these gases are not necessary in patients' individual rooms. However, since some patients require the administration of oxygen or air, pipes running within the walls or the ceilings of the hospital, deliver these two gases into the patients' rooms via wall or ceiling outlets. These rooms are typically arranged in a manner which is not subject to change. Therefore, to efficiently utilize the space, the gas modules are mounted on or in one of the walls of the room. The primary disadvantage of these wall mounted units is that they cannot be easily relocated.
As previously mentioned, moveable gas modules are preferred for use in examination rooms and operating rooms. Unfortunately, gas modules which receive gas from pipes running within the hospital ceiling or walls typically have a very limited range of motion. Commercially available ceiling-mounted gas modules are supported by bulky arms which have gas-carrying hoses running therethrough, and typically weigh over 500 pounds. The bulkiness and heaviness restricts the length and articulation of the arms, thus preventing the gas module from being conveniently positioned. Furthermore, the weight of the arms often prohibits manual operation and instead requires mechanical or electrical assistance.
Moreover, these ceiling-mounted gas modules cannot be used efficiently in examination rooms which contain a plurality of devices mounted above the examination table. In catheter laboratories, for instance, two X-ray tubes having opposed image intensifiers are used to produce two-dimensional images of a patient's internal organs. Each X-ray tube and its associated image intensifier is mounted onto a respective positionable U-shaped member so that an operator can accurately position each of the tubes and intensifiers about a patient. One of these U-shaped members, such as a LARC, positions one X-ray tube and image intensifier on either side of a patient. The LARC slides along the length of an examination table on two parallel tracks attached to the ceiling. The other of these U-shaped members, such as a Poly-C, positions the other X-ray tube and image intensifier above and below a patient, respectively. The Poly-C has two parallel arms that move the length of the examination table, and its base is attached to the floor. After considerable processing, the images produced by the image intensifiers are sent to monitors which are mounted on the ceiling on two parallel tracks which extend across the examination table, generally perpendicular to the LARC's tracks. Moreover, a physiologic monitor is also mounted above the examination table to relay the patient's vital statistics to the physician, as is, of course, a surgical light. Therefore, there is no room to mount a gas module on the ceiling above the examination table.
In rooms such as these, the ceiling mount of the gas module would have to be located away from the examination table because there is no room for the mount above the table. Therefore, the ceiling-mounted gas module must have a long reach so that it can be positioned reasonably near a patient. However, length is not the only concern. A ceiling-mounted gas module having long, bulky support arms cannot be easily positioned between the other devices in the room.
Due to the poor maneuverability, bulkiness, and restricted reach of commercially available ceiling-mounted gas modules, floor standing gas modules are typically used in crowded examination rooms and laboratories. The floor standing gas modules which receive gas from the network of pipes typically require long hoses which extend between the wall and the gas module. These hoses limit the range of motion of floor standing gas modules, and obstruct a large amount of the floor space in an examination room. Thus, they are not well suited for use in a crowded room. Many floor standing gas modules, however, use gas stored in tanks that are carried on the module. While these types of gas modules move on rollers, and therefore have a greater range of motion than the previously described floor standing models, they are quite heavy and large due to the tanks of gas which must be carried with the gas module. An additional problem stems from the fact that floor standing units are quite susceptible to contamination by dirt and fluids.
Accordingly, the prior art has various drawbacks and disadvantages.
SUMMARY OF THE INVENTION
The present invention overcomes many of these drawbacks and disadvantages by providing a low-bulk gas delivering apparatus for use in a catheter laboratory. The apparatus includes a universally articulatable support arm, one end of which is adapted to mount onto a ceiling and the other end of which is mounted to a gas module. The gas module is adapted to deliver gas received from a hose which connects the gas module to a source of gas. The hose generally extends along the support arm and is disposed outside of the support arm. Therefore, the support arm is lighter, slimmer, and less bulky than previously used support arms.
In accordance with a more specific aspect of the present invention, a ceiling-mounted gas delivering apparatus for use in a catheter laboratory is provided where the articulatable support member includes: a first support arm having a first end and a second end, the first end being adapted to attach to the ceiling so that the support arm extends downwardly from the ceiling toward the floor and is generally perpendicular to the floor; a second support arm having a first end and a second end, the first end of the second support arm being pivotally connected to the second end of the first support arm to permit the second support arm to pivot horizontally about the first support arm; and a third support arm having a first end and a second end, the first end of the third support arm being pivotally connected to the second end of the second support arm to permit the second end of the third support arm to move vertically upwardly toward the ceiling and downwardly away from the ceiling and to permit the third support arm to pivot horizontally about the second end of the second support arm. A gas module is rotatably mounted onto the second end of the third support arm, and a hose connects the gas module to a source of gas. The hose generally extends along the support member and is disposed outside of the support member.
Preferably, the articulatable support member is manually positionable, and is fully moveable throughout its range of motion by manually moving the gas module. Moreover, a self-leveling linkage which connects the gas module to the second end of the third support arm maintains a selected orientation of the gas module throughout the range of motion of the articulatable support member.
By supporting a gas module from a universally articulatable support arm, providing the support arm with at least two pivotable interconnections which enable the gas module to be moved horizontally and vertically, and providing a hose exterior to the support arm and which supplies gas from a source to the gas module, the gas module is adapted to be positioned around a patient.
BRIEF DESCRIPTION OF THE DRAWINGS
Other advantages of the invention will become apparent upon reading the following detailed description and upon reference to the drawings in which:
FIG. 1 is a side view of a ceiling-mounted gas delivering unit in accordance with the present invention;
FIG. 2 is a cross-sectional view of a gas module associated with the ceiling-mounted gas delivering unit taken generally along line 2--2 FIG. 1;
FIG. 3 is a perspective view illustrating a ceiling module which routes gas from gas carrying pipes to the gas delivering unit of the present invention; and
FIG. 4 illustrates a preferred range of motion of the gas delivering unit of FIG. 1.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof have been shown by way of example in the drawings and will be described in detail herein. It should be understood, however, that it is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning now to the drawings and referring initially to FIG. 1, a ceiling-mounted gas delivering unit is generally designated by a reference numeral 10. The ceiling-mounted gas delivering unit 10 includes a gas module 12 which is preferably mounted to the ceiling 14 by an articulatable linkage 16. Since the ceiling mounted gas delivering unit 10 is specifically designed for use in a room having a plurality of ceiling mounted devices, such as a catheter laboratory, the articulatable linkage 16 allows the gas module 12 to be moved easily to a wide variety of locations. Moreover, the gas module 12 is made quite small due to the fact that most catheterization procedures are performed on patients without the use of anesthesia. Therefore, only a few selected gases, such as air, compressed air, oxygen and a vacuum, are delivered to the gas module 12.
The gas module 12 receives these gases from a suitable source, and controllably delivers selected gases to a patient. As shown in FIG. 1, the gas module 12 preferably receives these gases from gas-carrying pipes 18 (20,22,23) which are disposed within the ceilings or walls of the examination room in which the ceiling-mounted gas delivering unit 10 is installed. Referring to FIG. 2, the gas module 12 includes four gas outlets 24,26,28, and 30, each of which is held in place by a suitable cover plate 25,27,29, and 31. As shown, outlets 24 and 26 provide a vacuum for anesthesia scavenging, outlet 28 delivers oxygen, and outlet 30 delivers compressed air. Alternatively, the compressed air outlet 30, which is seldom used in catheterization procedures, may be replaced with a holder (not shown) which is suitable to retain a container into which vacuumed fluids are deposited. The outlets 24,26,28, and 30 preferably include pressure regulating valves or flow regulating valves which help to control the pressure or amount of gas discharged from the outlets, as is known in the art.
Preferably, control valves and gauges (not shown) are attached to at least the oxygen and vacuum outlets 24,26,28 so that an attendant can control the amount of gas or vacuum being delivered to a patient. Since the exact amount of compressed air is not critical, a gauge is preferably not attached to the outlet 30.
The outlets 24,26,28, and 30 receive the gases from the respective pipes 22,18,20, and 23 through respective hoses 36,32,34, and 38, as illustrated in FIG. 3. A ceiling module 40 includes a plurality of connection tubes 42,44,46, and 48 which are connected to the respective gas carrying pipes 18,20,22, and 23 by a suitable means, e.g., by using a T-shaped junction or a perforating, self-sealing clamp. The connection tubes 42,44,46,48 connect to respective outlets 43,45,47,49 in the ceiling module 40. The hoses 32,34,36, and 38 are attached to the respective outlets 43,45,47, and 49 within the ceiling module 40, and are routed through an outlet tube 50, which serves as a passageway between the ceiling 14 and the room. The hoses 32,34,36, and 38 extend between the outlet tube 50 and an inlet tube 51 of the gas module 12 within a conduit 52. The conduit is connected to the outlet tube 50 and the inlet tube 51 by any suitable means, e.g., using band clamps 53,55. The conduit 51 is preferably corrugated to provide flexibility so that it generally extends along the articulatable linkage 16, and the conduit 52 and the hoses 32,34,36, and 38 are preferably made of rubber or of a flexible plastic material. The conduit 52 is secured to the articulatable linkage 16 by a plurality of clamps 54 which hold the conduit 52 onto the articulatable linkage 16 at preselected locations. Since the gas is delivered to the gas module 12 using the flexible conduit 52, instead of by routing the hoses within the linkage member, the articulated linkage 16 is much smaller, slimmer and lighter than commercially available ceiling-mounted gas modules.
The articulatable linkage 16 includes a base 56 which mounts the linkage 16 onto the ceiling 14. A vertical support arm 58 which is connected to the base 56 extends downwardly from the ceiling 14. The lower end of the vertical support arm 58 carries a linkage member 66 which connects a horizontally disposed arm 68 to the vertical support arm 58. The linkage member 66 preferably includes an upwardly extending post 70 (as shown by the phantom lines in FIG. 1), and the arm 68 includes a sleeve member 72 which slides over the post 70. The arm 68 is then secured to the vertical support arm 58 by attaching a cap 73 to top of the post 70. Therefore, the horizontal arm 68 is pivotable about the longitudinal axis 74 of the post 72, and the range of motion of the arm 68 is limited due to the obstruction of the vertical support arm 58, as shown by dashed line 75 in FIG. 4. This limited range of motion prevents the conduit 52 from wrapping around the articulatable linkage 16.
The outer end of the horizontal arm 68 includes a sleeve member 76 through which a post 78 (as shown by phantom lines in FIG. 1) extends. The post 78 is part of a connecting member 80 which connects the horizontal arm 68 to a tilting arm 82. The sleeve member 76 is secured to the connecting member 80 by attaching a cap 88 to the top of the post 78.
The connecting member 80 allows the tilting arm 82 to move with two degrees of freedom; the first degree of freedom being about the longitudinal axis 84 of the post 78, and the second being upwardly or downwardly about a spring-loaded joint 86. As illustrated in FIG. 4, at the limits (dashed lines 77 and 79) of the range of motion of the horizontal arm 68, the range of motion of the tilting arm 82 about the longitudinal axis 84 is shown by dashed lines 83,85 to be about 360°. However, the range of motion is advantageously limited to slightly less than 360° to prevent the conduit 52 from wrapping around the articulatable linkage 16.
The outer end of the tilting arm 82 is connected to the gas module 12 via a self-leveling linkage 90. The tilting arm 82 allows the gas module 12 to be moved upwardly or downwardly as shown by the phantom lines in FIG. 1, while the attitude or orientation of the gas module 12 remains relatively unchanged between the upper and lower positions of the tilting arm 82. This is due to the self-leveling linkage 90 which maintains the desired attitude of the gas module 12 through the range of motion of the tilting arm 82. The accuracy of sensitive gauges, such as mercury gauges, which are attached to the outlets, is maintained, since the attitude of the gas module 12 remains relatively unchanged. The self-leveling linkage 90 includes a shaft 92 which connects the control module 12 to the tilting arm 82, and the shaft 92 includes a bearing portion 94 which allows the gas module 12 to rotate about the longitudinal axis 96 of the shaft 92.
The ability of the horizontal arm 68 to pivot about the post 70 and the ability of the tilting arm 82 to pivot about the post 76, allows the gas module 12 to be positioned horizontally anywhere within the region bounded by the solid line 87 (FIG. 4). The vertical positioning of the gas module 12 is determined by the length of the vertical support arm 58, and by the vertical range of motion of the tilting arm 82 about the spring-loaded joint 86. In rooms where a greater vertical range of motion is desirable, the vertical support arm 58 could be adapted to slide axially and, thus, alter the length of the vertical support arm 58.
The movement of the gas module 12 is controlled solely by forces applied to a handle 98 which is preferably connected to the bottom of the control module 12. Because the spring-loaded joint 86 biases the gas module 12 upwardly, the gas module 12 acts as a counter-weight to overcome the spring force of the joint 86. Once the gas module 12 is moved into a desired position, the weight of the gas module 12 maintains the desired vertical position of the tilting arm 82. Should the gas module 12 be of an inappropriate weight, however, an additional counterweight 100 or counter-balance may be used to control the vertical positioning of the gas module 12. Preferably, any additional counter-weight is attached to the gas module 12.
Overall, the gas delivering unit 10 is lightweight by virtue of the slimness of the support members, i.e., the linkages and arms, which are used to make the articulatable linkage 16. Moreover, the support members are preferably made of a lightweight material, such as aluminum, to further reduce the weight of the gas delivering unit 10. Experimental units have been made using a commercially available articulatable linkage from Burkhart Roentgen Inc., 3 River Rd. South, Cornwall Bridge, Conn. 06754, which is referred to as an "overhead counterpoise". The weight of the articulatable linkage 16 is between about 30 pounds and about 80 pounds (depending on length), the weight of the gas module 12 is between about 20 pounds and about 40 pounds, the weight of the hoses 32,34,36,38 and conduit 52 is between about 10 pounds and about 30 pounds. Therefore, the weight of the entire gas delivering unit 10 is between about 60 pounds and about 150 pounds.
The range of motion and the slim profile of the articulatable linkage 16, allows the gas delivering unit 10 to be mounted onto a ceiling in an examination room having a plurality of devices mounted on the ceiling above a patient, because the articulatable linkage 16 is able to position the gas module 12 near the patient by winding between the other devices in the room.
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A low-bulk gas delivering apparatus for use in a catheter laboratory is provided. The apparatus includes a universally articulatable support arm, one end of which is adapted to mount onto a ceiling and the other end of which is mounted to a gas module. The gas module is adapted to deliver gas received from a hose which connects the gas module to a source of gas. The hose generally extends along the support arm and is disposed outside of the support arm. Therefore, the support arm is lighter, slimmer, and less bulky than previously used support arms.
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CROSS REFERENCE
[0001] The present application is a divisional of and claims priority under 35 U.S.C. §121 of U.S. patent application Ser. No. 13/826,628, filed on Mar. 14, 2013, which is incorporated by reference in its entirety.
BACKGROUND
[0002] This invention relates generally to an integrated circuit having at least two vertically stacked semiconductor substrates, and more specifically to TSV (through substrate via) structures formed in such an integrated circuit.
[0003] Integrated circuits have become ubiquitous. Today ‘complimentary metal on semiconductor’ (CMOS) technology can create billions of devices such as transistors for logic or memory (or both) on a single semiconductor substrate; which single substrate is known as a ‘monolithic integrated circuit’ and will be referred to herein as a chip. Hundreds of chips can be formed together as regions of a single semiconductor wafer and then diced to separate the individual chips. The devices are formed on a ‘front-side’ surface of a wafer by so-called ‘front end of the line’ processing (FEOL) of a wafer, with wafer processing typically continuing to form a contact layer (so called ‘middle of the line’ or MOL) and wiring to interconnect the devices of the single substrate (so-called ‘back end of the line’ or BEOL) before the wafer is diced.
[0004] In order to continue to improve performance and functionality of integrated circuits, the industry has recently been developing technology to vertically integrate two or more chips into a single vertically integrated component. In some embodiments, the two or more chips can each have active semiconductor devices (such as field effect transistors). In other embodiments, at least one of such two or more chips can be an ‘interposer’ which may not have any semiconductor devices or might only have passive semiconductor devices (such as a capacitor). Whereas the ‘monolithic IC’ includes a single semiconductor substrate (but could have other structural layers such as an organic laminate packaging), the single vertically integrated component is referred to herein as a three-dimensional (3D) integrated circuit (3D IC). A 3D IC includes at least two chips stacked together (and could similarly have additional layers such as a packaging laminate). Like the monolithic IC, many 3D ICs can theoretically be formed simultaneously by bonding entire (or partial) wafers and then singulating the individual 3D ICs by dicing the stack, each 3D IC having two or more chips vertically bonded together.
[0005] Whereas the device face (front-side) of a single chip IC can be directly against the packaging structure which delivers power and carries signals between the chip and the outside world, the 3D IC has at least one chip that is separated from the packaging by another chip. Power can be delivered to the devices of the at least one remote chip or devices on different chips of the same 3D IC can be interconnected using conductive elements that extend entirely through intermediate chips, referred to as ‘through substrate vias’ (TSVs). Put another way, a TSV is a conductive path within a 3D IC that passes through a chip and conductively connects elements located on opposite sides of that chip. A 3D IC can theoretically include any number of chips (C1, C2, . . . Cx, x>=2) and a TSV can theoretically connect any one chip of the stack to any other chip of the stack or to the packaging interface by passing through the one or more chips in between (e.g., if x=4, C1 can be connected to C4 by a TSV that passes through C2 and C3).
[0006] The intermediate substrates must be thinned to enable forming TSVs. TSVs can be formed into the substrate during fabrication of the front side, for example by etching a TSV cavity into a substrate, forming an insulating layer, depositing barrier and seed layers, plating to fill the cavity (which can be achieved by bottom-up techniques to avoid forming voids in the very high aspect ratio TSV cavity), CMP (chemical mechanical planarization), and building interconnects to connect to the TSV in a subsequent BEOL level. In such a flow scheme, the back side of the substrate can subsequently be thinned to expose the remote end of the TSV. Further processing can include cleaning and passivating the grind side.
[0007] Semiconductor wafers are produced by growing a single crystalline ingot that is sliced into wafers and polished. Crystal defects, which can agglomerate to form ‘crystal originated particles’ (COPs), and contaminants such as oxygen and metals are inevitably incorporated in the ingot. It is known to form semiconductor devices in a region free of any COPs that have a size larger than or commensurate to the semiconductor devices. One approach is to form a “denuded zone” on the device face of a wafer. For example, US Publ. 2002/0009862 to Mun (hereafter “Mun”) is directed to a two step heat treatment to remove grown-in defects to a required depth (10 to 100 um in claim 11 ). Another approach disclosed by U.S. Pat. No. 8,231,725 to Sattler et al is to form the crystalline ingot wafer having COP defects with a size not more than 30 nm.
[0008] Oxygen and certain other contaminants within the semiconductor ingot are not entirely undesirable since they can form so called precipitates known as ‘bulk micro defects’ (BMD) which can getter metal contaminants. Mun's method also purportedly forms a high density of BMD. U.S. Pat. No. 8,357,939 discloses process conditions to create a denuded zone while retaining a density of BMD above 1e11/cc at depth greater than 50 um and having an equivalent diameter within the range of 10-50 nm.
[0009] Additional metal contamination (above and beyond that incorporated during growth of the single crystalline ingot) can be introduced by thinning a wafer such as for incorporation in a 3D IC. U.S. Pat. No. 7,915,145 to Kurita et al discloses to address the additional contamination by careful CMP processing to add ‘extrinsic gettering’ on the grind side of a wafer having an ‘intrinsic gettering’ capability with BMD density in the range of 1e6 to 1e11 and size in the range of 10 to 100 nm.
[0010] Before thinning the wafer to expose the TSV, testing is performed to identify (and remove) those chips having flawed circuitry or excessive electrical leakage to the substrate. Electrical leakage can be tested by imposing a high voltage stress, known as ‘time dependent dielectric breakdown’ (TDDB) testing. Many TSVs appear to be structurally sound according to the front side ‘post fab’ testing but apparently contain latent TSV defects which can be triggered by the thinning process because they exhibit unacceptable leakage once the back side has been thinned to expose the TSV. A need remains to reduce the occurrence of such latent flaws within TSVs.
SUMMARY
[0011] According to a first embodiment, the invention provides a semiconductor chip comprising a semiconductor substrate with a first major surface in which a semiconductor device has been formed and a second major surface opposite to said first major surface, where the second major surface is created by thinning the semiconductor substrate, and bulk micro defects (BMD) having an average size less than 55 nm (nanometers) within a region of said semiconductor substrate. The region with BMD can extend from the second major surface through the semiconductor chip or to a lesser depth just adjacent to the grind side, such as to a depth of about ten microns from the said second major surface. The semiconductor chip can include COPs and can also include a TSV.
[0012] According to a second embodiment this invention provides an integrated circuit structure that includes a first chip bonded to a second chip, where the said first chip includes a plurality of semiconductor devices, the second chip includes a front surface in which at least one semiconductor device is formed, a back surface opposite to said front surface, and a through substrate via (TSV) that extends at least from said front surface to said back surface, and the second chip has a BMD density between 1e4/cc and 1e7/cc in a region bounded by said back surface. The first substrate of the 3D IC can include BMD at a density greater than 1e9/cc.
[0013] According to another aspect, the present invention provides a 3D IC having a first chip bonded to a second chip, where the first chip includes first BMD having an average equivalent diameter greater than 70 nm in an interior region and the second chip includes second BMD having average equivalent diameter smaller than 50 nm. In embodiments the first chip includes active semiconductor devices while the second chip includes no semiconductor devices or only passive semiconductor devices.
[0014] Yet another embodiment of the present invention provides a method to form a 3D IC by bonding a first chip to a second chip, where the first chip includes a plurality of BMD particles having an equivalent diameter in the range of 70 nm to 130 nm and the second chip includes BMD, such BMD having equivalent diameter in the range of 20 nm to 50 nm.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0015] FIGS. 1 illustrates a cross-sectional view of a 3D IC structure, according to one embodiment.
[0016] The drawings are not necessarily to scale. The drawings are merely schematic representations, not intended to portray specific parameters of the invention. The drawings are intended to depict only typical embodiments of the invention. In the drawings, like numbering represents like elements.
DETAILED DESCRIPTION
[0017] As noted above, a significant number of TSVs which pass front side testing can exhibit unacceptable electrical leakage when tested after grinding or otherwise thinning the chip. The present inventors investigated these failures. Results of this investigation are presented in Table 1.
[0000]
TABLE 1
TSV Yield vs Substrate Type
Substrate type
A (990)
B (582)
C (246)
D (217)
E (136)
COP-free?
denuded zone
no
yes
no
yes
(10-30 um)
BMD density
5e8-4e9/cc
~6.6e6/cc
BMD size
60-~140 nm
25-55
REI spikes
defects
No Defects
No Defects
No Defects
No Defects
Frontside yield
70-75%
100%
100%
100%
100%
Backside yield
~75 +/− 16%
~95 +/− 3%
[0018] As shown in Table 1, substrate A has a denuded zone and BMD density consistent with a high temperature anneal. Substrates C and E are COP-free substrates whereas substrates B and D both include COPs. Several of each of the substrate types were processed to form TSVs and tested from the front side. About 25% of the TSVs formed in substrate A failed front side testing. In contrast, nearly 100% of TSVs formed in substrates B, C, D, or E passed front side testing.
[0019] Continued processing was performed with those TSVs of substrates A that passed front side testing and also the TSVs of substrate C. Back side electrical leakage testing was conducted after thinning these substrates to expose the TSV on the back side. Another roughly 25% of the substrate A TSVs failed backside testing after grinding to expose the TSV on the back side.
[0020] The unexpected finding was low TSV yield in substrate A, which consistent with a high temperature processing to create a denuded zone, had no COPs and a moderate BMD density of 5e8 to 4e9 /cc, yet high TSV yield in wafers that contain COPs and have low BMD density such as substrate C.
[0021] Without wishing to be bound by theory, it appears that high BMD density formed according to a conventional high temperature anneal can lead to such latent TSV flaws. The inventors have discovered that TSV yield can be significantly improved by utilizing a substrate (e.g., FIG. 1 : substrate 101 ) in which throughout the region traversed by a TSV (e.g., FIG. 1 : TSV 112 ), i.e., the ‘3D region’ extending from the device layer (e.g., FIG. 1 : device layer 109 ) on the front side (e.g., FIG. 1 : front side 108 ) of a wafer to the back side (e.g., FIG. 1 : back side 111 ) exposed after thinning, BMD density is within a narrow range of 1e4-1e7/cc and BMD size is less than 55 nm (size calculated as the diameter of a sphere having equal volume, i.e., equivalent diameter). In embodiments the 3D zone is a region that extends the length of a TSV 112 from a denuded zone 110 to the remote end (e.g., FIG. 1 : end 116 ) of the TSV 112 , which could be e.g., 20 to 100 um below the front side 108 . In embodiments, about 85-90% of all BMD larger than 10 nm are between 25 and 35 nm. In embodiments, the substrate need not be free of COPs.
[0022] The substrate herein may comprise any conventional or future semiconductor wafer (or part thereof) with an epitaxial layer formed of, e.g., Si, SiGe, SiGeC, SiC, Ge alloys, GaAs, InAs, InP and other IIIIV or II/VI compound semiconductors. The substrate can optionally include a bulk material that may be the same or a different composition from the epitaxial layer, such as polycrystalline, amorphous, or single crystalline silicon, and the substrate can also optionally include an insulating layer which may be SiO2 or other insulating material under the epitaxial layer.
[0023] The TSVs described herein comprise a highly conductive core which may comprise e.g., copper, and also may comprise additional layers such as a seed layer, SiO2 or other dielectric to provide electrical isolation, and one or more materials to prevent metal migration into the substrate. The conductive path of the TSV may extend with a nearly uniform diameter from the front surface to the grind side surface of a substrate, or such uniform diameter can extend also through a dielectric or passivation and into a BEOL layer, such that a cross section of the TSV is coplanar with one of the major surfaces of the substrate. This conductive path can be formed as a solid conduit which may, e.g., have a circular cross section, or it can be an annular conduit surrounding a nonconductive core.
[0024] As further depicted in FIG. 1 , 3 D ICs 100 described herein include a thinned chip 102 and at least one more semiconductor chip 104 , 106 bonded together. The thinned chip 102 may include one or more semiconductor devices on a front side. In embodiments, the thinned chip 102 can be e.g., an interposer having only passive semiconductor devices such as capacitors. In other embodiments the thinned chip 102 semiconductor devices can be active (e.g., field effect transistors) or can be a combination of active and passive semiconductor devices. In embodiments the at least one more semiconductor chip 104 can have a denuded zone 110 on the front side 108 . For example the denuded zone 110 can be free of COP and BMD larger than 10 nm. The denuded zone 110 can extend several microns from the front side, such as to a depth of 10 um or even 25 or 30 um.
[0025] While the present invention has been described in terms of particular embodiments, the scope of the invention is not to be limited to the foregoing details but by the claims. It should be understood that an element claimed as being “on” or “over” another element can be directly on the other element or intervening elements may also be present, whereas when an element is claimed as being “directly on” or “directly over” another element, there are no intervening elements present. Similarly, elements claimed as being “connected” or “coupled” can be directly connected or coupled through intervening elements, whereas “directly connected” or “directly coupled” means no intervening elements are present.
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The formation of TSVs (through substrate vias) for 3D applications has proven to be defect dependent upon the type of starting semiconductor substrate employed. In addition to the initial formation of TSVs via Bosch processing, backside 3D wafer processing has also shown a defect dependency on substrate type. High yield of TSV formation can be achieved by utilizing a substrate that embodies bulk micro defects (BMD) at a density between 1e4/cc (particles per cubic centimeter) and 1e7/cc and having equivalent diameter less than 55 nm (nanometers).
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This is a continuation of application Ser. No. 961,047 filed Nov. 15, 1978, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method of manufacturing a ribbon type thin wafer of semiconductor material selected from the group consisting of germanium, silicon, selenium, tellurium, PbS, InSb, ZnTe, PbSe, InAs, CdS, GaAs, InP, GaSb, PbTe, ZnS, Bi 2 Te 3 , and mixtures thereof with additional elements for improving their properties, wherein said method comprises melting semiconductor material and rapid cooling the melt on the surface of travelling cooling substrate and forming a ribbon type thin wafer of semiconductor material having a fine and compact microscopic structure and homogeneous composition.
2. Description of the Prior Art
In the prior art, it is known that a thin plate of semiconductor such as selenium can be obtained by pressing the melt. Further, it is known that the polycrystalline silicon can be obtained on a substrate such as iron plate or stainless plate by the vapour deposition or glow-discharging. It is also known to obtain a thin film of single crystal silicon semiconductor material by taking up slowly from silicon melt. It is known in the prior art to produce the thin film by spattering or electrodepositing semiconductor material other than silicon on a substrate. However, it is unknown to produce at a high speed a thin wafer of semiconductor such as thin flake or thin ribbon which is not deposited on the substrate.
Accordingly, in the prior art, the producing speed of thin film of semiconductor was very low and it is very difficult to produce said thin film of semiconductor by industrial scale of mass production.
A very large scale of power station utilizing solar energy or numerous power sources of solar cells for use of air conditioning in individual houses should be realized for supporting the lack of future energy. While, in the prior art, the producing speed of thin wafer of semiconductor is too slow to produce a large scale of solar cell elements sufficient for supplying necessary energy lack. It is therefore highly requested to develop a high speed manufacturing method of a thin ribbon wafer of semiconductor material in a mass production.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a method of manufacturing a thin ribbon wafer of semiconductor material having a fine microscopic structure of high density in a high speed, by melting semiconductor material, ejecting the melt of semiconductor material through a nozzle and quickly cooling said melt on a surface of a moving or rotating cooling substrate. The method of producing a thin ribbon wafer of semiconductor material according to the invention is of extremely higher speed than that of the prior art. The raw material of crystalline semiconductor is selected from single or polycrystal element such as silicon, gelmanium, selenium tellurium, and III-V Group compound semiconductor material such as GaAs, InSb, GaSb, InAs, InP, and II-VI Group compound semiconductor material such as CdS, ZnTe, ZnS and other compounds such as PbSe, PbTe, Bi 2 Te 3 and mixtures thereof. According to the invention, various elements or compounds may be added in a melt of semiconductor material so as to produce a thin ribbon wafer of semiconductor having a fine and condensed microscopic structure in a solid solution.
According to the present invention, the ribbon thin wafer of semiconductor having a fine and compact microscopic structure may be obtained by quickly cooling the melt of a plurality of semiconductor elements such as Ge-Si which become a similar crystal structure in a solid solution over a wide range of mixing. A thin ribbon wafer of compound semiconductor having a fine and compact crystalline structure can be also obtained by quickly cooling the melt of a plurality of similar compounds of semiconductor material. As this example, ZnS-ZnTe can be illustrated.
As solid-soluble additive elements, use may be made of Sn, As, B, P, Sb, Al, Ga or composite clad material thereof.
As further additive elements, use may be made of metals and halogens which have been included in original semiconductor material.
The range of amount of these additive elements in the thin ribbon wafer of the semiconductor is considerably wider than the solubility limit in an ordinary crystalline state of the semiconductor.
In addition, all the additive elements soluble into the melt of semiconductor material are effective for changing electrical-, magnetic-, optical-, crystal structural- and elastic characteristics of the thin ribbon wafer of the semiconductor.
B, P, BP, SbAl, etc., are very effective as a flux as described hereinafter and serve to obtain the thin wafer of semiconductor. It is noted that B, P etc. are available to increase the viscosity of melt of semiconductor material.
In case of melting semiconductor material, attention should be given to the following points. That is, it is necessary to provide a sufficient viscosity for ejecting a melt of semiconductor material through a nozzle, and if a melting temperature becomes higher than a melting point of the semiconductor material, the viscosity becomes too low, so that the melt spontaneously drops out of the nozzle by the gravity and forms liquid drops. Further, if semiconductor material is molten at a much higher temperature, the melt continuously flows out of the nozzle and thus a thin ribbon wafer of semiconductor of good quality cannot be obtained. Accordingly, semiconductor material should be molten substantially at the melting point of material or at a higher temperature up to 300° C. above the melting point. In order to melt semiconductor material, use may be made of a resistance heating method and a high frequency heating method, but any other heating method may be employed.
The melt semiconductor material is ejected from the nozzle, and it is preferable to start this ejecting operation when the nozzle reaches immediately above a moving or rotating surface of moving or rotating cooling substrate. This can be controlled with the aid of a micro-switch and the like which detects a distance between the nozzle and the surface. Further, in order to obtain a semiconductor thin ribbon wafer of good quality, the nozzle should be made of material which hardly react with a melt of semiconductor material. The nozzle for use in an oxidizing atmosphere such as the air use may be made of platinum, platinum-rhodium and the like.
In vacuum or reducing atmosphere, it is preferable to use carbon, tungsten, molybdenum or their alloys and boron nitride for nozzle material.
In case of treating semiconductor material having a comparatively low melting point such as 1,400° C., fused silica may be used, if an operating time is limited. Further, as the top end configuration of the nozzle, use may be made of circular, elliptic, slit and the like, but any configuration can be selected in accordance with a width of semiconductor thin ribbon wafer to be obtained. A wide or broad thin ribbon wafer can be obtained by properly selecting the nozzle configuration. When the inner surface of a nozzle is lined with for example boron nitride, the melt semiconductor material can easily be ejected and the manufacture thereof becomes easy.
The melt semiconductor material should be ejected through the nozzle under a given pressure. If the ejection pressure is too high or too low, a configuration of thin ribbon wafer becomes deteriorated or irregular. Therefore the ejection pressure is preferably within the range of 0.01-1.5 atm.
In order to obtain the semiconductor thin wafer of excellent quality, the melt should be rapidly cooled upon being ejected on the moving or rotating surface of the moving or rotating substrate and thus the moving or rotating substrate having good machinability and thermal conductivity should be used. For instance, use may be made of the moving or rotating substrate consisting of copper, copper alloys, aluminum, iron, steel, stainless steel, fused silica, semisintered porcelain and the like.
If a revolution speed of this rotating member is too slow, a thickness of the semiconductor thin ribbon wafer becomes thick to flaky or powdery, so that the linear velocity of the surface of the rotating member is preferably more than 5 m/sec.
A diameter of the moving or rotating substrate may be determined depending upon each condition, such as the melting temperature of semiconductor material, the revolution speed of the rotating member and the ejecting pressure through the nozzle. For instance, even if linear velocities of surfaces of two rotating drums having different diameters are made identical with each other, centrifugal force produced by the rotating substrate of larger diameter is smaller than that of the rotating substrate of smaller diameter, so that the semiconductor thin wafer of good quality cannot be obtained from material having large adhesivity to the rotating surface. Further if a semiconductor material melt has small adhesivity, a good semiconductor thin wafer cannot be produced, because a cooling time is too short and at least a part of the melt state is contained in an atmosphere.
As the rotating substrate, use may be made of a disc or a drum, and in both cases, it is preferable to use a smooth and flat rotating surface as a cooling surface.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be explained in more detail referring to the accompanying drawings.
FIG. 1 is a fundamental diagrammatical view of an apparatus for manufacturing a thin ribbon wafer of semiconductor material according to the invention;
FIG. 2 is a sectional diagrammatical view showing experimental apparatus comprising a vacuum chamber;
FIG. 3 illustrates a heat resisting tube having a single round ejecting nozzle hole for carrying out the method of the present invention;
FIG. 4 illustrates a nozzle having a laterally extended elliptical ejecting nozzle hole for carrying out the present invention;
FIG. 5 shows a nozzle having two round holes arranged in a lateral direction for carrying out the present invention;
FIG. 6 illustrates a nozzle having two rectangular ejecting nozzle holes arranged in a lateral direction for carrying out the present invention;
FIG. 7 illustrates a nozzle having two laterally extended rectangular ejecting nozzle holes arranged in one direction;
FIG. 8 illustrates a nozzle having H-shape ejecting nozzle hole in a cross section for carrying out the present invention;
FIG. 9 illustrates a nozzle having two laterally extended elliptical ejecting nozzle holes arranged in parallel direction for carrying out the present invention;
FIG. 10 illustrates a nozzle having a plurality of longitudinally extended rectangular ejecting nozzle holes arranged in parallel direction for carrying out the present invention;
FIG. 11 illustrates a nozzle having a plurality of three longitudinally extended elliptical ejecting holes arranged in parallel direction for carrying out the present invention;
FIG. 12 illustrates a nozzle having a plurality of longitudinally extended rectangular ejecting holes arranged in lateral direction and having a pair of sub-ejecting holes arranged in both outermost portions for carrying out the present invention;
FIG. 13 is a graph showing a relation of an impurity concentration between raw semiconductor material and the thin ribbon wafer; and
FIG. 14 is a graph expressing hall mobilities of the thin ribbon wafer, single crystal and chemical vapour deposited polycrystal of silicon.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1, a reference numeral 1 designates a heat resisting tube, 2 a melt of semiconductor material, 3 a nozzle, 4 a heater, 5 a thermocouple, 6 moving or rotating cooling substrate, 7 a thin ribbon wafer of semiconductive material, respectively.
In FIG. 1, a melt of semiconductor material 2 consisting of germanium is contained in a heat resisting tube 1. The heat resisting tube 1 is composed of a fused silica tube lined with boron nitride. The heat resisting tube 1 is provided with a nozzle 3 having a diameter of 0.1-0.5 mm at its free end. The melt of semiconductor material 2 in the heat resisting tube 1 is maintained at a temperature of 940°-980° C. by means of a heating resistor 4. Below the heat resisting tube 1 is rotatably arranged a cooling substrate 6 made of stainless steel. The cooling substrate 6 is 300 mm in diameter and rotated at a speed of 2,000 rpm. The cooling substrate 6 is formed by a drum having a smooth and flat peripheral surface. The nozzle 3 is arranged close to the smooth and flat rotating surface of the drum 6. The melt of germanium in the heat resisting tube 1 is ejected on the rotating surface through the nozzle 3 with adjusting the ejecting pressure within a range of 0.03-1.5 atmospheric pressure. As soon as the melt germanium is made in contact with the rotating surface of the drum 6 the melt is quickly cooled on the rotating surface and a semiconductor thin ribbon wafer having a fine and compact microscopic structure is obtained in a continuous manner.
The thus obtained thin ribbon wafer of semiconductor is 5-30 μm in thickness and 0.1-0.8 mm in width. It was ascertained by an X-ray diffraction image that this thin ribbon wafer was substantially composed of a uniformly fine crystalline texture over the whole or on a substantial part.
Further, the thin ribbon wafer of silicon semiconductor was manufactured in vacuum with the use of a device shown in FIG. 2. In FIG. 2, a silicon material 12 is inserted into a heat resisting silica tube 9 and heated to be molten at a temperature of 1,650° C. in an electric furnace 14. A temperature can be measured by a thermocouple 24. In this case, the vacuum chamber 11 placed on a base 23 is evacuated from an outlet 16 by a vacuum pump (not shown) and maintained at high vacuum of 10 - 4 Torr. The chamber is provided thereon with a terminal plate 25 and is further provided therein with a cooling device comprising a rotating cooling drum 18 made of copper having a diameter of 40 mm and a thickness of 10 mm secured to a variable speed motor 19, arranged on a support 20, whose speed varies 0-30,000 rpm. The pressures in the vacuum chamber 11 can be reduced within the range of 10 -4 -760 Torr, and the atmosphere can be replaced by nitrogen, argon gas and the like for further pressure reduction. Prior to ejecting the silicon melt 12, a shutter 13 is opened by handing a knob 15. The shutter 13 is made closed before ejecting for preventing the drum 18 from being heated. Then, an electromagnetic valve (not shown) is turned on to actuate a cylinder 8 so as to lower the tube 9 to a position immediately above the rotating drum 18 which is rotated at a speed of 0-30,000 rpm, and argon gas at 0.5 atmospheric pressure is forced into the tube through a gas inlet 22. The melt of silicon is rapidly cooled on a rotating substrate drum and is throwing away in a form of thin wafer and gathered together in a collecting port 21 for taking out after the completion of the ejecting. In this experimental device, it is possible to charge a raw material into an inlet 17 after the tube 9 has been heated. This device has an advantage in that any damage such as deformation or oxidation in the thin ribbon wafer due to collision with the fluid in atmosphere resulting from the rapid formation of the thin wafer by the evacuation of vacuum chamber is considerably mitigated by reducing an atmospheric pressure, so that this device is very effective for obtaining long thin ribbon wafers. In order to prevent an excessive oxidation, it is preferable to use an inert gas as the atmosphere at the reduced atmospheric pressure.
The thus obtained silicon thin ribbon wafer by rapidly cooling the melt of silicon was 2.0 mm in width, 10 μm in thickness and more than 10 cm in length. The thin wafer was made into a thinner one of about 0.5 μm in thickness by etching, whose electron beam diffraction pattern was observed by a 1,000,000 V perspective electron microscope. As a result, it has been found that the thin wafer of silicon semiconductor was of a fine homogeneous crystalline texture.
In another embodiment, 0.40 of germanium, 0.5 of silicon, 0.05 of boron and 0.05 of phosphorus in atomic ratio were heated together in a molybdenum tube by means of a tungsten heater to form a melt and the melt was ejected onto a smooth and flat outer surface of a drum type rotating cooling substrate made of beryllium copper alloy having 50 mmφ in diameter rotating at 2,000-20,000 rpm with the aid of argon gas at 0.03-1 atmospheric pressure through a nozzle having a diameter of 0.1-0.5 mmφ to obtain a thin ribbon wafer consisting of 0.4 germanium, 0.5 silicon, 0.05 boron and 0.05 phosphorus in atomic ratio and having 10-40 μm in thickness and 0.2-1.0 mm in width. In this case, the whole device was put into the above vacuum chamber 11 which was maintained at 1 atmospheric pressure or 10 -3 Torr. Further, the vacuum chamber was previously filled with argon gas and the pressure in the chamber was reduced. The non-oxidizing atmosphere is effective to prevent an oxidation of the surface of the thin ribbon wafer. Further, the effect of pressure reduction is remarkable in this embodiment. The damage such as deformations or creases due to the collision of the thin ribbon wafer with the gas is reduced to vacuum or the reduced pressure, and as a result, a long thin ribbon wafer having a good quality becomes obtainable.
In a further embodiment, ZnTe was molten in a platinum-rhodium tube and kept at a temperature immediately above the melting point of 1,239° C. and was ejected through a nozzle of 0.1-0.4 mmφ onto a smooth and flat surface of a stainless steel drum of 20 mmφ in diameter, rotating 6,000 rpm at 0.03-1 atmospheric pressure to obtain a semiconductor thin ribbon wafer. When a part of this thin ribbon wafer was observed by a polarizing metal microscope, it was in the dark grey state under the cross nicol state, and a boundary of crystal of the thin wafer was only visible, and a characteristic of the fine and compact crystalline texture close to amorphous state was observed. The electric and magnetic properties of these thin semiconductor ribbon wafers were examined and it is found that these electric and magnetic properties are comparatively superior than that of the conventional semiconductor thin wafers.
Besides the above properties, the characteristics of the semiconductor thin ribbon wafer obtained by the method according to the invention will be explained as follows.
As mechanical strength, if thin wafers having same thickness and same size are bent, its bending strength upto a fracture limit shows a high value of 2-3 times of those of semiconductors with a common crystalline texture. In other words, the mechanical strength of the thin ribbon wafer according to the invention is considerably higher.
As described above, according to the invention, a semiconductor thin ribbon wafer is obtained under the fine texture state by ejecting a melt of semiconductor material through a nozzle and rapidly cooling it on the moving surface of a cooling substrate at a cooling rate of more than 1,000° C./sec up to 1,000,000° C./sec. The thus obtained thin ribbon wafer can be manufactured at a remarkably high speed as compared with the conventional method for manufacturing a conventional semiconductor wafer with the polycrystal texture and thus is very effective for use in such an apparatus that a great number of semiconductor elements are required.
The semiconductor thin ribbon wafer having the fine and compact crystalline texture is usable as rectifiers, junction element by ion implantation, varisters, thermistors, memory elements, photoelectric elements, photo cells, thermo electric elements, electronic cooling elements, atomic cell elements and the like, and remarkably valuable in industry.
The present invention can be carried out not only by a nozzle having a single nozzle hole, but also by a nozzle having multi nozzle holes.
The embodiment with respect to the multi nozzle according to the invention will be explained in detail with reference to the following embodiments illustrated in FIGS. 3-12.
A nozzle according to the present invention can have a circular single hole as shown in FIG. 3; a longitudinally extended elliptical hole shown in FIG. 4; but also a nozzle having two round holes aligned in FIG. 5. Further, according to the invention, a thin ribbon wafer of semiconductor having large width is manufactured with the use of a laterally or longitudinally extended multi-hole nozzle parallelly arranged in lateral or longitudinal direction as shown in FIGS. 6, 7, 8, 9, 10, 11 and 12.
FIGS. 3a and 3b are bottom and cross sectional views showing a regular nozzle. This nozzle has a circular ejecting nozzle hole 3a having a diameter of 0.1-1 mm and its characteristic is to be capable of obtaining a thin ribbon wafer of semiconductor 7 having a width not smaller than the diameter even by ejecting a melt of semiconductor material having high viscosity through the nozzle hole.
FIGS. 4a and 4b show a nozzle having an elliptical hole 3b. A characteristic of this nozzle is that the nozzle is suitable for manufacturing a thin ribbon wafer of semi-conductor 7 having a comparatively large width and capable of manufacturing a thin ribbon wafer of semiconductor having a fairly large width.
FIGS. 5a and 5b; FIGS. 6a and 6b show other embodiments of a nozzle 3 having two ejecting nozzle holes aligned adjacent to each other in a lateral direction. FIGS. 5a and 5b show a nozzle 3 having two circular ejecting nozzle holes 3c-1, 3c-2 viewing from the end of nozzle, and FIGS. 6a and 6b show the nozzle 3 having two longitudinally extended rectangular holes 3d-1, 3d-2 arranged in parallel. A rotary axis of a rotating cooling substrate 6 is aligned in parallel to the direction for connecting the centers of these ejecting nozzle holes 3c-1 and 3c-2, 3d-1 and 3d-2, respectively. The principle for using this nozzle 3 is as follows. As described above, the width of a thin ribbon wafer of semiconductor is generally wider than that of the nozzle hole. That is, a closely ejected melt 2 is widened in diameter when impinged upon a rotating cooling substrate 6 from the ejecting nozzle hole of the nozzle 3. As shown in FIG. 5, if two ejecting nozzle holes 3c-1 and 3c-2 are closely aligned, two parallel jet flows 2a and 2b of melt are impinged upon the rotating cooling substrate 4 and amalgamated with each other thereon. As shown in FIG. 6, if the longitudinally extended rectangular ejecting nozzle holes 3d-1 and 3d-2 are closely aligned, the two parallel jet flows 2a and 2b of melt get close the circular cross-section by surface tension during flowing down and amalgamated around at the surface of rotating cooling substrate 6. In this manner, a thin ribbon wafer of semiconductor having a substantially twice time larger width than that of the image nozzle hole can be obtained. Semiconductor material thus becomes a thin ribbon wafer of semiconductor having a large width. A size of the ejecting nozzle holes employed in this case is 0.6 mmφ in diameter and 70 μm in nozzle hole space in case shown in FIG. 5 and 1 mm in length, 0.5 mm in width and 60 μm in nozzle hole space in case shown in FIG. 6. In both cases, use is made of a fused silicate tube as nozzle material and the ejecting nozzle holes are manufactured by means of an ultrasonic processor. The above semiconductor material is molten at a temperature of 1,300° C. and cooled in super high speed by means of a rotating copper drum type substrate 6 under a pressure of 1 atom., a radius of 300 mmφ, a thickness of 10 mm and a number of rotation of 2,000 rpm.
A nozzle 3 having elongated two nozzle holes 3e-1 and 3e-2 sufficiently closed with each other as shown in FIGS. 7a and 7b is suitable for manufacturing a comparatively thin ribbon wafer. This nozzle 3 can be applied to the manufacture of a semiconductor thin ribbon wafer having a large width under the condition similar to that for manufacturing the thin ribbon wafer with using the conventional single hole nozzle. In particular, a semiconductor thin ribbon wafer having a width of 7 mm was obtained by ejecting the melt heated at a temperature of 1,300° C. under 0.6 atmospheric pressure through the nozzle 3 made of molten quartz provided with two rectangular holes 3e-1 and 3e-2 of 0.6 mm in length and 3 mm in width spaced apart from each other by 50 μm and by rapidly cooling the melt by bringing it in contact with the rotating cooling drum type substrate 6. In case that the viscosity of the molten jet is low, if use is made of the nozzle 3 having the ejection nozzle hole 3f, in which a center portion of the partition for spacing two elongated square type ejection nozzle holes 3e-1 and 3e-2 is removed by 50-100 μm as shown in FIGS. 8a and 8b, a more preferable result can be obtained.
FIGS. 9a and 9b show another embodiment of the nozzle in which two elongated elliptical type ejection holes 3g-1 and 3g-2 are arranged side by side viewed in the direction of the rotation of the cooling substrate 6. Each of these nozzle holes is located in a chamber formed by a partition 1a for containing two kinds of semiconductor materials. When melts are ejected through these nozzle holes 3g-1 and 3g-2, it is possible to produce a double-layered thin ribbon wafer. In the embodiment of this nozzle, provision is made of two ejection nozzle holes having 0.2 mm in length and 0.7 mm in width vertically spaced apart from each other by 50 μm. With the use of this nozzle, germanium and silicon are separately charged into the nozzle chamber and separately molten in the above two nozzle chambers at a temperature of 1,500° C., these two chambers are communicated to a common pressure source for ejecting at a common atmospheric pressure of 0.7 and rapidly cooled by ejecting onto said rotating cooling substrate 6 at a cooling rate of 1,000°-1,000,000° C./sec. Further, P-type silicon and N-type silicon are cooled under the similar condition with the use of this nozzle at a temperature of 1,500° C. and an atmospheric pressure of 0.5. The thus obtained thin ribbon wafer is of a double-layered structure having about 0.8 mm in width and about 50 μm in thickness. In this manner it is possible a semiconductive thin ribbon wafer having a p-n junction.
FIGS. 10a and 10b illustrate another embodiment of the nozzle having three elliptical ejection nozzle holes 3h-1-3h-3. In this case, as far as three nozzle holes are not spaced apart from each other, a thin ribbon wafer three times wider than the width of ejection nozzle holes can be obtained. That is, for example, three elliptical ejection nozzle holes having 1 mm in length and 0.7 mm in width are spaced apart from each other by 100 μm, the thin ribbon wafer having a width of 2.3 mm was produced. This embodiment is suitable for manufacturing a comparatively thick ribbon type thin wafer of semiconductor. The multi-hole nozzles of the present embodiment and the preceding embodiments are not preferable, if a space between the ejection nozzle holes is too wide, because creases might be formed in the finally obtained thin ribbon wafers. In case, except the positive use of this crease, it is preferable to make a thickness of the partition between the ejection nozzle holes at least less than 1/3 of the longest size of the ejection nozzle hole, and it is more preferable to make the thickness 1/5 to 1/10. By using such a nozzle, the thin ribbon wafers of semiconductor having a desired width were obtained. However, if a thickness of the partition is too thin, such as less than 40 μm, the partition is easily broken.
FIGS. 11a and 11b show still another embodiment of the multi-hole type nozzle having five long elliptical ejection nozzle holes 3i-1-3i-5 laterally aligned in a row. With the aid of such a nozzle, a thin ribbon wafer of semiconductor having a width about 5 times larger than the diameter of the ejection nozzle hole is formed. The principle of this nozzle is as follows. For comparison, in the nozzle shown in FIG. 4, a length of the laterally elongated elliptical ejection nozzle hole 3b is same as a total length of the ejection nozzle hole row of the nozzle shown in FIG. 11. When the jet of the melt is flown down through the wide elliptical nozzle hole 3b, the width of the molten jet flow becomes gradually narrow as flowing down and at the same time a thickness of the molten jet flow measured in a direction perpendicular to the width becomes thick. If the width of the molten jet flow becomes large, the defect might often occur at the center position or any other position of the thin ribbon wafer. It means that the molten jet flow is not uniformly flown down over the width but both side portions of the jet flow are obliquely flown down toward the center, so that the jet flow is concentrated into the center portion. In the embodiment shown in FIG. 11, however, the ejection nozzle holes 3i-1-3i-5 are laterally aligned in a row, each jet flow is flown down in parallel to each other, and all the jet flows are amalgamated on the surface of rotating cooling substrate 6. This principle is same as the embodiments shown in FIGS. 5 and 6. The nozzle shown in FIG. 11 has the following specification as compared with the embodiment shown in FIG. 10. Three central holes 3i-2, 3i-3, 3i-4, form a main hole row and two slightly small sub-holes 3i-1 and 3i-5 on both sides of the main hole row have about 80% hole width as compared with three main holes for reducing an edge effect on both sides of the thin ribbon wafer. In one embodiment of the invention, the width of the main hole is 0.8 mmφ, the width of the sub-hole is 0.7 mm and the space of the ejection nozzle holes is 80 μm. The ejection holes of this embodiment can easily be formed with the aid of an untrasonic machine. By rapidly cooling a silicon melt with the use of the present nozzle under the condition previously found by the inventor, thin ribbon wafers of silicon semiconductor having about 5 mm to 10 mm in width were obtained.
FIG. 12 shows a nozzle comprising a plurality of rectangular main holes 3j-1 and two auxiliary holes 3j-2 arranged on each side of main hole array for ignoring an edge effect to a great extent. According to this nozzle, a thin ribbon wafer an optional with can be formed in principle. As the main nozzle hole 3j-1, use may be made of a merely rectangular hole, a long circular elliptical hole, and any shape which can uniformly combine said melt jet flows over the whole width of wide thin ribbon wafer. With the aid of this nozzle, thin ribbon wafer of semiconductor having any desired width can be obtained.
As nozzle material, each kind of material can be selected in accordance with purposes. For example, fused quartz can be used over the range of 1,000° C. or more than that, i.e., several hundred degrees in centigrade. As nozzle material, use is made of heat resisting ceramics such as Al 2 O 3 , MgO, beryllium oxide, etc. The nozzle made of such ceramics is preferably lined with boron nitride at a lower portion, particularly on an inner surface. In this case, semiconductor material can be molten at a high temperature. Particularly, a nozzle made of boron nitride has been found preferable for manufacturing the semiconductor thin ribbon wafer. Particularly, when a reduced atmosphere or vacuum is required, this nozzle material is effective and preferably available for a vacuum tank. The lining of the lower portion, particularly the inner surface of the nozzle lined with niobium nitride, is very effective for weakening a reaction of the melt with nozzle material.
The embodiment with respect to manufacture a ribbon type thin wafer of semiconductor material will be explained in detail with reference to the following examples.
EXAMPLE 1
In a transparent quartz tube having a nozzle at its end, a pure silicon having a purity of 10 -8 was heated to 1,550° C. to form a uniform melt thereof. The melt thus formed was ejected through the nozzle onto a drum made of beryllium copper alloy and having a diameter of 300 mm, said drum being placed in a vacuum of 10 -8 Torr, and rotated at a speed of 2,500 rpm.
A silicon thin ribbon wafer obtained in this example has a typical thickness of 30 μm and a length of 10 cm. A resistivity of the wafer is 10 8 Ω-cm and a greater part i.e. more than 50% by volume is formed by grains having diameters of about 3 to 50 μm. Fine and condensed crystalline structure is grown in such a manner than an axis [110] situates within ±40° with respect to a normal to the wafer surface. It should be noted that the thickness of wafer can be varied within a range of 5-200 μm. The break down test for the wafer expressed that bending radii of the wafers having thicknesses of 5 μm, 30 μm and 200 μm are 0.5 cm, 5 cm and 20 cm, respectively. Such a strength against bending is sufficient for manufacturing actual semiconductor devices. Such a large bending strength can be conceived by the fact that crystal axes of the fine crystalline grains have orientated substantially in the same direction. Such an orientation of the crystal axes is very suitable for electrical properties of the semiconductor thin ribbon wafer, because a property of the crystal surface such as a surface potential density can be determined simply and a recombination probability at a crystal interface is reduced.
EXAMPLE 2
In the transparent quartz tube raw materials consisting of pure silicon having added thereto P, Sb, B and Sn, respectively by an as much amount as can form a solid solution was heated over a melting point. A melt was ejected through the nozzle onto a copper drum rotating at 2,300 rpm. The drum had a diameter of 400 mm and was placed in a vacuum of 10 -8 Torr.
Thin ribbon wafers obtained in this example 2 have substantially same thickness, length and grain diameter as those of the first example 1. However the resistivity was reduced as compared with the example 1 to a greater extent. The resistivities and impurity concentrations of the thin ribbon wafers are shown in the following table.
______________________________________Added ImpurityElement Resistivity Concentration______________________________________P 10.sup.-3 Ωcm 10.sup.18 /cm.sup.3Sb 10.sup.-2 cm 10.sup.18 /cm.sup.3B 10.sup.-2 cm 10.sup.18 /cm.sup.3Sn -- --______________________________________
It should be noted that even if tin was added to silicon by 25%, it was possible to form a flexible thin ribbon wafer.
EXAMPLE 3
In the transparent quartz tube pure silicon having added B thereto was heated to form a melt thereof. The melt was ejected through the nozzle onto a stainless steel drum and a stainless steel endless belt, respectively arranged in the air. The drum has a diameter of 180 mm and was rotated at a speed of 3,000 rpm. The belt was travelled at a linear speed of 20 m/s.
In the present example thin ribbon wafers of p conductivity type having a width of about 6 mm and a length of several centimeters were obtained. An oxygen distribution into a depth direction was measured by a combination of an ion etching and an Anger's electron spectroscopic method and it was found that below a hundred and several ten A from the surface of silicon oxide was observed and in a deeper region an oxide concentration was abruptly decreased. The resistivity of the deeper region was about 0.01 Ω-cm. It was found that the wafer has a preferable property for forming semiconductor devices such as a substrate for growing a semiconductor crystal including polycrystal, a thin film wafer, a ribbon, sheet and the other material for semiconductor elements. From a light absorption spectrum measurement it was further found that the thin ribbon wafer obtained in this example situates at an intermediate position between a single crystal state and an amorphous state.
EXAMPLE 4
The thin ribbon wafers obtained in the example 3 were subjected to a heat treatment in a vacuum and inert gas under the various conditions. A first sample of the thin ribbon wafer was heated at 500° C. for one week, a second one was heated at 1,100° C. for 48 hours and a third one was heated at about a melting point for 0.1 second. The last sample was dropped through a pipe type furnace heated at 1,420° C. The heat treatment has resulted in that the grain of the crystalline structure was grown. That is to say in the first, second and third samples, the grain size was increased by 1.1, 5 and 2 times, respectively as compared with the that of the ribbon wafer before the heat treatment. In the wafer thus treated there were grains having diameters of 5-500 μm. It was also found that the columnar structure of the ribbon wafer was improved by the heat treatment and the [110] axes of almost all grains were directed in a direction normal to the wafer surface. A light absorption spectrum was deflected towards the single crystal side. The electrical property of the ribbon wafer subjected to the heat treatment becomes similar to that of the single crystal. That is the resistivity of the wafer thus treated was decreased by more than 80% of that of the wafer as grown. When the grain size becomes large and the resistivity is decreased, a possibility of a recombination of electrons and holes situated at a boundary of grain surfaces is reduced and thus a recombination rate is decreased so as to prolong a life time of electrons and holes. Further a mobility is increased by the heat treatment.
When all samples were further heated at 1,400° C. for 24 hours the substantially whole width of the wafer was occupied by a single grain.
From the various experiments it is found that the grains of the thin ribbon wafer as grown are extremely increased in size by the heat treatment at a temperature within a range from 500° C. to a melting point for a time period within a range from 0.1 second to one week. Particularly the better result can be obtained by heating the wafer at about the melting point thereof. The heating may be effected in vacuum or in an inert gas such as argon.
FIG. 13 is a graph showing an impurity concentration characteristic of the thin ribbon wafer according to the invention. In the graph, an abscissa represents an impurity concentration of raw material, i.e. starting material and an ordinate an impurity concentration of the thin ribbon wafer as grown. Black dots express an electron density and vacant dots a hole density. As can be clearly seen from the graph the both concentrations correlate linearly to each other. This means that when the impurity concentration of the charge is selected to a desired value, the thin ribbon wafer as grown can also have the same desired impurity concentration. This is very preferable to manufacture various semiconductor devices.
FIG. 14 illustrates a graph showing a hall mobility of the thin ribbon wafer as grown according to the invention. In the graph curves A and B show n-type and p-type mobilities, respectively of the single crystal of silicon. A curve C represents a hall mobility of a polysilicon formed by a chemical vapour deposition. Black dots and vacant dots express n-type and p-type mobilities, respectively of the thin ribbon wafer according to the invention. As can be understood from the graph, the hall mobility of the thin ribbon wafer is superior to that of the known CVD polysilicon and is comparative with that of the single crystal thereof. It has been further found experimentally that the hall mobility of the wafer according to the invention can be increased by about two times by subjecting it to the heat treatment.
It is very important to select the material of cooling substrate depending upon semiconductor material to be used by taking into account a wettability between the melt of semiconductor material and the cooling substrate. The wettability is mainly determined by surface tensions of the melt and the substrate, and the viscosity of the melt. When the melt temperature is too high more than 300° C. above the melting point, the melt might spread over the cooling surface of the substrate so that the ribbon wafer becomes too thin and some times a greatly notched ribbon similar to a rattan blind might be produced, while when the melt temperature is too low, the jet flow of the melt might not creep along the surface of the substrate, so that the jet flow is divided into a number of small particles having irregular configuration. According to the invention, it is preferable to select such a viscosity of the melt that edges of the melt are made in contact with the substrate at an angle from 10° to 170° with respect to the substrate surface. For this purpose, a temperature of the melt should be selected within the range from the melting point to 300° C. above the melting point, particularly 100° C. to 150° C. above the melting point.
It is also very important that the melt of semiconductor material should be instantaneously very rapidly cooled on the cooling substrate at a suitable cooling rate of at least 1,000° C./sec, preferably 1,000 to 1,000,000° C./sec by taking account of wettability between the melt of semiconductor material and the cooling substrate.
According to the invention, it has been found that the pressure under which the melt is ejected through the nozzle should be within the range of 0.01-1.5 atm.
The ejection of the melt is preferably effected in a vacuum but it may be carried out in an inert gas or reducing gas atmosphere. Even in the latter case, it is preferable to reduce the pressure.
According to the invention, it is possible to manufacture the thin and flexible ribbon wafer of semiconductor material of a fine microscopic structure of high density having a large mechanical strength and an excellent electrical property. Therefore, various semiconductor devices can be manufactured with using such a ribbon wafer in a simple and reliable manner.
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A method for manufacturing a thin and flexible ribbon wafer of semiconductor material such as germanium, silicon, selenium, tellurium, PbS, InSb, ZnTe, PbSe, InAs, InP, GaSb, PbTe, ZnS, Bi 2 Te 3 , and mixtures thereof comprises melting the semiconductor material at a temperature within the range from a melting point thereof to 300° C. above the melting point to form a uniform melt; ejecting under a pressure the melt through a nozzle against a cooling surface of a moving substrate to cool very rapidly a jet flow of the melt at a cooling rate of 1,000° C. to 1,000,000° C./sec to form the ribbon type thin and flexible wafer of fine and compact microscopic structure having a large mechanical strength and an excellent electrical property. It is possible to add to the melt various additives as fluxes or impurities such as B, P, BP, Sb Sn, As, B, P, Sb, In, Al and alloys intermetallic compounds, and conjugates thereof. The thin ribbon wafer as grown is preferably heated at a temperature from within the range 500° C. to the melting point for a time within the range from 0.1 second to one week. The invention also provides a thin and flexible ribbon wafer of semiconductor material manufactured by the above mentioned process.
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FIELD OF THE INVENTION
[0001] The present invention relates generally to the field of oil and gas exploration. More particularly, the invention relates to methods for determining at least one property of a subsurface formation penetrated by a wellbore using a formation tester.
DESCRIPTION OF THE PRIOR ART
[0002] Over the past several decades, highly sophisticated techniques have been developed for identifying and producing hydrocarbons, commonly referred to as oil and gas, from subsurface formations. These techniques facilitate the discovery, assessment, and production of hydrocarbons from subsurface formations.
[0003] When a subsurface formation containing an economically producible amount of hydrocarbons is believed to have been discovered, a borehole is typically drilled from the earth surface to the desired subsurface formation and tests are performed on the formation to determine whether the formation is likely to produce hydrocarbons of commercial value. Typically, tests performed on subsurface formations involve interrogating penetrated formations to determine whether hydrocarbons are actually present and to assess the amount of producible hydrocarbons therein. These preliminary tests are conducted using formation testing tools, often referred to as formation testers. Formation testers are typically lowered into a wellbore by a wireline cable, tubing, drill string, or the like, and may be used to determine various formation characteristics which assist in determining the quality, quantity, and conditions of the hydrocarbons or other fluids located therein. Other formation testers may form part of a drilling tool, such as a drill string, for the measurement of formation parameters during the drilling process.
[0004] Formation testers typically comprise slender tools adapted to be lowered into a borehole and positioned at a depth in the borehole adjacent to the subsurface formation for which data is desired. Once positioned in the borehole, these tools are placed in fluid communication with the formation to collect data from the formation. Typically, a probe, snorkel or other device is sealably engaged against the borehole wall to establish such fluid communication.
[0005] Formation testers are typically used to measure downhole parameters, such as wellbore pressures, formation pressures and formation mobilities, among others. They may also be used to collect samples from a formation so that the types of fluid contained in the formation and other fluid properties can be determined. The formation properties determined during a formation test are important factors in determining the commercial value of a well and the manner in which hydrocarbons may be recovered from the well.
[0006] The operation of formation testers may be more readily understood with reference to the structure of a conventional wireline formation tester shown in FIGS. 1A and 1B . As shown in FIG. 1A , the wireline tester 100 is lowered from an oil rig 2 into an open wellbore 3 filled with a fluid commonly referred to in the industry as “mud.” The wellbore is lined with a mudcake 4 deposited onto the wall of the wellbore during drilling operations. The wellbore penetrates an earth formation 5 .
[0007] The operation of a conventional modular wireline formation tester having multiple interconnected modules is described in more detail in U.S. Pat. Nos. 4,860,581 and 4,936,139 issued to Zimmerman et al. FIG. 2 depicts a graphical representation of a pressure trace over time measured by the formation tester during a conventional wireline formation testing operation used to determine parameters, such as formation pressure.
[0008] Referring now to FIGS. 1A and 1B , in a conventional wireline formation testing operation, a formation tester 100 is lowered into a wellbore 3 by a wireline cable 6 . After lowering the formation tester 100 to the desired position in the wellbore, pressure in the flowline 119 in the formation tester may be equalized to the hydrostatic pressure of the fluid in the wellbore by opening an equalization valve (not shown). A pressure sensor or gauge 120 is used to measure the hydrostatic pressure of the fluid in the wellbore. The measured pressure at this point is graphically depicted along line 103 in FIG. 2 . The formation tester 100 may then be “set” by anchoring the tester in place with hydraulically actuated pistons, positioning the probe 112 against the sidewall of the wellbore to establish fluid communication with the formation, and closing the equalization valve to isolate the interior of the tool from the well fluids. The point at which a seal is made between the probe and the formation and fluid communication is established, referred to as the “tool set” point, is graphically depicted at 105 in FIG. 2 . Fluid from the formation 5 is then drawn into the formation tester 100 by retracting a piston 118 in a pretest chamber 114 to create a pressure drop in the flowline 119 below the formation pressure. This volume expansion cycle, referred to as a “drawdown” cycle, is graphically illustrated along line 107 in FIG. 2 .
[0009] When the piston 118 stops retracting (depicted at point 111 in FIG. 2 ), fluid from the formation continues to enter the probe 112 until, given a sufficient time, the pressure in the flowline 119 is the same as the pressure in the formation 5 , depicted at 115 in FIG. 2 . This cycle, referred to as a “build-up” cycle, is depicted along line 113 in FIG. 2 . As illustrated in FIG. 2 , the final build-up pressure at 115 , frequently referred to as the “sandface” pressure, is usually assumed to be a good approximation to the formation pressure.
[0010] The shape of the curve and corresponding data generated by the pressure trace may be used to determine various formation characteristics. For example, pressures measured during drawdown ( 107 in FIG. 2 ) and build-up ( 113 in FIG. 2 ) may be used to determine formation mobility, that is the ratio of the formation permeability to the formation fluid viscosity. When the formation tester probe ( 112 FIG. 1B ) is disengaged from the wellbore wall, the pressure in flowline 119 increases rapidly as the pressure in the flowline equilibrates with the wellbore pressure, shown as line 117 in FIG. 2 . After the formation measurement cycle has been completed, the formation tester 100 may be disengaged and repositioned at a different depth and the formation test cycle repeated as desired.
[0011] During this type of test operation for a wireline-conveyed tool, pressure data collected downhole is typically communicated to the surface electronically via the wireline communication system. At the surface, an operator typically monitors the pressure in flowline 119 at a console and the wireline logging system records the pressure data in real time. Data recorded during the drawdown and buildup cycles of the test may be analyzed either at the well site computer in real time or later at a data processing center to determine crucial formation parameters, such as formation fluid pressure, the mud overbalance pressure, i.e. the difference between the wellbore pressure and the formation pressure, and the mobility of the formation.
[0012] Wireline formation testers allow high data rate communications for real-time monitoring and control of the test and tool through the use of wireline telemetry. This type of communication system enables field engineers to evaluate the quality of test measurements as they occur, and, if necessary, to take immediate actions to abort a test procedure and/or adjust the pretest parameters before attempting another measurement. For example, by observing the data as they are collected during the pretest drawdown, an engineer may have the option to change the initial pretest parameters, such as drawdown rate and drawdown volume, to better match them to the formation characteristics before attempting another test. Examples of prior art wireline formation testers and/or formation test methods are described, for example, in U.S. Pat. Nos. 3,934,468 issued to Brieger; 4,860,581 and 4,936,139 issued to Zimmerman et al.; and 5,969,241 issued to Auzerais. These patents are assigned to the assignee of the present invention.
[0013] Formation testers may also be used during drilling operations. For example, one such downhole tool adapted for collecting data from a subsurface formation during drilling operations is disclosed in U.S. Pat. No. 6,230,557 B1 issued to Ciglenec et al., which is assigned to the assignee of the present invention.
[0014] Various techniques have been developed for performing specialized formation testing operations, or pretests. For example, U.S. Pat. Nos. 5,095,745 and 5,233,866 both issued to DesBrandes describe a method for determining formation parameters by analyzing the point at which the pressure deviates from a linear draw down.
[0015] Despite the advances made in developing methods for performing pretests, there remains a need to eliminate delays and errors in the pretest process, and to improve the accuracy of the parameters derived from such tests. Because formation testing operations are used throughout drilling operations, the duration of the test and the absence of real-time communication with the tools are major constraints that must be considered. The problems associated with real-time communication for these operations are largely due to the current limitations of the telemetry typically used during drilling operations, such as mud-pulse telemetry. Limitations, such as uplink and downlink telemetry data rates for most logging while drilling or measurement while drilling tools, result in slow exchanges of information between the downhole tool and the surface. For example, a simple process of sending a pretest pressure trace to the surface, followed by an engineer sending a command downhole to retract the probe based on the data transmitted may result in substantial delays which tend to adversely impact drilling operations.
[0016] Furthermore, delays also increase the possibility of tools becoming stuck in the wellbore. To reduce the possibility of sticking, drilling operation specifications based on prevailing formation and drilling conditions are often established to dictate how long a drill string may be immobilized in a given borehole. Under these specifications, the drill string may only be allowed to be immobile for a limited period of time to deploy a probe and perform a pressure measurement. Due to the limitations of the current real-time communications link between some tools and the surface, it may be desirable that the tool be able to perform almost all operations in an automatic mode. For example, U.S. Patent Application No. 2004/00457006 assigned to the assignee of the present invention describes a method for determining formation parameters by using a tool being able to perform operations in an automatic mode in a limited period of time. Nevertheless, in this automatic mode, some steps are sometimes redundant or useless, increasing the time spends on non useful information during this limited period of time and increasing the possibility of tool becoming stuck in the wellbore.
[0017] Therefore, the aim of the present invention is to describe a method to perform formation test measurements downhole within a minimum period of time and that may be easily implemented using wireline or drilling tools resulting in minimal intervention from the surface system.
SUMMARY OF THE INVENTION
[0018] The invention provides a method for estimating type of a build up pressure phase, the build up pressure phase being done after a drawdown pressure phase, said both drawdown and build up phases being done to determine formation pressure using a formation tester disposed in a wellbore penetrating a permeable formation, said permeable formation being able to create a formation flow, said method being characterized by using an index to determine the contribution of formation flow on the pressure build up phase.
[0019] In a further aspect of the invention, a method is disclosed for estimating a formation pressure using a formation tester disposed in a wellbore penetrating a formation, said method comprising: (a) establishing fluid communication between a pretest chamber in the downhole tool and the formation via a flowline, the flowline having an initial pressure therein; (b) moving a pretest piston in a controlled manner in the pretest chamber to reduce the initial pressure to a drawdown pressure during a drawdown phase; (c) terminating movement of the piston to permit the drawdown pressure to adjust to a stabilized pressure during a build-up phase and measuring simultaneously in relation to time, pressure P(t) and temperature T(t) in the pretest chamber; (d) extracting an index i(t) dependent of the pressure P(t) and the temperature T(t) informing on the build-up phase; (e) analyzing index i(t) and repeating steps (b)-(d) or going to step (f); (f) determining the formation pressure based on a final stabilized pressure in the flowline. The method can be directly applied to all formation tester known in the art.
[0020] Preferably, the index is a function dependent of the effects of thermodynamic equilibrium in the formation tester and the effects of formation flow into the formation tester. When the build up phase occurs after a drawdown of pressure, the thermodynamic equilibrium in the formation tester plays a part in the build up phase; and the formation flow, which enters into the formation tester, plays a part in the build up phase.
[0021] Preferably, the index is a function dependent of the effects of temperature variation in the formation tester and the effects of formation flow into the formation tester. For the thermodynamic equilibrium, the variation in temperature plays a major rule.
[0022] Preferably, the index i(t) is equal to:
Δ T Δ P · δ 2 ( log ( Δ P ) ) δ t 2 ,
where ΔT is the temperature variation, ΔP is the pressure variation and t the time. When the index function tends towards zero, the build up phase is due to contribution of formation flow and when not, the build up phase is due to contribution of temperature equilibrium.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Further embodiments of the present invention can be understood with the appended drawings:
[0024] FIG. 1A shows a conventional wireline formation tester disposed in a wellbore from Prior Art.
[0025] FIG. 1B shows a cross sectional view of the modular conventional wireline formation tester of FIG. 1A .
[0026] FIG. 2 shows a graphical representation of pressure measurements versus time plot for a typical prior art pretest sequence performed using a conventional formation tester.
[0027] FIG. 3 shows a graphical representation of a pressure measurements versus time plot for performing a pretest including a modified investigation phase the pretest as defined in U.S. Patent Application No. 2004/00457006.
[0028] FIG. 4 shows a graphical representation of a pressure measurements versus time plot containing non-formation build up and formation build up.
[0029] FIG. 5 shows a schematic of components of a module of a formation tester suitable for practicing embodiments of the invention.
[0030] FIG. 6A shows a first example of the method applied to a pressure measurement versus time according to the present invention.
[0031] FIGS. 6B, 6C and 6 D show the index according to the present invention applied to a part of the pressure measurement versus time of FIG. 6A .
[0032] FIG. 7A shows a second example of the method applied to a pressure measurement versus time according to the present invention.
[0033] FIGS. 7B and 7C show the index according to the present invention applied to a part of the pressure measurement versus time of FIG. 7A .
[0034] FIG. 8A shows a third example of the method applied to a pressure measurement versus time according to the present invention.
[0035] FIGS. 8B, 8C and 8 D show the index according to the present invention applied to a part of the pressure measurement versus time of FIG. 8A .
DETAILED DESCRIPTION
[0036] An embodiment of the present invention relating to a method for estimating formation properties (e.g. formation pressures and mobilities) may be applied with any formation tester known in the art, such as the tester described with respect to FIGS. 1A and 1B . Other formation testers may also be used and/or adapted for embodiments of the invention, such as the wireline formation tester of U.S. Pat. Nos. 4,860,581 and 4,936,139 issued to Zimmerman et al. and the downhole drilling tool of U.S. Pat. No. 6,230,557 B1 issued to Ciglenec et al. The method of the present invention is an improvement of the method of U.S. Patent Application No. 2004/00457006 which discloses a method including an investigation phase and a measurement phase to estimate formation properties.
[0037] In U.S. Patent Application No. 2004/00457006, the method consists in performing an investigation phase 13 b with several drawdown steps. Referring to FIG. 3 , the method comprises the step of starting the drawdown 810 and performing a controlled drawdown 814 . It is preferred that the piston drawndown rate be precisely controlled so that the pressure drop and the rate of pressure change be well controlled. However, it is not necessary to conduct the pretest (piston drawdown) at low rates. When the prescribed incremental pressure drop (Δp) has been reached, the pretest piston is stopped and the drawdown terminated 816 . The pressure is then allowed to equilibrate 817 for a period t i 0 , 818 which may be longer than the drawdown period t pi 817 , for example, t i 0 =2 t pi . After the pressure has equilibrated, the stabilized pressure at point 820 is compared with the pressure at the start of the drawdown at point 810 . At this point, a decision is made as to whether to repeat the cycle. The criterion for the decision is whether the equalized pressure (e.g., at point 820 ) differs from the pressure at the start of the drawdown (e.g., at point 810 ) by an amount that is substantially consistent with the expected pressure drop (Δp). If so, then this flowline expansion cycle is repeated.
[0038] To repeat the flowline expansion cycle, for example, the pretest piston is re-activated and the drawdown cycle is repeated as described, namely, initiation of the pretest 820 , drawdown 824 by exactly the same amount (Δp) at substantially the same rate and duration 826 as for the previous cycle, termination of the drawdown 825 , and stabilization 830 . Again, the pressures at 820 and 830 are compared to decide whether to repeat the cycle. As shown in FIG. 3 , these pressures are significantly different and are substantially consistent with the expected pressure drop (Δp) arising from expansion of the fluid in the flowline. Therefore, the cycle is repeated, 830 - 834 - 835 - 840 . The “flowline expansion” cycle is repeated until the difference in consecutive stabilized pressures is substantially smaller than the imposed/prescribed pressure drop (Δp), shown for example in FIG. 3 as 840 and 850 .
[0039] After the difference in consecutive stabilized pressures is substantially smaller than the imposed/prescribed pressure drop (Δp), the “flowline expansion” cycle may be repeated one more time, shown as 850 - 854 - 855 - 860 in FIG. 3 . If the stabilized pressures at 850 and 860 are in substantial agreement, for example within a small multiple of the gauge repeatability, the larger of the two values is taken as the first estimate of the formation pressure. One of ordinary skill in the art would appreciate that the processes as shown in FIG. 3 are for illustration only. Embodiments of the invention are not limited by how many flowline expansion cycles are performed. Furthermore, after the difference in consecutive stabilized pressures is substantially smaller than the imposed/prescribed pressure drop (Δp), it is optional to repeat the cycle one or more times.
[0040] The point at which the transition from flowline fluid expansion to flow from the formation takes place is identified as 800 in FIG. 3 . If the pressures at 850 and 860 agree at the end of the allotted stabilization time, it may be advantageous in certain conditions to allow the pressure 860 to continue the build up in order to obtain a better first estimate of the formation pressure. The process by which the decision is made to either continue the investigation phase or to perform the measurement phase, 864 - 868 - 869 , to obtain a final estimate of the formation pressure 870 depends on certain criterions described in U.S. Patent Application No. 2004/00457006. After the measurement phase is completed 870 , the probe is disengaged from the wellbore wall and the pressure returns to the wellbore pressure 874 within a time period 895 and reaches stabilization at 881 .
[0041] As it can be understood the unknown value is the formation pressure 870 , and a precise and quick method of measurement of this value is seeking. When the difference between wellbore pressure ( 801 , 881 ) and natural formation pressure 870 is typically of 1500 psi (10 MPa), the method according to U.S. Patent Application No. 2004/00457006 is applicable: for example, with a prescribed incremental pressure drop (Δp) of 300 psi (2 MPa) the investigation and measurement phases will have the same aspect as shown in FIG. 3 . Nevertheless, when the difference between wellbore pressure ( 801 , 881 ) and formation pressure 870 is typically of 5000 psi (34.5 MPa), as for low or very low permeability rocks, the method according to U.S. Patent Application No. 2004/00457006 with a prescribed incremental pressure drop (Δp) of 300 psi (2 MPa) will take a very long time. Also, there is a possibility to increase the prescribed incremental pressure drop (Δp) for example by using a pressure drop of 1500 psi (10 MPa), however this solution will increase the time needed for a build up phase, because the time needed for the stabilization of the pressure will also be longer if using the same criterions described in U.S. Patent Application No. 2004/00457006. The build up phase depending on the formation mobility, if the formation mobility is smaller as for low or very low permeability rocks, the build up time will be longer. Therefore there is a need to find a quicker method to perform investigation and measurement phases.
[0042] The method according to the present invention is based on the use of an index, which will inform on the nature and the behavior of the build up phase. Effectively, if an index could directly inform at the beginning of the build up phase what is contributing to the pressure build up: contribution of the formation flow or thermodynamic equilibrium of the flowline, the further steps of investigation phase 13 b on FIG. 3 could be reduced.
[0043] As defined in FIG. 2 , the formation pressure is obtained from the formation tester stabilized pressure build up value 115 after a given pretest drawdown 107 . The stabilized pressure build up value is representative of the formation pressure at the condition that the pretest drawdown 107 is made lower than said stabilized pressure build up. This condition is nevertheless verified a priori, and in practice “pseudo build up” may occur when this condition is not verified ( FIG. 4 ). Firstly, some formation testers feature a filter inside the probe; when the tool is not set a piston block the fluid path to the filter to avoid probe plugging. At the end of the tool set sequence, this piston retracts and allows access to the flowline. Thus, the flowline volume increases slightly and creates a pressure drop. The setting sequence continues for a few seconds until the final hydraulic pressure is reached. And during this few seconds the packer element of the formation tester is pressed against the formation and therefore causes the pressure in the flowline to increase. This first type of “pseudo build up” occurs only at the beginning of the pretest 41 . Secondly, the pressure drop created during a drawdown cools the flowline, this cooling will be followed by a heating at the build up phase. This effect introduces a temperature gradient in the pressure sensor, affecting the measured pressure read. Furthermore, when the drawdown ends, thermodynamic equilibrium begins and the flowline tends to heat up to go back to the ambient temperature of the formation tester. This effect introduces an expansion of the flowline fluids, affecting also the measured pressure. This second type of “pseudo build up” can occur every time for a pretest drawdown 42 . In FIG. 4 , the time spent between 100 s and 400 s on a “pseudo build up” or non-formation build up 42 was useless.
[0044] In order to speed up the formation pressure measurement, it is essential to be able to define in real time in a build up phase whether the pressure should be let to increase or whether a further drawdown phase is necessary. The index is based on intrinsic characteristics of the pseudo build up phase of second type and on intrinsic characteristics of a genuine formation build up phase. So, the index takes into consideration the effects in variation of temperature (pseudo build up phase of second type) and the contribution of the formation flow on the pressure build up observed.
[0045] For the temperature effects, a relationship exists between temperature and pressure; and the value of the ratio ΔT/ΔP—the change in the pressure sensor temperature versus the change in pressure during a given time period—is used as an index. For a build up phase entirely governed by thermal effects, i.e. a non-formation build up, this ratio will be larger than for the case where the formation flow is contributing to the build up phase.
[0046] For the contribution of the formation flow, the early part of the build up phase is dominated by wellbore storage effects and the expression for the difference between the actual reservoir pressure P i and the pressure after Δt elapsed time into the build up is:
Δ P = P i - P ( Δ t ) = [ P i - P 0 ] - Δ t τ ( 1 )
where P 0 is the pressure at the onset of the build up and τ is a time constant defined as:
τ = μ k · ( 2 C + S ) · V · C f r p ( 2 )
with: m fluid viscosity k formation permeability C flow geometry coefficient S skin V flowline volume C f fluid compressibility
The equation (1) can be written in the following form:
log ( Δ P ) = - log ( P i - P 0 ) · Δ t τ ( 3 )
As it can be observed log(ΔP) is a linear function of the elapsed time Δt. And it results that for the case where the formation flow is contributing alone to the build up phase, the condition (4) is satisfied:
δ 2 ( log ( Δ P ) ) δ t 2 = 0 ( 4 )
[0053] The index takes into consideration the both effects and is the product of the index contributing to thermal effects and on the index contributing to formation flow effects:
i ( t ) = Δ T Δ P · δ 2 ( log ( Δ P ) ) δ t 2 ( 5 )
In the case where there is no formation flow effects, but only thermal effects, the
δ 2 ( log ( Δ P ) ) δ t 2
part will be non-null and the
Δ T Δ P
part will also be non-null. The index function (5) will therefore be non-null. And in the case where there is formation flow effects, and also thermal effects, the
δ 2 ( log ( Δ P ) ) δ t 2
part will have a value practically null or will tend towards zero, and the
Δ T Δ P
part will still be non-null. The index function (5) will therefore tend towards zero. So when the index function (5) tends towards zero, the build up phase is a genuine formation build up and when not, the build up phase is a non-formation build up.
[0054] As said before the method may be practiced with any formation tester known in the art. A version of a probe module usable with such formation testers is depicted in FIG. 5 . The module 101 includes a probe 112 a , a packer 110 a surrounding the probe, and a flow line 119 a extending from the probe into the module. The flow line 119 a extends from the probe 112 a to probe isolation valve 121 a , and has a pressure gauge 123 a and/or temperature gauge 123 b . A second flow line 103 a extends from the probe isolation valve 121 a to sample line isolation valve 124 a and equalization valve 128 a , and has pressure gauge 120 a and/or temperature gauge 120 b . A reversible pretest piston 118 a in a pretest chamber 114 a also extends from flow line 103 a . Exit line 126 a extends from equalization valve 128 a and out to the wellbore and has a pressure gauge 130 a and/or temperature gauge 130 b . Sample flow line 125 a extends from sample line isolation valve 124 a and through the tool. Fluid sampled in flow line 125 a may be captured, flushed, or used for other purposes.
[0055] Probe isolation valve 121 a isolates fluid in flow line 119 a from fluid in flow line 103 a . Sample line isolation valve 124 a , isolates fluid in flow line 103 a from fluid in sample line 125 a . Equalizing valve 128 a isolates fluid in the wellbore from fluid in the tool. By manipulating the valves to selectively isolate fluid in the flow lines, the pressure gauges 120 a and 123 a may be used to determine various pressures and temperature gauges 120 b and 123 b may be used to determine various temperatures. For example, by closing valve 121 a formation pressure may be read by pressure gauge 123 a when the probe is in fluid communication with the formation while minimizing the tool volume connected to the formation. And for example, by closing valve 121 a formation sample temperature may be read by temperature gauge 123 b when the probe is in fluid communication with the formation while minimizing the tool volume connected to the formation.
[0056] In another example, with equalizing valve 128 a open mud may be withdrawn from the wellbore into the tool by means of pretest piston 118 a . On closing equalizing valve 128 a , probe isolation valve 121 a and sample line isolation valve 124 a fluid may be trapped within the tool between these valves and the pretest piston 118 a . Pressure gauge 130 a may be used to monitor the wellbore fluid pressure continuously throughout the operation of the tool and together with pressure gauges 120 a and/or 123 a may be used to measure directly the pressure drop across the mudcake and to monitor the transmission of wellbore disturbances across the mudcake for later use in correcting the measured sandface pressure for these disturbances.
[0057] Among the functions of pretest piston 118 a is to withdraw fluid from or inject fluid into the formation or to compress or expand fluid trapped between probe isolation valve 121 a , sample line isolation valve 124 a and equalizing valve 128 a . The pretest piston 118 a preferably has the capability of being operated at low rates, for example 0.01 cm 3 ·s −1 , and high rates, for example 10 cm 3 ·s −1 , and has the capability of being able to withdraw large volumes in a single stroke, for example 100 cm 3 . In addition, if it is necessary to extract more than 100 cm 3 from the formation without retracting the probe, the pretest piston 118 a may be recycled. The position of the pretest piston 118 a preferably can be continuously monitored and positively controlled and its position can be “locked” when it is at rest. In some embodiments, the probe 112 a may further include a filter valve (not shown) and a filter piston (not shown).
[0058] Various manipulations of the valves, pretest piston and probe allow operation of the tool according to the described methods. One skilled in the art would appreciate that, while these specifications define a preferred probe module, other specifications may be used without departing from the scope of the invention. While FIG. 5 depicts a probe type module, it will be appreciated that either a probe tool or a packer tool may be used, perhaps with some modifications. The following description assumes a probe tool is used. However, one skilled in the art would appreciate that similar procedures may be used with packer tools.
[0059] The techniques disclosed herein are also usable with other devices incorporating a flowline. The term “flowline” as used herein shall refer to a conduit, cavity or other passage for establishing fluid communication between the formation and the pretest piston and/or for allowing fluid flow there between. Other such devices may include, for example, a device in which the probe and the pretest piston are integral. An example of such a device is disclosed in U.S. Pat. No. 6,230,557 B1 and U.S. Patent Application Ser. No. 2004/0160858, assigned to the assignee of the present invention.
[0060] FIG. 6A is a first example of the use of the index function ( 5 ) according to the present invention, to determine if a build up phase is of the type of non-formation build up or formation build up. The values of the index function ( 5 ) are plotted for build up phases 6 B, 6 C and 6 D of pressure measurements of FIG. 6A . As it can be shown, the build up 6 B is a non-formation build up, the index function being not null; the build up 6 C is a non-formation build up, the index function being also not null; and the build up 6 D is a formation build up, the index function being null.
[0061] FIG. 7A is a second example of the use of the index function ( 5 ) according to the present invention. The values of the index function ( 5 ) are plotted for build up phases 7 B and 7 C of pressure measurements of FIG. 7A . As it can be shown, the build up 7 B is a formation build up, the index function being null and the build up 7 C is also a formation build up, the index function being also null.
[0062] FIG. 8A is a third example of the use of the index function ( 5 ) according to the present invention. The values of the index function ( 5 ) are plotted for build up phases 8 B, 8 C and 8 D of pressure measurements of FIG. 8A . As it can be shown, the build up 8 B is a non-formation build up, the index function being not null; the build up 8 C is a non-formation build up, the index function being also not null; and the build up 8 D is a formation build up, the index function being null.
CROSS REFERENCE TO RELATED APPLICATIONS
[0000]
This application claims priority to European patent application 05290452.1 filed Feb. 28, 2005.
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A method is disclosed for estimating a formation pressure using a formation tester disposed in a wellbore penetrating a formation, said method comprising: (a) establishing fluid communication between a pretest chamber in the downhole tool and the formation via a flowline, the flowline having an initial pressure therein; (b) moving a pretest piston in a controlled manner in the pretest chamber to reduce the initial pressure to a drawdown pressure during a drawdown phase; (c) terminating movement of the piston to permit the drawdown pressure to adjust to a stabilized pressure during a build-up phase and measuring simultaneously in relation to time, pressure P(t) and temperature T(t) in the pretest chamber; (d) extracting an index i(t) dependent of the pressure P(t) and the temperature T(t) informing on the build-up phase; (e) analyzing index i(t) and repeating steps (b)-(d) or going to step (f); (f) determining the formation pressure based on a final stabilized pressure in the flowline. And more generally a method could be used for estimating type of a build up pressure phase, the build up pressure phase being done after a drawdown pressure phase, said both drawdown and build up phases being done to determine formation pressure using a formation tester disposed in a wellbore penetrating a permeable formation, said permeable formation being able to create a formation flow, said method being characterized by using an index to determine the contribution of formation flow on the pressure build up phase.
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BACKGROUND OF THE INVENTION
This invention relates to a liquid crystal color display device, and more particularly to a liquid crystal color display device which includes locally different color display elements in one and the same device.
A liquid crystal color display device designed, for example, for automobile use, includes, for example, a bar-type display part for displaying the speed of an automobile in different colors. The bar is divided into, for example, four zones consisting of a green color zone, a yellow color zone, an orange color zone and a red color zone, and these color zones are progressively illuminated in the order of from the green color zone to the red color zone with an increase in the speed of the automobile.
As a means for exhibiting such locally different hues or exhibiting desired hues at desired portions only of a display pattern in one and the same display element in a liquid crystal color display device, a method is known in which a polarizing plate disposed on an upper side or a lower side of a twisted nematic type liquid crystal panel is locally colored in different colors, as disclosed in, for example, JP-A-No. 57-102611 laid open on June 25, 1982.
However, the method disclosed in the publication is defective in that, when it is desired to form a plurality of color display elements displaying colors other than the neutral color with one and the same polarizing plate means, the polarizing plate means must include polarizing plates dyed with the corresponding number of different dyes, and an increase in the cost is inevitable. In addition, the colored polarizing plate must then be bonded to the liquid crystal panel after the panel is formed. In this step, difficulty is encountered in accurately positioning the colored polarizing plate with respect to patterned display electrodes provided on the panel, and failure of accurate positioning leads to great degradation of the quality of display.
Also, a method as disclosed in, for example, JP-A-No. 57-172386 laid open on Oct. 23, 1982 is also widely known and used. According to the disclosed method, ink containing a pigment or a dye is printed as by screen printing on the surface of one of polarizing plates which is disposed nearer to a light source of a completed liquid crystal display device than the other. Three or four colors are usually printed in the same display device. In the disclosed method, black ink is printed on the area other than that occupied by the colored sections and display elements, in order to prevent misregister in printing and also to ensure a distinct display.
However, according to this method, the number of printing steps increases corresponding to the number of colors to be printed, and, when the black ink is used for the purpose of contouring, an extra printing step is additionally required. Also, since the colors are printed on the outer surface of the polarizing plate, the resistance to light is generally stressed as a matter of impartance, and, from this aspect, pigments instead of dyes are selected as coloring materials. However, the use of pigments lowers the transmittance of the ink and provides a display darker than when dyes are used. Further, there is the possibility of parallax between the ink films and the electrodes due to the spacing therebetween caused by the thickness of the substrate.
SUMMARY OF THE INVENTION
It is a primary object of the present invention to provide a liquid crystal color display device which is capable of displaying multiple colors, which can be produced by a simplified manufacturing process and which is excellent in its durability and quality of display.
According to one aspect of the present invention, two or more kinds of plural filter members are specifically combined with each other to form a filter layer which is disposed in an optical path of incident light in the color liquid crystal display device, and the area ratio of the color filter members constituting the filter layer is locally changed thereby changing the hue of light passing through the filter layer.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1a and 1b are schematic sectional views of major parts of embodiments of the liquid crystal color display device of the present invention, respectively.
FIGS. 2a, 2b and 2c show other embodiments of the present invention.
FIGS. 3a and 3b show the major part of other embodiments of the present invention respectively.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
EMBODIMENT 1
FIG. 1a shows part of a preferred embodiment of the liquid crystal color display device of the present invention. Referring to FIG. 1a showing only one of a pair of opposed transparent substrates 10 of a liquid crystal color display device, for example, a liquid crystal display device of a twisted nematic type in which nematic liquid crystal material is sandwiched between electrodes, and further two parallel polarizing plates are placed one across the liquid crystal from the other, so that activated areas of the liquid crystal material transmit light and unactivated areas do not, patterned electrodes 20 are formed on the transparent substrate 10, and a filter layer 30 is formed on each of the electrodes 20. A structure shown in FIG. 1b is a modification of the structure shown in FIG. 1a in that a single filter layer 30' is formed on the electrodes 20 provided on the transparent substrate 10.
The electrodes 20 of desired pattern are first formed by photolithography on the upper or lower transparent substrate 10 of the liquid crystal color display device constituting a liquid crystal color panel. Then, in order to form the filter layers 30 or filter layer 30' on the patterned electrodes 20 provided on each substrate 10, a dyeable material consisting essentially of, for example, an acrylic resin is coated on the substrate 10 and electrodes 20, and, after pre-curing the dyeable material, ultraviolet radiation is directed through a masking pattern to cure necessary portions of the dyeable material. This filtering material may be coated on only the display electrodes 20 as shown in FIG. 1a or may be coated on substantially the entire surface of the substrate 10 as shown in FIG. 1b, except the portions where opposed electrodes are to be electrically connected with each other on the substrate 10 for the purpose of making external connections to the display device on only one of the substrates and where a sealing agent is to be provided.
FIG. 2a shows a bar graph display for displaying the speed of an automobile. In FIG. 2a, it is supposed, for example, that a speed lower than and including 80 Km/h is displayed by a green color, a speed between 90 Km/h and 120 Km/h is displayed by a yellow color, and a speed between 130 Km/h and 160 Km/h is displayed by a red color. For this purpose, a red color display element 41, a yellow color display element 42 and a green color display element 43 are formed in a single liquid crystal color display device 40. A process for forming a filter layer for each individual electrode will now be described. First, a filter material coated and then cured on a transparent substrate is covered with a positive type photoresist except the area to be dyed in a first color, for example, the red color. FIG. 2b shows one of the transparent substrates 10 of the liquid crystal color display device 40. In FIG. 2b, sections 51, 52 and 53 correspond to the display elements 41, 42 and 43 in FIG. 2a respectively, and the section 52 is divided into stripe-shaped segments 52A and 52B. The section 51 and the stripe-shaped segments 52A of the section 52 are to be dyed in the red color. The positive type photoresist material suitable for this purpose is, for example, AZ-111S made by Farbwerke Hoechst AG. The substrate 10 (including electrodes, filter layers and photoresist coating) is then immersed in a dye solution to be dyed in red. This dye solution was prepared by dissolving a red dye of trade name RED 1P made by Nippon Kayaku Co., Ltd. into pure water (deionized water) so that the dye dissolution had a concentration of 0.1%, and the resulting structure was immersed in the dye solution for a period of time of 5 to 10 minutes at a dyeing temperature of 65° C. ±5° C.
Then, the photoresist coating is removed by a solvent, an alkaline solution or the like. After removal of the photoresist, a photoresist similar to that described above is used to mask the area except that to be dyed in a second color which is, for example, the green color. That is, the photoresist masks the areas except the section 53 in FIG. 2b corresponding to the display element 43 in FIG. 2a and except the stripe-shaped segments 52B in the section 52 in FIG. 2b corresponding to the display element 42 in FIG. 2a. In a manner similar to that described above, the assembly is immersed in a dye solution to be dyed in green. This dye solution was prepared by dissolving a green dye of trade name GReen IP made by Nippon Kayaku Co., Ltd. into pure water (deionized water) so that the dye solution had a concentration of 0.1%, and the resulting structure was immersed in the dye solution for a period of time of 15 minutes at a dyeing temperature of 65° C. ±5° C.
In the manner described above, a red color filter layer (51) for the display element 41, a green color filter layer (53) for the display element 43 and a yellow color filter layer (52) for the display element 42 which yellow color filter layer includes red and green color filtering segments 52A (31) and 52B (32) are formed on the electrodes. The filter layer for the red color display element 41 is entirely colored in red, and the filter layer for the green color display element 43 is colored in green. In the case of the yellow color display element 43, the red color filtering segments 52A (31) and the green color filtering segments 52B (32) are arranged in a stripe pattern as shown in FIG. 3a. However, the red color filtering segments and the green color filtering segments may be arranged in a mosaic pattern as shown in FIG. 3b. The ratio between the area occupied by the red color filtering segments 31 and that occupied by the green color filtering segments 32 is preferably selected to be about 1:1. FIG. 2c shows, in an exploded view, constituent elements of a color liquid crystal display device corresponding to the illustration in FIGS. 2a and 2b. Further, the common electrode may be replaced by a plurality of electrodes in association with the upper segment electrodes. The numbers of the upper and lower electrodes may or may not be the same.
The yellow color display in the embodiments of the present invention utilizes the principle of additive mixture of colors which teaches that, when light from a fine pattern such as a stripe or mosaic pattern which is too fine to be distinguished by the naked eye is incident on the eyes of a man, he senses a color different from the original color of the light. When the embodiment of the liquid crystal color display device of the present invention is used as a meter or the like for automobile use, the width of the stripes is preferably not larger than about 150 μm. This stripe width is preferably as small as possible from the viewpoint of the quality of display. Similarly, when the mosaic pattern is employed for such display devices as for automobile use, the dimension of each segment of the mosaic are preferably not larger than about 200 μm×200 μm. Further, when the number of the red color filtering segments 31 and green color filtering segments 32, that is, the ratio between the total area occupied by the red color filtering segments 31 and that occupied by the green color filtering segments 32 is suitably changed from the value of 1:1, any desired hue between the red color and the green color can be displayed by the display element 42.
Further, in this embodiment of the present invention, the color filter layers 30 and color filtering segments 31, 32 are directly formed on the electrodes. Therefore, the problem of parallax due to the distance between the color filters and the electrodes does not arise, thereby ensuring a display of good quality. However, the color filter layers 30 and the color filtering segments 31, 32 may be formed on the other surface of the transparent substrate on which the electrodes are not provided. This applies also to other embodiments which will be described later.
In this embodiment, two kinds of (e.g., red and green) filter layers and filtering segments are used for attaining a multicolor display. However, it is apparent that three kinds of, or, for example, red, green and blue filter layers and filtering segments may be used.
EMBODIMENT 2
Gelatine type photosensitive films widely used hitherto are dyed in, for example, red and green to provide patterned color filtering films, and such films are laminated on electrodes with a protective film interposed therebetween to provide color filter layers. By such an arrangement, a minimum number of, or only two kinds of color filter layers can provide a display element capable of displaying any desired intermediate hue between one of the colors and the other color, as in the case of EMBODIMENT 1. The color filter layers provided by the laminated films are disposed as in the case of EMBODIMENT 1.
EMBODIMENT 3
A filter layer is formed on substantially the entire surface of a transparent substrate as shown in FIG. 1b, and the portion of the filter layer except the area required for display is rendered opaque by dyeing such a portion with, for example, a black dye, so as to provide a distinct display. Also, such a black color can be generally obtained by consecutive dyeing with dyes of three primary colors.
In the embodiments of the present invention, formation of the filter layers on the electrodes provided on the inner surface of the transparent substrate is effective as described already in that parallax between the filter layers and the electrodes due to the thickness of the substrate does not occur unlike the case where the filter layers are formed on the outer surface of the substrate or on another polarizing plate. However, in order to prevent direct contact between the filter layers and the liquid crystal layer, a material which will not adversely affect the optical properties of the liquid crystal color display device or deteriorate the liquid crystal material even when it makes contact with the liquid crystal, for example, an acrylic or epoxy resin showing a high transmittance, may be coated on the surface of the filter layers to provide a protective coating.
Further, it is possible to reverse the abovementioned order of forming electrodes and thereafter filter layers on the substrates in EMBODIMENTS 1, 2 and 3.
It will be understood from the foregoing description of the present invention that a multi-color display can be attained by formation of a small number of kinds of color filtering segments or color filtering films. Also, by suitably changing the area ratio between the filtering segments of different colors arranged in a stripe pattern or a mosaic pattern, a display element capable of displaying a hue between the colors of the color filtering segments. Therefore, a liquid crystal color display device capable of displaying multiple colors can be provided by a simple manufacturing process. Further, lamination of the color filtering films with protective films interposed therebetween provides the effect similar to that described above.
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A liquid crystal color display device comprising at least two kinds of plural color filter members provided for patterned electrodes serving to apply an electric field across a liquid crystal layer sandwiched therebetween, each of the above-mentioned at least two kinds of color filter members transmitting light having wavelengths representative of a particular color, in which at least one of the color filter members is constituted by a combination of at least two kinds of filter members segmented to a degree unresolvable by the eyes specifically arranged.
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FIELD OF THE INVENTION
This invention pertains to Raman amplifiers and, more particularly, to Raman amplifiers having a bandwidth which exceeds the peak Raman Stokes gain shift of the transmission medium with which the Raman amplifier is utilized.
BACKGROUND OF THE INVENTION
Optical fiber technology is currently utilized in communications systems to transfer information, e.g., voice signals and data signals, over long distances as optical signals. Over such long distances, however, the strength and quality of a transmitted optical signal diminishes. Accordingly, techniques have been developed to regenerate or amplify optical signals as they propagate along an optical fiber.
One well-known amplifying technique exploits an effect called Raman scattering to amplify an incoming information-bearing optical signal (referred to herein as a “signal wavelength”). Raman scattering describes the interaction of light with molecular vibrations of the material through which the light propagates (referred to herein as the “transmission medium”). Incident light scattered by molecules experiences a downshift in frequency from the power-bearing optical signal (referred to herein as the “pump wavelength”). This downshift in frequency (or increase in wavelength) from the pump wavelength is referred to as the “Stokes Shift.” The downshift of the peak gain from the pump wavelength is referred to herein as the “peak Stokes shift.” The extent of the downshift and the shape of the Raman gain curve is determined by the molecular-vibrational frequency modes of the transmission medium. In amorphous materials, such as silica, molecular-vibrational frequencies spread into bands which overlap and provide a broad bandwidth gain curve. For example, in silica fibers, the gain curve extends over a bandwidth of about 300 nm from the pump wavelength and has a peak Stokes shift of about 100 nm.
The overall concept of Raman scattering is well known and is described in numerous patents and publications, for example, R. M. Stolen, E. P. Ippen, and A. R. Tynes, “Raman Oscillation in Glass Optical Waveguides,” Appl. Phys. Lett, 1972 v. 20, 2 PP62-64; and R. M. Stolen, E. P. Ippen, “Raman Gain in Glass Optical Waveguides,” Appl. Phys. Lett, 1973 v. 23, 6 pp. 276-278), both of which are incorporated herein by reference. With respect to the present invention, the most relevant aspect of Raman scattering is its effect on signal wavelengths traveling along the transmission medium.
FIG. 1 illustrates prior art optical amplifier which utilizes Raman scattering to amplify a signal wavelength. Referring to FIG. 1, a pump wavelength ωp and a signal wavelength ωs are co-injected in opposite directions into a Raman-active transmission medium 10 (e.g., fused silicon). Co-propagating pumps may be used, although a counter-propagation pump scheme reduces polarization sensitivity and cross talk between wavelength division multiplexed (WDM) channels. Providing the wavelength of the signal wavelength ωs is within the Raman gain of power wavelength ωp (e.g., about 300 nm in silica), the signal wavelength ωs will experience optical gain generated by, and at the expense of, the pump wavelength ωp. In other words, the pump wavelength ωp amplifies the signal wavelength ωs and, in so doing, it is diminished in strength. This gain process is called stimulated Raman scattering (SRS) and is a well-known technique for amplifying an optical signal. The two wavelengths ωp and ωs are referred to as being “SRS coupled” to each other. A filter 16 transmits all signals of the signal wavelength ωs and blocks signals of the pump wavelength cop thereby filtering out the pump wavelength.
FIG. 1A illustrates the gain curve for a signal wavelength ωs amplified using a single pump wavelength ωp. As shown in FIG. 1A, while gain occurs over a broad bandwidth (e.g. 300 nm in silica), only a portion of it (e.g., about 50 nm) is, from a practical standpoint, useable to effectively amplify the signal wavelength ωs. This useable bandwidth is referred to herein as the“effective Raman gain.” The effective Raman gain is determinable by one skilled in the art and depends on a number of factors including the desired degree of amplification and the desired flatness across the amplification bandwidth. In silica, the effective Raman gain having less than 3 dB gain variation extends about 25 nm on either side of the peak Raman Stokes shift of about 100 nm. Therefore, the bandwidth of the effective Raman gain occurs from about 75 to about 125 nm from the pump wavelength as shown between points A and B on the Raman gain curve in FIG. 1 A.
FIG. 2 is a schematic drawing illustrating the relationship between pump wavelengths and the signal wavelengths of a prior art Raman amplifier. The schematic of FIG. 2 shows multiple pump wavelengths cop through ωp+n which are used to amplify signal wavelengths ωs through ωs+m. Because the effective Raman gain occurs about 75to about 125 nm from the pump signal, signal wavelengths separated from a pump wavelength within this range will be effectively SRS coupled to the pump wavelength. In FIG. 2, pump wavelength ωp (1370 nm) is separated from signal wavelength ωs (1470 nm) by approximately 100 nm. Thus, assuming that the transmission medium 10 of FIG. 1 is silica, pump wavelength ωp will be SRS coupled to and amplify signal wavelength ωs.
If only a single pump wavelength ωp is used, only signals in the bandwidth from ωs−25 nm to ωs+25 nm would be within the effective Raman gain. However, the use of multiple pump wavelengths ωp through ωp+n as shown in FIG. 2 allows the gain bandwidth to be expanded to amplify signal wavelengths ωs through ωs+m. Furthermore, the use of multiple pump wavelengths serves to reduce gain variation (improve flatness) within this bandwidth due to the cumulative effect of multiple gain curves.
Despite multiple pump configurations, prior art Raman amplifiers are nevertheless limited in bandwidth, which in turn limits the capacity of WDM systems. More specifically, because the effective Raman gain tails off at about 125 nm from the pump wavelength, signal wavelengths beyond this point are not effectively amplified. Furthermore, the applicants have found that in multi-pump systems, where excellent flatness in amplification is achievable through the cumulative effect of multiple gain curves, signal wavelengths preferably should be within the peak Stokes shift of a pump wavelength, e.g., about 100 nm, for optimum flatness. This limitation in SRS coupling limits the bandwidth of signals, e.g. ωs from ωs+m as shown in FIG. 2, to the peak Stokes shift of a pump wavelength since extending the signal bandwidth beyond ωs+m would require introducing pump wavelengths into the signal bandwidth, beyond ωs.
Injecting pump wavelengths into the signal bandwidth, however, has traditionally been avoided due to backward Rayleigh scattering (BRS) resulting from the pump signals. BRS results from random localized variations of the molecular positions in glass that create random inhomogeneities of the reflective index that act as tiny scatter centers. Although the pump and signal wavelengths can be easily separated by filtering in a counter-propagating scheme, the BRS from the pump wavelengths, which propagates in the direction of the signals, is not easily filtered. Furthermore, BRS from longer pump wavelengths falls into the Raman gain generated by shorter pump wavelengths, thereby causing this BRS to be amplified such that it equals or exceeds the intensity of the signal wavelengths. For example, a pump wavelength generated at point A and intended to amplify a signal wavelength at point B would coincide with signal wavelength ωs+2. The BRS from the pump wavelength at point A is affected by the Raman gain of the lower pump wavelengths, thus introducing undesired noise into the signal wavelengths near point A (FIG. 2 ). Thus, BRS both decreases the Raman amplification of the adjacent signals by depleting the pump wavelengths' power, and diminishes signal quality by introducing noise and cross-talk between the channels.
BRS also causes a four-wave-mixing effect. Four-wave-mixing is defined by third order susceptibility in the relation between the induced polarization from the electric dipoles and electric field. In a particular case of four-wave-mixing in optical fibers, a strong pump wave at a frequency ω 1 creates two side bands located symmetrically at the frequencies ω 2 and ω 3 . The frequency shift of the side bands is given by Ω s =ω 1 −ω 2 =ω 3 −ω 1 , where ω 2 <ω 3 . The phase matching requirement for this process is k 2 −k 3 −2k 1 =0, where k is the wave number. The two side bands may also introduce undesired noise into the signal wavelengths.
Accordingly, it would be desirable to have a method and apparatus for expanding the gain bandwidth of a Raman amplifier beyond the maximum gain Raman Stokes Shift of the transmission medium without the attendant problems of BRS.
SUMMARY OF THE INVENTION
In accordance with the present invention, the amplification bandwidth of a Raman amplifier is expanded by interleaving narrow pump wavelengths between signal wavelengths, thereby avoiding interaction between the signal wavelengths and the BRS of the interleaved pump wavelengths. The line width of the pump signals are narrow enough (e.g., less than 1 GHz) compared to the wavelength spacing of the signal wavelengths (e.g., as low as 25 GHz) so that the BRS of the interleaved pump wavelengths is readily distinguishable from signal wavelengths and can be efficiently filtered out.
One aspect of the present invention is a method of Raman amplification employing interleaved pump and signal wavelengths. In a preferred embodiment, the method comprises effecting a plurality of pump wavelengths on a Raman-active transmission medium which is transmitting counter-propagating signal wavelengths, wherein one or more of the pump wavelengths are interleaved between the signal wavelengths. Preferably, the plurality of pump wavelengths spans a bandwidth that exceeds the peak Raman Stokes Shift of the transmission medium. In a preferred embodiment, the method further comprises the step of reducing BRS generated from the interleaved pump wavelengths.
Another aspect of the present invention is a Raman amplification system for amplifying signal wavelengths propagating on a transmission medium by interleaving signal and pump wavelengths. In a preferred embodiment, the system comprises: (a) a pump for generating a plurality of pump wavelengths wherein at least one of the pump wavelengths is between two of the signal wavelengths; and (b) a coupler for coupling the pump wavelengths to the transmission medium such that the pump wavelengths and the signal wavelengths are counter-propagating. Preferably, the pump is adapted to generate pump wavelengths over a bandwidth greater than that of the peak Raman Stokes Shift.
Yet another aspect of the present invention is a long-haul cable system employing the amplification system as described above. In a preferred embodiment, the cable system comprises: (a) a transmission path; (b) a signal transmitter coupled to the transmission path and adapted for transmitting signal wavelengths; (c) a signal receiver coupled to the transmission path and adapted for receiving the signal wavelengths; and (d) at least one amplifier system as described above disposed along the transmission path between the signal transmitter and the signal receiver.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a prior art Raman amplifier;
FIG. 1A illustrates the gain curve for a signal wavelength, amplified using a single pump wavelength in accordance with the prior art;
FIG. 2 is a schematic drawing illustrating the relationship between the pump wavelengths and the signal wavelengths of a prior art multiple-pump Raman amplifier;
FIG. 3 is a schematic drawing illustrating the relationship between the pump wavelengths and the signal wavelengths of a Raman amplifier using the method and apparatus of the present invention;
FIG. 3A is a simplified schematic drawing illustrating the relationship between the pump wavelengths and the signal wavelengths of a Raman amplifier using the method and apparatus of the present invention;
FIG. 4 is a block diagram of a Raman amplifier in accordance with the present invention; and
FIG. 5 is a graph showing the gain ripple of the output of a Raman amplifier in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 3 is a schematic drawing illustrating the relationship between the pump wavelengths and signal wavelengths of a Raman amplifier using the method and apparatus of the present invention. Referring to FIG. 3, a band of pump wavelengths ωp 1 through ωp 1 +n are shown. The bandwidth BWP of the pump wavelengths ωp 1 through ωp 1 +n exceeds one maximum gain Raman shift of the transmission medium. Preferably, the bandwidth of the pump wavelengths exceeds about 10% of the peak Stokes Shift, and more preferable, exceeds about 20% of the peak Stokes Shift. In the example of FIG. 3, the bandwidth BWP of the pump wavelengths ωp 1 through ωp 1 +n is 120 nm which exceeds one Raman maximum gain shift of silica by approximately 20 nm.
As can be seen in FIG. 3, the pump wavelengths ωp 1 +10, ωp 1 +11, ωp 1 +n which overlap the signal wavelengths ωs 1 , ωs 1 +1, ωs 1 +2, ωs 1 +3, ωs 1 +4, and ωs 1 +5 are situated between the signal wavelengths. The line width of the pump wavelengths is narrow enough compared to the wavelength spacing of the signal wavelengths that the BRS generated from the pump wavelengths can be identified as such and efficiently filtered out. The minimum wavelength separation between the signal wavelengths, referred to herein as the“stop bandwidth” or the “100% rejection band of the filter,” is related to the repetition rate, modulation format, signal strength, and transmission distance of the signal wavelength. For example, for a 10 Gb/s repetition rate, the separation between signal wavelengths may be no less than 0.2 nm (25 GHz at 1550 nm). A wider channel spacing is typically used in conventional transmission systems. A pump signal is preferably no wider than about {fraction (1/50)} of the channel separation, and, more preferably, no wider than about {fraction (1/100)} of the channel separation. Furthermore, the pump wavelength is positioned between signal wavelengths such that it appears in the middle between the adjacent signals. The accuracy to which a distributed feedback (DFB) laser can be tuned to a particular wavelength can be better than 0.01 nm (approximately 1.3 GHz).
FIG. 3A illustrates, in a simplified manner, the relationship between the pump wavelengths and signal wavelengths of a Raman amplifier using the method and apparatus of the present invention. As can be seen in FIG. 3A, the stop bandwidth is the area between the effective transmission bandwidth of the signal bandwidth, and within the stop bandwidth, a significantly narrower pump linewidth is effected. As described herein, this allows effective filtering of any BRS generated from the pump wavelengths.
FIG. 4 illustrates an exemplary embodiment of a Raman amplifier system in accordance with the present invention. As shown in FIG. 4, pump source 44 injects pump wavelengths onto a fiber span 40 . In a preferred embodiment, pump source 44 comprises a DFB laser, which can provide wavelength stability of better than 0.01 nm. Wavelength stability depends partially on the filter characteristic, that is, the breadth of the 100% rejection band. It is in this area that, in accordance with the present invention, the narrow pump wavelengths are effected. In an ideal step-like (i.e., rectangular shape) filter, this will require a stability of better than ¼ of the filter stop bandwidth with the line width of the pump being less than {fraction (1/10+L )} of the filter stop bandwidth. This bandwidth should be as narrow as possible so as not to decrease the effective channel transmission bandwidth. At the same time, it should be broad enough to allow for a given pump wavelength to be filtered out with maximum efficiency. Assuming the bandwidth and the wavelength stability of a pump equal to 1 GHz, the estimate for the filter stop bandwidth will be 4 GHz. It is desirable in practice to utilize an even smaller bandwidth, especially for a channel separation of less than 0.5 nm. The requirements when amplifying nonmodulated signals are broader because the line width of a CW signal is more than three orders of magnitude narrower than the bandwidth of a modulated RZ format signal at 10 Ghz.
DFB lasers emit wavelengths having line widths of less than 100 MHz and can deliver up to 20-30 mW of average power at the wavelength region of 1550 nm. These power levels are sufficient for amplification of the signal wavelengths when a pump scheme is used employing numerous, closely-packed pump wavelengths (e.g., when pump wavelength separation is less than 4 nm). As the wavelength separation between pumps increases, so must the power per pump wavelength. Pump power will also depend on signal power and the separation of the signals. The higher the required signal power and the smaller the separation between signal channels, the more pump power will be needed.
Filter 45 is tuned to transmit only signal wavelengths and not pump wavelengths. Suitable filters include, for example, Fabry-Perot filters and Mach-Zehnder wavelength multiplexers. Ideally, the transmission characteristics of the filter 45 are such that it permits maximum transmittance at the signal wavelengths and minimum transmittance at the pump wavelengths. Thus, the filter will pass the signal wavelengths and filter any signals occurring between the signal wavelengths, including BRS of the pump signals preferably in the 20 nm or more overlap area.
Isolator 46 provides unidirectional propagation and eliminates any multipath Rayleigh scattering effect and any reflection of the counter-proprogating radiation from the filter.
Pump source 42 and filter 43 are illustrative of a portion of another fiber span.
EXAMPLE
FIG. 5 illustrates the results of a numerical simulation of a Raman amplifier having 120 nm bandwidths. As shown, a gain ripple of less than 0.3 dB is achieved with 38 pump wavelengths (only 10 pump wavelengths are interleaved with signal wavelengths) situated at 4 nm spacing, illustrated by the relatively stable amplitude of the amplified signals at approximately −7 dBm. This numerical simulation is performed for 61 channel signals separated by 2 nm widths, thereby providing −7 dBm (0.2 mW) power per channel. The fiber span is represented as being 50 km long and consisting of standard telecommunication fiber with losses of 0.2 dB/km at 1550 nm. The total span loss at 1550 nm is 10 dB. Pump wavelengths start from 1360 nm (not shown) and end at 1512 nm. Signals start from 1475 nm and end at 1595 nm, covering three telecommunication bands (S, C, and L). The pump power starts at approximately 130 mW per pump and drops to below 10 mW above 1430 nm. Total pump power in the simulation is 1185 mW. This means that for the majority of pump wavelengths there will be no limitation on line width and precise positioning. These limitations will only apply for the wavelength region where the pump and signal bandwidths intersect (10 pumps for the simulation under discussion). In practice the number of pump wavelengths which coincide with signal bandwidths can be reduced. Utilization of fibers with smaller cross sections will reduce the required pump power.
While there has been described herein the principles of the invention, it is to be understood by those skilled in the art that this description is made only by way of example and not as a limitation to the scope of the invention. Accordingly, it is intended by the appended claims, to cover all modifications of the invention which fall within the true spirit and scope of the invention.
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A method of Raman amplification comprising the step of effecting a plurality of pump wavelengths on a Raman-active transmission medium transmitting counter-propagating signal wavelengths, wherein at least one of said pump wavelengths are interleaved between said signal wavelengths.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to a process for the catalytic aldol condensation of aldehydes, in particular for preparing α,β-unsaturated aldehydes, in a multiphase reactor.
PRIOR ART
[0002] Unsaturated aldehydes are starting materials for the preparation of many organic compounds and are used in many applications. They can, inter alia, be hydrogenated to produce saturated alcohols which in turn serve as starting materials for the production of plasticizers, detergents or solvents. In addition, the unsaturated aldehydes can be converted by selective hydrogenation into the saturated aldehydes and by subsequent oxidation into carboxylic acids.
[0003] Unsaturated aldehydes are prepared industrially by aldol condensation of saturated aldehydes with elimination of water. Important aldol condensations are the reaction of n-butyraldehyde with elimination of water to form 2-ethylhexenal or the reaction of n-valeraldehyde with elimination of water to form 2-propylheptenal. The starting materials can comprise not only the linear aldehydes but also branched aldehydes which can undergo an aldol condensation with themselves, with other branched aldehydes or with linear aldehydes, Likewise, aldehydes having different numbers of carbon atoms can be condensed with one another in an aldol reaction. The two hydrogenation products of the aldehydes 2-ethylhexenal and 2-propylheptenal (or isomer mixtures thereof) obtained by aldol condensation are 2-ethylhexanol and 2-propylheptanol (or isomer mixtures thereof) and are used on a large scale, inter alia as plasticizer alcohols.
[0004] As catalyst for the aldol condensation, use is generally made of a base, often NaOH, dissolved in water, with the aqueous base forming a second liquid phase in addition to the organic starting material/product mixture. The water of reaction liberated during the reaction becomes concentrated in the heavier, aqueous phase. The organic starting materials and products form the lighter, organic phase. The reaction temperature of the aldol condensation is typically in the range from 80 to 180° C. The reaction is generally carried out under a superatmospheric pressure which, in the presence of a gas phase, corresponds to the sum of the vapor pressures of aqueous and organic phases and is typically below 10 bar. Heat is liberated during the reaction and has to be removed from the process. The aldol condensation typically proceeds with high selectivity (>95%) to the desired products. An important secondary reaction is the formation of high-boiling by-products. A further possible secondary reaction is the Cannizzaro reaction which also leads to consumption of the catalyst.
[0005] Since the catalyst used in the aldol condensation is present essentially in the aqueous phase, the reaction likewise takes place mainly in the aqueous phase. To achieve a sufficiently rapid reaction, the starting materials therefore have to be similarly readily soluble in the aqueous phase. This is no longer the case for aldehydes having more than 6 carbon atoms, so that economical operation without solvent and/or solubilizer is often no longer possible here.
[0006] The reaction volume available for the aldol condensation is set by the volume of the aqueous phase. It is therefore desirable to operate the reactor with the highest possible proportion of aqueous phase. In the case of a continuous reaction, the aqueous phase leaving the reactor is usually, after phase separation, recirculated to the reactor for this reason. Such a mode of operation is described, for example, in EP 1106596 A2. Owing to the dilution of the aqueous phase by the water of reaction formed, part of the aqueous phase has to be continually discharged from the process and catalyst has to be replaced.
[0007] To ensure sufficiently good mass transfer between the two liquid phases, an appropriately large phase interface should also be made available in the reactor. This is typically achieved by introducing mixing energy by means of a dispersing apparatus. However, this mixing energy should not be too great since otherwise a stable emulsion of the two phases can be formed; this emulsion then cannot be separated completely by simple methods, e.g. in a simple gravity separator, after the reaction mixture leaves the reactor.
[0008] Various types of reactor have been used in the past for carrying out the aldol condensation of aldehydes. The aldol condensation can, for example, be carried out in a stirred reactor in which the two liquid phases are dispersed. Such processes are described, for example, in DE 927626 and WO 1993/20034. A disadvantage of this process is the use of mechanically susceptible rotating parts. Furthermore, removal of the heat of reaction via structurally complicated internal heat exchanger tubes is necessary.
[0009] U.S. Pat. No. 5,434,313 describes the use of three mixing circuits in series for the aldol condensation of n-butyraldehyde. The mixing energy is provided by the three pumps of the mixing circuit. To increase the residence time, a vessel is integrated into each of the second and third circuits. Disadvantages of this reaction system are the large outlay for installation of the tubes and the large number of circulation pumps required.
[0010] Furthermore, U.S. Pat. No. 5,434,313 describes carrying out the aldol condensation in a tube reactor. To achieve better dispersion of the two liquid phases, static mixing elements or packing are/is provided. The removal of heat is said to occur via the tube wall. Disadvantages of this concept are the large tube length required and the complicated way in which heat is removed.
[0011] EP 1106596 A2 likewise proposes the use of a tube reactor which is equipped with mixing elements. The discharge from the tube reactor is fed to a phase separator for separation of the two liquid phases. Part of the aqueous phase is recirculated together with the catalyst dissolved therein to the reactor, and the remainder is discharged from the process. As a result of this mode of operation, an excess of aqueous phase is established in the reactor, and the organic phase is present as a dispersion in the aqueous phase. The heat of reaction is removed from the recirculated aqueous phase by means of an external heat exchanger. To achieve sufficient dispersion of the organic phase, a high flow velocity in the tube reactor used is necessary; this leads to a relatively high pressure drop. An advantage of this reactor concept is the backmixing-free reaction of the organic starting materials. However, this is associated with a number of disadvantages such as the large tube length required and the associated large number of mixing elements. In addition, a high energy input is necessary for dispersing the organic phase and this requires the use of larger pumps and thus a higher power consumption. The typical pressure drop for the packing elements indicated, e.g. SMV2 from Sulzer and VFF, is 150 mbar/m. A typical power input of from 50 to 80 kW/m 3 of liquid volume can be calculated therefrom for the process described in EP 1106596 A2.
[0012] It is an object of the invention to provide an improved process for the catalytic aldol condensation in a two-phase liquid reaction mixture. This should be suitable for the aldol condensation of aldehydes with high selectivity to form the unsaturated aldol condensation product (unsaturated aldehyde). In particular, it is an object of the invention to provide a process for the catalytic aldol condensation
which has a compact reactor construction, in which a large proportion of aqueous phase can be set in the reactor in a simple way without aqueous phase having to be recirculated to the reactor from an external separator, in which the removal of heat is carried out in a simple manner, and in which satisfactory dispersion of the organic phase can be achieved with a very low energy input.
[0017] It has surprisingly been found that the stated object can be achieved effectively when both the reaction and the coalescence of the two liquid phases are combined in one apparatus. For this purpose, the settling out of the heavier aqueous phase is made possible by means of an unmixed disengagement zone through which flow occurs slowly in an upward direction in the upper part of the apparatus. As a result, this aqueous phase becomes concentrated in the mixed reaction zone underneath.
SUMMARY OF THE INVENTION
[0018] The invention provides a process for the catalytic aldol condensation of at least one aldehyde in a two-phase liquid reaction mixture in a reactor which has a reaction zone and a disengagement zone located directly above the reaction zone, wherein an aldehyde-comprising phase dispersed in a continuous aqueous catalyst-comprising phase is produced and a stream of the two-phase reaction mixture is allowed to rise from the reaction zone into the disengagement zone and coalesce, with a continuous organic phase being formed in the upper region of the disengagement zone.
[0019] The invention further provides for the use of an apparatus comprising a reactor which has reaction zone and a disengagement zone located directly above the reaction zone, wherein the reaction zone has a device for producing an organic phase dispersed in a continuous aqueous phase and the disengagement zone allows the coalescence of the two-phase reaction mixture and the formation of a continuous organic phase in the upper region of the disengagement zone, for reaction of a two-phase liquid reaction mixture.
DESCRIPTION OF THE INVENTION
[0020] For the purposes of the invention, the term “aqueous phase” refers to the phase which comprises water as main component. If the organic compounds comprised in the reaction mixture have some miscibility with water, the aqueous phase can accordingly comprise proportions of dissolved organic compounds. Correspondingly, the term “organic phase” refers, for the purposes of the invention, to the phase which comprises organic compounds, e.g. the aldehydes used for the aldol condensation and the products of the aldol condensation, as main component.
[0021] The process of the invention makes it possible for reaction zone and disengagement zone to be located in a single reaction vessel.
[0022] The process of the invention is preferably carried out continuously.
[0023] The aqueous catalyst-comprising phase comprises largely water. If desired, the aqueous phase can additionally comprise at least one organic, water-miscible solvent. Organic solvents which can be used are, for example, propanediol, glycerol, diethylene glycol and dimethylformamide.
[0024] The proportion of water and organic solvent in the aqueous phase is preferably at least 60% by weight, particularly preferably at least 80% by weight, based on the total weight of the aqueous phase.
[0025] In a preferred embodiment, the aqueous phase does not comprise any added organic solvents. For the purposes of the invention, the amount of aldehyde starting material, products of the aldol condensation and reaction-typical impurities dissolved in the aqueous phase do not count as added organic solvents. The proportion of water in the aqueous phase is then preferably at least 60% by weight, particularly preferably at least 80% by weight, based on the total weight of the aqueous phase.
[0026] The aqueous phase can optionally comprise phase transfer agents, surface-active or amphiphilic reagents or surfactants.
[0027] Preferred catalysts for the process of the invention are water-soluble, basic compounds such as hydroxides, hydrogencarbonates, carbonates, carboxylates or mixtures thereof in the form of their alkali metal or alkaline earth metal compounds. Preference is given to using alkali metal hydroxides, such as sodium hydroxide.
[0028] The concentration of the catalyst in the continuous aqueous phase in the reaction zone is preferably in the range from 0.1 to 15% by weight, particularly preferably from 0.2 to 5% by weight, in particular from 1 to 3% by weight.
[0029] The process of the invention is suitable for the reaction of aldehydes or aldehyde mixtures which can undergo a condensation reaction. If only one aldehyde is used, this has to have two α-hydrogen atoms on the same carbon atom next to the CO group. If two or more different aldehydes are used, at least one of the aldehydes has to have two α-hydrogen atoms on the same carbon atom.
[0030] Suitable aldehydes for the process of the invention are aldehydes having from 1 to 15, preferably from 3 to 15, particularly preferably from 4 to 6, carbon atoms.
[0031] Suitable aldehydes having two α-hydrogen atoms are, for example, acetaldehyde, propanal, n-butyraldehyde, n-valeraldehyde, 3-methylbutyraldehyde, n-hexanal, 3-methylpentanal, 4-methylpentanal, n-heptanal, n-octanal, n-nonanal and n-decanal. These aldehydes are also suitable for a homocondensation.
[0032] Suitable aldehydes having one α-hydrogen atom are, for example, isobutyraldehyde, 2-methylbutyraldehyde, 2-methylpentanal, 2-ethylhexanal, cyclohexylaldehyde.
[0033] Preferred starting materials for the process of the invention are: n-butyraldehyde, n-valeraldehyde, mixtures of n-butyraldehyde and isobutyraldehyde, mixtures of n-valeraldehyde with 2-methylbutyraldehyde and/or 3-methylbutyraldehyde. It is likewise possible to use a mixture of C 4 - and C 5 -aldehydes. These aldehydes can be prepared, for example, by hydroformylation of olefins.
[0034] When more than one aldehyde or an aldehyde mixture are/is used, the individual components can be fed separately into the stream of the catalyst solution. It is likewise possible to mix all starting materials before they are fed in and to feed them in together. Furthermore, the aldehydes can be used as a solution. Solvents which can be used are inert liquids which are sparingly soluble in the catalyst solution, for example hydrocarbons such as pentane, hexane, ligroin, cyclohexane or toluene.
Reaction Zone
[0035] According to the invention, the aqueous phase forms the continuous phase of the two-phase reaction mixture in the reaction zone. The proportion by volume of the aqueous phase in the reaction zone is preferably at least 70%, particularly preferably at least 80%, based on the total volume of the two-phase reaction mixture in the reaction zone.
[0036] In the process of the invention, the proportion of aqueous phase in the reaction zone is thus generally substantially greater than in a mixed reactor of the prior art without disengagement zone at the same reaction conversion. In the latter, an organic continuous phase would be established in the reaction zone without an externally introduced aqueous stream; such an organic continuous phase would have adverse consequences for the conversion and selectivity of the reaction.
[0037] The proportion by volume of the aqueous phase in the reaction zone can be set by, inter alia, appropriate design of the disengagement zone (e.g. the volume, type and extent of any internals and/or packing) so that the aqueous phase represents the continuous phase in the reaction zone.
[0038] The reaction zone is preferably backmixed. In particular, use is made of a reaction zone which is fluid-dynamically backmixed in respect of the aqueous phase and in respect of the organic phase (i.e. virtually equal concentrations of the aqueous phase and the organic phase are present at all points in the reaction zone). Mixing serves for macroscopic mixing of the reaction zone and for dispersing the organic phase as small droplets in the continuous aqueous phase. It has been found that backmixing in the reaction zone has a positive effect on the selectivity of the process. As a result of backmixing, the steady-state concentration of starting material is low and high-boiling condensation products are therefore formed to a lesser extent. Likewise, the removal of the heat of reaction from a circulated backmixed system is simpler since, for example, it is possible to employ an external heat exchanger.
[0039] In a specific embodiment of the process of the invention, at least one stream fed into the reaction zone and/or at least one stream from the reaction zone conveyed in an external circuit (circulation stream) is/are used for backmixing.
[0040] Suitable mixing devices are, for example, dynamic mixers (i.e. mixers whose mixing elements comprise movable parts) and static mixers (i.e. mixers without moving parts in the interior, which, in particular, operate according to the in-line principle). Preference is given to using at least one mixing device selected from among mixing nozzles, stirrers, mixing pumps, static mixing elements, beds of random packing elements, etc. Suitable types of stirrer comprise, for example, propeller stirrers, impeller stirrers, disk stirrers, blade stirrers, anchor stirrers, inclined blade stirrers, crossed-beam stirrers, helical stirrers, stirring screws, etc.
[0041] Preference is given to using at least one mixing nozzle for producing the aldehyde-comprising phase dispersed in the continuous aqueous catalyst-comprising phase in the reaction zone. Here, only a low power input is preferably effected by means of the mixing power of the nozzle. The total mixing power introduced into the reactor is preferably not more 0.5 kW per m 3 of liquid volume, particularly preferably not more than 0.3 kW per m 3 of liquid volume. This is a substantial difference from the process described in EP 1 106 596, in which, as indicated above, the mixing power is from 50 to 80 kW/m 3 and thus two orders of magnitude greater.
[0042] The reaction zone is preferably configured as a loop reactor or as a stirred vessel. Suitable loop reactors are, for example, free jet reactors, jet loop reactors, jet nozzle reactors, etc.
[0043] In a preferred embodiment, the reaction zone is configured as a free jet reactor. Free jet reactors and their design are described, for example, in K. H. Tebel, H.-O. May, Chem.-Ing.-Tech. 60 (1988), No. 11, pp. 912-913, and the references cited therein, which are hereby incorporated by reference.
[0044] The aldehyde is preferably introduced into the reaction zone in the region of the high local mixing energy of the mixing device, for example in the vicinity of the stirrer blades of a stirrer or at the nozzle tip of a mixing nozzle. This ensures good dispersing and mixing-in of the aldehyde in the aqueous reaction zone.
[0045] The introduction and mixing-in of the aldehyde occurs particularly advantageously when it is introduced via a two-fluid nozzle. A diagram of a suitable two-fluid nozzle may be found in Ullmann's Encyclopedia of Industrial Chemistry, 5th Edition, Volume B 4, page 280, FIG. 6 , A and is referred there as “two-phase jet nozzle”. The associated article describes two-phase streams composed of a gas phase and a liquid phase. However, the nozzle depicted can be used for liquid/liquid two-phase streams in the process of the invention. The aqueous phase is then preferably introduced where “liquid” is indicated in the drawing and the organic phase is fed into the annular space where “gas” is indicated in the drawing.
[0046] As an alternative, it is possible to feed the aldehyde into a stream from the reaction zone conveyed in an external circuit (circulation stream).
[0047] In addition to the aldehyde, catalyst also has to be fed into the reaction zone. The introduction of the catalyst is preferably effected into a stream from the reaction zone conveyed in an external circuit (circulation stream). The introduction of the catalyst is then preferably carried out on the suction side (upstream) of the transport device comprised in the circulation stream. If the catalyst is added on the suction side of, for example, a circulation pump, good mixing advantageously takes place in the pump. The catalyst is generally introduced in the form of a concentrated aqueous solution.
[0048] In a preferred embodiment of the process of the invention, the reaction zone is configured as a free jet reactor. Here, part of the reaction mixture is taken off from the reaction zone and returned via a nozzle in the upper region of the reaction zone. Preference is given to taking off part of the reaction mixture in the lower region of the reaction zone and especially at the bottom end. This produces circular flow in the reaction zone. A two-fluid mixing nozzle is preferably used as nozzle. The introduction of the circulation stream and the introduction of the aldehyde into the reaction zone are preferably effected via the two-fluid mixing nozzle. The nozzle is preferably directed axially downward in the reaction zone. In a preferred embodiment, an impingement plate is present at the lower end of the reaction zone.
[0049] The heat of reaction evolved in the aldol condensation can, in a useful embodiment, be removed directly in the reaction zone by means of integrated heat exchangers. In a preferred embodiment, an external heat exchanger integrated into a circuit is used for removal of heat.
[0050] The removal of heat is in this case effected inexpensively via an external heat exchanger which is integrated into the circuit leading to and from the reactor. The circulated stream preferably at the same time provides the driving jet of the nozzle and thus ensures mixing of the apparatus. The circulation pump of the external circuit draws in predominantly aqueous phase from the lower region of the reaction zone, as a result of which the risk of formation of a stable emulsion which can no longer be coagulated by simple settling is minimized.
Disengagement Zone
[0051] In the disengagement zone, a phase inversion takes place, i.e. the emulsion composed of a continuous aqueous phase and a disperse organic phase in the reaction zone is inverted to form an emulsion composed of a continuous organic phase and a disperse aqueous phase in the disengagement zone.
[0052] The cross-sectional area of the disengagement zone has to be sufficiently large for a phase separation to be able to take place and the aqueous phase to be able to settle in countercurrent. The diameter of the part of the apparatus in which the disengagement zone is located can therefore differ from the diameter of the part of the apparatus in which the reaction zone is located.
[0053] The upward-directed superficial velocity of the two liquid phases in the disengagement zone should preferably be less than 10 mm/s. It should particularly preferably be less than 5 mm/s. The velocity reported is calculated on the basis of the empty tube even when using internals and/or packing.
[0054] In a preferred embodiment, the disengagement zone comprises internals and/or packing. Packing can be used in the form of (ordered) packing or as a bed of random packing elements. This enables better coalescence of the two phases to be achieved in the disengagement zone.
[0055] Examples of internals are filter plates, baffles, column trays, perforated plates or other devices also used as mixing devices. Further suitable internals are a plurality of narrow, parallel tubes to form a multitube reactor. Particular preference is given to structured mixer packings or demister packings. Suitable packing elements are, for example, Raschig rings, saddles, Pall rings, Tellerettes, wire mesh rings or woven wire meshes. Steel has been found to be an advantageous material for packings and packing elements since it promotes coalescence particularly well because of its surface properties.
[0056] A discharge is preferably taken from the continuous organic phase in the upper region of the disengagement zone.
[0057] The discharge from the disengagement zone can, in a useful embodiment, be subjected to a work-up in order to isolate a fraction enriched in the aldol condensation product.
[0058] The discharge from the disengagement zone is preferably subject to a reaction in at least one further reactor. This enables the conversion into aldol condensation product(s) to be increased further. In particular, the further reaction is carried out in only one further reactor.
[0059] The further reaction is preferably carried out using at least one reactor having plug flow characteristics, i.e. a reactor which has very little backmixing in the flow direction. In a preferred variant, this reactor is tubular. To avoid backmixing and provide a relatively large surface area for the reaction, the reactor preferably comprises internals, i.e. ordered packing, e.g. sheet metal or woven packing, and/or a disordered bed of packing elements. Packings and packing elements are preferably composed of steel. The reactor having plug flow characteristics can be configured as a separate apparatus. In a specific embodiment, the reactor having plug flow characteristics is arranged directly above the first reactor which is operated in a backmixed manner.
[0060] The reactor used for the further reaction is preferably operated adiabatically. In a preferred embodiment, the reactor used for the further reaction comprises ordered packing, e.g. sheet metal or mesh packings, and/or a disordered bed of packing elements. Packings and packing elements are preferably composed of steel.
[0061] For the purposes of the present invention, the term “adiabatic” is used in the engineering sense rather than in the physicochemical sense. Adiabatic reaction conditions refer to a mode of operation in which the heat liberated in the reaction is taken up by the reaction mixture in the reactor and no cooling by means of cooling devices is employed. The heat of reaction is therefore discharged with the reaction mixture from the reactor, apart from a residual proportion which is given off from the reactor to the surroundings by natural heat conduction and thermal radiation.
[0062] A high final conversion in the reaction discharge can be achieved by means of the process of the invention. The reaction discharge is the discharge from the disengagement zone or, if present, the last reactor in the flow direction used for the aldol condensation. The conversion obtained by the process of the invention is preferably at least 95% by weight, preferably at least 97% by weight, based on the total weight of the linear aldehyde used for aldol condensation.
[0063] After the product mixture has been discharged from the disengagement zone or the after-reactor, it can be subjected to cooling, e.g. in a downstream heat exchanger.
[0064] The liquid reaction discharge is preferably separated into catalyst phase and product phase in a liquid-liquid separation vessel. This can be carried out in settling vessels of various construction types or centrifuges.
[0065] The water of reaction formed in the aldol condensation dilutes the catalyst solution and therefore has to be continually removed from the process. In the process of the invention, the removal of water preferably occurs exclusively with the liquid discharge from the disengagement zone or, if present, the (last in the flow direction) after-reactor. The aqueous catalyst phase obtained after liquid-liquid separation can be discharged as wastewater from the process. In an alternative embodiment, the aqueous catalyst phase which has been separated off can, optionally after discharge of a small proportion and corresponding replacement by fresh catalyst solution, also be recirculated to the aldol condensation.
[0066] The product obtained after the catalyst phase has been separated off can be purified by known methods, e.g. by distillation.
[0067] The aldol condensation products prepared by the process of the invention can advantageously be used for preparing saturated alcohols by hydrogenation. The saturated alcohols obtained in this way are employed, for example, for preparing plasticizers, detergents or solvents. The unsaturated C 8 - and C 10 -aldehydes are especially useful as precursors for plasticizer alcohols. Furthermore, the aldol condensation products can be converted by selective hydrogenation into the saturated aldehydes and these can be converted by subsequent oxidation into carboxylic acids, i.e. be used for the preparation of carboxylic acids. In addition, unsaturated aldehydes are used in many syntheses because of their reactivity. A further field of use of saturated and unsaturated aldehydes is use as fragrance.
DESCRIPTION OF FIGURES
[0068] The invention is illustrated below with the aid of FIGS. 1 and 2 .
LIST OF REFERENCE NUMERALS
[0000]
( 1 ) feed line for aldehyde
( 2 ) two-fluid nozzle
( 3 ) backmixed reaction zone
( 4 ) circulation stream
( 5 ) circulation pump
( 6 ) external heat exchanger
( 7 ) feed line for catalyst solution
( 8 ) impingement plate
( 9 ) disengagement zone
( 10 ) reactor discharge
( 11 ) after-reactor
[0080] One possible embodiment of the invention is shown for the purposes of illustration in FIG. 1 . The aldehyde feed ( 1 ) goes via a two-fluid nozzle ( 2 ) into the backmixed reaction zone ( 3 ) of the reactor. Mixing of the reaction zone and dispersion of the organic phase are effected by the introduced momentum of the driving jet of the nozzle. The circulation stream ( 4 ) which has been taken off in the lower region of the reactor and has previously been compressed by means of a circulation pump ( 5 ) and conveyed through an external heat exchanger ( 6 ) to remove the heat of reaction serves as driving jet. The concentrated catalyst solution ( 7 ) is introduced into the circulation stream. An impingement plate ( 8 ) can be provided at the bottom of the reactor in order to aid precipitation of organic droplets. The reaction zone is predominantly filled with aqueous phase in which the dissolved catalyst is present. Organic droplets comprising the reaction starting materials and reaction products are dispersed therein. Coalescence of the organic droplets and settling of the aqueous phase occur in the disengagement zone ( 9 ). This can be filled with ordered packing or with random packing elements which promote coalescence. In addition, residual conversion takes place here, i.e. the disengagement zone also serves as after-reactor. In particular, branched aldehyde isomers which react more slowly are reacted here. Within the disengagement zone or at the outlet of the reactor, phase inversion takes place, i.e. a continuous organic phase in which aqueous droplets are dispersed is formed. The reactor output ( 10 ) is taken off at the top of the reactor. It comprises predominantly organic phase. The aqueous phase comprises the dissolved catalyst and also water of reaction and water which was introduced via the catalyst stream.
[0081] A further possible embodiment of the invention is shown in FIG. 2 . There, an after-reactor ( 11 ) is installed downstream of the product outlet from the disengagement zone in order to achieve a higher conversion. The after-reactor can like the disengagement zone (( 9 ) in FIG. 1 ) of the main reactor be provided with ordered packing or random packing elements in order to minimize axial backmixing, which leads to a higher reaction conversion and promotes coalescence of the two phases.
Example 1
[0082] An apparatus analogous to FIG. 2 was used. The first reactor had a height of 5.6 m and a diameter of 0.8 m in the lower part. This lower part was superposed by a second part having a height of 2.0 m and a diameter of 1.1 m. The lower part was mixed by means of a nozzle. In the upper part, 1 m 3 of packing elements (Pall rings composed of V2A steel (1.4541) and having a diameter of 35 mm) were installed. The second reactor had a height of 16.3 m and a diameter of 0.5 m and was filled with 3.0 m 3 of packing elements (Pall rings composed of V2A steel (1.4541) and having a diameter of 35 mm). The plant was supplied continuously with 8.4 t/h of an aldehyde mixture (88.8% of n-valeraldehyde; 9.8% of 2-methylbutanal; 0.2% of 3-methylbutanal, balance dissolved butanes and butenes). 20 t/h were conveyed through the pumped circuit. The two-fluid nozzle had an internal diameter of 26.7 mm and produced a pressure drop of 0.45 bar. The specific power input is 0.09 kW/m 3 . A superficial velocity of 3.2 mm/s is obtained in the packing in the first reactor. The sodium hydroxide concentration in the aqueous phase was maintained at 2.5% by weight by addition of 20% sodium hydroxide solution. A pressure of Pe=6 bar and a temperature of 145° C. were set in the two reactors.
[0083] The composition of the discharge was determined by GC analyses.
[0000]
Component
GC-% by area
n-Valeraldehyde
1.4
2-Methybutanal
4.9
3-Methylbutanal
0.01
2-Propylheptenal
81.2
4-Methyl-2-propylhexenal
9.7
5-Methyl-2-propylhexenal
0.4
High boilers
1.5
[0084] The conversions of the individual components were determined:
[0000]
Component
Conversion
n-Valeraldehyde
98.6%
2-Methybutanal
55%
3-Methylbutanal
95%
Example 2
[0085] An apparatus analogous to FIG. 1 was used. The reactor had a diameter of 1.5 m and a height of 14 m. The lower part was mixed by means of a nozzle. In the upper part, 8 m of structured packing composed of stainless steel (304 L) was installed. The plant was supplied continuously with 25 t/h of an aldehyde mixture (99.85% of n-butyraldehyde; 0.07% of isobutyraldehyde, balance is dissolved propane and propene). 135 t/h were conveyed through the pumped circuit. The two-fluid nozzle had an internal diameter of 50 mm and produced a pressure drop of 2.2 bar. The specific power input is 0.75 kW/m 3 . A superficial velocity of 6 mm/s is obtained in the packing in the reactor. The sodium hydroxide concentration in the aqueous phase was maintained at 4.0% by weight by addition of 25% sodium hydroxide solution. A pressure of Pe=2.75 bar and a temperature of 90° C. were set in the reactor.
[0086] The composition of the discharge was determined by GC analyses.
[0000]
Component
GC-% by area
n-Butyraldehyde
0.4
Isobutyraldehyde
0.01
2-Ethylhexenal
96.9
4-Methyl-2-ethylpentenal
0.15
High boilers
2.2
[0087] The conversions of the individual components were determined and found to be as follows:
[0000]
Component
Conversion
n-Butyraldehyde
96.4%
Isobutyraldehyde
86%
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The present invention relates to a process for the catalytic aldol condensation of aldehydes, in particular for preparing α,β-unsaturated aldehydes, in a multiphase reactor.
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GOVERNMENT CONTRACT
The government has rights in this invention pursuant to Contract No. N00140-79-C-6282 awarded by the Department of the Navy.
This is a division of application Ser. No. 249,805, filed Apr. 1, 1981, now U.S. Pat. No. 4,428,808.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to thin films used for fabricating bulk wave and surface acoustic wave transducers and more particularly to thin films of polycrystalline material or crystallites each having a crystalline orientation oriented in a preferred direction.
2. Description of the Prior Art
Bulk and surface acoustic wave transducers are fabricated with thin layers of piezoelectric material such as zinc oxide (ZnO). The transducers are used, for example, to fabricate delay lines when the delay medium is non-piezoelectric. For high frequencies greater than 100 MHz the piezoelectric material such as zinc oxide is usually sputtered onto the substrate or medium for propagation. In most bulk wave devices and in some surface acoustic wave devices the substrate or propagation medium is first coated with a thin metal layer such as gold which serves as one electrode of the piezoelectric transducer. The piezoelectric material is sputtered onto the gold and then a second metal film such as gold is deposited on top of the piezoelectric material to form the second electrode.
In order for the sputtered piezoelectric material such as zinc oxide to be useful as a piezoelectric transducer, the piezoelectric material or zinc oxide layer must have a high degree of crystalline C-axis orientation normal to the plane of the layer. The sputtered piezoelectric material may comprise many crystallites, but each crystallite should have its C-axis oriented normal to the plane of the layer. The other axes of the piezoelectric material, such as in the basal plane of a hexagonal crystalline material such as zinc oxide, does not have to be aligned with respect to other crystallites for good transduction to take place, so long as the C-axis of the hexagonal crystalline material is aligned normal to the layer of the piezoelectric material.
It is known that zinc oxide will have good crystalline C-axis orientation if it is sputtered onto thermally evaporated gold which itself has good <111> axis orientation normal to the metal layer. In other words, in the prior art, good piezoelectric transducers could be obtained by using a bottom electrode of gold having its <111> axis oriented normal to the gold layer followed by a zinc oxide layer having its crystalline C-axis of the various crystallites oriented normal to the plane of the layer or close thereto, as measured by reflection electron diffraction patterns. A top layer of gold forms the top of electrode of the transducer.
It is known that thermally evaporated gold will have its <111> axis oriented normal to the gold layer on the following materials: spinel, sapphire, lithium niobate, fused quartz and ordinary microscope slides.
The deposition of piezoelectric films having their C-axis perpendicular to the film is described in U.S. Pat. No. 3,655,429 which issued on Apr. 11, 1972 to John DeKlerk and assigned to the assignee herein. In U.S. Pat. No. 3,655,429 at column 12 the formation of zinc oxide films were found to have a high degree of orientation on an oriented substrate such as crystalline material. The degree of orientation was also affected by the rate of deposition and the temperature of the substrate during deposition.
U.S. Pat. No. 3,825,779 which issued on July 23, 1974 entitled "Interdigital Mosaic Thin Film Shear Transducer" by John DeKlerk describes depositing cadmium sulfide or zinc oxide on a layer of gold on a substrate of aluminum oxide (Al 2 O 3 ). A mosaic thin film shear transducer was described having the C-axis inclined at an angle of 40 degrees to the normal to the piezoelectric film layer.
U.S. Pat. No. 3,689,784 which issued on Sept. 5, 1972 entitled "Broadband, High Frequency, Thin Film Piezoelectric Transducers" by John DeKlerk and assigned to the assignee herein describes a transducer comprising a single layer of piezoelectric material such as cadmium sulfide and electrode structures of gold formed on a substrate of lithium niobate.
U.S. Pat. No. 3,632,439 which issued on Jan. 4, 1972 entitled "Method Of Forming Thin Insulating Films Particularly For Piezoelectric Transducer" by John DeKlerk and assigned to the assignee herein describes the formation of cadmium sulfide films on single crystal substrates with oriented A and C axes. The desirability of having the C-axis normal to the plane of the film is described as desirable to form high frequency piezoelectric transducer films.
U.S. Pat. No. 3,543,058 which issued on Nov. 24, 1970 entitled "Piezoelectric Transducer" by P. G. Klemens and assigned to the assignee herein describes the formation of a acoustic transducer having alternate layers of piezoelectric material wherein at least one layer has different electromechanical properties.
It is therefore desirable to form layers of gold having a predetermined orientation among its crystallites on substrate materials where heretofore only unoriented gold layers were formed.
It is further desirable to form an electrode of gold having its <111> axis oriented normal to its layer on films of thermally formed silicon dioxide and of sputtered silicon dioxide.
It is further desirable to form oriented layers of piezoelectric material on substrate materials where heretofore only poor orientation was obtained.
It is further desirable to form electro-acoustic transducers having superb characteristics of oriented piezoelectric material on substrate materials where heretofore only transducers having poor characteristics typical of unoriented piezoelectric material were formed.
SUMMARY OF THE INVENTION
In accordance with the present invention, a method is described for depositing a layer of gold having a preferred crystalline orientation on the surface of a material which normally produces a layer of gold having no preferred crystalline orientation by sputtering a layer of glass over the surface of the material and depositing a layer of gold over the layer of sputtered glass.
The invention further provides a method for depositing piezoelectric material having a predetermined crystalline orientation by the steps of sputtering a layer of glass over the upper surface of a substrate, depositing a layer of gold over the layer of sputtered glass and depositing the piezoelectric material over the layer of gold.
The invention further provides a transducer for generating acoustic waves in a substrate in response to electrical signals comprising a substrate having an upper surface which previously provided unoriented gold, a layer of glass deposited or sputtered thereover, a layer of oriented gold deposited thereover, a layer of piezoelectric material deposited over the gold, a layer of conductive material deposited over the piezoelectric material and means for coupling an input signal to the layer of gold and the conductive layer.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of a transducer;
FIG. 2 is a cross-section view along the lines II--II of FIG. 1;
FIG. 3 is a pattern formed utilizing reflection electron diffraction of unoriented gold; and
FIG. 4 is a pattern for reflection electron diffraction of oriented gold.
FIG. 5 is a reproduction of a photograph of a reflection electron diffraction pattern from which FIG. 3 was derived.
FIG. 6 is a reproduction of a photograph of a reflection electron diffraction pattern from which FIG. 4 was derived.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawing and in particular to FIGS. 1 and 2, an electro-acoustic device such as the delay line 10 is shown having a substrate 12 suitable for propagating acoustic waves and a transducer 14 suitable for generating acoustic waves. Substrate 12 may, for example, be a semiconductor material such as silicon, germanium, gallium arsenide or it may be nonsemiconducting material suitable for propagating acoustic waves. A layer of dielectric 16 is formed on the upper surface 18 of substrate 12. Dielectric layer 16 may, for example, be silicon dioxide thermally grown or sputtered on the upper surface of a silicon substrate 12 or deposited by chemical vapor deposition on the upper surface 18.
Dielectric layer 16 or substrate 12 without dielectric layer 16 may, for example, have an upper surface 20 which may or may not result in a layer of oriented gold having its <111> axis normal to the plane of the layer when deposited thereon. Therefore, in place of depositing gold directly on upper surface 20 of dielectric layer 16 or substrate 12 without dielectric layer 16, a layer 22 of glass such as Corning 7059 glass is deposited thereon. Corning 7059 glass obtained from Corning Glass Works, Corning, N.Y. was chosen because from tests it was found that gold films deposited thereon are oriented with the <111> axes normal to the film layer. The target used for sputtering was 1/8" thick by 6" in diameter. Other materials which orient the <111> axes of gold normal to the film layer may be deposited such as by sputtering to form layer 22. The composition of Corning 7059 glass includes silicon dioxide 50.2%, barium oxide 25.1%, boron oxide 13.0%, aluminum oxide 10.7%, arsenic oxide 0.4% and other constituents 1.6% as measured by other. The glass 7059 may be deposited by sputtering and may have a thickness of 1,000 Angstroms. Glass layer 22 has been formed by sputtering Corning 7059 glass at the rate of 1,000 Angstroms/hour for one hour. The thickness of the glass 7059 was chosen arbitrarily as being thick enough at least 400 Angstroms to buffer the underlying layer of dielectric 16 and thin enough to be acoustically thin at the frequency of interest of a completed transducer.
By acoustically thin, glass layer 22 should have a thickness less than λ/10 where λ is the wavelength of the frequency designed for transducer operation. For example, at 1 GHz, λ is 5 micrometers. For a thickness of 1000 Angstroms at 1 GHz, the thickness corresponds to λ/50. At 3 GHz, the thickness corresponds to λ/16.7.
A thin layer of chrome (not shown) having a thickness of about 400 Angstroms was deposited over layer 22 for adherence followed by a deposition of 1,200 Angstroms of gold to form gold layer 24 over layer 22. The thickness of the gold depends upon acceptable ohmic loss of the transducer and the acceptable acoustic loading. The gold was deposited at a rate of about 100 Angstroms/second. The deposition of the gold was performed by thermally evaporating the gold which is well known in the art. The resulting gold layer 24 over layer 22 was highly oriented having its <111> axis orientation normal to the layer 24 within a small angle α. It is desirable for angle α to be less than 5 degrees.
In FIG. 2, the upper surface 23 of glass layer 22 is shown to contain reference line 25 which is parallel to glass layer 22 and gold layer 24. Arrow 27 is normal to glass layer 22 or at an angle θ=90 degrees to reference line 25. Arrow 29 is at an angle α with respect to arrow 27. Arrow 29 may be rotated around the axis of arrow 27 to form a cone representing all possible orientations within an angle α to arrow 27.
A layer of piezoelectric material 26 is deposited over gold layer 24. The piezoelectric material 26 may, for example, be zinc oxide which may be sputtered. A more detailed description of forming piezoelectric layers may be found in U.S. Pat. No. 3,655,429 which issued on Apr. 11, 1972 entitled "Method Of Forming Thin Insulating Films Particularly For Piezoelectric Transducers" by John DeKlerk and assigned to the assignee herein which is incorporated herein by reference.
Piezoelectric layer 26 has a preferred crystalline orientation which results from its deposition over oriented gold wherein the gold layer has a preferred crystalline orientation. For example, where the piezoelectric material is zinc oxide the C-axis of the zinc oxide has a preferred orientation normal to the layer of zinc oxide.
In FIG. 2, the lower surface of piezoelectric layer 26 is shown to contain reference line 30 which is parallel to reference line 25 and piezoelectric layer 26. Arrow 31 is normal to piezoelectric layer 26 or at an angle φ=90 degrees to reference line 30. Arrow 32 is at an angle β with respect to arrow 31. Arrow 32 may be rotated around the axis of arrow 31 to form a cone representing all possible orientation within an angle β to arrow 31. The degree of orientations within a small angle β of the many crystallites with respect to the normal to the layer, arrow 31, of zinc oxide is an important factor in achieving high quality transducers. The better the orientation of the zinc oxide or the smaller the angle β to the normal of layer 26, the more efficient the resulting transducer 14 will be.
A layer of conductive material 28 is formed over the piezoelectric layer 26 to form the upper electrode of transducer 14. As shown in FIGS. 1 and 2 transducer 14 is suitable for generating bulk acoustic waves into substrate 12. Electrical signals may be coupled between the upper electrode layer 28 and the lower electrode layer 24 to provide a voltage across piezoelectric layer 26. Piezoelectric material 26 in response to receiving bulk acoustic waves may generate electrical signals across layer 26 which are coupled out through upper electrode layer 28 and lower electrode layer 24.
FIG. 3 shows a reflection electron defraction pattern for thermally evaporated gold deposited over a layer of sputtered SiO 2 having a thickness of about 1,000 Angstroms. In FIG. 3 curves 34, 36, 38, 40 and 42 show circular arcs having a common origin 3 and a radius of various amplitudes shown by arrows 35, 37, 39, 41 and 43. The extension of the arcs through an angle of over 90 degrees with respect to the origin 33 show that the gold is unoriented and that the crystal axes such as [111] of various crystallites within the gold layer point in many directions.
FIG. 4 shows a reflection electron diffraction pattern for thermally evaporated gold on a layer of sputtered Corning 7059 glass having a thickness of about 1,000 Angstroms. FIG. 4 shows sharp spots 53 through 60 with respect to the origin 52 showing a high degree of <111> axis orientation normal to the plane or layer of the sputtered glass and gold. The many crystallites in the gold layer all have their <111> axes normal to the gold layer 24 within a small angle α resulting in a very high degree of orientation. Angle α may be as small as 11/2 degrees for oriented gold. If the gold was unoriented, then the spots 53 through 60 would degenerate into a number of arcs the length of which would depend upon the degree of unoriented gold. Angle α may be measured from the pattern as equal to 1/2 the angular width of the spot with respect to the origin 52.
FIG. 5 is a reproduction of a photograph showing in fine detail a reflection electron diffraction pattern from which FIG. 3 was derived. In FIG. 5 a film of unoriented gold was measured.
FIG. 6 is a reproduction of a photograph showing in fine detail a reflection electron diffraction pattern from which FIG. 4 was derived. In FIG. 6 a film of oriented gold was measured.
Since gold films thermally evaporated on certain materials have a high degree of orientation or order, oriented layers of gold on substrates on which gold normally does not orient itself may be achieved by covering the substrate with thin layers of material on which gold orients itself. The thin layer provides a buffer between the substrate and results in a layer of oriented gold when thermally deposited thereon. One example of a thin layer is Corning 7059 glass which may be deposited to a thickness of 1,000 Angstroms by sputtering.
The invention describes a method for depositing a layer of gold having a preferred crystalline orientation on the surface of a material which normally produces a layer of gold having no preferred crystalline orientation by sputtering a layer of glass over the surface of the material prior to depositing a layer of gold over the layer of glass.
The invention further describes a method for depositing piezoelectric material having a predetermined crystalline orientation by sputtering a layer of glass over the upper surface of the substrate, depositing a layer of gold over the layer of glass, and depositing the piezoelectric material over the layer of gold.
The invention further provides a transducer for generating acoustic waves in a substrate in response to electrical signals comprising depositing a layer of silicon dioxide on the upper surface of the substrate, depositing a layer of glass over the layer of silicon dioxide, depositing a layer of gold over the glass, depositing piezoelectric material over the gold layer, depositing a layer of conductive material over the piezoelectric material and coupling input lines to the gold layer and the top conductive layer for coupling electrical signals to and from the transducer.
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A transducer with thin films of gold having a high degree of orientation on surfaces previously yielding only unoriented gold has a layer of glass over the surface of the substrate material followed by a layer of oriented gold over the layer of glass. The added layer of piezoelectric material over the layer of oriented gold provides piezoelectric material having good orientation due to the oriented gold. Addition of a top conductive electrode forms a transducer wherein the piezoelectric material has a high degree of orientation.
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CROSS-REFERENCE TO RELATED APPLICATIONS
U.S. patents disclosing methods of sulfonating thin films of organic liquids by related means include U.S. Pat. No. 3,902,857 filed by John E. Vander Mey and Frank J. Kremers on Aug. 13, 1973 and U.S. Pat. No. 4,163,751, a division of the above, filed on Aug. 7, 1979.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a process and to apparatus for reacting a thin film of an organic liquid with a gaseous medium under reduced pressure. In particular this invention relates to a process and apparatus for continuously reacting a sulfonatable or sulfatable organic liquid with sulfur trioxide.
2. Description of the Prior Art
In recent years several processes and several types of apparatus have been suggested for reacting thin films of sulfonatable and sulfatable organic liquids with sulfur trioxide. Hereinafter when reference is made to sulfonation processes and to sulfonatable materials, it is to be understood that sulfation processes and sulfatable materials are also included, where their inclusion is applicable.
As the need for developing more forms of energy has grown, sources of oil, once considered too difficult or uneconomical to recover have now assumed much greater importance. This fact has now provided great impetus for improving sulfonating processes and apparatus, for large quantities of sulfonated oil detergents are now used in the "tertiary" oil treatment for the recovery of residual oil from the ground, as can be obtained, for example, from otherwise exhausted oil wells.
This technique, also known as the "Marathon Process" is presently employed to recover some of the vast amount of oil still remaining in the ground. The process involves the use of large quantities of oil-soluble detergents for solubilizing oil remaining in the ground which has not been attainable by the methods used in the past.
But there are also many other uses for sulfonated organics, and whereas color is unimportant when sulfonated oil detergents are employed for oil recovery, the lack of color becomes important in the manufacture of detergents and surface active agents from alkyl aryl hydrocarbons or aliphatic alcohols. Where the final product is designed for household use, a colorless or substantially colorless product is of prime importance.
Sulfonation with sulfur trioxide has advantages over sulfonation procedures using oleum, but the reaction between sulfur trioxide and sulfonatable organic compounds is generally violent and difficult to control. The uncontrolled exothermic reaction provides an undesirable colored product, hence various means to control the reaction have been suggested.
Some of the suggested processes require large quantities of an inert carrier gas such as air, introduced at high velocities to move a thin film of organic liquid along a cooled surface during the reaction. Such processes require air compressors and dryers, becoming costly both because of equipment and power requirements.
A process and apparatus for reacting a thin film of an organic liquid with a gaseous reactant which minimizes the problems discussed above is described in U.S. Pat. Nos. 3,902,857 filed on Aug. 13, 1973, and 4,163,751, a division of the above, filed on Aug. 7, 1979. Another such process is disclosed in U.S. patent application, Ser. No. 285,382 filed Aug. 30, 1972, now abandoned.
It would be desirable, however, to provide an improved process and apparatus for reacting a thin film of an organic liquid with a gaseous sulfur trioxide in a manner to increase production, reduce the cost of operation, reduce the amount of plant space required and provide a high quality substantially colorless product. It would be desirable to provide a sulfonating apparatus so compact as to be readily constructed as a mobile unit, capable of movement to any location where a continuing supply of a sulfonated product is required. Further, it would be desirable to provide such a compact unit capable of still higher production rates in those instances where product color is of secondary importance.
SUMMARY OF THE INVENTION
The present invention is directed to an improved process for reacting a thin film of an organic liquid with a gaseous medium. The process comprises the steps of introducing the organic liquid onto the inner curved surface of a rotating spheroidal reaction chamber at is axis or polar area, rotating the reaction chamber at a velocity such that the organic liquid is continuously formed into a thin film on the curved reaction surface, dividing the film covered curved reaction surface into three or more successive concentric reaction areas, depositing over each reaction area a controlled amount of said gaseous medium to thereby control the rate of reaction as the liquid film proceeds from one curved reaction area to the next under the urging of centrifugal force, reacting the organic liquid and the gaseous medium stepwise, under subatmospheric pressure on the rotating curved reaction surface, moving the resulting reaction product to the equatorial region of the rotating reaction chamber, and collecting the reaction product from the equatorial region of the spheroidal reaction chamber.
The apparatus of this invention for reacting a thin film of an organic liquid with a gaseous medium comprises an oblate or substantially spheroidal reaction chamber mounted on a supporting frame for rotation on its axis in a substantially horizontal position, with an inner reaction surface; evacuating means for maintaining the reaction chamber under subatmospheric pressure; separating means to divide the reaction surface into successive reaction areas or segments, thus forming corresponding individual chambers to which the reaction areas are exposed; a first depositing means to deposit the organic liquid on the reacting surface, a second depositing means for depositing controlled quantities of the gaseous reactant within the individual chambers; rotating means to rotate the reaction chamber at a speed such that the organic liquid is continuously moved by centrifugal action as a thin film, successively, over the concentric reaction areas for exposure to the gaseous reactant, and the resultant reaction product is continuously moved to the inner periphery of the reaction chamber where it accumulates; cooling means for controlling the reaction temperature; and means for removing the reaction product from the reactor.
When the gaseous reactant is sulfur trioxide, this may be introduced as a substantially undiluted gas, with the subatmospheric pressure being maintained below 100 mm Hg, preferably below 25 mm Hg. The sulfur trioxide may also be introduced as a mixture of sulfur trioxide and an inert gas such as air. The output of a sulfur burner system designed to deliver "converter gas" of about 8% SO 3 may be used, and in fact satisfactory results may be obtained even if the SO 3 content is as low as 4%. With the employment of such low strength sulfur trioxide the subatmospheric pressure of the reaction chamber may be maintained at about one-half atmosphere or less. The process of this invention can therefore be operated successfully employing a gaseous sulfur trioxide of from about the concentration of "converter gas" to pure sulfur trioxide obtained from such sources as stabilized liquid sulfur trioxide, oleum, or other conventional sources. Preferably, substantially pure sulfur trioxide is used with the pressure within the reaction chamber maintained below about 25 mm Hg.
The process of my invention produces far less air pollution than is obtained from conventional sulfonating apparatus, less power is required, a small vacuum pump is employed rather than a large air compressor and only a small scrubber is required.
Still another advantage of the apparatus of my invention is that it is small, compact, produces a high quality product in good yield, and can be constructed as a mobile unit for ready removal to any point where the product is required.
Although the present invention may be used for a variety of chemical reactions between organic liquids and gaseous reactants, in a preferred embodiment of this invention the gaseous medium is sulfur trioxide and the organic liquid comprises a sulfonatable or sulfatable organic liquid.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 of the drawings is a simplified cross sectional diagram of the rotary spherical reaction chamber of the present invention.
FIG. 2 is a partially exploded perspective view of the preferred embodiment of the present invention. This version has an oblate reaction chamber, the cross section being substantially eliptical. This drawing and those to follow are based on an actual prototype reactor.
FIG. 3 is a broken, partially exploded view of a detail of the stationary central column through which the gaseous reactant enters, and the product is withdrawn.
FIG. 4 is a perspective view of one type of screen diffuser which can be used between the separator discs to improve the uniformity of the distribution of the gaseous reactant within each separated chamber.
FIG. 5 is a cross sectional view in elevation of the assembled reaction chamber, being the same embodiment as the exploded view of FIG. 2.
FIG. 6 of the drawings is a cross sectional view taken through 6--6 of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The process and apparatus of the present invention are particularly applicable in the sulfonation or sulfation by gaseous sulfur trioxide of appropriate organic liquids. Such compounds include saturated alcohols, phenols, olefinic compounds and monocyclic and polycylic aromatic compounds. For example, compounds suitable for sulfation by sulfur trioxide include those fatty acids containing 8 to 20 carbon atoms such as lauryl, myristyl and cetyl alcohol; ethoxylated derivatives of the above fatty acids and the ethoxylated derivatives of alkyl phenols wherein the alkyl group contains from about 8 to about 16 carbon atoms such as octene, decene, dodecene, tetradecene, hexadecene, etc; aromatic hydrocarbons such as those containing benzene, anthracene, or like structures and alkyl substituted derivatives thereof, such as toluene, ethylbenzene, dodecyl benzene, etc. The advantages of the present method of sulfonation are particularly evident in the production of alkyl aromatic sulfonic acids which when neutralized with an alkali metal hydroxide, an amine or an alkanol amine form highly effective detergent compounds. Thus the process of the present invention will be preferably applied to those alkylated aromatic compounds in which the alkyl groups contain a total of from 8 to 22 carbon atoms and in particular, 12 to 14 carbon atoms. In those instances where the organic compound is a solid at room temperatures, it may be preheated to the liquid state, or liquefied by any other desired procedure.
The sulfur trioxide used as the active ingredient may be obtained from any suitable source. It may be vaporized from stabilized liquid sulfur trioxide, obtained from oleum or from other conventional sources. When such gaseous sulfur trioxide is undiluted with other gases, the sulfonation or sulfation is preferably maintained at a subatmospheric pressure of below about 100 mm Hg, or better still, below 25 mm pressure Hg.
However, dilute sulfur trioxide is also applicable. Converter gas containing about 8% sulfur trioxide with the balance being air gives good results, and in fact the sulfur trioxide content can be as low as about 4%. In those instances where such a dilute sulfur trioxide is used, the subatmospheric pressure is maintained at about half an atmosphere (380 mm Hg.) or lower. With other dilutions of higher concentration, intermediate pressures would apply.
An important benefit offered by the present invention stems from its compact structure and relatively high product output. It is compact enough to be rendered mobile, and sulfonators made according to the principles here disclosed can be moved to wherever a supply of a sulfonated product is required. This is especially important today when sulfonated oils are of such importance in the recovery of oil from shale, exhausted oil wells and oil-bearing sands and tars.
With reference to the drawings of FIGS. 1, 2 and 5, there is shown as a preferred embodiment, a rotatable spherical, spheroidal or oblate sulfonation reactor indicated generally at 10. This includes reaction chamber 13 comprising hemispherical sections 12 and 14. These hemispheres are of a material such as stainless steel, resistant to the reactants to be employed. This is also true of all those surfaces which come in contact with the reactants, with the possible exception of a few small parts mentioned below which may be fabricated of a resistant polymeric material such as Teflon. In the prototype reactor, 304 stainless steel was found to be satisfactory.
When ready for assembly the rims or perimeters of these two hemispheres 12 and 14 are brought together, separated only by a metal product-collector ring 21 having an outside diameter substantially equal to that of hemispheres 12 and 14, but an inner diameter up to about 2 inches less than the inner diameter of the hemispheres at their perimeters.
In the prototype sulfonator those sections herein referred to as "hemispheres" are actually 42 inch dish heads of 7/32 inch 304 stainless steel. The stainless steel product collector ring 21 is a circle or ring of channel steel with the sides of the channel extending outwardly, with the uppermost side of the channel having an outside diameter equal to the outer diameter of the hemispheres, and the lower side of the channel having a diameter just under that of the inside diameter of the hemispheres so that when ready for assembly, the lower side of the channel will fit inside the rim of the lower hemisphere and the upper side of the channel will extend over the rim, lying gasket-like between the butted rims of both hemispheres. The inner diameter of this collector ring 21 in the prototype is about 3/4 inch less than the inside diameter of the hemispheres at their rims so that the product-collector ring extends inwardly, 3/8 inch beyond the rims of the hemispheres. A clear view of the cross section of product-collector ring 21 as positioned in the prototype reactor is shown in FIG. 6. Although this is the preferred type of ring, a flat ring of sheet stainless steel would serve as well.
In the center of the bottom of the lower hemisphere 14 there is a circular opening at the perimeter of which is fixed a strong hollow shaft 11 extending downwardly from the reaction chamber. This shaft supports and rotates reaction chamber 13. Shaft 11 is journaled in bearing 15 shown fixed to supporting frame 17. Sheave 19 is fixed concentrically to the hollow shaft 11 below frame 17 whereby power transmitted from a motor not shown can rotate shaft 11 journaled at 15, and the reaction chamber 13 on a substantially vertical axis.
Hollow shaft 11 surrounds a stationary column 35 which extends below the rotary hollow shaft and is fixed with respect to supporting frame 17. The rotary hollow shaft 11 is journaled and sealed by a conventional ceramic-carbon mechanical seal 34. Such mechanical seals are marketed by the Crane Packing Co., and others. (FIG. 1)
This stationary column 35 also extends upwardly almost to the top of reaction chamber 13 and contains a plurality of conduits, 36 and 38. Extending from the lower end of this column are at least two tubes 36 for conducting sulfur trioxide up into the reaction chamber. Three are shown in FIG. 1, and four in FIGS. 2 and 3. If desired, still more can be used for fine reaction control, although about four is preferred. It would also be within the scope of the present invention to introduce the sulfur trioxide into the stationary column 11 through one conduit and use the column as a manifold to divide the sulfur trioxide into two or more streams within the column or as it leaves the column, within reaction chamber 13.
Also, extending from the lower end of the column is a product line 38 (FIGS. 1, 2 and 3), and a spent gas outlet 40 (FIGS. 1 and 2) which is connected with a small scrubber and vacuum pump, not shown. Still another conduit 41 (FIG. 2) can be included to withdraw any small amount of colored product which, if formed, can be collected in the lower hemisphere.
Preferably, one of the conduits of the group or bundle 36 extends to an opening 42 at the top of column 35 and enters a distributing head 44. In the preferred embodiment of the present invention, as shown in FIGS. 2 and 5, and detailed in FIG. 3, the upper portion of column 35 is shown as Teflon or any other suitable resistant material, and the conduits therein are cast or drilled within the solid Teflon. Stainless steel bolt 46 passing through stainless steel washer 48, Teflon disc 50 and stainless steel separator disc 52 engages threaded opening 54 to draw disc 52 tightly against distributing head 44. Sulfur trioxide or other gaseous reactant ascending a conduit, being one of the bundle 36 and escaping through opening 42 would be distributed by distributing head 44 through notches 56.
The type of distributing head is not essential. It can be a ring or cylinder of fritted glass, stainless steel, or a perforate ring of suitable material, stainless or Teflon woven screening, or it can be dispensed with entirely without affecting the end product to a marked degree.
In the embodiment of FIG. 1, Teflon disc 50 is adjacent to, and becomes a part of the distributing head; and the separator disc 52 is above rather than below it. Whether the Teflon disc 50 is above or below separator disc 52 is inconsequential.
Separator disc 52 has a diameter such that it leaves an annular space of no more than about an inch, preferably about a quarter of an inch between its perimeter and the adjacent wall of the upper hemisphere 12. Since the disc is attached to the stationary column 35, it too, remains stationary as the rotating reaction chamber turns about it.
Below separator disc 52 there is a second separator disc 60, also fixed to the stationary column 35. It is parallel to disc 52 and also extends almost to the wall of the upper hemisphere leaving an annular space of no more than about an inch, but preferably about one quarter of an inch. The vertical distance between the two discs is such that the annular area defined by these two circular separator discs comprises between about 5% and 15% of the total inner curved reaction surface of the upper hemisphere 12, or preferably about 7%.
The thickness of the circular separator discs is not critical provided they are heavy enough to remain substantially rigid. In the prototype sulfonator, 304 stainless steel was used having a thickness of 0.049 inches. Supporting separators 66 (FIGS. 2 and 3) can be employed if desired but are not essential.
Just below circular separator plate 60 there is an opening 58 in communication with a second conduit of the bundle 36, also for the introduction of the gaseous reactant such as sulfur trioxide.
Below circular separator disc 60 and opening 58 there is a third circular separator disc 70, also fixed to the column 35 at its center. It is parallel with separator disc 60 and also extends almost to the wall of the upper hemisphere leaving an annular space of no more than about an inch, preferably about one quarter of an inch.
The vertical distance between the two circular separator discs 60 and 70 is such, that the annular area of the wall or reaction surface defined by circular separator discs 60 and 70 comprises between about 7 to 20% of the total inner curved reaction surface of the upper hemisphere 12, or preferably about 10%.
Preferably a cylindrical screen 62 or porous or perforate cylinder surrounds column 35 between separator discs 60 and 70 to aid in producing an even distribution of the gaseous reactant leaving opening 58. Details of a suitable 304 stainless screen cylinder attached to a Teflon ring 64 is shown in FIG. 4. The inner surface of ring 64 can be threaded to cooperate with matching threads on column 35 for precise positioning of the distributing screen 62 (FIGS. 3 and 5) and for positioning separator disc 60.
Just below circular separator disc 70 there is another opening 68 in communication with a third conduit of the bundle 36, for the introduction of the gaseous reactant. Below this there is a forth circular separator disc 74 also fixed to the stationary column. It is parallel to discs 60 and 70 and extends almost to the wall of the upper hemisphere, also leaving an annular space of less than about one inch, preferably about one quarter of an inch.
The vertical distance between separator discs 70 and 74 is such that the annular area defined by separator discs 70 and 74 comprises between about 10% and 25% of the total inner curved reaction surface of the upper hemisphere 12, or preferably about 15%. As in the case of circular separator discs 60 and 70, preferably a cylindrical screen 72 (FIG. 5) or other type of distributor surrounds column 35 between separator discs 70 and 74.
Just below separator disc 74 in the case of the embodiment shown in FIG. 3, there is still another opening 75 in communication with the last conduit shown of the bundle 36 for the introduction of a gaseous reactant. Below this there is a fifth circular separator disc 76 also fixed at its center to the stationary column 35. It too, is parallel to discs 60, 70 and 74, and as with the latter, extends almost to the wall of the upper hemisphere 12, leaving an annular space of less than about an inch, preferably about one quarter of an inch. (FIGS. 2 and 5) The vertical distance between discs 74 and 76 is such that the annular area defined by separator discs 70 and 76 comprises between about 20 and 30% of the total inner curved reaction surface of the upper hemisphere 12, or preferably about 25%.
The above circular separator discs divide the reaction surface into three concentric reaction zones in the case of the embodiment of FIG. 1, and into four concentric reaction zones in the modified reaction chamber of FIGS. 2,3 and 5. In the case of the preferred embodiment of FIGS. 2 and 5, still another circular disc 78 is shown, but this serves only as a baffle and not as a separator disc. It is positioned just above collector ring 21 and has a diameter between about one half inch to 4 inches less than the inside diameter of the product collecting ring 21 which is just below it. Preferably, the diameter is about 2 inches less than the inner diameter of the product collecting ring. Baffle disc 78 is not critical to the present invention but serves to prevent any oversulfonated mist from reaching the final colorless, or essentially colorless product.
Hollow shaft 11 to which the driving pulley 19 for the rotary reaction chamber 13 is fixed, is adjustable within limits, so that it may be raised or lowered, and with it, the entire reaction chamber which is fixed thereto. It is clear, then, that by thus raising or lowering the reaction chamber in relation to the fixed column 35 which supports the separator discs, the annular clearances of these circular discs, and the concentric areas of reaction surface can be altered within limits. The bearing 15 and the seal 34 permit this adjustment.
The amount of sulfur trioxide or other gaseous reactant that can be delivered to each of the partitioned spaces between the circular separator discs can be controlled. Each of the conduits of bundle 36 can have its own control valve, not shown, as does my prototype sulfonator. These control valves are preferably in communication with a manifold supplied with the reactant gas of the concentration and pressure desired. Further, each can have its own flow meter and even automated equipment which is readily available, to mechanically control the flow of gas, independently, to each partitioned space.
In the preferred embodiment there is fixed, at the top center of the upper hemisphere 12 a bubble or bell-shaped appendage 16, the lower edge of which is joined smoothly to a circular opening at the top center of the upper hemisphere 12, said circular opening having the same diameter as that of the skirt or perimeter of bubble 16. The inner surface of the bubble 16 and the inner surface of the upper hemisphere 12, which is the reaction surface, are preferably highly polished.
An inlet feed pipeline 18 for the introduction of the organic liquid to be reacted with a gaseous reactant such as sulfur trioxide, passes through an opening in the top center of bubble 16 where it is journaled for longitudinal rotation. It is preferably supplied with suitable bearings for high speed rotation and passes through a substantially pressure-tight seal 20. Rotatable inlet feed pipeline 18 is in communication with a stationary conduit, the connection being made through a gas tight seal into which pipeline 18 is journaled. The conduit communicating with rotatable pipeline 18 is in communication with a controlled source of the liquid feed to be sulfonated or sulfated.
The lower end of feed line 18 terminates perpendicularly between two parallel discs, the diameter of which can be approximately half the diameter of the walls of the bubble 16 at its perimeter. Feed line 18 is sealed into a central opening in the first disc, the second disc of substantially the same diameter, being blank. These parallel discs are fastened together at three or more points. The vertical distance between these discs is related to the size of the sulfonator and to the amount of organic liquid to be fed into the reaction chamber. Assuming that the diameter of the feed inlet pipeline is chosen to be commensurate with the rate of flow of organic liquid to be handled, the distance between the discs is preferably about one quarter of the diameter of the feed inlet pipeline 18, or less. If desired, the parallel discs can have a plurality of perpendicular radiating impeller blades, straight or curved, as in a centrifugal pump, but these are not essential. Other types of spinning distributor heads can be used. A very effective type consists of two to four or more tubes in communication with the feed pipeline and radiating outwardly and perpendicularly from it. These may extend quite close to the wall of the bubble, being perpendicular to it, or they may turn away from their direction of rotation so as to be substantially parallel to the wall of the bubble and close to it.
Other types of spinning distributors are also satisfactory such as a hollow disc, sphere, or other shape having openings in its perimeter through which the liquid feed can be distributed by centrifugal force to the walls of the bubble. Furthermore, the bubble itself could be eliminated, with the distributing head dispersing the liquid feed directly into the top of the upper hemisphere 12.
A sheave is fixed to the rotary inlet feed pipeline 8 for driving the distributing head 22 and 24. The spinning distributing head is spun at an appreciably greater speed than that of the rotary reaction chamber, and preferably in the direction opposite to that of the rotary reaction chamber to insure uniform distribution of the liquid organic reactant.
There is also provided a product take-off line 80 terminating in a scoop 82 to collect product as it builds up as a result of centrifugal force above product collector ring 21. The take-off line 80 conducts the product to a take-off pump, not shown, for removal. A lute, not shown, can be included in the line to insure a good seal. A gear pump for product removal is preferred. The pump can deliver the product to a product receiver not shown. Alternately, the receiver can be maintained at a subatmospheric pressure to thus eliminate the need for a pump.
In FIG. 5 there is shown as an option, a discolored product take-off line 84 with scoop 86 positioned to collect any material collected below the collecting ring 21 coming from the lower hemisphere 14. An important feature of my invention is that all reacting surfaces face downwardly as well as inwardly, so that any mist formed which would not benefit from the cooling of the reaction surface, and would therefore be prone to overheating, over sulfonation and discoloration, would not fall back to the reaction surfaces, but would rapidly fall, because of the subatmospheric pressure, to the upper surface of the separator discs 60,70,74 or 76, or to the upper surface of baffle disc 78. All such material ultimately reaching the baffle disc would drop through the annular space surrounding baffle disc 78, to lower hemisphere 14. Here it would collect because of centrifugal force, below collector ring 21. So little such discolored product would be accumulated that it could easily be recovered from the bottom of the reactor after a short run, but the scoop 86 and discolored product take-off line 84 are shown in FIGS. 2 and 5 for the continuous removal of discolored product during a prolonged run, thus a novel method of continuously removing the bulk of substantially colorless product, and the small amount of discolored product, is provided. Any discolored product recovered can be combined with the main product when color is not critical, but kept separate where a colorless product is desired for use in household detergents and the like.
Recycling of any incompletely sulfonated product is easily accomplished by pumping all or part of the product back to feed line 18, but with all the adjustments provided, variation of the area of the several reaction surfaces, adjustment of the several streams of gaseous reactant and of the amount of liquid feed, incomplete sulfonation need not be encountered.
The opening 88 in the stationary column 35 of FIGS. 1,3 and 5, leads to the scrubber and vacuum pump not shown. It is the outlet for spent gas and provides the means for maintaining the system under reduced pressure.
When the reactor is to be closed, a band of suitable gasket material 23 of FIGS. 5 and 6, surrounds the juncture of the two hemispheres 12 and 14, so that the resulting reaction chamber 13 can be maintained at subatmospheric pressures. This band 23 is surrounded in turn by steel bellyband 26 of FIGS. 2,5 and 6, with a simple tightening device 28 of FIG. 2.
The hemispheres 12 and 14 are bolted together by two or more bolts passing through aligned drilled projections 32 fixed to the sides of each hemisphere.
In operating the equipment as in sulfonating a sulfonatable oil, the reaction chamber is evacuated. If substantially pure sulfur trioxide is to be used, a pressure of less than about 100 mm Hg is maintained, preferably between about 4 and 25 mm Hg. The oil is then introduced through feed inlet pipeline 18 while the feed line and disc distributor head 22-24 is spun at high speed. The sulfonatable oil is introduced into the reaction chamber while it is revolving in the direction opposite to that of the distributor 22-24 at a velocity of between about 25 and 400 RPM, preferably between about 100 and 200 RPM.
The liquid feed is thrown against the almost vertical polished inner wall of the bubble 16, and by centrifugal force, flows as a thin uniform film over the polished curved reaction surface toward the collector ring 21 at the equator or inner periphery of the rotating reaction chamber 13. In doing so it passes consecutively over the concentric annular areas separated by the circular separator disc 52, 60, 70, 74 and 76. Separate streams of sulfur trioxide, preferably independently controlled, are delivered to each partitioned chamber. Within each chamber the atmosphere provided does not supply sufficient sulfur trioxide to more than partially sulfonate that portion of the film of organic liquid momentarily exposed to that gaseous reactant. As the film of organic liquid flows over the annular reaction surfaces and passes one partitioned chamber after another, the ordinarily rapid reaction is slowed down. By the time it passes over the annular reaction surface exposed to the gaseous reactant between circular separator discs 74 and 76, the sulfonation has been virtually completed.
During the continuous process, zone heating or cooling as required is provided exteriorly by cold water jets or sprays, heated or cooled water or air, or heat lamps. The sulfonated product forced toward the reactor's inner perimeter collects above the collector ring 21 where it is continuously scooped up by scoop 82 of product line 80 and preferably directed to a gear pump and product receiver not shown. A product receiver maintained at subatmospheric pressure may be employed rather than a gear pump if desired.
A small sulfonator such as the 42 inch (diameter) prototype could be expected to produce between about 250 and 350 lbs of high quality product per hour. Any discolored product which may form from mist as previously explained could, if present in sufficient quantity, be scooped up by scoop 86 of pipeline 84 of FIG. 2 and collected by a separate gear pump and/or receiver not shown.
When treating highly viscose or solid sulfonatable materials, they can be fluidized by preheating, and if necessary, heat lamps or other sources of radiant energy can be used initially on the reaction surface.
The primary aim of this process and apparatus is to produce an essentially colorless high quality product. However, for some sulfonated products such as the sulfonated oils of value in the Tertiary process for the recovery of oil from exhausted oil wells, shales and oil bearing sands, color is of little concern.
Where there is no need for the separation of darkened product, no collector ring is required within the reaction chamber. The product can be scooped from the inner periphery or equator of the rotating reaction chamber.
It is also possible, where color in the product is of no consequence, to operate the apparatus in an inverted position with the reaction chamber suspended downwardly from its driving mechanism, or constructed as shown, but with the liquid organic feed and the partitioning separator discs being located in the lower hemisphere. The reaction chamber can also be fabricated and operated with a set of separator discs in each of the two hemispheres, with or without baffle discs, and with the fluid organic feed entering through rotating distributors at both poles of the rotating reaction chamber. The inner surface of both hemispheres is preferably a highly polished surface, and no collector ring is then required. The sulfonated product is continuously scooped from the inner periphery of the apparatus.
Quite apart from the use of the apparatus described as a sulfonator, it has also been found effective as a flash evaporator, either at atmospheric or subatmospheric pressures. Because of the thin film of liquid distributed over the evaporating surface, and the low evaporating temperatures possible, especially when the apparatus is used as a vacuum flash evaporator, products ordinarily discolored or chemically altered by heat can be effectively concentrated or evaporated in the apparatus described.
It will be apparent that the process and apparatus of my invention will permit the continuous production of an especially high quality product at a reasonably high rate of production, and this from a small compact apparatus which could be handled as a mobile unit and moved to those locations where a continuous supply of such product is required.
It is to be understood that variations and modifications of the present invention may be made without departing from the scope of this invention. It is also to be understood that the scope of the invention is not to be interpreted as limited to the specific embodiment disclosed herewith, but only in accordance with the appended claims when read in the light of the foregoing disclosure.
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A continuous process is disclosed which comprises introducing a sulfonatable or sulfatable organic liquid onto a rotating reaction surface as a thin film, rotating the reaction surface at a velocity such that the thin film is continuously moved toward the periphery of the reaction surface, dividing the reaction surface into a plurality of areas, depositing within each area a controlled quantity of gaseous sulfur trioxide over the liquid film, maintaining the pressure during the reaction at subatmospheric levels, controlling the temperature of the reaction surface, moving the reaction product by centrifugal action to the periphery of the reaction surface and continuously collecting the reaction product.
An apparatus for carrying out such a process is also disclosed.
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BACKGROUND
[0001] The present invention relates to the formation of coated surfaces which may be used in semiconductor processing.
[0002] In semiconductor material processing facilities, plasma processing chambers are often used, for example, for etching and deposition. The walls of these chambers, as well as liners, process kits, and dielectric windows, are often exposed to corrosive and erosive process gases, as well as plasma. Therefore, plasma chambers, typically composed of aluminum, are sometimes coated with protective layers to increase the life of the chamber.
[0003] U.S. Pat. No. 8,619,406 B2 describes a coating of is yttrium oxide (yttria, Y 2 O 3 ), which has been applied directly to aluminum or with an intermediary layer of aluminum oxide. An improvement over yttria is yttria-stabilized zirconia (YSZ, ZrO 2 :Y 2 O 3 ). It is also possible to layer either of these components with other components. For example, U.S. Pat. No. 6,942,929 describes a coating of yttrium aluminum garnet (YAG, Y 3 Al 5 O 12 ) over aluminum. U.S. Patent Pub. No. 2008/0169588 A1 describes a coating in which there is an outer layer of yttria and an intermediate layer of YAG, above a third layer of alumina. Another example is U.S. Patent Pub. No. 2014/0295670 A1, which describes a coating of yttria over aluminum oxide, over aluminum or aluminum alloy.
[0004] Given the expense and lost time in shutting down plasma processing chambers after they wear out, there is an interest in chamber coatings that have longer lifetimes, and which may have better protection against corrosive process chemicals.
SUMMARY
[0005] Various inventive embodiments are described herein. One embodiment is a substrate processing apparatus comprising a chamber configured to contain a plasma, wherein the apparatus may comprise one or more multi-layer surfaces oriented to face the plasma, the one or more multi-layer surfaces may each comprise: a base material; a first layer over the base material comprising zirconia stabilized with a dopant oxide; and a second layer over the first layer, comprising a yttrium-aluminum composite.
[0006] In another embodiment, at least one of the one or more multi-layer surfaces may be a transparent quartz window. The embodiment may further comprise: a spectrometric sensor positioned to take spectrometric measurements inside the chamber, through the quartz window; an analog to digital converter configured to convert signals corresponding to the spectrometric measurements into one or more digital signals; and a general purpose computer, which may comprise: one or more processors; a digital memory system; and an I/O bus in communication with the analog to digital converter and configured to receive the one or more digital signals; and one or more interconnection busses configured to transmit data between the one or more processors, the data receiver, the digital memory system, and the I/O bus.
[0007] In another embodiment, a method of operating the above apparatus or related apparatuses disclosed herein may comprise: using the spectrometric sensor to repeatedly take spectrometric measurements of the level of zirconium within the chamber, through the quartz window, wherein the spectrometric measurements are converted into the one or more digital signals by the analog to digital converter and transmitted to the I/O bus of the general purpose computer; causing the general purpose computer to run computer executable program instructions comprising instructions to monitor the digital signals until the signals reflect a spike in the level of zirconium in the chamber, and then to transmit a signal indicating the failure of a coating on a surface within the apparatus.
[0008] In another embodiment, a method of making any of the above apparatuses or related apparatuses disclosed herein may comprise, for each surface of the one or more surfaces: providing the base material; forming the first layer over the base material by exposing the surface to a plasma thermal spray; and after the first layer is formed, forming the second layer over the first layer by exposing the surface to a plasma thermal spray.
[0009] These and other features of the present inventions will be described below in the detailed description and in conjunction with the following figures.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The disclosed inventions are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar elements and in which:
[0011] FIG. 1 is a schematic cross-sectional view of a multi-layer coating.
[0012] FIG. 2 is a schematic view of a processing chamber that may be used in practicing the disclosed inventions.
[0013] FIG. 3 is a flowchart illustrating a process for creating a multi-layer coating.
[0014] FIG. 4 is a schematic illustration of a computer system for implementing a sensor processing system used in embodiments of the disclosed inventions.
DETAILED DESCRIPTION
[0015] Inventions will now be described in detail with reference to a few of the embodiments thereof as illustrated in the accompanying drawings. In the following description, specific details are set forth in order to provide a thorough understanding of the present invention. However, the present invention may be practiced without some or all of these specific details, and the disclosure encompasses modifications which may be made in accordance with the knowledge generally available within this field of technology. Well-known process steps and/or structures have not been described in detail in order to not unnecessarily obscure the present disclosure.
[0016] In plasma process chambers with a particular prior art coating of yttrium oxide, the inventors have observed an average lifetime of 3700 RF hours. This failure can be much earlier, depending on the chemistry of the plasma process. Failure mechanisms for such coatings may include delamination during the cleaning process upon, for example, exposure to chlorine or fluorine. The inventors have observed, however, that a coating of YSZ over aluminum may last approximately 10 times longer than a Y 2 O 3 coating in the test involving HF solution to mimic fluorine plasma exposure in a reactor. However, in a similar test involving an HCl solution to mimic chlorine plasma exposure in a reactor, there is minimal improvement in the lifetime of the coating. A coating of YAG over aluminum may last approximately 6 times longer than the Y 2 O 3 coating in a test involving HCl solution to mimic chlorine plasma exposure in a reactor, but a similar test involving HF solution only approximately doubles the lifetime with respect to Y 2 O 3 . Thermal cycling does not appear to substantially affect these results. The inventors have determined that there are advantages to combining the benefits of YAG with the benefits of YSZ in a single coating which, among its other benefits, would be resistant to both HCl and HF.
[0017] FIG. 1 shows one embodiment of such a coating 100 that combines the advantages of YSZ and YAG in the same coating. In this example, aluminum is the base/bulk material to be coated 101 , which is an interior surface of a plasma chamber. Above the aluminum is a layer of Al 2 O 3 102 . Above that is a layer of YSZ 103 . Finally, on the top is a layer of YAG 104 . The YAG layer 104 in this example is facing the plasma side of a chamber.
[0018] In other embodiments, zirconia may be stabilized with other oxides than yttria in layer 103 , such as magnesia (MgO), calcium oxide (CaO), and cerium(III) oxide (Ce 2 O 3 ), iridium(IV) oxide (IrO 2 ), titanium(IV) oxide (TiO 2 ), or oxides of elements from atomic numbers 57 (La) to 71 (Lu). In another embodiment, the Al 2 O 3 layer 102 may be omitted. Also, other embodiments may include other yttrium-aluminum composites, such as yttrium aluminum monoclinic (YAM) and yttrium aluminum perovskite (YAP). In some cases, coatings of YAG may contain small amounts of other components such as YAP and/or YAM, while still considered to be YAG.
[0019] In other embodiments, there may be intermediate layers of other materials, or multiple layers of any of the above materials, arranged in any order. Various plasma processing chamber base materials 101 may be used, including aluminum (Al), aluminum oxide (Al 2 O 3 ), an Al 2 O 3 film on Al (created, for example, by anodization), a non-aluminum containing metal, quartz, or other known plasma chamber materials.
[0020] The layers of the coating 103 and 104 may, in one embodiment, be applied by plasma thermal spraying. In other embodiments, they may be applied by sputtering, plasma enhanced chemical vapor deposition or other chemical vapor deposition, electron beam physical vapor deposition or other physical vapor deposition, chemical solution deposition, atomic layer deposition, pulse laser deposition, cathodic arc deposition, electrohydrodynamic deposition, sol-gel precursor deposition, aerosol deposition, and the like.
[0021] In one embodiment, the total thickness of layers 103 and 104 is about 0.2 mm (8 mils). The total thickness of the layers may be more or less; however, there is a trade-off relating to the thickness of the layers. The thicker the layers, the greater the corrosion resistance and lifetime of the coating is likely to be. However, as the layer gets thicker, the adhesion to the underlying layer(s) may decrease. Thus, a thinner layer may be better, assuming the surface can be coated uniformly. In one embodiment, layer 103 can be approximately 0.05-0.1 mm (2-4 mils) thick, and layer 104 can be approximately 0.05-0.15 mm (2-6 mils) thick.
[0022] Surfaces, as described, may in one embodiment be configured to withstand a lifetime of approximately 6,000 to 10,000 RF hours before failure, or in another embodiment, higher than 10,000 RF hours. The surfaces may also be designed to fail within a given expected range, such as 6,000 to 8,000 RF hours, 7,000 to 9,000 RF hours, or 8,000 to 10,000 RF hours.
[0023] The chamber may be configured in various ways known in the art. Suitable chambers may include 2300® Versys® Kiyo45™ chambers provided by Lam Research Corporation, or the like. The surfaces may be formed by any method known in the art. In addition, in one embodiment, both an intermediate zirconium-containing layer and an outer yttrium-aluminum composite layer may be deposited by plasma thermal spray. In one embodiment, the interior of plasma chamber composed of aluminum and/or one or more quartz windows may be coated by plasma thermal spray, to produce at least two coatings.
[0024] In another embodiment, a plasma chamber may comprise one or more replaceable linings. These linings may be coated in a controlled environment, and then inserted into the plasma chamber. FIG. 2 is a schematic, simplified view of an embodiment of a plasma processing chamber showing replaceable coated liners. Inside the chamber 200 , a chuck 201 may be used for holding substrates. An injector 202 may be used to inject process gasses into the chamber. Liners 204 , 205 , and 206 may be used in any configuration to protect the chamber from corrosion. Such liners may be made of any suitable material. In one embodiment, the liners may be composed of aluminum, and coated in accordance with one of the coatings described herein.
[0025] The embodiment of FIG. 2 includes a quartz window 203 , which may also be coated as described herein, with the coating facing the plasma-side of the chamber. In one embodiment, a sensor 207 may be placed behind the quartz window, and connected via sensor circuitry to a processor 208 for processing signals from the sensor 207 .
[0026] In one embodiment, the failure of a surface coated as described herein may be recognized by the use of sensors to monitor the presence of zirconium in the chamber. In a configuration where zirconium is only a component within an intermediate layer, zirconium may thus serve as a signal that layers above the zirconium layer have been breached. In one example, a zirconium spike may be recognized in the plasma, or on the surface of a substrate being processed. Such a spike may indicate, for example, that there has been a significant corrosion through an outer YAG layer and that an intermediate YSZ layer is being corroded. This could therefore result in a marked increase in the measured zirconium level. A spike may be recognized in several ways, including by setting a predetermined threshold for zirconium concentration in the chamber, such that when the threshold is met, this may be an indication that a surface coating within the chamber has failed. In an alternate embodiment, a threshold can be set for the rate of change in zirconium concentration as a function of time.
[0027] When a coating in the interior of a chamber fails, the chamber may be replaced or re-coated, or a part of the chamber may be replaced or re-coated. In one embodiment, the chamber may contain replaceable coated liners, and when the coating on one of the liners fails, the liner may be replaced. In another embodiment, a quartz window insert may similarly be coated, and the window replaced when the coating fails. In another embodiment, a gas injector into the chamber may be coated as described above, and when the coating on the gas injector fails, the injector may be replaced.
[0028] FIG. 3 shows an embodiment of an algorithm for determining when a surface inside a chamber, and in particular a replaceable liner surface, has failed. In step 301 , sensor 207 may be used to measure the zirconium level in the chamber. The process loops ( 302 ) so long as a spike in the zirconium level has not been detected. If a spike is detected, however, the process may indicate to an operator that a chamber coating has failed, 303 . An operator may in one embodiment respond by stopping the process, inspecting the liners, and replacing all the liners, or just the liner or liners that have failed. The algorithm may be performed by analog alarm circuitry as known in the art, or by digital circuitry such as a special- or general-purpose computer. An operator may be notified by various means, including a visual display, an audible alarm, or a text message. Such notifications can, in one embodiment, be sent over a wired or wireless network or otherwise via any appropriate telecommunications medium.
[0029] FIG. 4 is a high level block diagram illustrating a computer system 400 for implementing a sensor processing system used in embodiments of the disclosed inventions. The computer system may have many physical forms ranging from an integrated circuit, a printed circuit board, and a small handheld device up to a huge super computer. The computer system 400 may include one or more processors 402 , and further can include an electronic display device 404 (for displaying graphics, text, and other data), a main memory 406 (e.g., random access memory (RAM)), storage device 408 (e.g., hard disk drive), removable storage device 410 (e.g., optical disk drive), user interface devices 412 (e.g., keyboards, touch screens, keypads, mice or other pointing devices, etc.), and/or a communication interface 414 (e.g., wireless network interface). The communication interface 414 may allow software and/or data to be transferred between the computer system 400 and external devices via a link. The system may also include a communications infrastructure 416 (e.g., a communications bus, cross-over bar, or network) to which the aforementioned devices/modules may be connected.
[0030] Information transferred via communications interface 414 may be in the form of signals such as electronic, electromagnetic, optical, or other signals capable of being received by communications interface 414 , via a communication link that carries signals and may be implemented using wire or cable, fiber optics, a phone line, a cellular phone link, a radio frequency link, and/or other communication channels. With such a communications interface, it is contemplated that the one or more processors 402 might receive information from a network, or might output information to the network in the course of performing the above-described method steps. Furthermore, method embodiments of the present invention may execute solely upon the processors or may execute over a network such as the Internet in conjunction with remote processors that shares a portion of the processing.
[0031] The term “non-transient computer readable medium” is used generally to refer to media such as main memory, secondary memory, removable storage, and storage devices, such as hard disks, flash memory, disk drive memory, CD-ROM and other forms of persistent memory and shall not be construed to cover transitory subject matter, such as carrier waves or signals. Examples of computer code include machine code, such as produced by a compiler, and files containing higher level code that are executed by a computer using an interpreter. Computer readable media may also be computer code transmitted by a computer data signal embodied in a carrier wave and representing a sequence of instructions that are executable by a processor.
[0032] The computer device 400 may serve as the processor 208 for processing signals from the sensor 207 in FIG. 2 . For example, signals from sensor 207 may be processed through an analog-to-digital computer, such that a digital signal may be transmitted to the computing device 208 , for example via the communications interface 414 , which may include an I/O bus.
[0033] While inventions have been described in terms of several preferred embodiments, there are alterations, permutations, and various substitute equivalents, which fall within the scope of this invention. There are many alternative ways of implementing the methods and apparatuses disclosed herein. It is therefore intended that the following appended claims be interpreted as including all such alterations, permutations, and various substitute equivalents as fall within the true spirit and scope of the present invention.
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In accordance with this disclosure, there are provided several inventions, including a substrate processing apparatus with multi-layer surfaces configured to face the plasma and resist against corrosion. These multi-layer surfaces may in one example include a base layer of aluminum, anodized aluminum, or quartz, a second layer of stabilized zirconia, and a second layer of a yttrium-aluminum composite such as yttrium aluminum garnet (YAG).
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FIELD OF THE INVENTION
The present disclosure relates to the technical field of oil and gas drilling, in particular to a downhole mud-driven rotating magnetic field generator.
BACKGROUND OF THE INVENTION
With the development of modern oil and gas drilling technology, measuring while drilling tool (MWD tool) is more and more widely used in the drilling process. The MWD tool transmits the underground data to the ground by means of mud pulse, electromagnetic wave, or sound wave, so that the technicians on the ground can analyze the data and then adjust the drilling progress accordingly.
In the prior art, power is supplied to a downhole MWD tool mainly in two ways, namely through battery pack and through generator. Because the capacity and safety of a battery pack are greatly affected by the temperature, when the temperature reaches 120° C., the capacity of the battery pack decreases by 20%. The temperature limit of a battery pack is about 175° C. In addition, the transducer and electronic circuits of the MWD tool only require a few or a dozen watts of power, however, part of the underground measuring and controlling system can consume as much as 700 watts. To prolong the operation time of the tool underground, downhole generator is mainly used as the power source for the MWD tool at present, which supplies power for the battery and/or the transducer group and the signal generating device.
U.S. Pat. No. 5,517,464 discloses an MWD tool which integrates a mud pulse generator and a turbine generator. The turbine generator comprises a turbine impeller, a drive shaft, a transmission, a three-phase alternator, and a rotational speed measurement device. Because the space underground is limited and the generator can only provide relatively low power, the turbine generator cannot meet the requirement of the drilling process. In addition, in this device, a gearbox is used to obtain the rotary speed response from the turbine and the generator, which adds complexity to the structure of the MWD tool. Moreover, since the coils directly contact the mud, it requires highly of the mud quality, bearing performance, and the insulation of the coils; and the coils are easy to be damaged at high speed under severe environment, such as high temperature and intense vibration, for long terms.
CN 201010533100.2 discloses a petroleum drilling mud generating system which comprises coil windings, a magnet, an impeller, an upper plug, a lower plug, a central shaft, and an isolation sleeve, wherein the magnet is embedded in the impeller hub; the coil windings are fixed in a closed cavity formed by the central shaft, the upper and lower plugs, and the isolation sleeve; and the impeller hub is in clearance fit with the isolation sleeve. When the mud with pressure flushes from top to bottom, the flushed impeller rotates so that the magnet embedded in the impeller hub rotates synchronously with the impeller, and the coils cut through the magnetic lines of force to generate power. Moreover, an abrasion-resistant alloy sleeve is provided between the impeller and the isolation sleeve, which provides supporting and straightening functions when the impeller rotates. And a shock absorber is provided between the alloy sleeve and the plugs, so as to reduce influence of the mud impact on the abrasion-resistant alloy sleeve.
This petroleum drilling mud generating system is advantageous in that it no longer uses dynamic seal. However, it adopts clearance fit between the rotor and the isolation sleeve, with mud as the lubricant, so as to fulfill the functions of supporting and straightening. When operating at high speed in the mud, because sand unavoidably exists in the mud, sand stuck can easily occur, causing the whole system to fail and mud lubrication failure. In addition, the metal isolation sleeve, which is placed between the magnet and the coil windings, suffers from eddy current loss in a changing magnetic field, making it very difficult for the system to generate high power. In the meantime, eddy current loss directly manifests as heat, causing temperature rise.
SUMMARY OF THE INVENTION
The present disclosure provides a downhole rotating magnetic field generator, comprising: a stator assembly, comprising a stationary cylindrical body and windings arranged in a first region of the body; and a rotor assembly, comprising a permanent magnet arranged radially outside of the windings and a turbine rotor arranged in a second region of the body which is axially adjacent to the first region, wherein the turbine rotor and the permanent magnet are fixedly connected with each other along an axial direction, and arranged on the body at both ends of the rotor assembly respectively through a first bearing and a second bearing.
In an embodiment according to the present disclosure, a first internal fluid passage and a second internal fluid passage, which are communicated with each other, are formed respectively between the turbine rotor and the body and between the permanent magnet and the windings, so that a part of fluid passing through the generator enters the first internal fluid passage through the first bearing and then is discharged through the second bearing after flowing through the second internal fluid flow passage.
In one embodiment, a first external fluid passage is arranged on the periphery of the turbine rotor.
According to the present disclosure, a guiding stator is arranged on a third region of the body which is axially adjacent to the second region, a second external fluid passage is arranged on the periphery of the guiding stator, and a third internal fluid passage communicated with the first internal fluid passage is arranged inside the guiding stator.
According to a preferred embodiment of the present disclosure, an adjusting ring is arranged between the turbine rotor and the body, the first internal fluid passage being arranged between the turbine rotor and the adjusting ring, and the first bearing being placed on the periphery of the adjusting ring.
According to another preferred embodiment of the present disclosure, a slip ring is arranged between the guiding stator and the first bearing.
According to the present disclosure, the first bearing comprises a rotor upper bearing and a radial bearing, and the second bearing comprises a rotor lower bearing and a body bearing.
According to a preferred embodiment, an insulation layer is formed radially outside of the windings.
According to another preferred embodiment, a yoke and a non-magnetically conductive shield are respectively arranged radially outside and inside of the permanent magnet, the second internal fluid passage being arranged between the insulation layer and the non-magnetically conductive shield.
According to the present disclosure, the body comprises an axial inner passage and a radial passage arranged in the first region thereof, an electrical lead, which passes through a radial passage in a sealed manner and connects to the windings, is used to output the electric power and/or signal generated.
BRIEF DESCRIPTION OF THE DRAWINGS
The present disclosure will be described in detail below with reference to the accompanying drawings. It should be understood that the drawings are provided only to better illustrate the present disclosure, and should not be construed as limitations thereto. In the drawings,
FIG. 1 schematically shows the structure of a downhole rotating magnetic field generator according to the present disclosure.
DETAILED DESCRIPTION OF THE EMBODIMENTS
A specific embodiment according to the present disclosure will be described below with reference to FIG. 1 .
The downhole rotating magnetic field generator 100 according to the present disclosure mainly comprises a stator assembly and a rotor assembly. The stator assembly comprises a stationary, cylindrical body 1 . The cylindrical body 1 , as a mounting base of the whole generator, is configured as an elongated shaft-shaped member. All the components of the generator 100 can be mounted on the cylindrical body 1 . Windings 20 are arranged on a certain region of the body 1 (namely a first region L1). In one specific embodiment, a projection 25 in form of an integral step is arranged on one end (the right end in FIG. 1 ) of the first region L1, so that the windings 20 can be positioned axially thereon.
In a preferred embodiment, an insulation layer 13 is arranged radially outside of the windings 20 , and a set of laminations 19 is arranged radially inside of the windings 20 . During operation, the body 1 does not rotate. Therefore, the windings 20 , the set of laminations 19 , and the insulation layer 13 do not rotate during operation, either.
According to the present disclosure, the rotor assembly comprises a permanent magnet 10 arranged in the first region L1 of the body 1 . The magnet 10 is also located radially outside of the windings 20 , and one end (the right end in FIG. 1 ) thereof is defined by a second bearing, namely a lower bearing 14 and a body bearing 15 .
A turbine rotor 8 is arranged on one side (the left side in FIG. 1 ) of a second region L2 of the body 1 which is adjacent to the first region L1. The turbine rotor 8 is axially adjacent to and fixed connected with the permanent magnet 10 . The rotor assembly is arranged on the body 1 at both ends thereof respectively through the first bearing and the second bearing. The first bearing and the second bearing can both be, for example, sliding bearings.
In a preferred embodiment, a yoke 9 can be arranged outside of the permanent magnet 10 . The yoke 9 is fixedly connected to both the turbine rotor 8 and the permanent magnet 10 , so that the turbine rotor 8 and the permanent magnet 10 can rotate as a whole. Preferably, a non-magnetically conductive shield 11 can be arranged inside of the permanent magnet 10 to protect the permanent magnet 10 .
A first external fluid passage 8 a is arranged on the periphery of the turbine rotor 8 . During operation of the generator 100 underground, fluid, such as mud, flows through the first external fluid passage 8 a , so as to drive the turbine rotor 8 to rotate. Because the permanent magnet 10 is fixedly connected to the turbine rotor 8 , it rotates therewith. Thus, the rotating permanent magnet moves relative to the stationary windings 20 by cutting through the magnetic lines of force, so as to generate power.
According to a preferred embodiment, a first internal fluid passage 12 a is arranged between the turbine rotor 8 and the body 1 , and a second internal fluid passage 12 b is arranged between the permanent magnet 10 and the windings 20 . The first internal fluid passage 12 a and the second internal fluid passage 12 b are communicated with each other.
In this case, during operation of the generator 100 underground, most of the mud passes through the first external fluid passage 8 a on the periphery of the turbine rotor 8 to drive the turbine rotor to generate power. A small portion of mud enters the first internal fluid passage 12 a through the first bearing, then passes through the second internal fluid passage 12 b , and finally flows out of the generator 100 through the second bearing. Thus, this small portion of mud can effectively lower the temperature at the windings 20 , thereby extending the service life of the generator 100 significantly. Furthermore, the small portion of mud can also act as lubricant for the first bearing and the second bearing, and also prevent sand from being deposited thereon, so that the service life of the generator 100 can be further extended significantly.
According to an embodiment of the present disclosure, the generator 100 further comprises a guiding stator 3 . The guiding stator 3 is arranged on a third region L3 of the body 1 , which is axially adjacent to the second region L2, towards a side of the second region L2 opposite to the first region L1. Therefore, the guiding stator 3 and the turbine rotor 8 are axially adjacent with each other. A second external fluid passage 3 a is arranged on the periphery of the guiding stator 3 . The second external fluid passage 3 a is aligned with the first external fluid passage 8 a arranged on the periphery of the turbine rotor 8 , or staggered therefrom at a certain angle.
With the guiding stator 3 , the impact of mud will be diverted from the turbine rotor 8 to the guiding stator 3 , so that the load on the turbine rotor 8 can be effectively decreased, thus the service life of the generator 100 can be further prolonged. In addition, a third internal fluid passage 12 c , which communicates with the first internal fluid passage 12 a , is arranged inside the guiding stator 3 . In this case, part of the underground fluid can flow past the generator 100 through the third internal fluid passage 12 c , the first bearing, the first internal fluid passage 12 a , the second internal fluid passage 12 b , and the second bearing in succession.
Between the turbine rotor 8 and the body 1 , an adjusting ring 17 can be arranged. Under this condition, the first internal fluid passage 12 a is provided between the turbine rotor 8 and the adjusting ring 17 , and the first bearing is provided on the periphery of the adjusting ring 17 . With this adjusting ring 17 , the size of the first internal fluid passage 12 a can be more easily controlled, and the manufacturing and assembly of the turbine rotor 8 can be convenient.
The first bearing can comprise, for example, a rotor upper bearing 6 and a radial bearing 7 . The rotor upper bearing 6 is arranged on one end of the turbine rotor 8 adjacent to the third region L3, and forms an axial bearing pair with one end of the guiding stator 3 adjacent to the second region L2. In the meantime, the rotor upper bearing 6 and the radial bearing 7 , which is arranged on the body 1 or on the adjusting ring 17 , form a radial bearing pair.
In one specific embodiment, the generator 100 further comprises a slip ring 5 arranged between the guiding stator 3 and the turbine rotor 8 . For example, the slip ring 5 can be fixedly connected with the guiding stator 3 by means of a combination of interference fit and adhesive, thus providing a stable positioning restriction. Thus, under intense vibration and impact underground, the slip ring 5 and the rotor upper bearing 6 of the first bearing will contact each other and form a sliding bearing pair, so that direct contact of the guiding stator 3 with the turbine rotor 8 can be avoided. Therefore, the possibility of turbine rotor 8 being damaged can be reduced.
The second bearing can comprise, for example, a rotor lower bearing 14 arranged on the lower end of the yoke 9 and a body bearing 15 arranged on the body 1 . The rotor lower bearing 14 and the body bearing 15 form a sliding bearing pair and an axial thrust bearing pair.
According to the present disclosure, an axial inner passage 18 is formed inside the body 1 . A passage 22 penetrating the sidewall of the body 1 is arranged in the first region L1. A sealed contact pin 16 is arranged inside the passage 22 , which connects with the windings 20 and extends into the inner passage 18 through an electrical lead 21 . According to the present disclosure, the inner passage 18 can be in form of a blind hole for directly outputting the power generated. The inner passage 18 can also be in form of a step shape through-hole along the axis thereof, under which case, when the generator supplies power to the underground system, the inner passage 18 can also serve as a signal passage passing through the generator.
Although the present disclosure has been described with reference to the preferred embodiments, various modifications can be made to the present disclosure without departing from the scope of the present disclosure and components in the present disclosure could be substituted by equivalents. Particularly, as long as there is no structural conflict, all the technical features mentioned in all the embodiments may be combined together in any manner. These combinations are not exhaustively listed and described in the description merely for saving resources and keeping the description concise and brief. Therefore, the present disclosure is not limited to the specific embodiments disclosed in the description, but includes all the technical solutions falling into the scope of the claims.
|
The present disclosure relates to a downhole rotating magnetic field generator, wherein a stator assembly is formed by fixedly connecting a guiding stator, windings, and a body together, and a rotor assembly is formed by mounting a turbine rotor and a permanent magnet together. Between the stator assembly and the rotor assembly, sliding bearings are arranged and small mud passages are formed. There is no metal isolation between the rotor and the stator for cutting through the magnetic lines of force, so that the eddy current loss is relatively small. Meanwhile, with mud flowing through the passages as lubricant, overheating of the generator can be prevented and high power output can be ensured.
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FIELD
[0001] The present invention relates to a method of downlinking to a downhole tool located in a borehole.
BACKGROUND
[0002] The bottom end of a drillstring has a bottom hole assembly (BHA). The BHA includes a drill bit and typically also sensors, control mechanisms, and associated circuitry. The sensors may measure properties of the formation and of the fluid that is contained in the formation. A BHA may also include sensors that measure the BHA's orientation and position.
[0003] The drilling operation is controlled by an operator at the surface. The drillstring is rotated at a desired rate by a rotary table, or top drive, at the surface, and the operator controls the weight-on-bit and other operating parameters of the drilling process.
[0004] Drilling fluid, or “mud”, is pumped from the surface to the drill bit by way of the drillstring. The mud serves to cool and lubricate the drill bit, and to carry the drill cuttings back to the surface. The density of the mud is carefully controlled to maintain the hydrostatic pressure in the borehole at desired levels.
[0005] In order for the operator to be aware of the measurements made by the sensors in the BHA, and for the operator to be able to control the operation of the drill bit, communication between the operator and the BHA is necessary. A downlink is a communication from the surface to tools comprising part of the drillstring, typically within the BHA. A downlink might typically command a change of parameters for a rotary steerable system, intended to modify the curvature or direction in which the hole is progressing, or the operational parameters of downhole sensing tools. Likewise, an uplink is a communication from the BHA to the surface. An uplink is typically a transmission of the data collected by the sensors in the BHA. For example, the data may provide the BHA orientation. Uplink communications are also used to confirm that a downlink command was correctly understood.
[0006] One common method of communication is called “mud pulse telemetry”. Mud pulse telemetry involves sending signals, either downlinks or uplinks, by creating pressure and/or flow rate pulses in the mud. These pulses may be detected by sensors at the receiving location. For example, in a downlink operation, a change in the flow rate of the mud being pumped down the drillstring may be detected by a sensor in the BHA. The pattern of the pulses may be detected by the sensors and interpreted as a command for the BHA.
[0007] A commonly used technique for downlinking includes timed variation of pump speed. The downhole tool either counts transitions from high speed flow to low speed flow (and vice versa) or measures the time between certain transitions.
[0008] However, pump adjustments made at the surface are not immediately detected downhole. This is a consequence not principally of wave speed, but a combination of pressure drops and fluid compliance. Further, it is usually necessary to ensure that pump speed variations do not lead to changes in surface flow rates or pressure which exceed safety limits
SUMMARY
[0009] Embodiments of the present invention are at least partly based on the recognition that reduced detection times can be achieved by adjusting pump rates to take account of factors such as fluid compliance. The adjusted rates can be arranged to avoid changes in fluid pressure which exceed safety limits.
[0010] Thus a first aspect of the invention provides a method of downlinking to a downhole tool (such as an element of a bottom hole assembly) located in a borehole, wherein the downhole tool detects transitions in the flow velocity of fluid circulating in the borehole at the downhole tool, the method including the steps of:
[0011] (a) pumping fluid into a drillstring to circulate fluid in the borehole at the downhole tool;
[0012] (b) increasing the pumping rate of fluid into the drillstring to a rate which overshoots a steady state pumping rate needed to produce a transition which the downhole tool will detect, or decreasing the pumping rate of fluid into the drillstring to a rate which undershoots a steady state pumping rate needed to produce a transition which the downhole tool will detect; and
[0013] (c) subsequently adjusting the pumping rate of fluid into the drillstring to approach or achieve said steady state pumping rate;
[0014] wherein steps (b) and (c) produce a transition which is detected by the downhole tool.
[0015] Using this method, the transition detected by the downhole tool can be achieved much more rapidly than is possible with conventional flow sequences.
[0016] Typically steps (b) and (c) are performed twice in sequence, firstly for one of overshoot and undershoot, and secondly for the other of overshoot and undershoot. Indeed, steps (b) and (c) can be performed repeatedly to produce corresponding transitions which are detected by the downhole tool.
[0017] As a result of detecting the transition or transitions, the downhole tool may alter its mode of operation.
[0018] Preferably, the increased or decreased pumping rate is optimised within operational limits associated with the borehole to minimise the time required to effect the detected transition. In this way, the fastest transition compatible with safe drilling operations can be achieved.
[0019] The method may include the step of calculating the steady state pumping rate and the increased or decreased pumping rate before performing step (b). For example, the calculation may be based on any one or any combination of: the compliance per unit length of the fluid circulating within the drillstring, the frictional pressure drop in the drillstring, the ratio of the frictional pressure drop at the downhole tool, and a characteristic time for the circulating fluid to respond to changes in pumping rate. Preferably, the calculation is based at least on said characteristic time, and the method further includes the preliminary step of determining said characteristic time by temporarily stopping the pumping of fluid into the drillstring.
[0020] The method may further include the steps of: measuring the surface pressure variation of the fluid after performing steps (b) and (c), comparing the measured pressure variation to a predicted surface pressure variation of the fluid, and adjusting the increased or decreased pumping rate and/or the steady state pumping rate before repeating steps (b) and (c). The adjustment may not necessarily be to the value of, for example, the increased or decreased pumping rate, but may include the period of time that the increased or decreased pumping rate is maintained. Typically the adjustment has the aim of increasing the over- or undershoot if the measured surface pressure variation is lower than predicted, or to decreasing the over- or undershoot if the measured surface pressure variation is higher than predicted. Further aspects of the invention respectively provide a computer system, a computer program and a computer program product which correspond to the method of the first aspect. Moreover, optional features of the first aspect result in corresponding optional features of these further aspects.
[0021] Thus, a second aspect of the invention provides a computer system for controlling a pumping system that pumps fluid into a drillstring to circulate fluid to a downhole tool located in a borehole, and being operable to effect transitions in the flow velocity of the circulating fluid which are detectable at the downhole tool to enable downlinking to the downhole tool;
[0022] the system being adapted to calculate:
[0023] (a) a steady state pumping rate into the drillstring needed to produce a transition which the downhole tool will detect, and
[0024] (b) either an increased pumping rate of fluid into the drillstring which overshoots said steady state pumping rate, or a decreased pumping rate of fluid into the drillstring which undershoots said steady state pumping rate;
[0025] the system further being adapted to issue control signals for controlling the pumping system to:
[0026] (i) adjust the pumping rate to said increased or decreased pumping rate, and
[0027] (ii) subsequently adjust the pumping rate of fluid to approach or achieve said steady state pumping rate;
[0028] wherein, in use, the adjustments produce a transition which is detectable by the downhole tool.
[0029] The system may be adapted to perform further calculations and to issue corresponding further control signals for controlling the pumping system, so that further transitions can be produced which are detectable by the downhole tool.
[0030] The system may be adapted to receive operational limits associated with the borehole, and the calculated increased or decreased pumping rate can be optimised within said operational limits to minimise the time required to effect the detectable transition.
[0031] A third aspect of the invention provides a pumping system for a borehole, the pumping system having the computer system according to the second aspect for enabling downlinking to a downhole tool located in the borehole.
[0032] A fourth aspect of the invention provides a computer program for controlling a computer-controlled pumping system that pumps fluid into a drillstring to circulate fluid to a downhole tool located in a borehole, and being operable to effect transitions in the flow velocity of the circulating fluid which are detectable at the downhole tool to enable downlinking to the downhole tool;
[0033] the computer program, when executed, calculating:
[0034] (a) a steady state pumping rate into the drillstring needed to produce a transition which the downhole tool will detect, and
[0035] (b) either an increased pumping rate of fluid into the drillstring which overshoots said steady state pumping rate, or a decreased pumping rate of fluid into the drillstring which undershoots said steady state pumping rate;
[0036] the computer program, when executed, further issuing control signals for controlling the pumping system to:
[0037] (i) adjust the pumping rate to said increased or decreased pumping rate, and
[0038] (ii) subsequently adjust the pumping rate of fluid to approach or achieve said steady state pumping rate;
[0039] wherein, in use, the adjustments produce a transition which is detectable by the downhole tool.
[0040] A fifth aspect of the invention provides a computer program product carrying the computer program of the fourth aspect.
BRIEF DESCRIPTION OF THE DRAWINGS
[0041] Embodiments of the invention will now be described by way of example with reference to the accompanying drawings, in which:
[0042] FIG. 1 shows surface flow rates against time for a conventional downlinking flow sequence (dashed line) and a downlinking flow sequence according to an embodiment of the present invention (solid line);
[0043] FIG. 2 shows predicted flow rates against time at a downhole tool for the conventional downlinking flow sequence (dashed line) and the downlinking flow sequence according to an embodiment of the present invention (solid line) of FIG. 1 ;
[0044] FIG. 3 shows predicted surface pressure against time for the conventional downlinking flow sequence (dashed line) and the downlinking flow sequence according to an embodiment of the present invention (solid line) of FIG. 1 ; and
[0045] FIG. 4 shows schematically a well having a computerised control system for controlling surface pumps during downlinking, in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
[0046] In order to optimise the amount of overshoot or undershoot to improve downlink times it is helpful first to estimate parameters associated the borehole so that the effects downhole of surface flow changes can be modelled.
[0047] The compliance per unit length Λ of the fluid circulating within the drillstring is generally known, or varies only within a defined range. The compliance per unit length of the fluid is the cross sectional area of the fluid within the drillstring, divided by the bulk modulus of the fluid. For a water based drilling fluid, and a pipe with a mean inner radius of 2 inches (50.8 mm), the compliance will be roughly 4×10 −12 Pa −1 per meter of drillstring. Oil based drilling fluids are generally 25% to 50% more compliant than water based drilling fluids.
[0048] Over most conditions encountered in practice, the frictional pressure drop in the drillstring and the frictional pressure drop at the downhole tool are proportional to the flow velocity squared. α, the ratio of the frictional pressure drop in the drillstring (in one direction) to the flow velocity squared, and β, the ratio of the frictional pressure drop through the downhole tool (e.g. the BHA and drill bit) to the flow velocity squared, are, therefore, generally known or can be determined by techniques familiar to the skilled person.
[0049] Formulae for frictional pressure drops along a drillstring can be found in references such as Bourgoyne, Millheim, Chenevert and Young, Applied Drilling Engineering , SPE Textbook series, volume 2, 1986, p. 147.
[0050] Typically, the bit pressure drop is close to one half of the fluid density, times the square of the fluid velocity through the bit nozzles. Appropriate formulae for other BHA components with significant pressure drops are normally supplied in the component specification sheets.
[0051] Approximate solutions can be found to following equations (1) and (2) and boundary condition (3) that describe the variation of fluid volumetric flow rate and pressure along the drillstring with time at low frequencies.
[0000]
∂
v
∂
x
=
-
λ
∂
P
∂
t
(
1
)
∂
P
∂
x
=
-
f
1
2
v
2
(
2
)
P
(
L
)
=
β
1
2
v
(
L
)
2
(
3
)
[0000] where v if the volumetric flow rate, P is the pressure, is the compliance per unit length, and f is a friction coefficient. The distance along the drillstring from the top is x, the time variable t, and the total drillstring length L. n terms of the parameter, for a constant cross-section drillstring:
[0000] fL=α (4)
[0052] Expressions (1) to (3) can be solved exactly for abrupt changes in the flow rate at surface, if the constant is zero. Using this exact solution, a series expansion solution in powers of ( ˜ )can be iteratively derived, yielding an expression (5) for a characteristic time τ for the circulating fluid to respond to changes in flow velocity:
[0000]
T
=
τ
2
(
1
+
α
2
β
+
1
c
)
(
5
)
[0000] where T is the time for the flow at the downhole tool to reach zero on cessation of pumping of fluid into the borehole, and c is the real solution to the following equation:
[0000]
0
=
c
(
1
-
c
)
-
(
α
β
)
(
c
2
2
-
c
3
3
+
c
4
12
)
+
(
α
β
)
2
(
c
3
12
-
c
4
12
+
c
5
36
-
c
6
252
)
-
(
α
β
)
3
(
c
4
72
-
c
5
63
+
5
c
6
672
-
5
c
7
3024
+
c
8
6048
)
+
(
α
β
)
4
(
c
5
504
-
25
c
6
9072
+
29
c
7
18144
-
c
8
2016
+
c
9
12096
-
c
10
157248
)
(
6
)
[0053] For a given borehole and downhole tool, T is proportional to the mean flow rate of fluid on which the variations are to be superimposed. Having determined Λ, α, β and τ, a pump flow sequence can be established. One approach is to model the fluid system as a series of n sections in series, at each section the difference between the fluid flow out of and into the section being balanced by the product of the fluid compliance within the section and the pressure change across the section. This is a numerical approximation to the set of analytic equations (1) to (3). The flow can be non-dimensionalised by dividing by the higher of the start and end flow of the pump sequence. Further, time can be expressed in terms of the characteristic time τ.
[0054] This approach provides a set of n differential equations which can be solved by iterative simulation.
[0055] The pressure drop along the pipe, instead of being regarded as a continuous pressure drop with length, is modelled as a set of discrete pressure drops along the drillstring. Between these pressure drops, the volume flow rate and pressures will be the same. Thus instead of continuous volume flow rate and pressures variables, if there are n pressure drops, there will be n+1 different flow rates in the different sections, and similarly there will be n+1 different pressures.
[0056] Using equations (2) and (3), the pressures may be written in terms of the volume flow rates, thus for example:
[0000]
P
(
L
)
=
β
1
2
v
(
L
)
2
(
7
)
[0000]
P
(
(
n
-
1
)
L
n
)
=
P
(
L
)
+
fL
2
n
v
(
(
n
-
1
)
L
n
)
2
=
β
1
2
v
(
L
)
2
+
fL
2
n
v
(
(
n
-
1
)
L
n
)
2
(
8
)
P
(
(
n
-
2
)
L
n
)
=
P
(
(
n
-
1
)
L
n
)
+
fL
2
n
v
(
(
n
-
2
)
L
n
)
2
=
β
1
2
v
(
L
)
2
+
fL
2
n
v
(
(
n
-
1
)
L
n
)
2
+
fL
2
n
v
(
(
n
-
2
)
L
n
)
2
(
9
)
[0000] etc.
[0057] Substituting into equation (1), and integrating gives:
[0000]
v
(
L
)
-
v
(
(
n
-
1
)
L
n
)
=
-
1
n
Bv
(
L
)
v
(
L
)
t
(
10
)
v
(
(
n
-
1
)
L
n
)
-
v
(
(
n
-
2
)
L
n
)
=
-
1
n
Bv
(
L
)
v
(
L
)
t
-
1
n
Av
(
(
n
-
1
)
L
n
)
t
v
(
(
n
-
1
)
L
n
)
(
11
)
v
(
(
n
-
2
)
L
n
)
-
v
(
(
n
-
3
)
L
n
)
=
-
1
n
Bv
(
L
)
v
(
L
)
t
-
1
n
Av
(
(
n
-
1
)
L
n
)
t
v
(
(
n
-
1
)
L
n
)
-
1
n
Av
(
(
n
-
2
)
L
n
)
t
v
(
(
n
-
2
)
L
n
)
(
12
)
[0000] etc.
[0058] The constants A and B which appear in the equations are given by:
[0000]
A
=
α
2
β
+
α
and
B
=
2
β
2
β
+
α
(
13
)
[0059] The number of sections necessary to model the actual flow depends on the ratio of A to B. Taking (n−1) as the smallest integer greater than A/B has been found to give good results.
[0060] The differential equations are discretised, with the surface flow rate, v( 0 ), at time zero set to a changed flow from the pumps, and the flow rate in the rest of the system at time zero being set at an initial value which typically corresponds to a steady state flow circulating through the system before the flow from the pump is changed. The discretised equations are then integrated in time, with an integration step of 1% of the characteristic time, τ, being sufficiently small to generally provide accurate results.
[0061] We have found that typically the fastest way to achieve a flow reduction transition downhole is to reduce the flow rate into the borehole as low as permitted, and then to bring the flow back to the level corresponding to steady state flow at the reduced flow rate. In order to optimise this transition, the time over which the flow into the borehole undershoots the steady state flow at the reduced flow rate is adjusted so that the flow downhole does not quite go below the reduced flow rate for the transition.
[0062] Similarly, for a flow increase transition downhole, the flow into the borehole is initially adjusted to as high a level as permitted, and then brought back to the level corresponding to steady state flow at the increased flow rate. Again, for an optimal transition, the time over which the flow into the borehole overshoots the steady state flow at the increased flow rate is adjusted so that the flow downhole does not quite go above the increased flow rate for the transition.
[0063] FIG. 1 shows surface flow rates against time for a conventional downlinking flow sequence (dashed line) and a downlinking flow sequence according to the present invention (solid line). In the conventional sequence, the flow is reduced to 75% of the initial level, held at that level and then increased to 100% of the initial level. In the flow sequence according to the present invention, the flow reduction transition is replaced by an undershoot to 50% of the initial level before increasing to the 75% steady state level for the reduced flow, and the flow increase transition is replaced by an overshoot to the 125% level before reducing to the 100% steady state level for the increased flow.
[0064] The surface flow rates of FIG. 1 were used in the iterative simulation described above. FIG. 2 shows predicted flow rates against time at the downhole tool for the conventional downlinking flow sequence (dashed line) and the downlinking flow sequence according to the present invention (solid line), and FIG. 3 shows predicted surface pressure against time for the conventional downlinking flow sequence (dashed line) and the downlinking flow sequence according to the present invention (solid line). The simulation assumed a drillstring pressure drop equal to the downhole tool pressure drop (i.e. α equal to β), and used a two pressure drop model, (i.e. n=2, and a set of three equations that was solved numerically).
[0065] From FIG. 2 , it is evident that the target downhole flow rates for both the flow reduction and flow increase transitions are achieved much more rapidly for the downlinking flow sequence using the undershoot and overshoot than for the conventional flow sequence.
[0066] FIG. 3 shows that despite the much larger changes in surface flow rates associated with the downlinking flow sequence using the undershoot and overshoot, the surface pressures do not drop excessively below (in the case of the undershoot) or excessively above (in the case of the overshoot) the steady state surface pressures at respectively the 75% and 100% flow levels. This is particularly significant in relation to the overshoot, as drilling operators generally aim to avoid upward pressure spikes which they associate with dangerous drilling conditions that might fracture underground formations or exceed the pressures ratings of components in the surface hydraulic system.
[0067] A computerised control system may be provided which calculates optimal downlinking transitions by applying Λ, α, β and τ for a particular borehole to the iterative simulation described above, the simulation taking account of site-specific factors, such as minimum and maximum acceptable surface flow rates and pressures. The system can then be used to automatically control surface pumps during downlinking.
[0068] Furthermore, having downlinked, the actual surface pressure can be measured and compared to the predicted values, and adjustments made to the downlinking parameters, either to increase the over or undershoot if the actual surface pressure variations are lower than predicted, or to decrease the over or undershoot if the actual surface pressure variations are higher than predicted.
[0069] FIG. 4 shows schematically a well having such a computerised control system. Mud pumps 2 , under the control of computer 1 , pump drilling fluid through surface pipework 3 connected to a drillstring 9 in well borehole 12 . A BHA 11 at the downhole end of the drillstring comprises components such as a measurement-while-drilling transmitter 5 , a logging-while-drilling tool 6 and a rotary steerable system 7 . The BHA connects to a bit 8 . As indicated by the arrows, drilling fluid flows down through the drillstring 9 , the BHA 11 , the bit 8 and back up to the surface through annulus 10 . As described above, computer 1 downlinks to the BHA 11 by controlling the pumping rate of mud pumps 2 to produce transitions which are detected by the BHA 11 .
[0070] While the invention has been described in conjunction with the exemplary embodiments described above, many equivalent modifications and variations will be apparent to those skilled in the art when given this disclosure. Accordingly, the exemplary embodiments of the invention set forth above are considered to be illustrative and not limiting. Various changes to the described embodiments may be made without departing from the spirit and scope of the invention.
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A method of downlinking to a downhole tool located in a borehole is provided. The downhole tool detects transitions in the flow velocity of fluid circulating in the borehole at the downhole tool. To provide for the detection of the transitions fluid is pumped into the drillstring so that it circulates in the borehole at the downhole tool and the pumping rate of fluid into the drillstring is either increased to a rate which overshoots a steady state pumping rate needed to produce a transition or is decreased to a rate which undershoots a steady state pumping rate needed to produce a transition.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a method for bounce suppression of a valve member operated by a piezo actuator during the closing phase in an internal combustion engine and a corresponding device for carrying out the method.
[0003] 2. Description of Related Art
[0004] In internal combustion engines, especially in Otto and Diesel engines, valves control the intake and the discharge of the combustion gases, the valve opening and closing times having a considerable influence on the power output, on the fuel consumption, on low-pollutant combustion and on the running properties of the internal combustion engine at a specified rotational speed. These valves are usually developed as flat-seat valves, in the closed state of the valve, a valve member being accommodated with its valve disk in a valve seat in a precisely fitting and sealing manner. To open the valve, the valve disk is lifted off from the valve seat, and in this context, an annular gap opens, through which the combustion gas is able to flow. The flat-seat valve is driven via the valve spindle, which is a part of the valve member. In modern engines, in order to open and close the valves, piezo actuators are used, which open and close again a valve at high speed. In particular during rapid closing of the flat-seat valve, the valve disk bumps into the valve seat, the sealing surfaces of the two elements striking each other. At higher closing speeds, the impact of the valve disk onto the valve seat leads to an elastic bump, as a result of which the flat-seat valve does not close abruptly, but rather opens slightly and closes again several times after the first closing. This impacting impairs the precision of the closing process, and thereby influences the abovementioned properties of the internal combustion engine in an undesired way. Furthermore, the impacting of the valve disk on the valve seat leads to rapid material wear. In particular, the exhaust valve of an internal combustion engine is especially exposed to corrosive conditions, because the sealing surfaces on the valve disk and the valve seat are exposed to high temperatures and the corrosive effects of the hot and combusted combustion gases.
BRIEF SUMMARY OF THE INVENTION
[0005] The present invention provides a method for bounce suppression of a valve member operated by a piezo actuator during the closing phase in an internal combustion engine and a corresponding device for carrying out the method.
[0006] According to the present invention, the piezo actuator is electronically controlled in such a way that, during the closing process, first of all it absorbs the kinetic energy of the valve member shortly before impact, is thereby deformed itself, generates a charge internally, and with that, it increases its restoring force. Even before the piezo actuator goes over into the elastic rebound phase, the charge built up internally in the piezo actuator is dissipated, so that the valve member is finally damped by an inelastic bump upon impact and guided into the valve seat having lower kinetic energy, where the valve disk then remains, without the undesired bouncing motion.
[0007] The method according to the present invention, during the closing phase, includes the steps: partial discharging of the piezo actuator, whereby the valve member is braked even before reaching the valve seat, interruption of the discharge of the piezo actuator, whereby the piezo actuator is upset by the valve member and builds up an electric charge, renewed discharging of the piezo actuator, a residual charge remaining in the piezo actuator is at least partially dissipated after partial discharge and the charge built up during the charge interruption. The method, according to the present invention, for bounce suppression of a valve member operated by a piezo actuator, during the closing phase in an internal combustion engine, also includes an interruption of the discharge process of the piezo actuator during closing of the valve, the selection of the points in time of the start of the interruption and the end of the interruption being significant for optimum bounce suppression.
[0008] In the embodiment of the present invention, it is alternatively also possible to repeat the process within a valve-closing cycle once or several times, whereby the valve member is returned into the valve seat in a stuttering manner. Each discharge process is interrupted in a controlled manner, in this context. During the respective interruption times, the valve member has a closing speed determined by the interruption time period, and this speed, as well as the mass of the valve member, determine the kinetic energy of the valve member. Beginning at the time of the interruption, the valve member, which is connected in a directly or indirectly force-locking manner to the piezo actuator, is braked via the elastic effect of the piezo actuator. During the braking, the piezo actuator is deformed by the impulse of the valve member, and in the process, the piezo crystal in the piezo actuator builds up a charging voltage which increases the restoring force of the piezo crystal. Even before the piezo crystal gets into the back swing, and therefore acts itself as an impact surface instead of the valve seat, the charge built up in the piezo actuator is discharged. Because of the discharge, the piezo actuator, that is mechanically stressed by the kinetic energy of the valve member, loses its restoring force, whereby the elastic back swing does not take place. This being the case, during the interruption of the discharge, the piezo actuator acts like an impact- cushion, in which the kinetic energy is converted into deformation energy and is dissipated.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0009] In the following, the present invention is explained in detail with reference to the attached drawings. The figures show:
[0010] FIG. 1.1 shows a diagram of the charging voltage curve of an undamped piezo actuator over one valve cycle.
[0011] FIG. 1.2 shows a diagram of the charging current and discharging current of an undamped piezo actuator over the same valve cycle.
[0012] FIG. 1.3 shows a diagram of the valve lift of an undamped piezo actuator over one valve cycle.
[0013] FIG. 2.1 shows a diagram of the charging voltage curve of a piezo actuator using the method according to the present invention for bounce suppression.
[0014] FIG. 2.2 shows a diagram of the charging current and the discharging current of a piezo actuator over the valve cycle according to FIG. 2.1 .
[0015] FIG. 2.3 shows a diagram of the valve lift having bounce suppression according to the present invention.
[0016] FIGS. 3 . 1 - 3 . 6 show a diagram for clarifying the automatic setting of the discharge interruption times.
[0017] FIG. 4 shows a block diagram of a simple device for charging, and discharging according to the present invention, a piezo actuator.
[0018] FIG. 5 shows a block diagram of a control device as an additional embodiment of the device according to FIG. 4 .
DETAILED DESCRIPTION OF THE INVENTION
[0019] FIG. 1 shows a diagram of the curve over time of charging voltage U p of a piezo actuator over a valve cycle Z along time t. Starting at time a in the diagram in FIG. 1.3 , at which the piezo actuator is not charged and the valve is closed, valve lift h v at time a thus amounting to zero, charging current I p begins to flow, according to the diagram in FIG. 1.2 . Charging current I p flows as a constant current from time a to time b. Within this time interval a-b, the piezo actuator builds up charging voltage U p at time b in the diagram in FIG. 1.1 . Because of the unbraked extension, and because of the masses connected with force-locking to the piezo actuator, the valve member still vibrates back and forth about the opening point at time b and shortly thereafter, according to the diagram in FIG. 1.3 . This mechanical vibration is reflected in charging voltage U p in charging voltage diagram in FIG. 1.1 . The valve, now opened, remains in the open position of time b until time c. Within this time interval b-c, neither valve lift h v , nor charging voltage U p , nor charging current and discharging current I p changes, apart from the slight mechanical vibrations of valve lift h v mentioned at the outset, and charging voltage U p corresponding to it. At time c, the piezo actuator is discharged by negative current pulse I p , which sets in at time c ( FIG. 1.2 ), from time c to time d. Within this time interval c-d, valve lift h v follows the negative leg in FIG. 1.3 between times c and d. At time d, according to the diagram in FIG. 1.3 , the valve member arrives at lift height zero, which means the same as the impact of the valve disk on the valve seat, where it is then bumped back elastically against the restoring force of a valve spring or of the piezo actuator, and still strikes several times and is thrown back elastically, until this bouncing vibration has ebbed out at point e in the diagram in FIG. 1.3 This bouncing vibration taking place-after the closing is reflected in the curve of charging voltage U p of the piezo actuator in the diagram in FIG. 1.1 . It is the subject matter of the present invention to suppress this bouncing vibration between times d and e after the end of the discharge process.
[0020] FIGS. 2.1 , 2 . 2 and 2 . 3 show the corresponding curve of charging voltage U p of the piezo actuator in FIG. 2.1 , the curve of the discharge current in FIG. 2.2 and valve lift h v over a valve cycle Z, the discharge of the piezo actuator being interrupted according to the present invention. The interruption is shown on the right side of the diagram in FIG. 2.2 . The valve cycle begins at time f, as in FIGS. 1.1 , 1 . 2 and 1 . 3 at point a, and runs via time g to time h. At this point, cycle part f-g-h in FIGS. 2.1 , 2 . 2 and 2 . 3 does not differ from cycle part a-b-c in FIGS. 1.1 , 1 . 2 and 1 . 3 . Beginning at point h, the discharge process of the piezo actuator begins by a first negative discharge current pulse according to the diagram in FIG. 2.2 of time h to time i. Within this time interval h-i, charging voltage U p of the piezo actuator drops off to approximately one-half to one-third of the maximum charging voltage, according to the diagram in FIG. 2.1 . In a corresponding manner, valve lift h v in FIG. 2.3 also decreases to about one-half to one-third of the maximum lift. At this point, at time i, discharge current I p ( FIG. 2.2 ) is interrupted. Following this, the piezo actuator is not discharged any further, and, from now on, it is further deformed by the kinetic energy of the valve member. Because of the deformation, that is, the further upsetting by the braked valve member mass, the piezo actuator builds up charge and increases its charging voltage U p in time interval i to j ( FIG. 2.1 ). This increase in charging voltage U p increases the restoring force of the piezo actuator, whereby the valve member is braked increasingly more strongly. Thus, the piezo actuator absorbs the kinetic energy of the valve member. The energy absorption is limited by the capacitance of the piezo actuator, that is, the maximum possible charging buildup within the piezo actuator. If this is sufficient to stop the valve completely for a while, then at this point the mechanical stress and the charging of the piezo actuator would lead to the piezo actuator carrying out a back swing during the reduction of the mechanical stress and the reduction of the internal charge. But, exactly at this point, at time j, the internal charge of the piezo actuator is dissipated by a renewed discharge current pulse ( FIG. 2.2 ) in time interval j-k, so that the back swing is prevented. Between time j and k, the valve member is again brought to a reduction in the valve lift, by the discharge of the piezo actuator. Depending on the intensity of the renewed acceleration or the kinetic energy still residually bound in the valve member, this renewed discharge and the renewed return stroke lead to a gentler impact of the valve disk onto the seat, without one or more rebounds taking place on account of this.
[0021] FIGS. 3.1 , 3 . 2 , 3 . 3 , 3 . 4 , 3 . 5 and 3 . 6 show how a device for bounce suppression finds the right time of the interruption of the charging process and the right time for a renewed discharge of the piezo actuator. On this matter, FIG. 3.1 shows a set of diagrams of four curves of charging voltage U p of the piezo actuator, curve 1 in FIG. 3.1 being associated with the discharge diagram in FIG. 3.2 , curve 2 being associated with the discharge diagram in FIG. 3.3 , curve 3 being associated with the discharge diagram in FIG. 3.4 and curve 4 being associated with the discharge diagram in FIG. 3.5 . The valve lift corresponding to the curves is shown i the diagram in FIG. 3.6 .
[0022] Beginning with curve 1 in FIG. 3.1 , the first discharge process, that is not yet optimized, starts at time 1 and the discharge pulse lasts until time o, according to FIG. 3.2 . Because of this long discharge pulse, the valve member builds up a high kinetic energy and upsets the piezo actuator, that is for the most part discharged, up to a maximum upset and up to the maximum charge buildup possible from this level of mechanical stress of the piezo actuator, corresponding to charging voltage U p . The renewed energy-absorbing charge buildup is too small, however, to soften the kinetic energy of the valve member. It is therefore necessary to shorten the first discharge pulse, so that the charge still possible to be built up by upset of the piezo actuator, at the end of the first discharge pulse, is raised to a minimum level. In this non-optimized discharge process according to curve 1 in FIG. 3.1 , a new discharge pulse begins only at time r, by which charging voltage U p , which was formerly at a stable level in time, is decreased. This level in time interval p-r is specifically to be avoided, however, and is therefore detected by a control electronics system, and the first discharge pulse is thereupon shortened in the next valve cycle.
[0023] During the next valve cycle, the discharge process begins again at time 1 , but is interrupted earlier than at time o, namely, at time n. The charge buildup then taking place in curve 2 , after time n, is correspondingly greater than after time o in curve 1 , because the piezo actuator still has sufficient capacitance for charge buildup and for mechanical upsetting. Thereafter, the same circumstances set in while a plateau in time forms in charging voltage U p , as in curve 1 of charging voltage U p .
[0024] In a still later valve cycle, the discharge diagram is shown in FIG. 3.4 , the curve of charging voltage U p is shown in curve 3 in FIG. 3.1 , charging voltage U p rises, beginning at time m, to the level at time o in FIG. 3.1 , after the discharge current has been interrupted at time o. This charge buildup, represented by the rise in charging voltage U p in curve 3 , is now great enough to absorb the kinetic energy bound to the valve member, the amount of the sufficient kinetic energy being predetermined, and cannot be derived from the diagram of the charging voltage curve itself.
[0025] In order to suppress the development of the level remaining the same in time, the second discharge pulse is advanced, at this point, to such an extent that directly after the maximum buildup of the charging voltage at time o, curve 4 in FIG. 3.1 and discharge diagram 3 . 5 , the renewed discharge of the piezo actuator begins, and charging voltage U p drops off again immediately to a minimum.
[0026] During the optimizing phase, the curves of valve lifts h v do not differ greatly from one another. The stress absorbed by the piezo actuator, however, does differ. In response to the optimized discharge, the piezo actuator is stressed in the elastic range and is destressed again.
[0027] FIG. 4 finally shows a device 10 , according to the present invention, for discharging a piezo actuator P, which has a charge/discharge switch S 1 and a switch S 2 for interrupting the charging process. During discharge of piezo actuator P by switch S 1 , switch S 2 interrupts the charging process, in order to damp the impact of the valve member. Alternatively, instead of using two switches S 1 and S 2 , it is also possible to use a single switch having 3 states, which charges piezo actuator P in a first state, is highly resistive in the second state and discharges piezo actuator P in a third state.
[0028] As is shown in FIG. 5 , for the automatic setting of the times of the discharge current pulse, a control device 20 is used in the embodiment of device 10 which monitors the charging voltage of piezo actuator P. Control device 20 for controlling a piezo actuator P for a valve member in an internal combustion engine has the following components to do this: at least one variable timing element 21 for setting a point in time for interrupting the discharge process of piezo actuator P, at least one variable timing element 22 for setting a point in time for renewed charging after interrupting the discharge of piezo actuator P, at least one device 25 for measuring the charging voltage of piezo actuator P, at least one device 24 for storing the measured data and at least one device 23 for the automatic variation of the time elements.
[0029] For the setting of the discharge current times, control device 20 detects a rise in the charging voltage of piezo actuator P after the interruption of the first discharge current, and measures the height of the charging voltage rise. Only when the height of the charging voltage rise reaches or exceeds a predetermined value does control electronics 20 control the point in time of the renewed discharge pulse, control device 20 in this case detecting a plateau development over time, and advancing in time the second discharge pulse in successive valve cycles until the plateau development of the charging voltage fails to appear. In order to set the two points in time, control device 20 controls the points in time according to the following strategy: First, the setting of the time of the first interruption takes place after a partial discharge by control device 20 , so that the interruption takes place so late that the upsetting of piezo actuator P, taking place after the interruption, is so slight that the accompanying charge buildup falls below a specified value. This ensures that control device 20 does not close the valve member at too early a closing time. Then the setting of the time of the renewed discharge by control device 20 begins so that the renewed discharge takes place so late that the charge of piezo actuator P, built up by upsetting, does not change over a specified time interval. A plateau over time is detected by this, which is minimized in the subsequent control cycle. From this non-optimal state, the control device controls the point in time again by the subsequent adjustment of the point in time of the interruption after a partial discharge, until it has been advanced in time so far that the charge buildup reaches or exceeds a specified value. Only after that does the adjusting of the point in time of the renewed discharge take place, until it has been advanced so far that the charge of the piezo actuator, built up by the upsetting, changes within a specified time interval by a specified amount, so that no plateau formation over time is detected.
[0030] Control device 20 used for the control, in an advantageous manner has a device which detects the impact of the valve member, preferably via the monitoring of the charging voltage after the discharge of piezo actuator P. When an impact is detected, control device 20 is activated for setting the discharge time, and if no further impact is detected, control device 20 is deactivated.
[0031] For the implementation of control device 20 , a microcontroller 23 may be used or a control electronics system, the input of the control devices being the charging voltage and the output being a signal for triggering the discharge process.
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A method for bounce suppression of a valve member operated by a piezo actuator during the closing phase of a valve in an internal combustion engine, having the following steps: partial discharging of the piezo actuator, whereby the valve member is braked even before reaching the valve seat, interruption of the discharge of the piezo actuator, whereby the piezo actuator is upset by the valve member and builds up an electric charge, renewed discharging of the piezo actuator, the residual charge after partial discharge and the charge built up during the charge interruption being at least partially dissipated. It is provided, according to the present invention, briefly to interrupt the discharge process, whereby the piezo actuator absorbs the energy of the valve member and, even before an elastic rebound takes place, the piezo actuator is discharged again, in order to dissipate the energy absorbed by the piezo actuator.
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TECHNICAL FIELD
[0001] This invention relates to damping the vibrations of a wind turbine blade. More specifically, this invention relates to an element for damping the edgewise vibrations of a wind turbine blade, a wind turbine blade including the element, and a method for damping edgewise vibrations with the element.
BACKGROUND
[0002] Long slim structures, such as wind turbines, will always sway in the wind. From an engineering viewpoint, swaying is the first fundamental vibration shape. Vibration shapes can occur in many different forms and at many different speeds, or more precisely frequencies. These frequencies are often called the natural frequencies, and each corresponds to a particular vibration shape.
[0003] Two major types of natural vibrations (i.e., resonant oscillations) associated with the blade of a wind turbine are flapwise and edgewise vibrations. Flapwise vibrations occur in a plane perpendicular to the leading and trailing edges of the blade. Edgewise vibrations occur in a plane through the leading and trailing edges. Both types of vibrations place significant loads on the blade that can intensify fatigue damage and lead to failure. Therefore, it is important to avoid exciting these vibrations, and/or damping these vibrations once being excited.
[0004] Edgewise vibrations refer to blade vibrations in the general direction of the chord of the airfoil of the blade and are characterized by a slender blade cross section in the direction of the vibration movement, so there is almost no air resistance force to dampen the movement once started, as contrasted with a flapwise movement which has relatively large aerodynamic damping. Thus, the natural damping of edgewise vibrations is very weak and consequently it takes a long time for the vibrations to dissipate. In some cases, the vibrations can even be perpetually self-sustaining or unstable (i.e., ever increasing until fracture of the blade).
[0005] To prevent, or at least reduce the likelihood of, such an outcome, it is desirable to dampen edgewise vibrations through some other mechanism or physical principle. In this regard, several ways to dampen edgewise vibrations of a structural blade have been developed. For example, WO 95/21327 discloses a blade having an oscillation-reduction element oriented in the direction of unwanted oscillations. The oscillation-reduction elements disclosed therein are tuned liquid dampers. These dampers are specifically designed (i.e., “tuned”) to have a natural frequency substantially corresponding to the dominating natural frequency of the blade. As such, their effectiveness at damping vibrations is frequency-dependent. They also typically require maintenance and can be difficult to access and install. Passive dampers are also known. One example of a passive damper is disclosed in WO 99/43955. However, because passive dampers are typically difficult to design and implement, the number of adequate solutions developed has been limited.
[0006] Accordingly, there remains a need for improvement in damping and controlling unwanted vibrations in wind turbine blades. More particularly, there is a need for an apparatus and method for damping edgewise vibrations in wind turbine blades in a manner that overcomes the drawbacks of existing apparatus and methods.
SUMMARY
[0007] This invention in one embodiment is a blade for a wind turbine. The blade generally includes a shell body, an inner spar supporting at least a portion of the shell body, and a damping element coupled to the inner spar. The damping element is configured to adjust the principal axes of the blade relative to the shell body to dissipate vibrations of the blade.
[0008] Different embodiments of the damping element are disclosed as examples. The term “damping element” refers to some or all of these embodiments, together with equivalents to such embodiments. The damping element may include, for example, an element coupled to the inner spar in a variety of different orientations and/or configurations.
[0009] In one of the various embodiments of this invention, a blade for a wind turbine includes a shell body with a leading edge and a trailing edge. A chord of the shell body extends between the leading and trailing edges. A spar is located within the shell body and supports at least a portion of the shell body. The spar has a generally tubular configuration over at least a portion of its length. In one embodiment, a damping element is coupled to the spar and contained within the tubular configuration of the spar and extends less than the entire length of the spar. The damping element is configured to orient a structural pitch of the blade obliquely relative to the chord so as to reduce edgewise vibrations of the blade. The damping element may have a generally linear or an arcuate cross-sectional configuration. The tubular configuration of the spar may have a generally rectangular cross section with a pair of spaced first walls each oriented generally parallel to the chord and joined at four corners to a pair of spaced second walls, each oriented generally perpendicular to the chord. In one embodiment, the damping element extends diagonally across the rectangular cross-section of the spar between a pair of the corners.
[0010] There may be a single damping element in the blade or a plurality of damping elements coupled to the blade. Additionally, the damping element may be at least partially formed with the blade or separately attached thereto. As such, the invention provides a stand-alone damping element in addition to a wind turbine blade incorporating such an element. The stand-alone damping element may be coupled to the inner spar or to only a portion of the spar to dissipate vibrations of the blade.
[0011] Finally, a wind turbine incorporating the blade and damping element is also provided, along with a method of dissipating edgewise vibrations in the blade of such a wind turbine. Thus, the method involves operating the wind turbine so that the blade experiences edgewise vibrations. In response, the damping element dissipates or dampens vibrations primarily in the flapwise direction.
[0012] This invention in other embodiments includes the ability to retrofit a wind turbine blade to include a damping element according to various embodiments to address and dampen edgewise vibrations.
[0013] These and other aspects will be made more apparent by the detailed description and claims below, as well as by the accompanying drawings. Note that when describing the same type of elements, numerical adjectives such as “first” and “second” are merely used for clarity. They are assigned arbitrarily and may be interchanged. As such, the use of these adjectives in the claims may or may not correspond to the use of the same adjectives in the detailed description (e.g., a “first element” in the claims might refer to any such “element” and not necessarily the ones labeled “first” in the detailed description below).
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The objectives and features of the invention will become more readily apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
[0015] FIG. 1 is a perspective view of one embodiment of a wind turbine;
[0016] FIG. 2 is a perspective view of a blade on the wind turbine of FIG. 1 ;
[0017] FIG. 3 is a sectional view taken along line 3 - 3 in FIG. 2 ;
[0018] FIG. 4 is a sectional view similar to FIG. 3 showing one example of a damping element;
[0019] FIGS. 4A-4B are sectional views similar to FIG. 4 showing alternative embodiments of a damping element;
[0020] FIG. 5 is a view similar to FIG. 2 with a portion of the shell body broken away to expose the spar; and
[0021] FIG. 6 is an enlarged view of the spar shown in phantom lines and a damping element of FIG. 5 .
DETAILED DESCRIPTION
[0022] FIG. 1 shows one embodiment of a wind turbine 10 . The wind turbine 10 generally includes a tower 12 , a nacelle 14 supported by the tower 12 , and a rotor 16 attached to the nacelle 14 . The rotor 16 includes a hub 18 rotatably mounted to the nacelle 14 and a set of blades 20 coupled to the hub 18 . More specifically, each blade 20 includes a root 22 coupled to the hub 18 and a tip 24 spaced from the hub 18 . The blades 20 convert the kinetic energy of the wind into mechanical energy used to rotate the shaft of a generator (not shown), as is conventional. However, as will be described in greater detail below, one or more of the blades 20 are specially designed to reduce certain vibrations that create loads and increase the potential of damage or failure.
[0023] FIGS. 2 and 3 schematically illustrate one of the blades 20 in further detail. The blade 20 , in one embodiment, includes a shell body 26 extending between a leading edge 30 and a trailing edge 32 and forming an airfoil cross section. A chord 34 ( FIG. 3 ) extends between leading edge 30 and trailing edge 32 . An inner spar 36 extends from the root 22 toward the tip 24 within the shell body 26 to support at least a portion of the shell body 26 . The blade 20 may be constructed using any materials and techniques suitable for wind turbines. For example, the shell body 26 may be constructed by laying materials in a mold and curing resin. The resin may be pre-impregnated in the materials (e.g., pre-preg glass fibers) and/or introduced separately (e.g., using an infusion process), depending on the technique used.
[0024] Certain conditions may cause the blade 20 to experience vibrations in the plane of its rotation. The tip 24 moves back and forth in an edgewise direction along the chord 34 between the leading and trailing edges 30 , 32 during these vibrations. The blade 20 may also experience vibrations in a flapwise direction, where the tip 24 moves perpendicular to the plane of rotation. As discussed above, flapwise vibrations have significant aerodynamic damping while edgewise vibrations have little to no aerodynamic damping. Previous attempts to dampen edgewise vibrations have focused on various mechanical apparatus, such as tuned liquid dampers or passive dampers, to apply forces in the opposite direction of movement of the tip 24 and thereby dampen the edgewise vibrations. However, in accordance with one embodiment of the invention, the edgewise vibrations of a wind turbine blade 20 are damped based on a different physical principle as compared to those described above.
[0025] In this regard, an important characteristic of a blade that largely influences the amplitude and damping (or possible instability) of edgewise vibrations is the structural pitch. The structural pitch refers to the direction in which the blade moves when it vibrates. If a blade vibrates only in the edgewise direction with zero flapwise motion, then the structural pitch is said to be zero. If edgewise motion and flapwise motion both occur, then the blade has some non-zero value of structural pitch which is determined by the relative level of flapwise and edgewise motion. The more flapwise motion the blade has during an edgewise movement (i.e., higher structural pitch), the more aerodynamic damping is placed on the blade. This increases the overall damping and can help prevent unstable edgewise vibrations.
[0026] The structural pitch is highly related to the principal axes of the blade cross section. The principal axes are the two directions in which the blade 20 is the stiffest and the most compliant. As shown in FIGS. 2 and 3 , a typical blade 20 has one principal axis 38 aligned with the chord 34 of the blade 20 , and another principal axis 40 oriented perpendicularly to the chord 34 and the other principal axis 38 . When the principal axes 38 , 40 are aligned perfectly with the edgewise and flapwise directions of the blade 20 then the structural pitch of the blade 20 is zero and there can be no aerodynamic damping of the edgewise vibrations. Changing the direction of the principal axes, however, will modify the structural pitch of the blade 20 to a non-zero value and thereby provide an increased level of damping of the edgewise vibrations.
[0027] Thus, in accordance with one embodiment of the invention, edgewise vibrations of a wind turbine blade are damped by altering the principle axes of the blade, which in turn alters the structural pitch. More specifically, when the tip 24 moves in the edgewise direction toward the leading edge 30 , a damping element 42 minimizes and/or reduces the edgewise vibrations by effectively introducing flapwise blade movement. In an exemplary embodiment, and as will be discussed in more detail below, the damping element 42 may include a relatively rigid structural member cooperating with or incorporated in the spar 36 of the wind turbine blade 20 .
[0028] In this regard, various embodiments of the damping element 42 according to this invention are shown in FIGS. 4-6 . The spar 36 , as shown in FIGS. 4-4B , has a generally tubular configuration with a generally rectangular cross section. A pair of spaced first walls 44 are each oriented generally parallel to the chord 34 and joined at four corners 46 to a pair of spaced second walls 48 , which are each oriented generally perpendicular to the chord 34 . The damping element 42 , according to various embodiments of this invention extends, generally diagonally across the rectangular cross section of the spar 36 between an opposing pair of the corners 46 . In the embodiment shown in FIGS. 4 and 4A , the damping element 42 is a generally planar, rigid structural element and, as shown in cross section in FIGS. 4 and 4A , is generally linear. The planar configuration of the damping element 42 is shown more clearly in FIG. 6 according to one embodiment.
[0029] In alternative embodiments, the damping element 42 is non-planar and, in a further modification of the damping element 42 according to this invention as shown in FIG. 4B , is curved or arcuate in cross section. In FIG. 4 , the orientation of the damping element 42 extends between a corner 46 of the spar 36 above the chord 34 adjacent the leading edge 30 of the blade 20 to a corner 46 of the spar 36 below the chord 34 and adjacent the trailing edge 32 of the blade 20 . In the embodiment shown in FIG. 4A , the damping element 42 is reoriented so that the corner 46 of the spar 36 , to which the damping element 42 is joined adjacent the leading edge 30 , is below the chord 34 and the corner 46 of the spar 36 , to which the damping element 42 is joined adjacent the trailing edge 32 of the blade 20 , is located above the chord 34 . Moreover, the orientation of the damping element 42 in FIG. 4B is similar to that shown in FIG. 4 , but in an alternative embodiment may be provided with an orientation similar to that shown in FIG. 4A .
[0030] As shown in FIG. 4 , the damping element 42 reorients the structural pitch of the blade 20 to be oblique relative to the chord 34 (i.e., non-zero structural pitch) so as to reduce edgewise vibrations of the blade 20 . In particular, the principal axis 40 is rotated to be generally more aligned with the orientation of the damping element 42 while the principal axis 38 is rotated to be generally more perpendicular to the plane of the damping element 42 . Likewise, the principal axes 38 , 40 of the embodiment shown in FIG. 4A have been reoriented into an oblique relationship relative to the chord 34 so as to reduce the edgewise vibrations of the blade 20 . A comparison of the principal axes 38 , 40 in FIGS. 4 and 4A relative to the orientation shown in FIG. 3 demonstrates the oblique orientation of the structural pitch according to any one of a variety of embodiments within the scope of this invention.
[0031] As shown in FIGS. 5 and 6 , damping element 42 , according to various embodiments of this invention, is coupled within the tubular configuration of the spar 36 and may extend along only a portion of the length of the spar 36 within the blade 20 . Alternatively, multiple damping elements 42 positioned at spaced locations along the blade 20 may also be utilized to dampen edgewise vibrations of the blade 20 according to this invention.
[0032] According to various embodiments of this invention, the spar 36 of the blade 20 is modified to include a diagonally oriented damping element 42 such that the principal axes 38 , 40 of the blade 20 are rotated to increase or decrease structural pitch and, thus, increase damping of the edgewise vibration. The damping element 42 is relatively stiff to add support to the spar 36 to thereby rotate the principal axes 38 , 40 to more generally align with the support provided by the stiff damping element 42 . The damping element 42 could be placed in alternative orientations within the spar 36 depending upon which direction the structural pitch rotation is needed. The damping element 42 , according to one embodiment of this invention, is advantageously added only to the longitudinal region of the blade 20 where the blade 20 experiences maximum curvature during edgewise vibrations. The more pronounced change to the structural pitch results from extended length damping elements 42 within the spar 36 .
[0033] The number and location of damping elements 42 within the shell body 26 may vary. Several of the damping elements 42 , according to the embodiment of FIG. 4 , may be located close to the root 22 of the blade 20 . The damping elements 42 may be strategically positioned in locations where they will not only be effective at damping edgewise vibrations, but also at providing additional support to the shell body 26 where it is needed. The damping elements 42 may also be positioned in locations where they are easier to construct or install.
[0034] Advantageously, the damping element 42 may include a material with relatively high damping capacity, such as fiber-reinforced rubber. The material may be surrounded on one or more sides by a shell (not shown) constructed from fiberglass or another material that provides some structural support. This type of damping element 42 may be provided as a separate component that is coupled to the spar 36 by glue or the like during the manufacturing process of the blade 20 .
[0035] The embodiments discussed above involve coupling the damping element 42 to the spar 36 . However, it is also possible to couple the damping element 42 to other parts of the blade 20 and still achieve a greater degree of freedom in the flapwise direction than in the edgewise direction.
[0036] Again, those skilled in the art will appreciate that there are different ways of constructing the damping element 42 within this invention. Indeed, the damping element 42 may be constructed similar to any of the embodiments discussed above or other embodiments.
[0037] Furthermore, associating the damping element 42 with the inner spar 36 enables the design and manufacture of the shell body 26 to be optimized without having to take into account the attachment of the damping element 42 . Loads created by the damping element 42 are transferred to the inner spar 36 rather than the shell body 26 . Coupling the damping element 42 along the inner spar 36 may also help increase the overall stiffness of the blade 20 . As a result, thinner blade designs may be possible.
[0038] During the manufacturing process of the blade 20 , the damping element 42 may be coupled to the inner spar 36 by gluing the damping element 42 thereto. This may come before positioning the inner spar 36 relative to the shell body 26 , or just prior to closing the mould (not shown) that assembles the shell body 26 together. The length of the damping element 42 may vary such that there may be one long damping element 42 or a plurality of damping elements 42 coupled to the inner spar 36 .
[0039] The embodiments described above are merely examples of the invention defined by the claims that appear below. Those skilled in the art will appreciate additional examples, modifications, and advantages based on the description. Additionally, those skilled in the art will appreciate that individual features of the various embodiments may be combined in different ways. Accordingly, departures may be made from the details of this disclosure without departing from the scope or spirit of the general inventive concept.
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A blade ( 20 ) for a wind turbine ( 10 ) generally includes a shell body ( 26 ) extending between a leading edge ( 30 ) and a trailing edge ( 32 ), an inner spar ( 36 ) supporting at least a portion of the shell body ( 26 ), and a damping element ( 42 ) coupled to the inner spar ( 36 ). The damping element ( 42 ) is configured to adjust the structural pitch of the blade ( 20 ) to dissipate edgewise vibrations of the blade ( 20 ). The damping element ( 42 ) may be incorporated into the spar ( 36 ) upon manufacture of the blade ( 20 ) or installed as a retro-fit modification to existing blades ( 20 ).
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CROSS REFERENCE TO RELATED APPLICATIONS
This application claims priority to U.S. Provisional Application No. 61/101,548 filed Sep. 30, 2008, and U.S. Provisional Application No. 61/117,448 filed Nov. 24, 2008, the entire disclosures of which are incorporated herein by reference.
BACKGROUND
Due to its excellent biocompatibility, biostability and physical properties, polyurethane or polyurethane-containing polymers have been used to fabricate a large number of implantable devices, including pacemaker leads, artificial hearts, heart valves, stent coverings, artificial tendons, arteries and veins. Formulations for delivery of active agents using polyurethane implantable devices, however, require a liquid medium or carrier for the diffusion of the drug at a zero order rate.
SUMMARY
Described herein are methods and compositions based on the unexpected discovery that solid formulations comprising one or more active agents can be used at the core of a polyurethane implantable device such that the active agent is released in a controlled-release, zero-order manner from the implantable device. The active agents and polyurethane coating can be selected based on various physical parameters, and then the release rate of the active from the implantable device can be optimized to a clinically relevant release rate based on clinical and/or in vitro trials.
One embodiment is directed to a method for delivering a formulation comprising an effective amount of risperidone to a subject, comprising: implanting an implantable device into the subject, wherein the implantable device comprises risperidone or a formulation thereof substantially surrounded by a polyurethane-based polymer. In a particular embodiment, the polyurethane-based polymer is formed from one or more polyols, wherein the general polyol structure is selected from the group consisting of
—[O—(CH 2 ) n ] x —O—;
O—(CH 2 —CH 2 —CH 2 —CH 2 ) x —O—; and
O—[(CH 2 ) 6 —CO 3 ] n —(CH 2 )—O—.
For the compositions and methods described herein, the values for n and x are integer values of between about 1 and about 1,000,000; of between about 2 and about 500,000; of between about 5 and about 250,000; and of between about 10 and about 100,000. In a particular embodiment, the polyol comprises —[O—(CH 2 ) n ] x —O—, wherein the polyurethane-based polymer has an equilibrium water content of between about 5% and about 200%, e.g., of at least about 15%. In a particular embodiment, risperidone is released at a zero-order rate of about 149 μg/day per square centimeter of the surface area of the implantable device. In a particular embodiment, the polyol comprises O—(CH 2 —CH 2 —CH 2 —CH 2 ) x —O—, wherein the polyurethane-base polymer has a flex modulus of between about 1000 and about 92,000 psi, e.g., of about 2,300 psi. In a particular embodiment, risperidone is released at a zero-order rate of about 146 μg/day per square centimeter of the surface area of the implantable device. In a particular embodiment, the polyol comprises O—[(CH 2 ) 6 —CO 3 ] n —(CH 2 )—O—, wherein the polyurethane-based polymer has a flex modulus of between about 620 and about 92,000 psi, e.g., of about 620 psi. In a particular embodiment, risperidone is released at a zero-order rate of about 40 μg/day per square centimeter of the surface area of the implantable device.
One embodiment is directed to a drug delivery device for the controlled release of risperidone over an extended period of time to produce local or systemic pharmacological effects, comprising: a) a polyurethane-based polymer formed to define a hollow space; and b) a solid drug formulation comprising a formulation comprising risperidone and optionally one or more pharmaceutically acceptable carriers, wherein the solid drug formulation is contained in the hollow space, and wherein the device provides a desired release rate of risperidone from the device after implantation. In a particular embodiment, the drug delivery device is conditioned and primed under conditions chosen to be consistent with the water solubility characteristics of the at least one active agent. In a particular embodiment, the pharmaceutically acceptable carrier is stearic acid. In a particular embodiment, the polyurethane-based polymer is formed from one or more polyols, wherein the general polyol structure is selected from the group consisting of:
—[O—(CH 2 ) n ] x —O—;
O—(CH 2 —CH 2 —CH 2 —CH 2 ) x —O—; and
O—[(CH 2 ) 6 —CO 3 ] n —(CH 2 )—O—.
In a particular embodiment, the polyol comprises —[O—(CH 2 ) n ] x —O—, wherein the polyurethane-based polymer has an equilibrium water content of between about 5% and about 43%, e.g., of at least about 15%. In a particular embodiment, risperidone is released at a zero-order rate of about 149 μg/day per square centimeter of the surface area of the implantable device. In a particular embodiment, the polyol comprises O—(CH 2 —CH 2 —CH 2 —CH 2 ) x —O—, wherein the polyurethane-base polymer has a flex modulus of between about 1000 and about 92,000 psi, e.g., of about 2,300 psi. In a particular embodiment, risperidone is released at a zero-order rate of about 146 μg/day per square centimeter of the surface area of the implantable device. In a particular embodiment, the polyol comprises O—[(CH 2 ) 6 —CO 3 ] n —(CH 2 )—O—, wherein the polyurethane-based polymer has a flex modulus of between about 620 and about 92,000 psi, e.g., of about 620 psi. In a particular embodiment, risperidone is released at a zero-order rate of about 40 μg/day per square centimeter of the surface area of the implantable device. In a particular embodiment, appropriate conditioning and priming parameters can be selected to establish the desired delivery rates of the at least one active agent, wherein the priming parameters are time, temperature, conditioning medium and priming medium.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of an implant with two open ends.
FIG. 2 is a side view of pre-fabricated end plugs used to plug the implants.
FIG. 3 is a side view of an implant with one open end.
FIG. 4 is a graph of the release rate of risperidone from Carbothane® PC-3575A polyurethane implants (Flex Modulus 620 psi) prepared from tubing sections representing the beginning, middle and end of a coil of tubing as part of an assessment of the uniformity of the material within a particular lot. Samples were evaluated weekly for one year. All implants were of equivalent geometry and drug load.
FIG. 5 is a graph of the release rate of risperidone from Carbothane® PC-3575A polyurethane implants (Flex Modulus 620 psi) as part of an assessment of the effect using saline versus aqueous hydroxypropyl betacellulose solution (15% in phosphate buffered saline) as the elution media. Samples were evaluated weekly for 11 weeks. All implants were of equivalent geometry and drug load.
FIGS. 6A and 6B are graphs comparing the release rates of risperidone from Carbothane® PC-3595A polyurethane implants (Flex modulus 4500 psi) to Tecophilic® HP-60D-20 polyurethane implants (EWC, 14.9%) as part of the evaluation of the release of the active from either hydrophilic and hydrophobic polyurethane materials. Samples were evaluated weekly for 22 weeks for the Carbothane® implant. Samples were evaluated weekly for 15 weeks for the Tecophilic® implant. All implants were of equivalent geometry and drug load. FIG. 11B is a graph of the release rate of risperidone from Tecophilic® HP-60D-20 polyurethane implants (EWC, 14.9%) alone, sampled weekly for 15 weeks.
FIG. 7 is a graph comparing the release rates of risperidone from Tecoflex® EG-80A polyurethane implants (Flex Modulus 1000 psi) and two grades of Tecophilic® polyurethane implants, HP-60D-35 and HP-60D-60 (EWC, 23.6% and 30.8%, respectively). All were sampled weekly for 10 weeks. All implants were of equivalent geometry and drug load.
FIG. 8 is a graph of the release rate of risperidone from Carbothane® PC-3575A polyurethane implants (Flex Modulus 620 psi) that served as in vitro controls for implants used in the beagle dog study described in Example 8. The in vitro elution study of these implants was initiated on the date of implantation of the subject implants as part of an assessment of in vivo-in vitro correlation.
FIG. 9 is a graph of the in vivo plasma concentration of risperidone in the beagle dog study described in Example 8. The lower plot represents the average plasma concentration achieved in dogs implanted with one Carbothane® PC-3575A polyurethane implant (Flex Modulus 620 psi). The upper plot represents the average plasma concentration achieved in dogs implanted with two Carbothane® PC-3575A polyurethane implants (Flex Modulus 620 psi).
FIG. 10 is a graph showing the in vitro release of risperidone from Tecoflex® and Carbothane® implants. The pellets comprising the risperidone formulation had a diameter of 3.5 mm, a length of about 4.5 mm and a weight of 5.4 mg. The implant had a reservoir length of about 39-40 mm, a wall thickness of 0.2 mm, and internal diameter of 3.6 mm and an overall length of about 45 mm.
FIG. 11 is a graph showing the in vivo release of risperidone from Tecoflex® and Carbothane® implants, as compared to a control. The pellets comprising the risperidone formulation had a diameter of 3.5 mm, a length of about 4.5 mm and a weight of 5.4 mg. The implant had a reservoir length of about 39-40 mm, a wall thickness of 0.2 mm, and internal diameter of 3.6 mm and an overall length of about 45 mm.
DETAILED DESCRIPTION
To take the advantage of the excellent properties of polyurethane-based polymers, the present invention is directed to the use of polyurethane-based polymers as drug delivery devices for releasing drugs at controlled rates for an extended period of time to produce local or systemic pharmacological effects. The drug delivery device can comprise a cylindrically shaped reservoir surrounded by polyurethane-based polymer that controls the delivery rate of the drug inside the reservoir. The reservoir contains a formulation, e.g., a solid formulation, comprising one or more active ingredients and, optionally, pharmaceutically acceptable carriers. The carriers are formulated to facilitate the diffusion of the active ingredients through the polymer and to ensure the stability of the drugs inside the reservoir.
A polyurethane is any polymer consisting of a chain of organic units joined by urethane links. Polyurethane polymers are formed by reacting a monomer containing at least two isocyanate functional groups with another monomer containing at least two alcohol groups in the presence of a catalyst. Polyurethane formulations cover a wide range of stiffness, hardness, and densities.
Polyurethanes are in the class of compounds called “reaction polymers,” which include epoxies, unsaturated polyesters and phenolics. A urethane linkage is produced by reacting an isocyanate group, —N═C═O with a hydroxyl (alcohol) group, —OH. Polyurethanes are produced by the polyaddition reaction of a polyisocyanate with a polyalcohol (polyol) in the presence of a catalyst and other additives. In this case, a polyisocyanate is a molecule with two or more isocyanate functional groups, R—(N═C═O) n≧2 and a polyol is a molecule with two or more hydroxyl functional groups, R′—(OH) n≧2 . The reaction product is a polymer containing the urethane linkage, —RNHCOOR′—. Isocyanates react with any molecule that contains an active hydrogen. Importantly, isocyanates react with water to form a urea linkage and carbon dioxide gas; they also react with polyetheramines to form polyureas.
Polyurethanes are produced commercially by reacting a liquid isocyanate with a liquid blend of polyols, catalyst, and other additives. These two components are referred to as a polyurethane system, or simply a system. The isocyanate is commonly referred to in North America as the “A-side” or just the “iso,” and represents the rigid backbone (or “hard segment”) of the system. The blend of polyols and other additives is commonly referred to as the “B-side” or as the “poly,” and represents the functional section (or “soft segment”) of the system. This mixture might also be called a “resin” or “resin blend.” Resin blend additives can include chain extenders, cross linkers, surfactants, flame retardants, blowing agents, pigments and fillers. In drug delivery applications, the “soft segments” represent the section of the polymer that imparts the characteristics that determine the diffusivity of an active pharmaceutical ingredient (API) through that polymer.
The elastomeric properties of these materials are derived from the phase separation of the hard and soft copolymer segments of the polymer, such that the urethane hard segment domains serve as cross-links between the amorphous polyether (or polyester) soft segment domains. This phase separation occurs because the mainly non-polar, low-melting soft segments are incompatible with the polar, high-melting hard segments. The soft segments, which are formed from high molecular weight polyols, are mobile and are normally present in coiled formation, while the hard segments, which are formed from the isocyanate and chain extenders, are stiff and immobile. Because the hard segments are covalently coupled to the soft segments, they inhibit plastic flow of the polymer chains, thus creating elastomeric resiliency. Upon mechanical deformation, a portion of the soft segments are stressed by uncoiling, and the hard segments become aligned in the stress direction. This reorientation of the hard segments and consequent powerful hydrogen-bonding contributes to high tensile strength, elongation, and tear resistance values.
The polymerization reaction is catalyzed by tertiary amines, such as, for example, dimethylcyclohexylamine, and organometallic compounds, such as, for example, dibutyltin dilaurate or bismuth octanoate. Furthermore, catalysts can be chosen based on whether they favor the urethane (gel) reaction, such as, for example, 1,4-diazabicyclo[2.2.2]octane (also called DABCO or TEDA), or the urea (blow) reaction, such as bis-(2-dimethylaminoethyl)ether, or specifically drive the isocyanate trimerization reaction, such as potassium octoate.
Isocyanates with two or more functional groups are required for the formation of polyurethane polymers. Volume wise, aromatic isocyanates account for the vast majority of global diisocyanate production. Aliphatic and cycloaliphatic isocyanates are also important building blocks for polyurethane materials, but in much smaller volumes. There are a number of reasons for this. First, the aromatically-linked isocyanate group is much more reactive than the aliphatic one. Second, aromatic isocyanates are more economical to use. Aliphatic isocyanates are used only if special properties are required for the final product. Light stable coatings and elastomers, for example, can only be obtained with aliphatic isocyanates. Aliphatic isocyanates also are favored in the production of polyurethane biomaterials due to their inherent stability and elastic properties.
Examples of aliphatic and cycloaliphatic isocyanates include, for example, 1,6-hexamethylene diisocyanate (HDI), 1-isocyanato-3-isocyanatomethyl-3,5,5-trimethyl-cyclohexane (isophorone diisocyanate, IPDI), and 4,4′-diisocyanato dicyclohexylmethane (H12MDI). They are used to produce light stable, non-yellowing polyurethane coatings and elastomers. H12MDI prepolymers are used to produce high performance coatings and elastomers with optical clarity and hydrolysis resistance. Tecoflex®, Tecophilic® and Carbothane® polyurethanes are all produced from H12MDI prepolymers.
Polyols are higher molecular weight materials manufactured from an initiator and monomeric building blocks, and, where incorporated into polyurethane systems, represent the “soft segments” of the polymer. They are most easily classified as polyether polyols, which are made by the reaction of epoxides (oxiranes) with an active hydrogen containing starter compounds, or polyester polyols, which are made by the polycondensation of multifunctional carboxylic acids and hydroxyl compounds.
Tecoflex® polyurethanes, Tecogel® polyurethanes and Tecophilic® polyurethanes are cycloaliphatic polymers and are of the types produced from polyether-based polyols. For the Tecoflex® polyurethanes, the general structure of the polyol segment is represented as,
O—(CH 2 —CH 2 —CH 2 —CH 2 ) x —O—
whereby an increase in “x” represents a increase in flexibility (decreased “Flex Modulus”; “FM”), yielding FM ranging from about 1000-92,000 psi. From the standpoint of drug release from these materials, the release of a relatively hydrophobic API decreases as the FM increases. For the compositions and methods described herein, the values for x are integer values of between about 1 and about 1,000,000; of between about 2 and about 500,000; of between about 5 and about 250,000; and of between about 10 and about 100,000. In still other embodiments, x may range from about 2-500, about 2-100, about 5-50, and 10-30.
For the Tecophilic® (hydrophilic) or Tecogel® polyurethanes, the general structure of the polyol segment is represented as,
—[O—(CH 2 ) n ] x —O—
whereby increases in “n” and “x” represent variations in hydrophilicity, and yield equilibrium water contents (% EWC) ranging from about 5%-200%. For the compositions and methods described herein, the values for n and x are integer values of between about 1 and about 1,000,000; of between about 2 and about 500,000; of between about 5 and about 250,000; and of between about 10 and about 100,000. In still other embodiments, n and x may have the same or different values, with those values ranging from about 2-500, about 2-100, about 5-50, and 10-30. From the standpoint of drug release from these materials, the release of a relatively hydrophilic API increases as the % EWC increases.
Specialty polyols include, for example, polycarbonate polyols, polycaprolactone polyols, polybutadiene polyols, and polysulfide polyols.
Carbothane® polyurethanes are cycloaliphatic polymers and are of the types produced from polycarbonate-based polyols. The general structure of the polyol segment is represented as,
O—[(CH 2 ) 6 —CO 3 ] n —(CH 2 )—O—
whereby an increase in “n” represents a increase in flexibility (decreased FM), yielding FM ranging from about 620-92,000 psi. For the compositions and methods described herein, the values for n are integer values of between about 1 and about 1,000,000; of between about 2 and about 500,000; of between about 5 and about 250,000; and of between about 10 and about 100,000. In still other embodiments, n may range from about 2-500, about 2-100, about 5-50, and 10-30. From the standpoint of drug release from these materials, the release of a relatively hydrophobic API will decrease as the FM increases.
Chain extenders and cross linkers are low molecular weight hydroxyl- and amine-terminated compounds that play an important role in the polymer morphology of polyurethane fibers, elastomers, adhesives and certain integral skin and microcellular foams. Examples of chain extenders include, for example, ethylene glycol, 1,4-butanediol (1,4-BDO or BDO), 1,6-hexanediol, cyclohexane dimethanol and hydroquinone bis(2-hydroxyethyl)ether (HQEE). All of these glycols form polyurethanes that phase separate well, form well-defined hard segment domains, and are melt processable. They are all suitable for thermoplastic polyurethanes with the exception of ethylene glycol, since its derived bis-phenyl urethane undergoes unfavorable degradation at high hard segment levels. Tecophilic®, Tecoflex® and Carbothane® polyurethanes all incorporate the use of 1,4-butanediol as the chain extender.
The current invention provides a drug delivery device that can achieve the following objectives: a controlled-release rate (e.g., zero-order release rate) to maximize therapeutic effects and minimize unwanted side effects, an easy way to retrieve the device if it is necessary to end the treatment, an increase in bioavailability with less variation in absorption and no first pass metabolism.
The release rate of the drug is governed by the Fick's Law of Diffusion as applied to a cylindrically shaped reservoir device (cartridge). The following equation describes the relationship between different parameters:
ⅆ
M
ⅆ
t
=
2
π
hp
Δ
C
ln
(
r
o
/
r
i
)
where:
dM/dt: drug release rate; h: length of filled portion of device; ΔC: concentration gradient across the reservoir wall; r o /r i : ratio of outside to inside radii of device; and p: permeability coefficient of the polymer used.
The permeability coefficient is primarily regulated by the hydrophilicity or hydrophobicity of the polymer, the structure of the polymer, and the interaction of drug and the polymer. Once the polymer and the active ingredient are selected, p is a constant, h, ro, and r i are fixed and kept constant once the cylindrically shaped device is produced. ΔC is maintained constant.
To keep the geometry of the device as precise as possible, the device, e.g., a cylindrically shaped device, can be manufactured through precision extrusion or precision molding process for thermoplastic polyurethane polymers, and reaction injection molding or spin casting process for thermosetting polyurethane polymers.
The cartridge can be made with either one end closed or both ends open. The open end can be plugged with, for example, pre-manufactured end plug(s) to ensure a smooth end and a solid seal, or, in the case of thermoplastic polyurethanes, by using heat-sealing techniques known to those skilled in the art. The solid actives and carriers can be compressed into pellet form to maximize the loading of the actives.
To identify the location of the implant, radiopaque material can be incorporated into the delivery device by inserting it into the reservoir or by making it into end plug to be used to seal the cartridge.
Once the cartridges are sealed on both ends with the filled reservoir, they are optionally conditioned and primed for an appropriate period of time to ensure a constant delivery rate.
The conditioning of the drug delivery devices involves the loading of the actives (drug) into the polyurethane-based polymer that surrounds the reservoir. The priming is done to stop the loading of the drug into the polyurethane-based polymer and thus prevent loss of the active before the actual use of the implant. The conditions used for the conditioning and priming step depend on the active, the temperature and the medium in which they are carried out. The conditions for the conditioning and priming may be the same in some instances.
The conditioning and priming step in the process of the preparation of the drug delivery devices is done to obtain a determined rate of release of a specific drug. The conditioning and priming step of the implant containing a hydrophilic drug can be carried out in an aqueous medium, e.g., in a saline solution. The conditioning and priming step of a drug delivery device comprising a hydrophobic drug is usually carried out in a hydrophobic medium such as, for example, an oil-based medium. The conditioning and priming steps can be carried out by controlling three specific factors, namely the temperature, the medium and the period of time.
A person skilled in the art would understand that the conditioning and priming step of the drug delivery device is affected by the medium in which the device is placed. A hydrophilic drug can be conditioned and primed, for example, in an aqueous solution, e.g., in a saline solution. The temperature used to condition and prime the drug delivery device can vary across a wide range of temperatures, e.g., about 37° C.
The time period used for the conditioning and priming of the drug delivery devices can vary from about a single day to several weeks depending on the release rate desired for the specific implant or drug. The desired release rate is determined by one of skill in the art with respect to the particular active agent used in the pellet formulation.
A person skilled in the art will understand the steps of conditioning and priming the implants are to optimize the rate of release of the drug contained within the implant. As such, a shorter time period spent on the conditioning and the priming of a drug delivery device results in a lower rate of release of the drug compared to a similar drug delivery device that has undergone a longer conditioning and priming step.
The temperature in the conditioning and priming step will also affect the rate of release in that a lower temperature results in a lower rate of release of the drug contained in the drug delivery device when compared to a similar drug delivery device that has undergone a treatment at a higher temperature.
Similarly, in the case of aqueous solutions, e.g., saline solutions, the sodium chloride content of the solution determines what type of rate of release will be obtained for the drug delivery device. More specifically, a lower content of sodium chloride results in a higher rate of release of drug when compared to a drug delivery device that has undergone a conditioning and priming step where the sodium chloride content was higher.
The same conditions apply for hydrophobic drugs where the main difference in the conditioning and priming step is that the conditioning and priming medium is a hydrophobic medium, more specifically an oil-based medium.
The delivery of risperidone can be useful, for example, to treat schizophrenia, manic states, bipolar disorder, irritability, autism, obsessive-compulsive disorder, severe treatment-resistant depression with or without psychotic features, Tourette syndrome, disruptive behavior disorders in children; and eating disorders. Risperidone belongs to a class of anti-psychotic drugs known as “atypical neuroleptics”. It is a strong dopamine antagonist. It has a high affinity for D2 dopaminergic receptors. It has actions at several 5-HT (serotonin) receptor subtypes. These are 5-HT2C, linked to weight gain, 5-HT2A, linked to its antipsychotic action and relief of some of the extrapyramidal side effects experienced with the “typical neuroleptics” through action at 5-HT1A. The latter action leads to an increased release of dopamine from mesocortical neurons in the brain. Effective levels of risperidone in the blood are known and established and can range, for example, about 0.1 to about 10 ng/ml, from about 0.5 to about 8 ng/ml or about 1.0 to about 5 ng/ml range.
One of skill in the art would be able to tailor risperidone release by altering a variety of implant factors. For example, as shown in the Examples, different classes of polyurethanes lead to different release rates of risperidone. Additionally, within classes of polyurethanes, the EWC and/or flex modulus of the polyurethane can be varied to achieve different risperidone release rates. Further still, one of skill in the art could vary the size of the implant to increase or decrease the surface area of the implant, thereby varying the release rate of risperidone from the implant. Such alterations lead to release rates in the physiologically-relevant range, e.g., of about 0.001 to about 15 mg/day, from about 0.1 to about 15 mg/day, from about 1 to about 12.5 mg/day, from about 7.5 to about 12.5 mg/day or at about 12.5 mg/day. Release rate from implants can also be varied, for example, by adjusting the amount and nature of excipients contained in the risperidone formulation.
Implants that achieve physiological release rates of risperidone can vary in size, depending on, for example, the nature of the polyurethane used. A cylindrical implant, for example, can have a range of internal diameters from about 1 mm to about 10 mm, from about 1.5 mm to about 5 mm, from about 1.8 mm to about 3.6 mm, about 3.6 mm or about 1.8 mm. An implant can range in length from about, for example, 5 mm to about 100 mm, from about 7.5 mm to about 50 mm, from about 10 mm to about 40 mm, from about 15 mm to about 30 mm, about 37 mm, about 40 mm or about 15.24 mm.
The current invention focuses on the application of polyurethane-based polymers, thermoplastics or thermosets, to the creation of implantable drug devices to deliver biologically active compounds at controlled rates for prolonged period of time. Polyurethane polymers can be made into, for example, cylindrical hollow tubes with one or two open ends through extrusion, (reaction) injection molding, compression molding, or spin-casting (see e.g., U.S. Pat. Nos. 5,266,325 and 5,292,515), depending on the type of polyurethane used.
Thermoplastic polyurethane can be processed through extrusion, injection molding or compression molding. Thermoset polyurethane can be processed through reaction injection molding, compression molding, or spin-casting. The dimensions of the cylindrical hollow tube should be as precise as possible.
Polyurethane-based polymers are synthesized from multi-functional polyols, isocyanates and chain extenders. The characteristics of each polyurethane can be attributed to its structure.
Thermoplastic polyurethanes are made of macrodiols, diisocyanates, and difunctional chain extenders (e.g., U.S. Pat. Nos. 4,523,005 and 5,254,662). Macrodiols make up the soft domains. Diisocyanates and chain extenders make up the hard domains. The hard domains serve as physical crosslinking sites for the polymers. Varying the ratio of these two domains can alter the physical characteristics of the polyurethanes, e.g., the flex modulus.
Thermoset polyurethanes can be made of multifunctional (greater than difunctional) polyols and/or isocyanates and/or chain extenders (e.g., U.S. Pat. Nos. 4,386,039 and 4,131,604). Thermoset polyurethanes can also be made by introducing unsaturated bonds in the polymer chains and appropriate crosslinkers and/or initiators to do the chemical crosslinking (e.g., U.S. Pat. No. 4,751,133). By controlling the amounts of crosslinking sites and how they are distributed, the release rates of the actives can be controlled.
Different functional groups can be introduced into the polyurethane polymer chains through the modification of the backbones of polyols depending on the properties desired. Where the device is used for the delivery of water soluble drugs, hydrophilic pendant groups such as ionic, carboxyl, ether, and hydroxyl groups are incorporated into the polyols to increase the hydrophilicity of the polymer (e.g., U.S. Pat. Nos. 4,743,673 and 5,354,835). Where the device is used for the delivery of hydrophobic drugs, hydrophobic pendant groups such as alkyl, siloxane groups are incorporated into the polyols to increase the hydrophobicity of the polymer (e.g., U.S. Pat. No. 6,313,254). The release rates of the actives can also be controlled by the hydrophilicity/hydrophobicity of the polyurethane polymers.
For thermoplastic polyurethanes, precision extrusion and injection molding are the preferred choices to produce two open-end hollow tubes ( FIG. 1 ) with consistent physical dimensions. The reservoir can be loaded freely with appropriate formulations containing actives and carriers or filled with pre-fabricated pellets to maximize the loading of the actives. One open end needs to be sealed first before the loading of the formulation into the hollow tube. To seal the two open ends, two pre-fabricated end plugs ( FIG. 2 ) can be used. The sealing step can be accomplished through the application of heat or solvent or any other means to seal the ends, preferably permanently.
For thermoset polyurethanes, precision reaction injection molding or spin casting is the preferred choice depending on the curing mechanism. Reaction injection molding is used if the curing mechanism is carried out through heat and spin casting is used if the curing mechanism is carried out through light and/or heat. Hollow tubes with one open end ( FIG. 3 ), for example, can be made by spin casting. Hollow tubes with two open ends, for example, can be made by reaction injection molding. The reservoir can be loaded in the same way as the thermoplastic polyurethanes.
To seal an open end, an appropriate light-initiated and/or heat-initiated thermoset polyurethane formulation can be used to fill the open end, and this is cured with light and/or heat. A pre-fabricated end plug, for example, can also be used to seal the open end by applying an appropriate light-initiated and/or heat-initiated thermoset polyurethane formulation on to the interface between the pre-fabricated end plug and the open end, and curing it with the light and/or heat or any other means to seal the ends, preferably permanently.
The final process involves the conditioning and priming of the implants to achieve the delivery rates required for the actives. Depending upon the types of active ingredient, hydrophilic or hydrophobic, the appropriate conditioning and priming media is chosen. Water-based media are preferred for hydrophilic actives, and oil-based media are preferred for hydrophobic actives.
As a person skilled in the art would readily know many changes can be made to the preferred embodiments of the invention without departing from the scope thereof. It is intended that all matter contained herein be considered illustrative of the invention and not it a limiting sense.
EXEMPLIFICATION
Example 1
Tecophilic® polyurethane polymer tubes are supplied by Thermedics Polymer Products and manufactured through a precision extrusion process. Tecophilic® polyurethane is a family of aliphatic polyether-based thermoplastic polyurethane that can be formulated to different equilibrium water contents (EWC) of up to 150% of the weight of dry resin. Extrusion grade formulations are designed to provide maximum physical properties of thermoformed tubing or other components. An exemplary tube and end cap structures are depicted in FIGS. 1-3 .
The physical data for the polymers is provided below as made available by Thermedics Polymer Product (tests conducted as outlined by American Society for Testing and Materials (ASTM), Table 1).
TABLE 1
Tecophilic ® Typical Physical Test Data
ASTM
HP-60D-20
HP-60D-35
HP-60D-60
HP-93A-100
Durometer
D2240
43D
42D
41D
83A
(Shore Hardness)
Spec Gravity
D792
1.12
1.12
1.15
1.13
Flex Modulus (psi)
D790
4,300
4,000
4,000
2,900
Ultimate Tensile Dry (psi)
D412
8,900
7,800
8,300
2,200
Ultimate Tensile Wet (psi)
D412
5,100
4,900
3,100
1,400
Elongation Dry (%)
D412
430
450
500
1,040
Elongation Wet (%)
D412
390
390
300
620
Example 2
Tables 2A-C show release rates of risperidone from three different classes of polyurethane compounds (Tecophilic®, Tecoflex® and Carbothane®). The release rates have been normalized to surface area of the implant, thereby adjusting for slight differences in the size of the various implantable devices. Risperidone is considered to be hydrophobic (not very water-soluble), as indicated by the Log P value; for the purposes of the data provided, a Log P value of greater than about 2.0 is considered to be not readily soluble in aqueous solution. The polyurethanes were selected to have varying affinities for water soluble active agents and varying flexibility (as indicated by the variation in flex modulus).
For applications of the polyurethanes useful for the devices and methods described herein, the polyurethane exhibits physical properties suitable for the risperidone formulation to be delivered. Polyurethanes are available or can be prepared, for example, with a range of EWCs or flex moduli (Table 2). Tables 2A-C show normalized release rates for various active ingredients from polyurethane compounds. Tables 2D-F show the non-normalized release rates for the same active ingredients, together with implant composition.
TABLE 2A
Polyurethane Type
Tecophilic
Polyurethane Grade
HP-60D-60
HP-60D-35
HP-60D-20
HP-60D-10
HP-60D-05
Relative Water
% EWC/Flex Modulus
Active
Solubility
31% EWC
24% EWC
15% EWC
8.7% EWC
5.5% EWC
Risperidone
Log P = 3.28
—
—
149
μg/day/cm 2
—
—
(M.W. 410)
10% CC,
2% SA,
28.5
mg API
TABLE 2B
Polyurethane Type
Tecoflex
Polyurethane Grade
EG-85A
EG 100A
EG-65D
Relative Water
% EWC/Flex Modulus
Active
Solubility
F.M.: 2,300
F.M.: 10,000
F.M.: 37,000
Risperidone
Log P = 3.28
146
μg/day/cm 2
7.6
μg/day/cm 2
1.9
μg/day/cm 2
(M.W. 410)
10% CC,
2% SA,
10% CC,
2% SA,
10% CC,
2% SA,
27.9
mg API
29.8
mg API
29.7
mg API
TABLE 2C
Polyurethane Type
Carbothane
Polyurethane Grade
PC-3575A
PC-3595A
Relative Water
% EWC/Flex Modulus
Active
Solubility
F.M.: 620
F.M.: 4,500
Risperidone
Log P = 3.28
40
μg/day/cm 2
11
μg/day/cm 2
(M.W. 410)
10% CC,
2% SA,
10% CC,
2% SA,
27.8
mg API
29.7
mg API
TABLE 2D
Polyurethane
Tecophilic
Grade
HP-60D-60
HP-60D-35
HP-60D-20
HP-60D-10
HP-60D-05
Relative Water
% EWC
Active
Solubility
31% EWC
24% EWC
15% EWC
8.7% EWC
5.5% EWC
Risperidone
Log P = 3.28
—
—
150
μg/day
—
—
(M.W. 410)
ID: 1.80
mm
Wall: 0.30
mm
L: 15.24
mm
1.005
cm 2
TABLE 2E
Polyurethane Type
Tecoflex
Polyurethane Grade
EG-85A
EG 100A
EG-65D
Relative Water
Flex Modulus
Active
Solubility
F.M.: 2,300
F.M.: 10,000
F.M.: 37,000
Risperidone
Log P = 3.28
150
μg/day
8
μg/day
2
μg/day
(M.W. 410)
ID: 1.85
mm
ID: 1.85
mm
ID: 1.85
mm
Wall: 0.20
mm
Wall: 0.20
mm
Wall: 0.20
mm
L: 16.0
mm
L: 16.4
mm
L: 16.2
mm
1.030
cm 2
1.056
cm 2
1.043
cm 2
TABLE 2F
Polyurethane Type
Carbothane
Polyurethane Grade
PC-3575A
PC-3595A
Relative Water
Flex Modulus
Active
Solubility
F.M.: 620
F.M.: 4,500
Risperidone
Log P = 3.28
40
μg/day
11
μg/day
(M.W. 410)
ID: 1.85
mm
ID: 1.85
mm
Wall: 0.20
mm
Wall: 0.20
mm
L: 15.6
mm
L: 16.2
mm
1.004
cm 2
1.043
cm 2
The solubility of an active agent in an aqueous environment can be measured and predicted based on its partition coefficient (defined as the ratio of concentration of compound in aqueous phase to the concentration in an immiscible solvent). The partition coefficient (P) is a measure of how well a substance partitions between a lipid (oil) and water. The measure of solubility based on P is often given as Log P. In general, solubility is determined by Log P and melting point (which is affected by the size and structure of the compounds). Typically, the lower the Log P value, the more soluble the compound is in water. It is possible, however, to have compounds with high Log P values that are still soluble on account of, for example, their low melting point. It is similarly possible to have a low Log P compound with a high melting point, which is very insoluble.
The flex modulus for a given polyurethane is the ratio of stress to strain. It is a measure of the “stiffness” of a compound. This stiffness is typically expressed in Pascals (Pa) or as pounds per square inch (psi).
The elution rate of an active agent from a polyurethane compound can vary on a variety of factors including, for example, the relative hydrophobicity/hydrophilicity of the polyurethane (as indicated, for example, by logP), the relative “stiffness” of the polyurethane (as indicated, for example, by the flex modulus), and/or the molecular weight of the active agent to be released.
Example 3
Elution of Risperidone from Polyurethane Implantable Devices
FIGS. 5-10 are graphs showing elution profiles of risperidone from various implantable devices over varying periods of time.
Release rates were obtained for risperidone from Carbothane® PC-3575A polyurethane implants (F.M. 620 psi) prepared from tubing sections representing the beginning, middle and end of a coil of tubing as part of an assessment of the uniformity of the material within a particular lot ( FIG. 5 ). Samples were evaluated weekly for one year. All implants were of equivalent geometry and drug load.
Release rates were obtained for risperidone from Carbothane® PC-3575A polyurethane implants (F.M. 620 psi) as part of an assessment of the effect using saline versus aqueous hydroxypropyl betacellulose solution (15% in phosphate buffered saline) as the elution media ( FIG. 6 ). Samples were evaluated weekly for 11 weeks. All implants were of equivalent geometry and drug load.
Release rates were compared for risperidone from Carbothane® PC-3595A polyurethane implants (F.M. 4500 psi) and Tecophilic® HP-60D-20 polyurethane implants (EWC 14.9%) as part of the evaluation of the release of the active from either hydrophilic and hydrophobic polyurethane materials ( FIGS. 7A and 7B ). Samples were evaluated weekly for 22 weeks for the Carbothane® implant. Samples were evaluated weekly for 15 weeks for the Tecophilic® implant. All implants were of equivalent geometry and drug load.
Release rates were compared for risperidone from Tecoflex® EG-80A polyurethane implants (F.M. 1000 psi) and two grades of Tecophilic® polyurethane implants, HP-60D-35 and HP-60D-60 (EWC, 23.6% and 30.8%, respectively) ( FIG. 8 ). All were sampled weekly for 10 weeks. All implants were of equivalent geometry and drug load.
Release rates were obtained for risperidone from Carbothane® PC-3575A polyurethane implants (F.M. 620 psi) that served as in vitro controls for implants used in the beagle dog study described in Example 4. The in vitro elution study of these implants was initiated on the date of implantation of the subject implants as part of an assessment of in vivo-in vitro correlation.
Example 4
Evaluation of Polyurethane Subcutaneous Implant Devices Containing Risperidone in Beagle Dogs
This study determines the blood levels of risperidone from one or two implants and the duration of time the implants release the drug. Polyurethane-based implantable devices comprising a pellet comprising risperidone were implanted into beagles to determine release rates of risperidone in vivo. The results of the sample analysis are summarized in Table 3 and FIG. 10 . Risperidone is still present at a high level in the dog plasma at the end of the third month. The study was conducted in accordance with WCFP's standard operating procedures (SOPs), the protocol, and any protocol amendments. All procedure were conducted in accordance with the Guide for the Care and Use of Laboratory Animals (National Research Center, National Academy Press, Washington, D.C., 1996), and approved by the Institutional Animal Care and Use Committee in WCFP.
The implants initially contained about 80 mg of risperidone and are designed to deliver approximately 130 mcg/day for 3 months. The test article was stored at between 2-8° C. before use.
The animals were as follows:
Species: Canine
Strain: Beagle dog
Source: Guangzhou Pharm. Industril Research Institute,
Certification No: SCXK(YUE)2003-0007
Age at Initiation of Treatment: 6˜9 months
Weight: 8˜10 kg
Number and Sex: 6 males
Prior to study initiation, animals were assigned a pretreatment identification number. All animals were weighed before administration once weekly, and received cage-side observations daily by qualified veterinarian during acclimation period. All animals were given a clinical examination prior to selection for study. Animals with any evidence of disease or physical abnormalities were not selected for study. The blood sampling was taken as Baseline at the 3rd and 2nd day before implant. Animals were then randomized into to 2 groups, with the dosing schedule provided as follows:
No. of Animals
Dose rate
Total Dose
Group
Dose Route
Male
(mcg/day)
(mg)
1
Subcutaneous
3
130
23 (single
implant
implant)
2
Subcutaneous
3
260
46 (double
implant
implants)
Each animal was anesthetized by general anesthesia via pentobarbital sodium at the dose of 30 mg/kg for device implantation. The drug was released at a steady rate for several months. Half the animals received one implant (group 1) and the others received two implants (group 2). A 5 cm2 area of the shoulder was shaved and 2 mL of marcaine infused under the skin to numb the area. A small incision was made on the shoulder and the device was slid under the skin. The small incision was closed and the animal was allowed to recover and return to his run. Over the next five to seven days, the implantation site was be monitored for signs of infection or reaction. The skin staples were removed when the skin has healed sufficiently. At the end of three months, the devices were removed, just as they would clinically.
Animals were fasted at least four hours prior to blood sampling. Since blood sampling was done in the morning, food was withheld overnight. Blood samples were drawn using a 20 G needle and collected directly into the 5 mL tubes containing sodium heparin and maintained chilled until centrifugation. Samples were then centrifuged at 5000 RPM for 5 minutes at 4° C. The separated plasma was then be transferred into two 3 mL cryo tubes. The samples were labeled with the actual date the sample was taken, the corresponding study day, the dog identification and the duplicate sample designator (either A or B). Samples were kept at −20° C. until ready for analysis.
On two consecutive days, prior to implantation of the delivery device, baseline blood samples were taken. In addition, daily blood samples were taken during the first week and weekly blood samples were taken for the three months following implantation. Two 5 mL blood samples were drawn at each time from each dog. Blood samples were drawn from the cephalic veins primarily; with the saphenous or jugular used as a backup. For both the single and double implant groups, blood samples were drawn at appropriate times as outlined in Table 3 below. Analysis required at least 2 mL of plasma, which required no less than 10 mL of blood drawn for each sample. Analysis of plasma concentrations of risperidone was performed using an LC/MS assay developed for this compound. A single assay was be run for each sample. Samples were collected, held at the appropriate condition and analyzed in batches.
TABLE 3
Concentration of Risperidone in Dog Plasma
Group 1(single implant)
Group 2(double implants)
Group 1
Group 2
Date
Week
Day
1M01
1M02
1M03
2M01
2M02
2M03
Mean
S.D.
Mean
S.D.
−3
—
—
—
—
—
—
−2
—
—
—
—
—
—
1.29
1
1
BLQ
BLQ
0.26
BLQ
0.54
BLQ
0.26
/
0.54
/
1.30
1
2
0.77
BLQ
0.24
0.53
1.86
0.46
0.51
0.37
0.95
0.79
1.31
1
3
1.16
0.78
0.37
1.15
2.70
0.92
0.77
0.40
1.59
0.97
2.01
1
4
1.26
0.79
0.66
1.21
3.85
0.94
0.90
0.32
2.00
1.61
2.02
1
5
1.15
0.66
1.03
1.02
3.13
0.77
0.95
0.26
1.64
1.30
2.03
1
6
1.14
0.58
0.52
0.97
2.96
0.79
0.75
0.34
1.57
1.20
2.04
1
7
1.17
0.72
0.44
0.89
3.27
0.73
0.78
0.37
1.63
1.42
2.11
2
14
1.26
1.03
0.38
1.15
2.81
1.01
0.89
0.46
1.66
1.00
2.18
3
21
1.09
0.70
0.62
1.38
3.09
0.91
0.80
0.25
1.79
1.15
2.25
4
28
1.34
0.84
1.02
1.71
3.55
1.10
1.07
0.25
2.12
1.28
3.03
5
35
2.07
2.23
1.65
1.97
4.54
1.12
1.98
0.30
2.54
1.78
3.10
6
42
1.53
1.13
1.87
1.86
3.34
1.40
1.51
0.37
2.20
1.01
3.17
7
49
1.33
1.09
1.16
1.67
2.23
1.29
1.19
0.12
1.73
0.47
3.24
8
56
1.56
1.29
1.30
1.28
2.09
1.54
1.38
0.15
1.64
0.41
3.31
9
63
1.06
0.83
1.39
1.13
2.27
0.97
1.09
0.28
1.46
0.71
4.07
10
70
1.39
1.00
1.36
1.42
3.51
1.48
1.25
0.22
2.14
1.19
4.14
11
77
1.23
1.15
1.41
1.61
3.47
1.07
1.26
0.13
2.05
1.26
4.21
12
84
1.29
1.10
1.21
1.23
3.47
1.23
1.20
0.10
1.98
1.29
4.28
13
91
1.38
0.88
1.10
1.09
3.22
1.38
1.12
0.25
1.90
1.16
5.05
14
98
1.94
1.01
1.32
1.28
3.76
1.19
1.42
0.47
2.08
1.46
5.12
15
105
1.54
0.98
1.23
1.37
3.48
1.31
1.25
0.28
2.05
1.24
5.19
16
112
1.61
0.94
1.30
1.22
3.98
1.59
1.28
0.34
2.26
1.50
5.26
17
119
1.36
0.97
1.49
1.48
2.66
1.65
1.27
0.27
1.93
0.64
6.02
18
126
1.40
0.93
0.95
0.99
3.25
1.16
1.09
0.27
1.80
1.26
6.09
19
133
1.47
1.19
1.33
1.36
3.36
0.98
1.33
0.14
1.90
1.28
6.16
20
140
1.16
1.25
0.85
3.2*
3.46
1.03
1.09
0.21
2.25
1.72
6.23
21
147
1.16
1.23
1.26
1.17
5.56
1.53
1.22
0.05
2.75
2.44
6.30
22
154
1.63
2.02*
1.44
1.41
5.21
1.34
1.54
0.13
2.65
2.21
7.07
23
161
1.26
1.04
0.92
1.41
44.82**
1.36
1.07
0.17
1.39
0.04
7.14
24
168
1.85
0.9
BLQ
1.5
3.78
1.26
1.38
0.67
2.18
1.39
7.21
25
175
1.69
1
BLQ
1.29
3.46
1.3
1.35
0.49
2.02
1.25
7.28
26
182
1.42
1.09*
0.34
1.7
4.48
1.82
0.88
0.76
2.67
1.57
*re-analysis
**re-analysis, abnormal data
FIG. 9 is a graph of the in vivo plasma concentration of risperidone in the beagle dog study. The lower plot represents the average plasma concentration achieved in dogs implanted with one Carbothane® PC-3575A polyurethane implant (F.M. 620 psi). The upper plot represents the average plasma concentration achieved in dogs implanted with two Carbothane® PC-3575A polyurethane implants (F.M. 620 psi).
Example 5
Evaluation of Polyurethane Subcutaneous Implant Devices Containing Risperidone in Beagle Dogs
Expanding on the data presented in Example 4, this study determines the blood levels of risperidone from one or two larger implants and the duration of time the implants release the drug. Polyurethane-based implantable devices comprising a pellet comprising risperidone were implanted into beagles to determine release rates of risperidone in vivo. The results of the larger implant data are summarized in FIG. 10 (in vitro elution profile) and FIG. 11 (elution in beagle dogs).
The pellets comprising the risperidone formulation used for this study had a diameter of 3.5 mm, a length of about 4.5 mm and a weight of 5.4 mg. The implant had a reservoir length of about 39-40 mm, a wall thickness of 0.2 mm, and internal diameter of 3.6 mm and an overall length of about 45 mm. initially contained about 80 mg of risperidone and are designed to deliver approximately 130 mcg/day for 3 months.
Equivalents
The present disclosure is not to be limited in terms of the particular embodiments described in this application, which are intended as illustrations of various aspects. Many modifications and variations can be made without departing from the spirit and scope of the disclosure, as will be apparent to those skilled in the art. Functionally equivalent methods, systems, and apparatus within the scope of the disclosure, in addition to those enumerated herein, will be apparent to those skilled in the art from the foregoing descriptions. Such modifications and variations are intended to fall within the scope of the appended claims. The present disclosure is to be limited only by the terms of the appended claims, along with the full scope of equivalents to which such claims are entitled. It is to be understood that this disclosure is not limited to particular methods, reagents, compounds compositions or biological systems, which can, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting. As will be understood by one skilled in the art, for any and all purposes, such as in terms of providing a written description, all ranges disclosed herein also encompass any and all possible subranges and combinations of subranges thereof.
While various aspects and embodiments have been disclosed herein, other aspects and embodiments will be apparent to those skilled in the art. All references cited herein are incorporated by reference in their entireties.
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This invention is related to the use of polyurethane-based polymer as a drug delivery device to deliver biologically active risperidone at a constant rate for an extended period of time and methods of manufactures thereof. The device is very biocompatible and biostable, and is useful as an implant in patients (humans and animals) for the delivery of risperidone to tissues or organs.
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FIELD OF THE INVENTION
The present invention relates to a safety net system and method for grain bins and grain carts, and, more particularly, to such a safety net system and method in which a large mesh safety net is attached to anchors positioned along the inside perimeter walls of a grain bin or grain cart such that the net extends over the entire grain storage area of the bin or cart to allow grain ingress while preventing a person from entering the grain storage area.
BACKGROUND OF THE INVENTION
Grain storage structures, including mobile grain carts and stationary grain storage bins are one of the leading causes of farm deaths in the United States. In 1992, the National Institute for Occupational Safety and Health (NIOSH) reported 9 fatalities in the United States from getting suffocated in grain or caught in grain augers in a bin or cart. The State of Illinois alone reported 22 deaths from grain bins, as well as an additional number from grain carts, in the years from 1986-1994. There are a number of causes for these accidents.
When grain is stored with a relatively high moisture content, the grain tends to cake or crust at the surface and form a “bridge” of caked grain which can extend all of the way between the sidewalls of the storage bin or cart. Such bridged grain is extremely hazardous because it prevents grain from flowing into the bin or cart and hides underlying pockets of air beneath the bridge. Farmers will often walk on the bridged grain in an effort to break it up and fall through the bridge, thus getting engulfed in the grain.
Farm workers are also often buried by stored grain as the grain is being emptied from the bottom of the bin or cart. The flowing grain acts much like quick sand, pulling the worker completely under the grain surface. According to NIOSH, forces created by a grain auger unloading grain are so great that, once a person is buried up to the waist, they stand virtually no chance of escaping from the auger force, even with the aid of a safety rope. The force required to remove a person buried to the chest in grain can exceed 2,000 pounds, i.e. about the weight of a small car. Typical unloading rates will fully bury an adult person within one minute. High capacity conveyors can move 5,000 bushels of grain in an hour. At these flow rates, a six foot adult will be totally buried in 15 seconds.
The risk of suffocation increases as grain ages in a bin due to the emission of carbon dioxide, which displaces the oxygen supply in the bin. Thus, even if a worker is not buried completely, he can suffocate due to the lack of oxygen in the bin.
NIOSH recommends the following steps to prevent such accidents, 1) Break up crusts of grain from outside the bin; 2) Avoid entering storage bins or grain carts; 3) If you must enter a bin or cart, stay above the material at all times, assume that all bridged material is unstable, wear safety harnesses with properly fastened life lines, stop the flow of grain prior to entering, and turn on any ventilators
It is clear, then, that a need exists for improved safety equipment for grain storage bins and grain carts. Such equipment should preferably be economical and easily installed, yet reliable, should not interfere with operation of the grain cart or bin and should be passive and not easily defeated in purpose.
SUMMARY OF THE INVENTION
The present invention is a grain storage safety net system and method which is designed to reduce or prevent accidents involving grain carts and grain storage bins. The safety net system is a wide mesh netting which is strong and durable. For example, for grain storage bins, the netting can be made of plastic coated steel cable while for grain carts it might be made of braided nylon or a similar material. The mesh is removably secured to the side walls of the grain storage bin or grain cart via a system of anchors attached about the periphery of the bin or cart. The wide mesh structure of the netting allows grain to freely drop through the netting into the bin or cart, yet prevents a person from intentionally or accidentally entering the bin or cart from above. The inventive method includes the steps of attaching a plurality of anchors to the sides of a grain storage bin or grain cart and then securing a wide mesh netting to the anchors such that it blankets the grain storage area to prevent human entry into the storage area from above, yet allows the free entrance of grain through the netting into the storage area.
OBJECTS AND ADVANTAGES OF THE INVENTION
The objects and advantages of the invention include: providing a grain storage safety netting system and method; providing such a system and method in which a series of anchors are attached to the inside periphery of a grain storage bin or grain cart; providing such a system and method in which a wide mesh netting is removably secured to the anchors in a position in which the netting blankets the top of the grain storage area of the bin or cart; providing such a system and method in which the netting allows the free ingress of grain into the storage area from above, while preventing human entry into the grain storage area from above; providing such a system and method which minimizes or prevents suffocation accidents involving grain storage bins or grain carts; and providing such a system and method which is reliable, easy to install, is economical to manufacture and which is particularly well suited for its intended purpose.
Other objects and advantages of this invention will become apparent from the following description taken in conjunction with the accompanying drawings wherein are set forth, by way of illustration and example, certain embodiments of this invention.
The drawings constitute a part of this specification and include exemplary embodiments of the present invention and illustrate various objects and features thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front elevational view of a stationary grain storage bin, with portions broken away to illustrate the placement of a netting system in accordance with the invention.
FIG. 2 is a greatly enlarged, fragmentary cross-sectional view of a portion of the grain bin, taken along line 2 — 2 of FIG. 1, and illustrating a side view of one of a plurality of net anchors secured to the corrugated side of the bin.
FIG. 3 is a greatly enlarged, fragmentary cross-sectional view of a portion of the grain bin, taken along line 3 — 3 of FIG. 2, and illustrating a top view of the net anchor of FIG. 3 along with a portion of wide mesh safety netting.
FIG. 4 is a cross-sectional view of the entire grain storage bin, taken along line 4 — 4 of FIG. 1, and illustrating the complete safety netting and anchor system.
FIG. 5 is a perspective view of a mobile grain cart equipped with a grain storage safety netting system in accordance with the present invention.
FIG. 6 is a greatly enlarged, fragmentary cross-sectional view of a portion of the grain cart sidewall, taken along line 6 — 6 of FIG. 5, and illustrating a top view of one of a plurality of net anchors secured to the side wall of the cart along with a portion of wide mesh safety netting.
FIG. 7 is a greatly enlarged, fragmentary cross-sectional view of a portion of the grain cart side wall, taken along line 7 — 7 of FIG. 6, and illustrating a side view of the net anchor of FIG. 6 with the safety netting secured thereby.
DETAILED DESCRIPTION OF THE INVENTION
As required, detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which may be embodied in various forms. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed structure.
Referring to the drawings, and particularly FIGS. 1-4, a grain storage safety net system, generally indicated at 1 is attached to a grain storage bin 2 . The safety netting system 1 includes a generally circular wide mesh net 3 , with preferred opening sizes approximately 4″ by 4″. The net 3 is preferably constructed of woven steel cable 4 with a plastic coating 5 . A plurality of net anchors 11 are arrayed about the inside periphery of a cylindrical side wall 12 of the bin 2 about 2-4 feet below a top 13 of the cylindrical side wall 12 . This position allows a person to enter the bin 2 via a ladder 14 , yet the net 3 prevents that person from entering the bin 2 far enough to be immersed in, and therefor suffocated by, a quantity of grain (not shown) stored in the bin 2 . The wide mesh structure of the net 3 allows grain to freely pass through the net 3 but will not allow a person to pass there through. The net 3 is made of a circular peripheral cable 15 and a plurality of attached, criss-crossing cables 16 .
FIGS. 2 and 3 illustrate details of one of the net anchors 11 . FIG. 2 shows a number of corrugations 17 of the bin side wall 12 , with the anchor 11 attached thereto. The anchor 11 includes a vertically oriented steel plate 21 of a length to cover a plurality of the corrugations 17 , with a plurality of attachment bolts 22 and nuts 23 extending through the side wall 12 and through the plate 21 . A pair of ears 24 are attached to and extend inward from the steel plate 21 about midway along the plate 21 . The ears 24 are separated by a distance 25 sufficient to easily accommodate a diameter of one of the peripheral cable 15 of the net 3 . Each of the ears 24 has a bore 32 extending vertically therethrough, with the bores 32 being aligned vertically to allow a keeper such as a retention bolt 33 to be placed therethrough inside the peripheral cable 15 to retain the peripheral cable 15 between the ears 24 . A nut 34 is attached to the bolt 33 to hold it in place.
Referring to FIG. 4, the anchors 11 thus removably secure the safety net 3 via the peripheral cable 15 in a manner such that it blankets an entire upper opening 35 formed by the cylindrical side wall 12 to prevent human ingress therein.
FIGS. 5-7 illustrate a grain storage safety net system, generally indicated at 41 , which is attached to a mobile grain cart 42 . The safety netting system 41 includes a generally rectangular wide mesh net 43 , with preferred opening sizes approximately 3″ by 4″. The net 43 is preferably constructed of attached strands 44 of, for example, braided nylon, but can be made of plastic coated stranded steel cable if additional strength is needed. A plurality of net anchors 51 are arrayed about an inside surface of each of four rectangular side walls 52 - 55 , preferably about 18″ to 24″ below an upper surface of each of the side walls 52 - 55 . Again, this position allows a person to access a generally rectangular top opening 61 of the cart 42 , yet the net 43 prevents that person from entering the cart 42 far enough to be immersed in, and therefor suffocated by, a quantity of grain (not shown) stored in the cart 42 . The wide mesh structure of the net 43 allows grain to freely pass through the net 43 but will not allow a person to pass there through. The net 43 is made of one or more peripheral cable(s) 56 forming a rectangle and a plurality of attached, criss-crossing cables 57 .
FIGS. 6 and 7 illustrate details of one of the net anchors 51 . Each anchor 51 includes a vertically oriented steel plate 62 of a length to accommodate a plurality of attachment screws 63 extending through the plate 62 and into the side wall 52 . The plate 62 is bent in the middle to form a semi-circular protrusion 65 which extends inward into the cart 42 . The protrusion 65 forms a recess 71 of a sufficient size to easily accommodate a diameter of the peripheral cable 56 of the net 43 .
Referring again to FIG. 5, the anchors 51 thus removably secure the safety net 43 in a manner such that it blankets the entire upper opening 61 formed by the side walls 52 - 55 to prevent human entrance therein while allowing the free flow of grain there through.
While certain forms of the present invention have been illustrated and described herein, it is not to be limited to the specific forms or arrangement of parts described and shown. For example, the design of the anchors 11 and 51 is exemplary only and many other variations of attachments could be employed equally effectively. For example, the steel plates could be circular instead of rectangular, which would yield more surface area of attachment. The individual anchors could be replaced with a continuous anchoring system which extends entirely about the periphery of the bin or cart. The anchors 11 and 51 could be reinforced on the opposite side of the respective side walls 12 and 52 - 55 . The nominal mesh opening sizes of the nets 3 and 43 can be any desired dimension, and the net material can be any suitable material as long as the mesh size and material strength are sufficient to prevent human ingress into the grain storage areas of the bin 2 or cart 42 . Other variations will occur to those of skill in the art.
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A grain storage safety net system and method is designed to reduce or prevent accidents involving grain carts and grain storage bins. The safety net system includes a strong and durable wide mesh netting which is secured to the inside periphery of either a grain cart or grain bin via a plurality of anchors. The netting thus blankets an upper ingress opening of the cart or bin, with the wide mesh netting allowing the ingress of grain while preventing human entry therein.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an alarm device for informing reduction of pneumatic pressure of vehicle tires by sensing abnormal change of tire internal pressure of a vehicle when running and by informing it to an operator.
2. Description of the Prior Art
An alarm device for informing an alarm to an operator by sensing abnormal change caused by reduced pressure of internal pressure of a tire in a vehicle, such as a puncture and the like, is well known by for example U.S. Pat. No. 3,810,090. Such device comprises a transmitter having an oscillator for generating a high frequency signal by sensing change of tire internal pressure and a transmitter antenna for radiating an electromagnetic wave by its output, a receiver having a receiver antenna attached on the chassis side of a vehicle for receiving the electromagnetic wave from the transmitter antenna and for processing the electromagnetic wave received by this antenna, and an alarm for generating a warning to an operator.
This kind of devices, however, is liable to be misoperated by receiving an influence of noises from a spark plug generated by a vehicle itself and noises from the outside and lacks reliability. In order to construct a device for receiving no influence of such noises, its mechanism becomes complicated and as a result, the device becomes expensive and impracticable.
SUMMARY OF THE INVENTION
An object of the present invention is to provide an alarm device for informing reduction of pneumatic pressure of a tire, which is simple in construction, light in weight and easy in production.
Another object of the present invention is to provide an alarm device for informing reduction of pneumatic pressure of a tire, which is cheap, reliable and practicable.
The alarm device for informing reduction of pneumatic pressure of a tire according to the present invention senses abnormal change of tire internal pressure of a vehicle by a pressure sensing switch, converts such abnormal change into an electric signal and generates an alarm to an operator. The device comprises an oscillator having an oscillation coil fixed on a chassis side of the vehicle; a resonator consisting of a resonance coil and a capacitor fixed to a peripheral portion of the rotating wheel having a tire adjacent the oscillation coil and for resonating with an electromagnetic wave radiated from the oscillation coil; a signal processing device containing a sensing means for sensing change in an oscillation condition generated in the oscillator due to a resonant condition of the resonator switched on and off in accordance with abnormal internal pressure of a tire and for processing a signal sensed by this sensing means; and an alarm for generating a warning by the output of this signal processing device.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing the principle of an alarm device for informing reduction of pneumatic pressure of tire according to the invention;
FIG. 2 is a block diagram showing the construction of the device according to the invention;
FIG. 3 is a waveform showing the oscillation state of an oscillator of the device according to the invention;
FIG. 4 is a waveform showing the oscillation state of the oscillator in case of receiving an influence of the resonator;
FIG. 5 is a waveform showing the output of a comparator of the device according to the invention;
FIG. 6 is a waveform showing the output of an integrator of the device according to the invention;
FIG. 7 shows cross-sectional view showing an embodiment of the device according to the invention, in which the resonant portion is fixed to a rim inclined portion of the wheel;
FIG. 8 is a cross-sectional view showing another embodiment of the device according to the invention in which the same resonant portion is fixed to a rim flange portion of the wheel;
FIG. 9 is a cross-sectional view showing a construction of the resonance section consisting of a pressure sensing switch and a resonator integrally formed at normal tire internal pressure in detail;
FIG. 10 is a cross-sectional view showing a construction of the resonator at abnormal tire internal pressure;
FIG. 11 is a partial cross-sectional view showing another construction of the pressure sensing switch and the resonator of the resonance section at the normal tire internal pressure; and
FIG. 12 is a partial cross-sectional view showing the pressure sensing switch and the resonator of the resonance section at abnormal tire internal pressure.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, a principal structure of the alarm device for informing reduction of pneumatic pressure of tire according to the invention is shown. The device comprises a resonance section 1, an oscillation section 2 and an alarm section 3. As shown in FIG. 2, the resonance section 1 comprises a pneumatic pressure sensing switch 4 for a change of tire internal pressure of a vehicle and a resonator 5 consisting of a series combination of a resonance coil and a capacitor. The switch 4 and the resonator 5 are integrally formed and rotatably mounted on each wheel of a vehicle as stated hereinafter. The oscillation section 2 comprises an oscillator 6 consisting of a series or parallel circuit of an oscillation coil and a capacitor, and a signal processing device 10 including a detector 7 for detecting the output of the oscillator 6, a comparator 8 for comparing the output of the detector 7 with a reference signal and an integrator 9 for integrating the output of the comparator 8. The oscillator 6 and the signal processing device 10 are mounted at the portion opposed to the chassis adjacent the resonance section 1. In this case, a preferable distance between the resonator 5 and the oscillator 6 is 5-40 mm, preferably 10-30 mm. An preferable oscillation frequency of the oscillator 6 is 20 KHz-10 MHz, preferably 100 KHz-5 MHz. The alarm section 3 comprises a logic circuit 11 for logically operating the output of the integrator 9, an indicator 12 for indicating the output of the circuit 11 and a power supply switch 13. The alarm section 3 is connected to the integrator 9 of the signal processing device 10 through a cable 14 and mounted on a dashboard of the vehicle.
Operation of the alarm device for informing reduction of pneumatic pressure of tire according to the invention will be explained with reference to FIGS. 3-6. The pneumatic pressure sensing switch 4 of the resonance section 1 shown in FIG. 2 senses change of tire internal pressure, particularly reduction of pneumatic pressure, closes during normal internal pressure and opens during abnormal internal pressure thereby to make the resonator 5 switch on or off. The construction of the pressure sensing switch 4 will be explained in greater detail hereinafter. The resonator 5 becomes in a resonating condition under the switched on state of the pressure sensing switch 4 during normal internal pressure and becomes in a non resonating condition under the switched off state of the pressure sensing switch 4 during abnormal internal pressure, i.e., reduced pressure state. FIG. 3 shows a waveform of an oscillating current which exhibits the oscillation condition of the oscillator 6 of the oscillation section 2. FIG. 4 shows the state that the oscillating current of the oscillator 6 of the oscillation section 2 has an amplitude changed by approach of the resonator 5 provided on the wheel side. In FIG. 4, a waveform A shows the state that the resonator 5 is open-circuited by reduction of the tire internal pressure when running and that the oscillator 6 is not influenced by the resonator 5 when the resonator 5 and the oscillator 6 are at positions separated from each other. That is, the resonator 5 has no influence on the oscillator 6 under such a state. A waveform B shows the state that the oscillation current of the oscillator 6 is changed by influence of the resonator 5 under the resonatable state when the tire internal pressure is normal while running.
In the section B of FIG. 4, a section B 1 shows a waveform when the resonator 5 fixed to the wheel approaches the oscillator 6 by rotation. That is, in this section B 1 , if the resonator 5 approaches the oscillator 6, oscillation energy is absorbed in the resonator 5, so that the current in the oscillator becomes abnormal and amplitude of the oscillation current becomes almost zero. A section B 2 shows a waveform when the resonator 5 is separated from the oscillator 6. That is, in the section B 2 , the oscillator 6 does not receive any influence from the resonator 5 so that the oscillation current has again original amplitude. Accordingly, the waveforms shown in the sections B 1 and B 2 correspond to the case when a signal having a certain amplitude is subjected to amplitude modulation.
The output of the oscillator 6 for generating the waveform shown in FIG. 4 is detected by the detector 7 of the signal processing device 10 and a voltage value of a certain amplitude (corresponding to sections A and B 2 shown in FIG. 4) and a voltage value of the modulated amplitude (corresponding to section B 1 shown in FIG. 4) are compared with each other in the comparator 8. The output of the comparator 8 is shown in FIG. 5. A section D shown in FIG. 5 corresponds to the sections A and B 2 shown in FIG. 4, and a section C shown in FIG. 5 corresponds to the section B 1 shown in FIG. 4. The comparator 8 is so constructed that it generates a pulse when a changed amount of an amplitude between the sections B 1 and B 2 becomes more than a certain level and generates no pulse when the amplitude difference between the sections A and B 2 and the sections B 1 becomes less than a certain level. In other words, the comparator compares successive outputs from the detector and provides pulses whenever a sufficient difference is present between successive detector outputs. If amplitude modulation does not occur, due to the opening of switch 4, the detector outputs will all be the same and no pulses will be supplied by the comparator 8.
The waveform shown in FIG. 5, i.e., the output of the comparator 8 is integrated by the integrator 9 of the signal processing device 10 and a waveform shown in FIG. 6 is obtained. That is, the integrator 9 starts integral operation by the leading edge of a pulse in the section C shown in FIG. 5 and completes the integral operation by the trailing edge. Therefore, pulses shown in FIG. 5 are continuously generated during normal running, so that the output of the integrator 9 becomes an integral waveform shown by a section E shown in FIG. 6 and finally saturated, but during abnormal running, i.e., when the tire internal pressure is lowered and the vehicle is stopped, there are waveforms of attenuation amplitude less than a predetermined level SL shown in a section F shown in FIG. 6 and zero amplitude.
When internal pressure of a tire becomes lower than the predetermined value for some reason or other during running of vehicle, the pressure sensing switch 4 of the resonance section 1 becomes the off state and the resonator 5 cannot be operated, the oscillator 6 generates a continuous oscillation signal as shown in the section A of FIG. 4, so that the output of the comparator 8 becomes zero amplitude as shown in the section D of FIG. 5; namely, no pulse is generated and as a result, the waveform shown in the section F of FIG. 6 has an amplitude attenuated to less than the predetermined level SL or zero amplitude. When the amplitude becomes less than the predetermined level SL the output of the integrator is detected by the logic circuit 11 and an alarm is generated from the indicator 12. When this indicator 12 is of an indicating lamp, the lighting of the lamp informs to an operator of vehicle that internal pressure of the tire is reduced to less than the predetermined value. In this case, as an indicating means, color indication can also be used in a manner such that the indicating lamp shows a blue color when neumatic pressure is normal and a red color when the pressure is abnormal.
A relation between the above described predetermined level SL and a discharge time constant of the integrator is so determined that a discharge characteristic curve of the integrator shown in FIG. 6 becomes not more than the predetermined level SL at low speed running, for instance a speed of 10 km/h.
There is shown means of securing the alarm device for informing reduction of pneumatic pressure of tire according to the invention as follows.
FIG. 7 shows means of securing the resonance section 1 of the alarm device according to the invention to a peripheral portion of a wheel, for instance a recessed inclining portion of a rim 21 for supporting a tire 20. In this embodiment, the oscillation section 2 is secured to a bracket 23 of a chassis 22 at the position opposed to the inclined portion of the rim. This oscillation section 2 is connected to the alarm section 3 through the cable 14. The alarm portion 3 is mounted to for instance a dashboard at the driver's seat.
FIG. 8 shows means of securing the resonance section 1 of the alarm device according to the invention to a rim flange portion 24 of the wheel. In FIG. 8 like parts of the component shown in FIG. 7 are denoted with like numerals. In this embodiment, the resonance section 1 is secured to the flange portion 24 of the rim 21, so that a valve 25 is communicated with the pressure sensing switch 4 of the resonance section 1 through a cap nut 26 screwed to the valve 25 and an air pipe 27.
FIGS. 9 and 10 show the states that the resonator 5 becomes in an operating condition and an inoperating condition by switching on and off of the pressure sensing switch 4 of the resonance section 1 shown in FIG. 7 in accordance with internal pressure of the tire.
FIG. 9 shows the case that the internal pressure of the tire 20 is normal and the pressure sensing switch 4 is closed. In this embodiment, the resonance section 1 comprises a resin molded body 33 having a rim flange portion 31 and a screw threaded step column 32, sealed a resonance coil 30 and a capacitor C therein, a cylindrical threaded spring case 34 threadedly mounted on a large threaded column portion 32', spring 36 provided in a spring chamber 35 formed between the cylindrical spring case 34 and a small column portion 32" of the resin molded body 33, a metal switch plate 37 engaged with a free end of the spring 36 and made into contact with coil ends 30', 30" projected to the end surface of the small column portion 32", a bellofram 38 for compressing the metal switch plate 37 to the coil ends 30', 30" against force of the spring 36 when the internal pressure of the tire is normal, and a bellofram press plate 40 having an air path 39 at the center and screwed into the cylindrical spring case 34. That is, the pressure sensing switch 4 of the resonance section 1 shown in FIG. 2 comprises the bellofram 38, the metal switch plate 37 and the spring 36. In case of securing such resonance section 1 to a wheel, the rim flange portion 31 and the cylindrical spring case 34 are fixed to the rim 21 of the wheel through two O-rings 41, 42. The step column 32 is inserted into a hole bored at the inclined portion of the rim 21 through the O-rings 41, 42 and the screw of the cylindrical spring case 34 is threaded into the screw portion of the step column 32 from the inside of the tire 30 and sealed. The spring 36 is inserted into the spring chamber 35 formed between the small column portion 32" and the cylindrical spring case 34 and the metal switch plate 37 and bellofram 38 are placed on the free end of the spring. The bellofram 38 is fixedly secured by screwing the bellofram press plate 40 into the end portion of the cylindrical spring case 34 thereby securing the periphery of the bellofram 38 to the cylindrical spring case 34.
When the internal pressure of the tire is normal, the bellofram 38 is pressed to the end portion of the small column portion 32" against force of the spring 36 by internal pressure of the tire 20 through the air path 39 at the center of the bellofram press plate 40, so that the ends 30' and 30" of the resonance coil are short-circuited by the metal switch plate 37.
When the internal pressure of the tire is abnormal, i.e., the internal pressure of the tire is reduced, however, the bellofram 38 and the metal switch plate 37 are pushed back in the direction of the bellofram press plate 40 by force of the spring 36 as shown in FIG. 10, so that the coil ends 30', 30" are separated from the metal switch plate 37 and as a result, the resonator 5 becomes in an inoperating condition.
FIGS. 11 and 12 show the construction of the pressure sensing switch 4 of the resonance section 1 when the resonance section 1 is secured to the rim flange portion 24 as shown in FIG. 8.
FIG. 11 shows the construction of the pressure sensing switch 4 when the internal pressure of the tire 20 is normal. In this embodiment, the pressure sensing switch comprises a bellofram 50, a piston 51 and a contact ring 52. A cylinder portion of the piston 51 is formed by threading a metal spring press member 53, an insulating ring 54, a metal case 55 and a bellofram press member 56 with each other. In this case, a spring chamber 57 is formed between the piston 51 and the metal spring press member 53, the insulating ring 54 and the metal case 55 of the cylinder, and a metal spring 58 is put in this chamber 57. The metal spring press member 53 and the bellofram press member 56 are provided with terminals 59, 60 and lead pieces 61, 62, respectively, and the resonance coil 30 and the capacitor C of the resonator 5 are connected to these lead pieces 61, 62 and integrally assembled. The bellofram press member 56 is bored with a hole at the center so as to form an air path 63 and the air path 63 is communicated to the valve 25 through the air pipe 27 and the cap nut 26 as shown in FIG. 8.
When the internal pressure of the tire is normal, the pressure is transmitted to the bellofram 50 through the valve 25, the cap nut 26, the air pipe 27 and the air path 63, thereby pressing the piston 51 against force of the metal spring 58, and then the contact ring 52 provided in the flange portion 51' of the piston 51 is made into contact with an extension 55' of the metal case 55. The resonator 5 is then closed through the lead piece 61, the terminal 59, the metal spring press member 53 made of metal, the metal spring 58, the contact ring 52, the metal case 55, the bellofram press member 56, the terminal 60 and the lead piece 62.
When the internal pressure of the tire is abnormal, i.e., the internal pressure is reduced, the bellofram 50 and the piston 51 are pushed back to the bellofram press member 56 against force of the metal spring 58 as shown in FIG. 12, so that the extension 55' of the metal case 55 is separated from the metal contact ring 52 and the resonator 5 is opened.
The invention is not limited to the above described embodiments but can be modified variously. For example, as a means for detecting change of the oscillation condition of the oscillator, use may be made of a frequency detection means. In this case, the detector 7 is used as a frequency detector, and the comparator must be constructed to generate output pulses in case of changing the frequency.
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An alarm device for informing reduction of pneumatic pressure of vehicle tires by sensing abnormal change of tire internal pressure of a vehicle when running by a pressure sensing switch, by converting the thus sensed abnormal change into an electric signal and by generating an alarm to an operator. This device comprises an oscillator having an oscillation coil fixed on a chassis side of the vehicle; a resonator consisting of a resonance coil and a capacitor fixed to a peripheral portion of the rotating wheel having tire adjacent the oscillation coil and for resonating with an electromagnetic wave radiated from the oscillation coil; a signal processing device containing a sensing means for sensing change in an oscillation condition generated in the oscillator due to a resonant condition of the resonator switched on and off in accordance with abnormal internal pressure of a tire and for processing a signal sensed by this sensing means; and an alarm for generating a warning by the output of this signal processing device.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This patent application claims the priority and benefit of U.S. provisional patent application 62/030,724, entitled “Automatic Creation of Applique Cutting Data from Machine Embroidery Data”, filed on Jul. 30, 2014 and which herein incorporated by reference in its entirety.
TECHNICAL FIELD
[0002] Embodiments are related to sewing, embroidery, embroidery machines, embroidery design software, and automated cutting machines.
BACKGROUND
[0003] Applique is often done by labeling the color steps with the words “Applique” and either “Position” or “Material”. The steps always have to be in order. The first sewn section is the Position. This sewing puts an outline on the project being embroidered. This outline is the location of the material applique which that will be applied to a project cloth at this point in time. The next sewing step is the “Material” which can vary in type of stitch, such as single run, double (out and back), or even zigzag. This sewing anchors the material of the applique to the project. The next step a sewer must do is to cut the applique around the outside of the stitches sewn by the “Material” step. They do this by hand using a pair of scissors generally. Once the excess fabric is removed, the sewing is completed to finish the project.
[0004] Alternatively, a sewer can run the outline of the design on some other item such as paper. This allows them to place the paper with the outline on the cloth that is to be the applique, allowing the sewer to cut the paper and cloth together. This saves loss of registration by the machine during the sewing process.
[0005] Yet another alternate method is to print out a precise template of the applique position color using a normal printer and software that is calibrated for this purpose. All of these methods require the user to hand-cut the applique cloth.
[0006] A different process also exists, wherein certain dies have been made to cut cloth. AccuQuilt.com has typical examples. The dies using manual or pneumatic or electrical means can cut the cloth. This means the cloth must be applied using a sewing machine, not with embroidery.
[0007] U.S. Pat. No. 6,600,966 titled “SOFTWARE PROGRAM, METHOD AND SYSTEM FOR DIVIDING AN EMBROIDERY MACHINE DESIGN INTO MULTIPLE REGIONAL DESIGNS” issued to Brian D. Bailie on Jul. 29, 2003. U.S. Pat. No. 6,600,966 is herein incorporated by reference in its entirety for its teachings of embroidery techniques, embroidery file formats, embroidery file reading/writing/modification, use of grids, analysis software applied to embroidery, identifying and using embroidery regions, and automated and computerized embroidery.
[0008] U.S. Pat. No. 6,633,794 titled “SOFTWARE PROGRAM AND SYSTEM FOR REMOVING UNDERLYING STITCHES IN AN EMBROIDERY MACHINE DESIGN” issued to Brian D. Bailie on Oct. 14, 2003. U.S. Pat. No. 6,633,794 is herein incorporated by reference in its entirety for its teachings of embroidery techniques, embroidery file formats, embroidery file reading/writing/modification, use of grids, analysis software applied to embroidery, identifying and analyzing individual stitches in their context in an embroidery design, and automated and computerized embroidery.
[0009] U.S. Pat. No. 6,732,008 titled “SOFTWARE PROGRAM AND SYSTEM FOR EVALUATING THE DENSITY OF AN EMBROIDERY MACHINE DESIGN” issued to Brian D. Bailie on May 4, 2004. U.S. Pat. No. 6,732,008 is herein incorporated by reference in its entirety for its teachings of embroidery techniques, embroidery stitches, embroidery file formats, embroidery file reading/writing/modification, use of grids, analysis software applied to embroidery, identifying and analyzing individual stitches in their context in an embroidery design, and automated and computerized embroidery.
[0010] U.S. Pat. No. 6,944,605 titled “EXPERT SYSTEM AND METHOD FOR CREATING AN EMBROIDERED FABRIC” issued to Brian D. Bailie on Sep. 13, 2005. U.S. Pat. No. 6,944,605 is herein incorporated by reference in its entirety for its teachings of embroidery techniques, stitches, fabrics, analysis. Further reasons for incorporating U.S. Pat. No. 6,944,605 in its entirety is its teaching of creating and applying rules in the context of embroidery, its teaching of analysis for offering recommendations to human operators, its approach to embroidery design flow, and its parametric selection teachings.
[0011] U.S. Pat. No. 7,457,683 titled “ADJUSTABLE EMBROIDERY DESIGN SYSTEM AND METHOD” issued to Brian D. Bailie on Nov. 25, 2008. U.S. Pat. No. 7,457,683 is herein incorporated by reference in its entirety for its teachings of embroidery techniques, embroidery stitches, embroidery file formats, embroidery file reading/writing/modification, analysis software applied to embroidery, identifying and analyzing individual stitches in their context in an embroidery design, and automated and computerized embroidery.
[0012] Prior art references having different authorship are now presented. The references are also incorporated by reference in their entirety for their teachings of certain aspects of embroidery, embroidery techniques, and the automation of aspects of embroidery processes.
[0013] U.S. Pat. No. 4,920,902 titled “Automatic pattern sewing machine” issued to Takenoya et al. on May 1, 1990. It is herein incorporated by reference for its teachings of a machine that automatically sews patterns, teaching of applique techniques, teachings of pattern data, and teachings of automatic or assisted modification of the pattern data.
[0014] U.S. Pat. No. 1,741,620 titled “Hemstitched applique work and process of making the same” issued to Fixler on Dec. 31, 1929. It is herein incorporated by reference in its entirety for its teachings of stitches, embroidery, and embroidery knowhow.
[0015] U.S. Pat. No. 8,557,078 titled “Applique printing process and machine” issued to Marino et al. on Oct. 15, 2013. It is herein incorporated by reference in its entirety for its teachings of automatically producing an applique based on a printing type process, for its teachings of certain embroidery/applique techniques, and for its teaching of cutting cloth/materials for appliques.
[0016] U.S. Pat. No. 5,438,520 titled “Method of creating applique data” issued to Satoh et al. on Aug. 1, 1995. It is herein incorporated by reference in its entirety for its teachings of applique techniques, applique data, generation and manipulation of applique data, and for the machinery and equipment (embroidery machine, computer, cutter, etc.) that can be used in association with designing and creating appliques.
[0017] U.S. Pat. No. 7,882,645 titled “System and method for making an applique” issued to Boring on Feb. 8, 2011. It is herein incorporated by reference in its entirety for its teachings of applique techniques, applique templates, and applique design.
[0018] U.S. Pat. No. 3,226,732 titled “Applique article and method of manufacture” issued to Zerilli on Jan. 4, 1966. It is herein incorporated by reference in its entirety for its teachings of applique techniques, applique layers, and applique design, cutting, stitching and application.
[0019] Three related patents are also incorporated herein by reference in their entirety. U.S. Pat. No. 5,430,658 titled “METHOD FOR CREATING SELF-GENERATING EMBROIDERY PATTERN” issued to Davinsky et al. on Jul. 4, 1995. U.S. Pat. No. 5,668,730 titled “METHOD FOR AUTOMATICALLY GENERATING CHAIN STITCHES” issued to Tsonis et al. on Sep. 16, 1997. U.S. Pat. No. 5,771,173 titled “METHOD FOR AUTOMATICALLY GENERATING A CHENILLE FILLED EMBROIDERY STITCH PATTERN” issued to Tsonis et al. on Jun. 23, 1998. These three patents largely have the same inventors and are included by reference herein in their entireties for their teachings of developments and refinements in defining, outlining, and filling embroidery shapes. They are also incorporated by reference for their teachings of automatic or algorithmic generation of chain stitch outlines, of automatic or algorithmic generation and of embroidery patterns, of computer aided design applied to embroidery, of embroidery techniques and processes, and for their detailed teachings of stitch types, properties, and uses.
[0020] A document titled “A Survey of Polygon Offseting Strategies” by Fernando Cacciola was incorporated into the filing of U.S. provisional patent application 62/030,724 and is thereby also herein incorporated by reference in its entirety. It is incorporated herein for its teachings of techniques for offsetting polygons and for other transformations and operations.
[0021] Applique is a popular technique and embroidery designs for applique exist in abundance. Systems and methods for saving the sewers time by producing properly cut out designs are needed.
BRIEF SUMMARY
[0022] The following summary is provided to facilitate an understanding of some of the innovative features unique to the disclosed embodiments and is not intended to be a full description. A full appreciation of the various aspects of the embodiments disclosed herein can be gained by taking the entire specification, claims, drawings, and abstract as a whole.
[0023] Aspects of the embodiments address limitations and flaws in the prior art by analyzing machine embroidery data to automatically produce cutting data that a cutting machine can interpret to cut out the applique. An applique data file specifies an applique design and contains sewing data. The sewing data can include sewing vectors and jump commands. The sewing vectors specify stitches as, for example, movements, stitch points, or needle penetrations. The jump commands split the sewing vectors into subsections. For example, one subsection can be an applique outline while a number of other subsections can be holes or openings in the applique outline. An embroidery machine can read and interpret the applique data file to thereby stitch a pattern onto a piece of cloth. A cutting machine can read the cutting data automatically created by the embodiments disclosed herein and cut the applique out of a piece of cloth.
[0024] Aspects of the embodiments can be a non-transitory memory containing program instructions readable by a computer for performing certain operations. Other aspects of the embodiments can be the steps or operations performed in automatically creating the cutting data from the applique data file.
[0025] It is, therefore, an aspect of the embodiments to access an applique data file and to create lists of sewing vectors. If there is only one subsection, then there is only one list. If a jump command splits the sewing vectors into two or more subsections, then there can be two more or lists.
[0026] It is also an aspect of the embodiments to normalize the lists. Normalizing the lists by discarding certain sewing vectors or data such as tie-off data, double stitches, and other sewing artifacts do not affect the applique outline that is to be cut.
[0027] It is a further aspect of the embodiments to close the lists. It is possible for the endpoint on a list to be far enough from the start point that one or more additional sewing vectors are needed to close the list so that it defines a closed outline.
[0028] It is a yet further aspect of the embodiments that an outline contains holes. The dosed paths specified by the lists specify at least one outline and may specify a number of holes for applique designs that contain openings. The embodiments can determine that a list is an outline and that another list is a hole. The embodiments can also create objects that include an outline list and one or more hole lists for holes inside the outline.
[0029] It is yet another aspect of the embodiments that the outlines are inflated by a positive amount to make them slightly larger and for the holes to be inflated by a negative amount to make them slightly smaller.
[0030] It is still yet another aspect of the embodiments to simplify the lists by removing points using certain known algorithms such as the Douglas-Peucker algorithm or any of its readily available derivatives. The outline can then be further simplified by fitting them to Bezier outlines using common fitting technique such as Newton-Raphson least squares fitting techniques or other line and curve fitting algorithms that are known in the arts of graphing or computer graphics.
[0031] It is a still yet further aspect of the embodiments to create a preview that can be seen by a person. An image can be produced by copying a first bitmap into the image sections outside of the applique outline and inside any holes in the applique. A second bitmap can be copied into image sections inside the applique outline and outside any holes in the applique.
[0032] An alternative embodiment can use the applique design to draw vectors onto a bitmap. The bitmap should be sized such that it is large enough to include all the vectors and also large enough that the shortest vector is at least two pixels long. The bitmap can then be conditioned to produce a better outline. Thinning algorithms and skeletonizing algorithms can condition the bitmap. The applique outline can then be traced by finding a first pixel in the outline and then simply following along the outline. Cutting data can be produced from the applique outline traced in the image. Those familiar with image processing and digital image manipulation are familiar with a number of common thinning an skeletonizing algorithms.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The accompanying figures, in which like reference numerals refer to identical or functionally similar elements throughout the separate views and which are incorporated in and form a part of the specification, further illustrate the present invention and, together with the background of the invention, brief summary of the invention, and detailed description of the invention, serve to explain the principles of the present invention.
[0034] FIG. 1 illustrates a high level diagram of a processor executing stored instructions to create a cutting data file from an applique data file in accordance with aspects of the embodiments;
[0035] FIG. 2 illustrates a high level block diagram of data transformations and processes to create a cutting data file from an applique data file in accordance with aspects of the embodiments;
[0036] FIG. 3 illustrates a high level block diagram of data transformations and processing of a bitmap to create a cutting data file from an applique data file in accordance with aspects of the embodiments;
[0037] FIG. 4 illustrates an image with irregular edges in association with automated global underlay in accordance with aspects of the embodiments;
[0038] FIG. 5 illustrates an image of needle penetrations in association with automated global underlay in accordance with aspects of the embodiments;
[0039] FIG. 6 illustrates the image of FIG. 5 after triad filtering in association with automated global underlay in accordance with aspects of the embodiments;
[0040] FIG. 7 illustrates the image of FIG. 6 after simplification of the outline and inflation in association with automated global underlay in accordance with aspects of the embodiments;
[0041] FIG. 8 illustrates a tatami fill of the image of FIG. 7 in association with automated global underlay in accordance with aspects of the embodiments;
[0042] FIG. 9 illustrates the tatami filled design of FIG. 8 with embroidered letters in association with automated global underlay in accordance with aspects of the embodiments;
[0043] FIG. 10 illustrates an echo quilting design with embroidered letters in association with automated echo quilting in accordance with aspects of the embodiments;
[0044] FIG. 11 illustrates an automatically generated pattern around embroidered letters in association with automated stippling in accordance with aspects of the embodiments;
[0045] FIG. 12 illustrates an automatically generated pattern from a “Drunkard” algorithm in association with automated stippling in accordance with aspects of the embodiments;
[0046] FIG. 13 illustrates an automatically generated less randomized version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments;
[0047] FIG. 14 illustrates an automatically generated “Leafy” version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments; and
[0048] FIG. 15 illustrates an automatically generated “Geometric” version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments.
DETAILED DESCRIPTION OF THE INVENTION
[0049] The particular values and configurations discussed in these non-limiting examples can be varied and are cited merely to illustrate embodiments and are not intended to limit the scope thereof.
[0050] The embodiments will now be described more fully hereinafter with reference to the accompanying drawings, in which illustrative embodiments of the invention are shown. The embodiments disclosed herein can be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Like numbers refer to like elements throughout. As used herein, the term “and/or” includes any and all combinations of one or more of the associated listed items.
[0051] The disclosed embodiments are described in part below with reference to flowchart illustrations and/or block diagrams of methods, systems, and computer program products and data structures according to embodiments of the invention. It will be understood that certain blocks of the illustrations, and combinations of blocks, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the block or blocks.
[0052] These computer program instructions may also be stored in a non-transitory computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function/act specified in the block or blocks.
[0053] The computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions/acts specified in the block or blocks.
[0054] FIG. 1 illustrates a high level diagram of a processor 104 executing stored instructions 102 to create a cutting data file 107 from an applique data file 105 in accordance with aspects of the embodiments. A non-transitory processor readable medium 101 contains the stored code representing instructions 102 that the processor 104 running in computer 103 accesses. The processor 104 accesses applique data file 105 and processes the sewing data 106 to produce cutting file 107 . A cutter 109 provided with applique cloth 108 can process the cutting data file 107 to thereby cut out an applique 110 . An embroidery machine 112 provided with cloth 111 and applique 110 can process applique data file 105 to thereby sew the applique onto the cloth 113 .
[0055] FIG. 2 illustrates a high level block diagram of data transformations and processes to create a cutting data file 107 from an applique data file in accordance with aspects of the embodiments. The applique data file contains sewing data 106 . The sewing data contains sewing vectors 201 and jump commands 202 . There are also sewing artifacts 203 in the sewing data 106 . Examples of sewing artifacts 203 include data for tie-offs, double stitching, and sewing paths that cross in on themselves without stopping.
[0056] Two lists 204 , 207 are created from the sewing data 106 because, in this example, the sewing data 106 contains a jump command 202 . The sewing vectors 205 before the jump command can go into list 1 204 while the sewing vectors 208 after the jump command can go into list 2 207 . In practice, more jump commands can result in more lists being created. Furthermore, list 1 204 and list 2 207 do not contain jump commands.
[0057] The lists 204 , 207 are normalized to remove sewing artifacts 206 , 209 . Analysis indicates that list 2 defines a closed path, meaning that the first and last points in the list of sewing vectors are closer than a predetermined threshold. Analysis indicates the list 1 204 does not define a closed path. List 1 204 is amended to produce list 1 209 containing sewing vectors 210 wherein the path is closed by adding additional sewing data to the list to thereby close the path. For example, a stitch can be added that connects the first and last points.
[0058] List 1 209 and list 2 207 are analyzed and it is determined that the closed path defined by sewing vectors 208 lies inside of the closed path defined by sewing vectors 210 . List 1 209 therefore defines an outline while list 2 207 defines a hole inside the outline. List 1 209 and list 2 207 are combined into object 1 211 because the hole is inside the outline. Object 1 211 can then be inflated by inflating the outline by a positive amount and inflating the hole by a negative amount. In the example, list 1 209 has been inflated by a positive amount into list 1 212 while list 2 207 has been inflated by a negative amount into list 2 213 .
[0059] Inflation is a common geometric term which is slightly different than scaling. It is also known as polygon offsetting and is well known in the art. Where there are ‘Holes’ the inflation uses a negative value, thus reducing the size of the hole.
[0060] Object 1 can be simplified to include simplified lists such as list 1 214 and list 2 215 . Simplification is the elimination of extra points in the sewing data. There are a number of well-known algorithms such as Douglas-Peucker and its derivatives that eliminate extra points. The outline and hole can also be fitted to Bezier outlines using common fitting techniques such as Newton-Raphson or least squares fitting techniques.
[0061] Object 1 can then be transformed into cutting data because the object's data is forward moving, non-repetitive, and possibly spline or cubic Bezier format that is useful to a cutter.
[0062] FIG. 3 illustrates a high level block diagram of data transformations and processing of a bitmap 307 to create a cutting data file 107 from an applique data file 105 in accordance with aspects of the embodiments. The applique data file 105 , in an embroidery file format, contains an applique design 301 with sewing data 106 . The sewing data can contain sewing vectors 201 , jump commands 202 , and sewing artifacts 203 . Exemplary sewing vectors 201 include stitches 302 , movements 303 , or needle penetrations 304 .
[0063] A bitmap 307 is created that is sized at least as large as the design size 306 and such that the shortest sewing vector 305 is at least two pixels long. The sewing vectors are then drawn onto the bitmap 308 . The bitmap can be conditioned 309 by applying a thinning algorithm or a skeletonizing algorithm. The bitmap can then be traced to find a point on the outline and then the outline traced 310 to produce a list, as discussed above. The list is closed if analysis finds that it is open. The cutting data 107 can then be produced from the list.
[0064] The embodiments can consist of the usual apparatus of a computer, a program, and an embroidery machine. The software can look for sections of the design with appropriate labels. It also allows the user to select a section for applique. The software uses the sewing data (stitches) which consist of a series of relative or absolute movements (vectors or stitch points or needle penetrations) to create an outline. That outline is then saved in a format that is useful to a cutting machine. Cutters, similar to the vinyl cutters used by sign shops everywhere, have been adapted to the purpose of cutting fabric recently. Currently, the cutters force the user to draw the outlines for the cut using a manual drawing process—using bezier or point input modes. In some cases, they can scan in a picture and auto-trace an outline. These are separate sets of steps which are prone to terrible inaccuracy when making the outline.
[0065] The process for converting is not a simple matter of converting formats of the sewing vectors into cutting vectors. The stitch data for an applique position may contain a set of vectors that handle multiple outlines, including holes in outlines, as well as sewing requirements such as tie-offs which are extra stitches that ensure the thread is working and able to be cut between sections. What's required is forward-moving-only data that forms dosed polygon outlines.
[0066] Exemplary descriptions of steps and instructions for performing the process are now provided.
[0067] The stitch data may contain both normal sewing vectors and “jump” commands. These jumps are non-sewing movement commands. When the process sees these commands in the data, it can separate the data into subsections, organized as linked lists with each subsection containing the sewing vectors between two jump commands. The end cases, obviously, are the sewing vectors from the stitch data start to the first jump command and the sewing vectors from the last jump command to the end of the stitch data. Note that here linked lists are used in the interests of a simple explanation whereas, in practice, different data structures such as arrays, trees, hash tables, key-value pairs, etc., can be used to similar effect.
[0068] The lists, aka subsections, are now processed into normalized data, which removes certain sewing artifacts.
[0069] For each list:
[0070] Advance a few stitches into the data, looking for a Euclidean distance of travel away from the start point, (2 mm best current) until a new point is found. Once that is reached, the skipped stitch data in between can be discarded. This process is referred to as ‘skipping tie-off data’ and is used throughout. This Euclidean distance and any of the other tolerances or distance discusses below can be user specified parameters having default values or can be constant values. Note, Euclidean distance is specified here as it has proven useful although other distance measures such as Mahalanobis, Manhattan, etc., can be used in appropriate circumstances.
[0071] It is entirely possible for the path to continue around its required outline and past the start point, and it frequently does. The process therefore scans the data iteratively and tracks its path. When and if the path comes back within a tolerance, the closing distance, of the start point, the shape is assumed closed at that point, and that section of data is saved for later processing. The closing distance is typically a distance from the current stitch end to the start point. If found, the stitch whose end is within the closing distance is the closing stitch for that particular shape.
[0072] If the length of the design, meaning the total length of all vectors is below a threshold, or the number of useable points is too small (a line, not a polygon), then the list is discarded. The data may be double-stitched, wherein the stitches travel to an endpoint, then reverse direction of travel to come back at or near the start point. Therefore the process scans the data looking for double-stitches and removes the double-back section. The process also discards any data beyond the closing stitch.
[0073] It is possible that the data at this point does not form a properly closed path and there is no closing stitch. The path is closed in the usual manner of adding a new tail point between the closing stitch and the start point which closes the outline.
[0074] It is also possible that a stitch other than a single or double stitch may exist in the stitch data. This can be determined by analyzing the points in the data and seeing how many are repeated within a certain tolerance, usually 0.2 mm. If there is a plurality of these, an alternate method must be used on this data to get a set of points that run in a forward direction. This can be accomplished with an alternate process, such as:
[0075] Alternate Method:
[0076] Create a 2-color (e.g., black and white) bitmap that will represent the image, using a pixel ratio that is known so that the vectors will have meaningful scale when drawn such as the shortest vector having a length of two or possibly more pixels. Draw the stitches into the bitmap. Apply a thinning algorithm to the bitmap which will provide sensible single-pixel data. Scan the bitmap for a starting pixel and follow the outline, tracing the path. Thinning algorithms are suggested here because they have been used with success. Other well-known image processing algorithms can similarly skeletonize an image or bitmap.
[0077] These steps are well known in all areas of computer graphics, but not used in the embroidery art for this purpose. Once a plurality of pixels has been discovered, the results are checked against the same steps as above for length and closure. If it is long enough, but open, then it is closed.
[0078] Alternate Method:
[0079] The user might use an image of the stitch data and draw on top of it using ordinary computer drawing tools to create an outline from scratch. This is also useful if the user wants to add an applique section to a design that currently does not have one, but is a good candidate (visually) for one.
[0080] Sequencing the resultant lists.
[0081] Now that we have a plurality of lists containing clean forward-moving-only vector data (cutters don't like a lot of reversals), we can now sort them into outlines and holes.
[0082] For each point-list, analyze the remaining point-lists to see if they wholly contain this list. This is achieved using the Winding Number rule, or any similar technique. Lists which are not wholly contained are separated into a group of ‘outline’ lists, and holes are left in the list of point-lists.
[0083] Next each hole is analyzed to see which outline contains it, and they are grouped together. This group is an ‘object’. Each object has a single outline and possibly a plurality of holes. There may be several objects.
[0084] Optionally:
[0085] As applique cloths will need to be attached to the cloth being embroidered, there are always stitches provided to do so in the applique design. These stitches are known as the ‘Material’ stitches. These stitches are either automatically generated or hand-laid by the artist who is creating the design. Often times the automatic creation of these material stitches uses the exact same form and size as the outline of the applique. This process can work if the applique is hand cut by the sewer after the applique has been sewn. However, if the applique is cut in advance, the material stitching may not penetrate the applique cloth, as the applique cloth will be the same size as the stitching. Therefore at the direction of the user, or automatically, the outline of the applique shape may be inflated before cutting. Making this decision can be done as simply as examining the size of the applique and the size of the material stitching, and if they are within a small tolerance (1-2 mm) then the inflation needs to occur.
[0086] Inflation is a common geometric term which is slightly different than scaling. It is also known as polygon offsetting and is well known in the art. Where there are ‘Holes’ the inflation uses a negative value, thus reducing the size of the hole.
[0087] Optional, depending on the needs of the cutter device:
[0088] Now, each point-list within each object is processed by simplification—thus eliminating extra points which can make the cut difficult. The algorithm used is one created by Douglas-Peucker or any readily available derivative. Then the outlines are fitted to Bezier outlines using a common fitting technique such as Newton-Raphson least squares fitting techniques.
[0089] Finally each object's data, now in forward-moving, non-repetitive, possibly spline or cubic Bezier format is ready for output to a cutter. The cutters each have a format for their data. A typical example is the HPGL.plt format, which is widely used, although there are many proprietary formats too.
[0090] Additionally:
[0091] Once a cut outline (cutline) has been created, it is possible to store this cutline alongside the sewing data in the apparatus. This adds a novel benefit of being able to allow the user to select an image, or for the software to create one, simulating fabric of a given or user-chose color, which image is then used in the display to the user for visualization of the applique. The process of display uses the cutline, which is always a closed shape as described, and a pair of bitmaps which will be used to represent the image. The first image is called a bitmap mask and this image is filled with a background color of known value. Then the cutline is drawn on the mask with a different color. The cutline is always at least one pixel smaller on each edge in its representation on the bitmap than the bitmap size.
[0092] A loop is run for each pixel in the bitmap and an evaluation is made—if the pixel is background colored data, a determination of that point and whether or not it is inside the actual object is made. Inside is determined true if the point is within the outline, and not within any holes. If it is determined that the point is inside the object shape, then a seeded fill operation is performed, which is a color that fills the inside area, and that color is not background. At the end of the loop the mask bitmap contains a binary image of pixels which are either background or contained in the object.
[0093] The next step is to use an image, represented by another bitmap, and placed over the mask bitmap, and a display bitmap. Where the mask bitmap contains drawn pixels, the matching pixel from the image is copied into the display.
[0094] In a previous step, the input image may be selected by the user, and certain transforms applied, including brightness, contrast, sepia tone, hue and saturation adjustments for the purpose of matching other colors and even editing may be performed. All of which steps are common to the computer graphics art, and included as a step in the process.
[0095] It is not assumed that masked bitmaps are novel. Just the implementation of them in the place is described. There are also transforms that can be applied, too numerous to mention, but by example: rotation, morphing, and alpha channel.
[0096] Another Addition:
[0097] Prior art (Bailie) has disclosed a method for removing overlapping stitches from a design. This improves the design by removing density which results in damage to equipment, downtime, and even simple production time. The new cutline and masked bitmap allows the process to be extended in such a way that the applique material is now an additional component of the occlusion—causing other stitches which are previously sewn to be unnecessary. Their removal is very useful for the same reasons just mentioned.
[0098] An additional item is useful: Tagging the sewing data which are Position and Material runs as NOT to be removed is useful. This stitch data which would be removed during the process normally can now be exempted from the removal. The reason is that Position and Material runs are required where applique materials will be overlapped, according to the designer of the embroidery design. In this case, the stitches that are not part of Position and Material stitches should be removed, and would be, as the subsequent applique would cover them.
[0099] Aspects related to automatic global underlay for embroidery designs:
[0100] It is often desired to place embroidery on towels or any other items that are composed of a cloth with a texture known as pile. This poses difficulty for the embroiderer as the process of embroidery on that kind of cloth requires a substantial number of stitches to flatten out that cloth before the design is sewn. If the underlying stitches are insufficient, the design will have the texture of the cloth protruding above the embroidery and/or making the texture of the embroidery irregular.
[0101] As most designs are not created with this intended purpose, it would be beneficial if there were a way to automatically add such an underlay to any design. This can be accomplished using (the usual apparatus) plus a set of bitmaps, and stitch-creation process.
[0102] First a masked bitmap is created. It is filled with no color (black). Then, using a single color, the design is drawn into it. This image when rendered usually has a very irregular edge, one not pleasing to the eye. Due to the nature of stitch data, the bitmap is rendered using LineTo and MoveTo commands, which leave “>” shaped gaps all along the edges of adjacent lines of stitching as can be seen in FIG. 4 .
[0103] If a path-following process around the image is used, these “<” or “>” shaped dents are formed. Nonetheless, a set of traces around the drawn design must be the start of the process. However, additional drawing in the form of a different color, only at points of needle penetration can be performed as shown in FIG. 5 .
[0104] This allows the outline to have more intelligent data and thus the resultant paths can have the pixels between the penetrated points removed. This makes the outline more regular and pleasing. Further improvement can be made by filtering triads of stitch points which are close together, often the result of embroidery short-stitching, which is commonly used as a method to turn the angle of lines of stitches. FIG. 6 is an image of such a filtered image.
[0105] Next a simplification of the outline can be made and conversion into Bezier or other outline form thus made.
[0106] As there are likely to be a plurality of outlines, it is important to create objects with outlines and holes, as described previously.
[0107] Once those outlines exist, a global underlay can be achieved by first, inflating the size of the shapes to some useful value (best practice is 3 mm) as seen in FIG. 7 .
[0108] Then those shapes can be passed to a tatami fill generator which is well defined in the art (best practice for Terry cloth is 3.5 mm stitch length, 1.5 mm line density). The output of the fill generator can then be sequenced as the earliest-sewn data in the design. Thus with a single user action, the process can adapt any design to the desired nappy cloth. Additionally, using the prior art, any stitch data from the original design which is interpreted as underlay may now be removed, as it has been replaced with a superior set of data. FIG. 8 illustrates a tatami fill pattern while FIG. 9 illustrates letters embodied over a tatami filled area.
[0109] Aspects related to automatic echo quilting for embroidery designs:
[0110] Using a similar process to creating a global underlay, wherein the outline and hole data is created for any embroidery design, we can achieve a different effect. The concept of echo quilting is not new to graphics, but in embroidery such items are manually created by a skilled artist. FIG. 10 illustrates an echo quilting design with embroidered letters.
[0111] Outlining stitches with new stitches can be done by taking the objects and handing them to a run stitch generator (or any stitch generator, such as satin, bean stitch, etc.). Further, if we optionally discard any holes, we can then expand the outlines using known polygon inflation techniques to create a single or plurality of outlines which ‘echo’ around the design. This is commonly used by quilters to provide stability to a quilt, using a set of running stitches known as echo quilting. It appears as ripples would in a pond. Further, as each embroidery is constrained by the hoop which will be used to create it, we can cause the echo lines to terminate within the bounds of the hoop, and add tie-off and jump to other echo lines as needed. The user of the software could control the distance and stitch type of the echo lines. Additionally, multiple designs within a hoop could have their outlines inflated together, producing a more visually complex result as the echo patterns interfere with each other, and each echo line can have other stitch actions applied, such as decorative motifs played on the line, etc.
[0112] Aspects related to automatic drop shadow embroidery:
[0113] Using a similar process to creating a global underlay, wherein the ‘outline’ and ‘hole’ data is created for any embroidery design, we can achieve a different effect. The concept of drop shadow is not new to graphics, but in embroidery such items are manually created by a skilled artist.
[0114] In this process, we take a complete set of outlines as proposed above and offset them in a manner described by a user, having little skill and requiring only a visual interest, and offset, inflate with rounding acute corners, monochromatize, and then use a graphical subtraction which created a resulting set of objects that can then have stitches applied. The subtraction includes steps for discovering intersections between the original and copied image, then discarding overlapped regions, however, the drop shadow is compensated such that its shape penetrates the original design by a small amount which is useful in embroidery to prevent gapping in designs, where the background shows through. The user inputs an offset of a vector, containing by definition a distance and an angle. This angle is then used as the angle for a tatami or other patterned fill, well known in the art.
[0115] Aspects related to automatic stipple embroidery:
[0116] Prior art exists, which has flaws that this overcomes.
1.) Using a similar process to creating a global underlay, wherein the ‘outline’ and ‘hole’ data is created for any embroidery design, we can achieve a different effect. or 2.) Using a user-defined area which typically includes an outer shape, which may be an embroidery hoop area, or some other defined polygon, and optionally an internal area of exclusion such as a design or plurality of designs placed in the hoop area, there is a need to automatically stitch down lines in a pseudo-random order known in the art as stippling. There are several variations on the pattern, but one requirement is near-uniform distance between lines of stitching. And they may not cross.
[0120] Prior art has been shown with fractals (Tsonis . . . , Pulse Microsystems, Mississauga, Canada), but that approach has a failure in that the fractal shape does not match the original shape, and thus there are dipped sections causing the stitch to either jump from section to section (undesirable because of time sewing and trimmer [a mechanical device in the machine] wear) or false paths which are too close.
[0121] Other prior art—Brother JP—uses a method where the pattern can be trapped and requires an exit to find its way out, which causes the lines of stitching to be closer together than optimal.
[0122] These embodiments solve that using maze theory and algorithms, with adaptations for embroidery.
[0123] A plurality of tessellated shapes, which may or not be identical in shape, is laid over the desired embroidery region at potentially a user-defined angle, with added spacing between the tessellations, defining graphical cells in a matrix. Each cell has data with it describing its center and the position and state of each edge, along with each edge's availability of an adjacent neighbor. Cells with fewer than two edges that are completely contained in the outline are discarded from the matrix.
[0124] As there is a minimal irregularity sometimes desired in stippling, the centers may be randomly offset by some small vector.
[0125] Shapes which are partially contained are flagged as such, along with the edges that are available for use in the design (those contained in the shape).
[0126] An initial starting point is defined, either randomly or by the user. The software then follows an algorithm (Drunkard's Path example) for selecting and adding cells to the sequence, labeling used cells as it goes, thereby ensuring that a single path can be traced into each and every useable cell in the matrix. Due to the nature of randomization added to the algorithm, the path is always different, although the seed used can be stable or user-altered to change the path. To ensure that the accidental use of continuous forward moves does not occur, the randomizer is presented with a reduced solution set where advancing forward in the same direction as the last move occurred happens. This makes the path turn frequently.
[0127] Once the path has been established, there needs to exist a return route in order to achieve the desired effect. For this reason, the actual entry and exit of each cell has its points set at evenly spaced intervals along the edge where travel exists. Thus, the path always forms a closed shape, running twice through each and every cell.
[0128] Where the path enters a cell is stable, as that maintains spacing between lines of stitching. Instead of following through the cell, however, the stitches run around the edges of the cell toward the exit edge. This provides additional shape and visual interest to the pattern. This is made possible by the cell spacing, which allows the edges not to touch.
[0129] Additional adjustment is made to the points discovered as the path travels through the cells. For each cell where the path enters and then exits, without going through another cell, this cell is flagged for shape adjustments.
[0130] The nodes of each entry, exit, and edge travel are set into a list, each given a Bezier handle set (or spline). In the case of Bezier, the handles may be adjusted in length and rotation by small amounts to create imperfect curvature, similar to what a skilled sewer would do by hand. Additional effects can be the lack of curvature and/or the erasure of nodes based on patterns. This produces a random, yet geometrically pleasing image.
[0131] Further, the resultant shape can now be taken as an outline and passed to other stitch generating apparatus. In this way motifs (or any other ornamentation) can be added.
[0132] A variation of this exists and is known in the industry as “Vermicelli Stitching.” This is similar in that it is random movements of small vector length and those movements are allowed to clip against the actual outlines. In this case we take the original stipple path and allow it to enter any cells that even touch the outline. A similar operation is performed, yet with a simple rule system for internal deformation of each cells travel route. The result is very similar to a manual process that is extremely time-consuming.
[0133] FIG. 11 illustrates an automatically generated pattern around embroidered letters in association with automated stippling in accordance with aspects of the embodiments.
[0134] FIG. 12 illustrates an automatically generated pattern from a “Drunkard” algorithm in association with automated stippling in accordance with aspects of the embodiments.
[0135] FIG. 13 illustrates an automatically generated less randomized version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments.
[0136] FIG. 14 illustrates an automatically generated “Leafy” version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments.
[0137] FIG. 15 illustrates an automatically generated “Geometric” version of the “Drunkard” pattern of FIG. 12 in association with automated stippling in accordance with aspects of the embodiments.
[0138] It will be appreciated that various of the above-disclosed and other features and functions, or alternatives thereof, may be desirably combined into many other different systems or applications. Also, that various presently unforeseen or unanticipated alternatives, modifications, variations or improvements therein may be subsequently made by those skilled in the art which are also intended to be encompassed by the following claims.
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Using an existing embroidery design that has been created for applique, data is automatically created for a cutting machine, which will cut the applique. Currently, the user currently has to cut these by hand—a labor intensive process or use a custom die that can be expensive. The process only requires that the applique steps in the sewing sequence are labeled as such. Generally, the applique steps are so labeled in order for the design creator to be able to let the sewer know what they are doing.
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FIELD OF THE INVENTION
The present invention relates in general to a method and apparatus for transferring digital information between electrical components and, in particular, to a method and apparatus for transferring digital information between electrical components without the use of a dedicated data clock or data over sampling.
BACKGROUND OF THE INVENTION
Presently, it is known for two or more electronic devices to exchange information or data using a serial data stream. Known methods of data transfer include a serial peripheral interface (SPI) that uses a dedicated data clock, data and enable signals to transfer serial data. Such interfaces are typically used in applications requiring data to be transferred from one electronic device or component to another electronic device or component.
One particular application in which data is transferred between electrical components is found in integrated circuit architectures used in wireless products that have a radio frequency integrated circuit (RF IC) and a baseband integrated circuit (BB IC). The RF IC receives and downconverts RF signals to baseband data signals that are coupled to the BB IC for further processing. The BB IC, among its various functions, may process the baseband data signals to develop a digital error or frequency control signal that is coupled to the RF IC. The RF IC may use the frequency control signal to correct and control its receive frequency synchronization. Additionally, the BB IC may generate a digital audio signal that may represent audio, such as voice, which is coupled to the RF IC for subsequent broadcast.
The use of an SPI to transfer the baseband data signals, the digital frequency control signal and the digital audio signal between the RF IC and the BB IC may require as many as nine dedicated pins on the integrated circuit chip (three pins for each signal to be transferred) and, therefore, may add cost and complexity to both the RF IC and the BB IC.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram illustrating a digital interface between a radio frequency integrated circuit (RF IC) and a baseband integrated circuit (BB IC).
FIG. 2 is a signal diagram illustrating the timing of various signals that may be used to couple data between the RF IC and the BB IC shown in FIG. 1 .
FIG. 3 is a block diagram of the clock synchronizers shown in FIG. 1
FIG. 4 is a model of a state machine employed by the clock synchronizer of FIGS. 1 and 3 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, a personal communication device 10 , such as a cellular telephone or the like, may generally include an antenna 12 , front end circuitry 14 , a radio frequency integrated circuit (RF IC) 16 , a baseband integrated circuit (BB IC) 18 , receive (RX) audio circuitry 20 and transmit (TX) audio circuitry 22 . The antenna 12 may receive an RF signal broadcast from a transmitter, such as a cellular base station (not shown), and may couple the RF signal to the front end circuitry 14 . The front end circuitry may process the RF signal and couple the processed RF signal to the RF IC 16 , wherein the processed RF signal may be fed to mixers 30 and 32 , which may be fed with local oscillator signals that may be 90° out of phase with respect to one another, due to a phase shifter 34 . The mixer 30 may generate a quadrature component of the RF signal and couple the quadrature component to a low pass filter 40 . Similarly, the mixer 32 may generate an in-phase component of the RF signal and couple the in-phase component to a low pass filter 42 . After the quadrature and the in-phase components are filtered by the low pass filters 40 , 42 , the in-phase and quadrature components may be each coupled to 10 bit analog to digital converters 44 , 46 . The output of the 10 bit analog to digital converter 44 is a 10 bit digital signal representative of the quadrature component of the RF signal. Similarly, the output of the 10 bit analog to digital converter 46 is a 10 bit digital signal representative of the in-phase component of the RF signal. The bit streams from the 10 bit analog to digital converters 44 , 46 may be coupled to a serializer 48 .
The serializer 48 may also receive a Sync signal and a clock signal, both of which may be used to control the output of the serializer 48 . The clock signal may be generated by a divider 60 that is coupled to an oscillator 61 . In one embodiment, the oscillator 61 may be separate from the RF IC 16 and may have a frequency of 7.68 megahertz (MHz). Alternatively, the oscillator 61 may be integrated with the RC IC 16 . Either way, the divider 60 may divide the oscillator frequency by a factor of six to generate a clock signal having a frequency of 1.28 MHz. The Sync signal may be generated by an I/Q Sync generator 62 that may divide the clock signal from the divider 60 by a factor of twenty to produce a 64 kilohertz (KHz) Sync signal. More detail regarding the timing of the clock and Sync signals will be described hereinafter in conjunction with FIG. 2 .
Upon receiving the bit streams from the 10 bit analog to digital converters 44 , 46 and the clock and Sync signals, the serializer 48 may generate an output bit stream having both the quadrature and the in-phase bits from the 10 bit analog to digital converters 44 , 46 therein. The output bit stream from the serializer 48 may be coupled to the BB IC 18 , where it may be received and processed in a manner described in detail below.
In addition to the output bit stream from the serializer 48 , the oscillator 61 output may be coupled to the BB IC 18 . A buffer 64 in the RF IC 16 may receive the Sync signal from the I/Q Sync generator 62 and may generate a Sync' signal that is also coupled to the baseband IC 18 . The Sync signal, which is generated by the I/Q Sync generator 62 , is a synchronization signal that is local only to the RF IC 16 and is used by the serializer 48 to transmit information from the RF IC 16 to the BB IC 18 . The Sync' signal may also be coupled to the baseband IC 18 . Due to circuit board capacitance or inductance and a finite output impedance of the buffer 64 , the Sync' signal may be slightly skewed with respect to the Sync signal. The Sync' signal and the oscillator signal may both be coupled to a clock synchronizer 66 , which generates an Sclock-RF signal representative of a synchronized clock in the RF IC 16 . The clock synchronizer 66 may be a divider that divides the oscillator signal by a factor of six, wherein the clock synchronizer 66 may be reset by the Sync' signal so that a negative edge of the Sclock-RF signal coincides with a state transition of the Sync' signal. Accordingly, the Sclock-RF signal may have substantially the same frequency as the clock signal (e.g., if the oscillator 61 frequency is 7.68 MHz, the clock signal will be 1.28 MHz) and may be synchronized with the Sync' signal. The RF IC 16 uses the Sync' signal and the Sclock-RF signal to receive information from the BB IC 18 .
The BB IC 18 may also contain a clock synchronizer 70 that may receive the oscillator signal and the Sync' signal from the RF IC 16 and may generate an Sclock-BB signal representative of a synchronized clock on the BB IC 18 . Like the clock synchronizer 66 , the clock synchronizer 70 may divide the oscillator signal by a factor of six and may be reset at every transition of the Sync' signal. The clock synchronizer 70 maintains the timing of the Sclock-BB signal because the periodic reset caused by the Sync' signal also resets the clock synchronizer 66 and thereby synchronizes the Sclock-BB signal with the Sclock-RF signal. Sclock-BB and Sclock-RF are then used to maintain alignment of data words that are transmitted between the RF IC 16 and the BB IC 18 .
The clock signals (e.g., the clock, the Sclock-BB and the Sclock-RF) are represented in FIG. 2 by a clock signal 76 . The clock signal 76 has a rising edge 78 , a high state 80 , a falling edge 82 and a low state 84 . As shown in FIG. 2, in one embodiment the clock signal 76 may have a period of 781.25 nanoseconds (ns), which corresponds to a clock frequency of 1.28 MHz. The synchronization signals (e.g., the Sync signal and the Sync' signal) are represented in FIG. 2 by a synchronization signal 90 , having a rising edge 92 , a high state 94 , a falling edge 96 and a low state 98 . The sychronization signal 90 changes states (from low to high or from high to low) every time 10 falling edges 82 of the clock signal 76 occur. Accordingly, the synchronization signal 90 has a period of 15.625 microseconds (μs), which corresponds to a frequency of 64 KHz.
Also shown in FIG. 2 is a data signal timing diagram 100 that represents the timing of the output bit stream generated by the serializer 48 of the RF IC 16 and received by the BB IC 18 . For example, returning to FIG. 1, the output bit stream that is coupled from the serializer 48 to the BB IC 18 may contain alternating sequences of in-phase information and quadrature information, wherein each sequence contains ten bits. The in-phase information may be clocked out of the serializer 48 while the synchronization signal 90 is high, and the quadrature information may be clocked out of the serializer 48 while the synchronization signal is low. In other alternative embodiments, the in-phase information may be clocked out of the serializer 48 while the synchronization signal 90 is low and the quadrature information may be clocked out of the serializer 48 while the synchronization signal 90 is high.
The BB IC 18 includes an I/Q to phase converter 110 that receives the output bit stream from the serializer 48 , the Sync' signal and the Sclock-BB signal. As shown in the data signal timing diagram 100 of FIG. 2, the I/Q to phase converter 110 clocks in data from the serializer 48 on every rising edge 78 of the clock signal 76 . As the I/Q to phase converter 110 clocks in the data bit by bit, the I/Q to phase converter 110 knows whether the clocked bits represent in-phase information or quadrature information based on the state of the Sync' signal represented in FIG. 2 by the synchronization signal 90 . For example, when the synchronization signal 90 is in the high state 94 , the I/Q to phase converter 110 may interpret the output data received from the serializer 48 as in-phase data. Conversely, when the synchronization signal 90 is in the low state 98 , the I/Q to phase converter 110 may interpret the output data received from the serializer 48 as quadrature information. Because the I/Q to phase converter 110 , which may be thought of as a data receiver, is synchronized with the serializer 48 , the I/Q to phase converter 110 can receive an output bit stream without the use of a dedicated data clock and without over sampling the output bit stream.
As the I/Q to phase converter 110 receives the data from the serializer 48 , it converts the data from in-phase and quadrature format to differential phase format and couples the differential phase formatted information to a demodulator 120 . The demodulator 120 may produce an audio signal that may be coupled to the RX audio circuitry 20 to produce an analog audio signal that may be coupled to, for example, an earpiece speaker. The demodulator 120 may also produce a signal representative of a baseband offset frequency between the personal communication device 10 and a base station (not shown) with which the personal communication device 10 is communicating.
The signal representative of the baseband offset frequency may be coupled from the demodulator 120 to a serializer 130 , which operates in substantially the same manner as the serializer 48 of the RF IC 16 . The serializer 130 clocks 10 bit data words to the RF IC 16 . The 10 bit data words are representative of the frequency control signal (referred to hereinafter as a 10 bit frequency control signal) and are clocked at a rate determined by the Sclock-BB signal. A data signal timing diagram 140 , shown in FIG. 2, illustrates the timing at which the 10 bit frequency control signal from the serializer 130 may be clocked. Specifically, on the first rising edge 78 of the clock signal 76 that occurs after the rising edge 92 of the sychronization signal 90 , a new data bit 142 may be set. The new data bit 142 informs the RF IC 16 as to whether it should expect information from the BB IC 18 . For example, if the new data bit 142 is a logical one, the RF IC 16 may be programmed to expect more data that will be clocked from the serializer 130 on subsequent clock pulses. Conversely, if the new data bit 142 is a logical zero, the RF IC 16 may be programmed to ignore any subsequent “data” that may appear to follow. When the new data bit 142 is set, 10 bits of information will be clocked from the serializer 130 on the next 10 rising edges 78 of the clock signal 76 . The data bits following the next data bit 142 may be arranged from least significant bit to most significant bit, or may be arranged from most significant bit to least significant bit.
As data is output from the serializer 130 , it is received by a multi-accumulator fractional-N modulator, which may also be referred to as a fractional-N synthesizer (frac-N synth) 150 . As will be appreciated by those having ordinary skill in the art, the frac-N synth 150 receives serial data that is used to program a rapidly tuning synthesizer. The frac-N Synth 150 has sufficient bandwidth so that it can be programmed to the baseband signal without introducing distortion. The frac-N synth 150 is clocked by the Sclock-RF signal and the Sync' signal and receives the 10 bit frequency control from the serializer 130 of the BB IC 18 . Because the Sclock-RF signal is synchronized by the Sync' signal, which is the same signal used to synchronize the Sclock-BB signal that is used to clock the serializer 130 , the frac-N synth 150 is sufficiently synchronized to the serializer 130 to receive the 10 bit frequency control signal without the use of a dedicated data clock and without oversampling the 10 bit frequency control signal.
The frac-N synth 150 receives the 10 bit frequency control signal and, based on that signal, reprograms its output frequency. The output signal from the frac-N synth 150 is coupled to a low pass filter 160 , which filters the output signal and couples the filtered signal to a second local oscillator (LO) 162 . Although, the low pass filter 160 and the LO 162 are shown in FIG. 1 as being separate from the RF IC 16 , those having ordinary skill in the relevant art will readily appreciate that the low pass filter 162 and the LO 162 could be integrated into the RF IC 16 . The filtered output signal from the low pass filter 162 provides frequency correction to the LO 162 to keep the LO 162 oscillating at the proper frequency and phase. The output of the LO 162 may be coupled to the mixer 32 and further coupled to the mixer 30 through the phase shifter 34 . As described above, the mixers 30 , 32 operate on the processed RF signal from the front end 14 to produce in-phase and quadrature components on the processed RF signal.
The BB IC 18 also includes a serializer 170 that is clocked by the Sclock-BB signal and that receives a digital audio signal from the TX audio circuitry 22 . The serializer 170 may couple the digital audio signal to the RF IC 16 in serial 9 bit words (referred to hereinafter as a 9 bit digital audio signal). Referring to a data signal timing diagram 172 shown in FIG. 2, on the first rising edge 78 of the clock signal 76 after a rising edge 92 of the synchronization signal 90 , the serializer 170 may clock a filler bit 174 to the RF IC 16 . In some applications the filler bit 174 provides no useful information to the RF IC 16 and is just used as a filler because the digital audio signal is only 9 bits long and 10 bits may be clocked out of the serializer 170 on each half cycle of the synchronization signal 90 . In other applications, the filler bit 174 may be used to carry useful information. The 9 bits following the filler bit 174 form the 9 bit digital audio signal, which transfers audio to the RF IC 16 so that the RF IC 16 may modulate the audio onto a carrier signal for broadcast. In some applications, the 9 bit digital audio signal may have its bits arranged from least significant to most significant. In other applications, the bits of the 9 bit digital audio signal may be arranged from most significant to least significant.
Because the 9 bit digital audio signal may need to be coupled to the RF IC 16 more frequently than the 10 bit frequency control signal, a second 9 bit word of digital audio is coupled from the serializer 170 to the RF IC 16 following the falling edge 96 of the synchronization signal 90 . A filler bit 176 , which may be followed by 9 digital audio bits, is clocked out of the serializer 170 on the first rising edge 78 of the clock signal 76 following the falling edge 96 of the synchronization signal 90 . Again, the 9 digital audio bits may be arranged from least significant to most significant or from most significant to least significant. Additionally, the filler bit 176 may or may not provide useful information to the RF IC 16 .
A frac-N synth 186 disposed within the RF IC 16 receives the 9 bit digital audio signal from the serializer 170 . Like the frac-N synth 150 , the frac-N synth 186 is clocked by the Sclock-RF signal and the Sync' signal. Because the Sclock-RF signal is synchronized by the Sync' signal, which is the same signal used to synchronize the Sclock-BB signal that is used to clock the serializer 170 , the frac-N synth 186 is sufficiently synchronized to the serializer 170 to receive the 9 bit digital audio signal without the use of a dedicated data clock and without the need to oversample the 9 bit digital audio signal. The frac-N synth 186 , upon receiving the 9 bit digital audio signal, changes its output frequency to create a frequency modulated signal representative of the information in the 9 bit digital audio signal. The analog signal may be coupled to transmitter (TX) circuitry 190 , which may be separate from or integrated with the RF IC 16 . The TX circuitry 190 may include an upconverter or a mixer and/or various other components known to those having ordinary skill in the art. The frequency modulated signal from the TX circuitry 190 is coupled to the antenna 12 , which broadcasts the signal.
Turning now to FIG. 3, the clock synchronizer 66 , 70 may include an inverter gate 200 , a first D flip-flop 204 , a second flip-flop 206 , an AND gate 208 and a state machine 210 . The output of the oscillator 61 , which may be 7.68 MHz, may be coupled to the inverter gate 200 and the state machine 210 . The output of the inverter gate 200 has the same frequency as the input to the inverter gate 200 , except that the output of the inverter gate 200 is 180° out of phase with the input to the inverter gate 200 . The output of the inverter gate 200 clocks the D flip-flops 204 , 206 at every negative edge of the output from the oscillator 61 . The Sync' signal is coupled to the first D flip-flop 204 . The non-inverting output (Q) of the first D flip-flop 204 is coupled to the input (D) of the second D flip-flop 206 and is further coupled to the AND gate 208 . The inverting output ({overscore (Q)}) of the second D flip-flop 206 is also coupled to the AND gate 208 . The output of the AND gate 208 , which is referred to herein as the Pos signal, is an edge detect of the Sync' signal running off the negative edge of the oscillator 61 . For example, when two consecutive states of the Sync' signal are the same, the output of the AND gate 208 is a logical zero and when two consecutive states of the Sync' signal are different, the output of the AND gate 208 is a logical one.
The state machine 210 , which receives inputs from the oscillator 61 and the AND gate 208 , can change the state of its output (Sclock) on each pulse of the oscillator 61 , wherein the state of the output Sclock signal is dependent on the state of the Pos signal provided to the state machine 210 . Further detail regarding the implementation and operation of the state machine 210 is given with respect to FIG. 4 below.
The state machine 210 may be implemented using combinational logic, application specific hardware or any other suitable electrical technology known to those having ordinary skill in the art. A register transfer language (RTL) such as VERILOG may be used to model the operation of the state machine 210 and to automatically produce the appropriate hardware to carry out the model. As shown in FIG. 4, the state machine model has seven states represented by seven circles labeled 0 - 6 , each state having an associated Sclock output that is produced at each pulse of the oscillator 61 (FIG. 1) and the state of which is determined by the Pos signal (FIG. 3 ). For example, states 0 - 3 have an Sclock output equal to 0 and states 4 - 6 have an Sclock output equal to 1.
The state machine 210 may begin operation in the 0 state and may remain in the 0 state so long as the Pos signal is equal to 1. However, when the Pos signal goes low (becomes equal to 0), the state machine 210 may transition from state 0 to state 2 as indicated by an arrow from state 0 to state 2 that is labeled “Pos=0.” As can be seen from FIG. 4, as long as the Pos signal is equal to 0, the state machine 210 will traverse from state 0 to state 2 , to state 3 and so on until the machine 210 reaches state 6 , wherein if the Pos signal is still equivalent to 0, the state machine 210 transitions from state 6 to state 1 . Accordingly, as long as the Pos signal is equal to 0, the state machine 210 repeatedly traverses from state 1 to state 6 through states 2 - 5 and back to state 1 again. When the Pos signal is equal to 1 , the state machine 210 will transition from whichever state it is currently in, to state 0 , which may be referred to as the reset state.
During operation of the clock synchronizer 66 , 70 , when the input to the second D flip-flop 206 and the output of the second D flip-flop 206 are both a logical 1 , the AND gate 208 generates a Pos signal equal to 1, which resets the state machine 210 to state 0 . When the state machine is at state 0 , Sclock equals 0. Therefore, each time the clock synchronizer 66 , 70 detects an edge on the Sync' signal, the clock synchronizer 66 , 70 creates a negative edge Sclock signal thereby synchronizing the Sclock signal with the Sync' signal. As shown in FIG. 4, states 1 , 2 and 3 have an associated Sclock signal equal to 0 in states 4 , 5 and 6 have an associated Sclock signal equal to 1. Accordingly, during periods of time, when no edges of the Sync' signal are detected, the state machine 210 repeatedly traverses from state 1 to state 6 , thereby tracing out a 50% duty cycle signal having a frequency that is one-sixth of the oscillator frequency. During such operation, states 1 , 2 and 3 represent the low state of the Sclock signal and states 4 , 5 and 6 represent the high state of the Sclock signal.
The foregoing description is one embodiment of a device constructed in accordance with the teachings of the present invention. Consequently, it will be understood by those of ordinary skill in the art, that the teachings of the present invention may be carried out in software resident on a processor such as a digital signal processor or by dedicated hardware that is designed to carry out the various functions disclosed herein. Accordingly, the foregoing description has been presented for the purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed. Many modifications and variations are possible in light of the above teachings. It is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto.
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A method of transferring data between a first electrical component ( 16 ) and a second electrical component ( 18 ), which are both coupled to a common oscillator ( 62 ) that oscillates at a first frequency, the first electrical component ( 16 ) generating a first bit stream having a second frequency that is a fraction of the first frequency and having a first number of bits, generating an indicator signal having a third frequency that is a fraction of the first frequency and that is indicative of a type of data represented by the first bit stream, and coupling the first bit stream and the indicator signal to the second electrical component. The second electrical component ( 18 ) sampling the first bit stream and the indicator signal at a fourth frequency that is substantially identical to the second frequency, thereby recovering the first bit stream generated by the first electrical component ( 16 ) and determining the type of data contained in the first bit stream.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to new bisphosphonic acid derivatives as represented by the following formula (I') or pharmaceutically acceptable salts thereof. ##STR2## in which
R 1 represents a hydrogen atom, an alkyl group having from 1 to 10 carbon atoms, a cycloalkyl group having from 3 to 10 carbon atoms, a phenyl group, an alkenyl group having from 2 to 10 carbon atoms which may be substituted by a phenyl group or a phenyl substituted alkyl group having from 1 to 5 carbon atoms which may be substituted by an alkoxy group having from 1 to 5 carbon atoms;
R 2 represents a hydrogen atom or an alkanoyl group having from 2 to 6 carbon atoms;
R 3 , R 4 , R 5 and R 6 may be the same or different, each represents a hydrogen atom or an alkyl group having from 1 to 5 carbon atoms; provided that when R 1 represents a methyl group, an ethyl group, an isopropyl group or a tert-butyl group, at least one of R 2 , R 3 , R 4 , R 5 and R 6 represents a substituent other than hydrogen atom.
The present invention also relates to a bone resorption-inhibitor and an anti-arthritis containing, as an active ingredient, a bisphosphonic acid derivative as represented by the following formula (I) or a pharmaceutically acceptable salt thereof. ##STR3## in which
R 1 represents a hydrogen atom, an alkyl group having from 1 to 10 carbon atoms, a cycloalkyl group having from 3 to 10 carbon atoms, a phenyl group, an alkenyl group having from 2 to 10 carbon atoms which may be substituted by a phenyl group or a phenyl substituted alkyl group having from 1 to 5 carbon atoms which may be substituted by an alkoxy group having from 1 to 5 carbon atoms;
R 2 represents a hydrogen atom or an alkanoyl group having from 2 to 6 carbon atoms;
R 3 , R 4 , R 5 and R 6 may be the same or different, each represents a hydrogen atom or an alkyl group having from 1 to 5 carbon atoms.
DESCRIPTION OF THE RELATED ART
Hitherto, various compounds have been synthesized as bisphosphonic acid derivatives, and there may be mentioned Japanese Patent Application (OPI) No. 89293/80 (the term "OPI" as used herein means a "published unexamined Japanese patent application") which discloses compounds having an aminomethylene-bisphosphonic acid residue as bonded at the 3-position of a substituted isoxazolyl group, like the compounds of the present invention.
The said Japanese Patent Application (OPI) No. 89293/80 (hereinafter referred to as "(OPI) No. 89293/80") mentions bisphosphonic acid series compounds of a formula: ##STR4## in which
R 1a represents a hydrogen atom, an alkyl group or a halogen atom;
R 2a represents a hydrogen atom or an alkyl group; and
Y represents an oxygen atom or an NH group.
However, the substituted isoxazolylaminomethylene-bisphosphonic acid derivatives which are concretely illustrated in the examples of (OPI) No. 89293/80 are those having methyl group, ethyl group, isopropyl group or tert-butyl group as the alkyl group for the substituent on the isoxazolyl group, and further, only free bisphosphonic acids are limitatedly illustrated therein.
Specifically, only the compounds of a general formula (I"): ##STR5## in which R 1' represents a methyl group, an ethyl group, an isopropyl group or a tert-butyl group, which may correspond to the compounds of the above-mentioned formula (I') of the present invention, are concretely illustrated in (OPI) No. 89293/80.
Further, (OPI) No. 89293/80 mentions that the substituted isoxazolylaminomethylene-bisphosphonic acid derivatives can be used as agricultural chemicals, especially as herbicide, but this is quite silent on the usability of the said derivatives as medicines.
Ordinary bones are living tissues which participate in resorption and precipitation of calcium for maintaining a constant inorganic equilibrium in a living body. In growing bones, the inorganic precipitation exceeds the inorganic resorption, but the bone resorption often exceeds the bone precipitation (ossification) in special diseases of some kinds, which would induce hypercalcemia, Paget's disease, etc. Hitherto, 1-hydroxyethylidene-1,1-bisphosphonic acid (etidronate), dichloromethylene-bisphosphonic acid (chlodronate), etc. have been used as remedial medicines for the diseases caused by the bone resorption, but these are insufficient from the viewpoint that the activity is not high and they have harmful side effects. Accordingly, sufficient medicines for the diseases are unknown up to the present.
Arthritides are inflammatory diseases of articulations, and the main diseases include rheumatic arthritis and the analogous diseases with articular inflammation.
Above all, the rheumatic arthritis is called a rheumatiod arthritis, which is a cryptogenetic chronic polyarthritis where the main lesion resides in the inflammatory lesion in the synovial membrane in the intracapsular layer. Arthritides such as rheumatic arthritis, etc. are progressive diseases which cause articular disorders such as articular deformation, ankylosis, etc. Accordingly, if these are deteriorated with no effective remedial treatment, these would often cause severe somatic disorders in some cases.
Various medicines have heretofore been used for the medicinal treatment for these arthritides, including, for example, steroids such as cortisone and other adrenocortical hormones; non-steriod series anti-inflammatory agents such as aspirin, piroxicam, indometacin, etc.; gold agents such as gold thiomalate, etc.; anti-rheumatic agents such as chloroquine preparations, D-penicillamine, etc.; anti-gouty agents such as colchicine, etc.; immunosuppressants such as cyclophosphamide, azathioprine, methotrexate, levamisole, etc.
However, these medicines have various problems in that they have harmful side-effects which are serious or which would make the long use difficult, or the effect is not sufficient, or they are not effective to the already expressed arthritides, etc.
Accordingly, in the clinical medicine for arthritides, the actual circumstances are that the provision of chemical medicines which are less toxic and which have an excellent preventive and remedial activity against arthritides is strongly desired.
The present inventors found that the compounds as represented by the above-mentioned formula (I') and salts thereof are new and additionally found, as a result of animal tests, that the compounds as represented by the above-mentioned formula (I) and salts thereof unexpectedly have a bone resorption-inhibitor activity to be able to inhibit hypercalcemia caused by bone resorption as well as have an excellent anti-arthritic activity, and accordingly have hereby achieved the present invention.
SUMMARY OF THE INVENTION
Specifically, the present invention provides the new bisphosphonic acid derivatives as represented by the above-mentioned formula (I') and salts thereof. Additionally, it provides a bone resorption-inhibitor as well as an anti-arthritis containing, as an active ingredient, the bisphosphonic acid derivative as represented by the above-mentioned formula (I) or its salt. (The derivatives of the formula (I) and their salts include the bisphosphonic acid derivatives of the formula (I') and their salts and the bisphosphonic acid derivatives of the formula (I") and their salts).
In the groups in the general formulae as herein referred to, the alkly group having from 1 to 5 carbon atoms (hereinafter this is described as "lower alkyl group") is a linear or branched carbon chain. Accordingly, the lower alkyl group includes a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, an isobutyl group, a sec-butyl group, a tert-butyl group, a pentyl (amyl) group, an isopentyl group, a neopentyl group, etc. The alkyl group having from 1 to 10 carbon atoms in the general formulae is a linear or branched carbon chain, which includes, in addition to the above-mentioned examples for the lower alkyl group, an n-hexyl group, an n-heptyl group, an n-octyl group, an n-nonyl group, an n-decyl group, an isoheptyl group, a 2-ethylbutyl group, a 2-ethylpentyl group, a 4-ethylheptyl group, etc. The cycloalkyl group having from 3 to 10 carbon atoms includes, for example, a cyclopropyl group a cyclobutyl group, a cyclopentyl group, a cyclooctyl group, a cyclodecyl group, etc. The alkenyl group having from 2 to 10 carbon atoms means a linear or branched hydrocarbon group, typically including a vinyl group, an allyl group, an isopropenyl group, a 2-butenyl group, a 2-methyl-2-propenyl group, a 3-pentenyl group, a 4-methyl-3-pentenyl group, a 4-methyl-3-hexenyl group, a 4-ethyl-3-hexenyl group, etc. These alkenyl groups may optionally be substituted by a phenyl group. Typical phenylalkenyl groups include a styryl group, a 3-phenyl-2-propenyl group, a 4-phenyl-2-butenyl group, etc.
The "phenyl substituted alkyl group having from 1 to 5 carbon atoms which may be substituted by an alkoxy group having from 1 to 5 carbon atoms (hereinafter this is described as "lower alkoxy group")" includes a benzyl group, a phenethyl group, a phenylpropyl group, a phenylbutyl group, etc. which are unsubstituted or substituted by a methoxy group, an ethoxy group, a propoxy group, a butoxy group, a pentyloxy group, an iso-propoxy group, an iso-butoxy group, an iso-pentyloxy group, a tert-pentyloxy group, etc. The said lower alkoxy group may be substituted in any position on the phenyl group.
The "alkanoyl group having from 2 to 6 carbon atoms (hereinafter this is described as "lower alkanoyl group")" includes, for example, an acetyl group, a propionyl group, a butanoyl group, etc. Among the said substituents, R 1 is preferably a lower alkyl group or a cycloalkyl group. This is more preferably a methyl group, a pentyl group, a cyclopropyl group, etc. The group R 1 may be substituted in the 4- or 5-position on the isoxazole ring in the above-mentioned general formulae. The compounds of the present invention include tetraesters in which R 3 to R 6 are all lower alkyl groups as well as monoesters, diesters and triesters in which one to three of R 3 to R 6 is(are) lower alkyl group(s).
The free phosphonic acids of the present invention can form the corresponding salts. Accordingly, the active ingredients of the present invention include pharmaceutically acceptable salts of the compounds of the formula (I). Concretely, there may be mentioned salts with inorganic bases, for example, salts with alkali metals such as sodium, potassium, etc., and salts with alkaline earth metals such as calcium, magnesium, etc.; ammonium salts; salts with organic bases such as methylamine, ethylamine, dimethylamine, diethylamine, trimethylamine, triethylamine, cyclohexylamine, ethanolamine, diethanolamine, etc.; and salts with basic amino acids such as lysine, ornithine, etc.
MANUFACTURE METHOD:
The compounds of the formula (I) of the present invention can be manufactured in accordance with the following reaction formulae. ##STR6## In these formulae, R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are the same significance as above, R 3' , R 4' , R 5' and R 6' may be the same or different, each represents an alkyl group having from 1 to 5 carbon atoms, R 7 , R 8 and R 9 may be the same or different, each represents an alkyl group having from 1 to 5 carbon atoms, and X represents a halogen atom.
FIRST METHOD:
In this method, the respective reaction components of a 3-aminoisoxazole (II), a lower alkyl ortho-formate (III) and a dialkyl phosphite (IV) are blended each in the corresponding reaction amount or excessive amount of (IV) and reacted under heating. A reaction solvent is not specifically required. The reaction is performed generally at 100° to 200° C., preferably at 150° C. or so, for 10 to 60 minutes.
For isolating and purifying the thus obtained reaction product (V), for example, the reaction mixture is purified on a silicagel column with a mixed solvent of methanol-chloroform.
In the reaction of the 3-aminoisoxazole (II) and the lower alkyl ortho-formate (III), an iminoether intermediate of a formula: ##STR7## (wherein R 1 , R 7 and R 8 are the same significance as above.) may be isolated.
The iminoether intermediate can be further reacted with the dialkyl phosphite (IV) to give the compound (V).
For isolation and purification of the thus obtained reaction product, for example, the reaction mixture is directly purified by silica gel column chromatography, or alternatively, this is washed with water in the form of a chloroform solution, and after the solvent was distilled out, the resulting residue can be purified by silica gel column chromatography.
For manufacture of the final products in which R 2 represents a lower alkanoyl group, the compound (V) (especially the ester thereof) is acylated. For the acylation, the compound (V) may be reacted with a reaction-equivalent amount or excessive amount of an acylating agent directly or in a solvent. As the acylating agent can be used acid anhydrides, acid halides, etc. As the reaction solvent can be used benzene, toluene, diglyme, etc. The reaction is desirably carried out under heating.
The bisphosphonates can be converted into the corresponding bisphosphonic acids by hydrolysis. The hydrolysis is generally carried out by heating under reflux in a concentrated hydrochloric acid. Alternatively, the bisphosphonates can be treated with a strong acid or a trimethylsilyl halide in a water-free solvent. For the method, in general, a commercial anhydrous hydrobromic acid in acetic acid can be used directly or in the form of a pertinently diluted solution, or a solution of an iodide trimethylsilane as dissolved in a solvent such as carbon tetrachloride, dimethylformamide, chloroform, toluene, etc. can be used. Regarding the temperature, the hydrolysis is carried out with cooling or heating. For example, when the ester is hydrolyzed with a trimethylsilyl halide with cooling at -10° C. or lower, a partially hydrolyzed product is obtained.
When the bisphosphonic acid is to be converted into its salt, the acid is treated with a base such as sodium hydroxide, potassium hydroxide, ammonia or organic amines, etc. in a conventional manner.
SECOND METHOD:
In this method, a mixture solution comprising 1 mol. of phosphorus trihalogenide (VI) and excessive amount, preferably 2 to 10 mol. of trialkyl phosphite (VII) is first reacted, for example, at 40° to 100° C., preferably at 60° to 80° C., for 15 to 30 minutes, and then a substituted isoxazole-3-formamide (VIII) is added to the resulting mixture solution and heated, for example, at 40° to 100° C., preferably at 60° to 80° C., for several hours. The progress of the reaction can easily be confirmed by TLC (thin layer chromatography, with developer system of chloroform-methanol). After the completion of the reaction, the excess trialkyl phosphite is removed out by distillation.
Then, the isolation and purification of the obtained product, and the acylation and hydrolysis can be performed by the same manner as the first method.
In addition to the above-mentioned manufacture methods, the compounds (I) can be produced by any other various methods. For instance, in accordance with the method described in Japanese Patent Application (OPI) No. 89293/80, a free bisphosphonic acid is first obtained and then esterified or is subjected to salt-formation reaction.
The isolation and purification of the final products (I) can be carried out by conventional chemical treatments which include extraction, crystallization, recrystallization, various chromatography operations, etc.
EFFECT OF THE INVENTION:
The compounds (I) and their salts provided by the present invention have a bone resorption-inhibitory action and also have an action of inhibiting hypercalcemia caused by bone resorption. Accordingly, the compounds (I) and their salts of the present invention are useful as a remedy or preventive to hypercalcemia caused by bone resorption, Paget's disease, metastatic osteocarcinoma, osteopsathrosis, sthenic bone resorption to follow inflammatory arthritides such as chronic rheumatoid arthritis, etc. In addition, these are recognized to have excellent anti-inflammatory action and sedative and analgesic action. Further, the anti-arthritic action of the compounds (I) and their salts of the present invention was demonstrated and confirmed by the preventive and remedial activity to adjuvant-induced arthritis.
The adjuvant-induced arthritis is widely utilized as a study model for arthritides in this technical field, as this results in polyarthritis chronica which is analogous to human rheumatic arthritis.
As mentioned hereinafter, the compounds provided by the present invention were demonstrated and confirmed to have prophylactic and therapeutic actions in the adjuvant arthritis. Although it is not clarified by what function and mechanism the compounds could have the anti-arthritic action, it is presumed that the compounds provided by the present invention could have a direct inhibitory action at least to the inflammatory symptoms of arthritides, in view of the reported fact that conventional immunosuppressants and immunomodulators could not be recognized to be effective on already expressed arthritides, while glucocorticosteroids could have an anti-arthritic action in both the prophylactic and the therapeutic experiment for arthritides.
Accordingly, the compounds can be applied to all arthritides which cause inflammation. Diseases for which the compounds are efficacious include rheumatic arthritic and the arthritides which cause inflammation, for example, cryptogenetic polyarthritides such as juvenile rheumatoid arthritis (including Still's disease), tetanic myelitis, psoriatic arthritis, Reiter's syndrome, etc.; rheumatic fever (acute rheumatic arthritis); diseases to cause arthritic symptom, amoung gouty and metabolic articular diseases such as gout, pseudogout, Wilson's diseases, etc.; diseases to cause arthritic symptom, among medical diseases except metabolic diseases, which are often accompanied by complicated arthritides, for example, pulmonary hypertrophic arthritis, sarcoidosis, ulcerative colitis, regional ileitis, Whipple's disease, liver diseases, hemophilic arthritis, hemoglobinopathy, hemochromatosis, accessory thyroid hyperergasia, hypothyroidism, etc.; diseases to cause arthritic symptom in collagen diseases (except rheumatic arthritis) such as systemic scleroderma (dermatosclerosis), systemic lupus erythematous, etc.; diseases to cause arthritic symptom in Bechcet's syndrome; traumatic arthritides and the analogous diseases thereof; infectious arthritides such as suppurative arthritis, etc. Experimental test methods and results are mentioned hereunder so as to support the pharmacological effect of the compounds (I) and their salts provided by the present invention.
(1) INHIBITORY EFFECT ON HYPERCALCEMIA:
Rats of hypercalcemia induced by administration of parathyroid hormone (hereinafter referred to as "PTH") were used, and the decrement of the serum calcium amount by administration of the compound was measured.
TEST METHOD:
30 μg/kg of human 1-34 PTH (manufactured by Peptide Laboratory) which was dissolved in a 0.1% BSA (bovine serum albumin)-containing physiological saline (content of the PTH is 6 μg/ml) was intravenously injected in an amount of 30 μg/kg (5 ml/kg as the solution) to 5-week male Wistar rats which had been fasting for 20 hours. Only 0.1% BSA-containing physiological saline was injected to the normal control group in the same manner. 45 minutes after the PTH injection, the rats were etherized and then subjected to celiotomy, whereby the blood was collected from the abdominal cava with a vacuum blood-collecting tube. The blood collected was immediately centrifuged by 3000 rpm, at 4° C. for 10 minutes to isolate the serum. The ionized calcium (Ca ++ ) concentration in the serum was immediately measured with a Ca ++ meter (Sera 250, manufactured by Horiba Manufacturing Co.).
The compounds of the present invention were dissolved using sodium hydroxide and hydrochloric acid, in physiological saline (pH 7.4), for subcutaneous administration, in such amounts that the dose amounted to 2 ml/kg, and for oral administration, in distilled water (pH 7.4) so that the dose amounted to 5 ml/kg. They were administered 24 or 72 hours before the PTH injection. A physiological saline or a distilled water was administered to the normal control group and the control group, in the same manner. Salmon calcitonin (SCT, manufactured by Armour Co.) was dissolved in physiological saline so that the dose amounted to 2 ml/kg, and then subcutaneously administered 30 minutes before the PTH injection.
The results for each group were expressed in terms of mean±S.E. (standard error) and comparison was made among the groups by testing by one-way analysis of variance. The significance level was taken at 5%.
RESULTS:
The results obtained by the subcutaneous administration and the oral administration are shown in Table 1 and Table 2, respectively.
TABLE 1 (1)______________________________________Subcutaneous administration(Administered 24 hours before the PTH injection) Dose Serum Ca.sup.++Compound Tested (/kg) N (m mole/liter)______________________________________Normal Control -- 5 1.40 ± 0.01**Control -- 5 1.56 ± 0.01Compound of 30 mg 5 1.44 ± 0.02**Example 12Compound of 30 mg 5 1.45 ± 0.02**Example 14Normal Control -- 5 1.38 ± 0.01**Control -- 5 1.49 ± 0.00SCT 0.3 IU 5 1.07 ± 0.02**Compound of 0.3 mg 5 1.43 ± 0.02**Manufacture 1.0 mg 5 1.40 ± 0.01**Example 1 3.0 mg 5 1.36 ± 0.02**Normal Control -- 5 1.40 ± 0.01**Control -- 5 1.52 ± 0.01Compound of 30 mg 5 1.41 ± 0.02**ManufactureExample 2______________________________________ Mean value ± S.E. **P <0.01
TABLE 1 (2)______________________________________Subcutaneous administration(Administered 72 hours before the PTH injection) Dose Serum Ca.sup.++Compound Tested (/kg) N (m mole/liter)______________________________________Normal Control -- 5 1.41 ± 0.01**Control -- 5 1.52 ± 0.00Compound of 0.1 mg 5 1.42 ± 0.02**Example 6 0.3 mg 5 1.25 ± 0.02**Compound of 0.1 mg 5 1.41 ± 0.02**Example 8 0.3 mg 5 1.27 ± 0.02**Normal Control -- 5 1.41 ± 0.01**Control -- 5 1.50 ± 0.02Compound of 0.01 mg 5 1.47 ± 0.02Example 21 0.03 mg 5 1.38 ± 0.01** 0.10 mg 5 1.22 ± 0.003**Normal Control -- 5 1.41 ± 0.02**Control -- 5 1.46 ± 0.02Compound of 0.01 mg 5 1.45 ± 0.01Example 22 0.03 mg 5 1.35 ± 0.01** 0.10 mg 5 1.21 ± 0.02**Normal Control -- 5 1.43 ± 0.00Control -- 5 1.48 ± 0.02Compound of 0.03 mg 5 1.40 ± 0.01**Example 23 0.1 mg 5 1.33 ± 0.01**Normal Control -- 5 1.34 ± 0.02**Control -- 5 1.43 ± 0.01Compound of 0.1 mg 5 1.39 ± 0.02**Example 25 0.3 mg 5 1.22 ± 0.01**Normal Conrtrol -- 5 1.35 ± 0.02**Control -- 5 1.44 ± 0.01Compound of 0.3 mg 5 1.43 ± 0.03Example 25 1.0 mg 5 1.36 ± 0.02*Normal Control -- 5 1.47 ± 0.02**Control -- 5 1.57 ± 0.02Compound of 0.1 mg 5 1.36 ± 0.01**Example 28 0.3 mg 5 1.18 ± 0.02**Known Compound 1.0 mg 5 1.43 ± 0.02**(note-1)Normal Control -- 5 1.35 ± 0.02**Control -- 5 1.44 ± 0.01Compound of 0.1 mg 5 1.20 ± 0.01**Example 31 0.3 mg 5 1.05 ± 0.03**Normal Control -- 5 1.36 ± 0.01*Control -- 5 1.45 ± 0.01Compound of 0.1 mg 5 1.41 ± 0.02Example 32 0.3 mg 5 1.27 ± 0.02**Normal Control -- 5 1.38 ± 0.01**Control -- 5 1.48 ± 0.02Etidronate 10 mg 5 1.44 ± 0.01 30 mg 5 1.40 ± 0.01**Compound of 0.03 mg 5 1.42 ± 0.02Example 1 0.1 mg 5 1.33 ± 0.01**Control -- 5 1.51 ± 0.03Compound of 0.1 mg 5 1.39 ± 0.02**Manufacture 0.3 mg 5 1.22 ± 0.02**Example 2Normal Control -- 5 1.42 ± 0.02*Control -- 5 1.54 ± 0.02Compound of 0.3 mg 5 1.45 ± 0.01Manufacture 1.0 mg 5 1.23 ± 0.05**Example 3Normal Control -- 5 1.47 ± 0.02**Control -- 5 1.57 ± 0.02Known Compound 0.1 mg 5 1.58 ± 0.00(note-2) 0.3 mg 5 1.49 ± 0.01* 1.0 mg 5 1.39 ± 0.02**Known Compound 0.3 mg 5 1.51 ± 0.03(note-1) 1.0 mg 5 1.43 ± 0.02**______________________________________ Mean value ± S.E. *P <0.05, **: P <0.01 (Note1): [(5t-butyl-3-isoxazolyl)amino]methylenebis(phosphonic acid) (disclosed in Japanese Patent Application (OPI) No. 89293/80) (Note2): [(5isopropyl-3-isoxazolyl)amino]methylenebis(phosphonic acid) (disclosed in Japanese Patent Application (OPI) No. 89293/80)
TABLE 2 (1)______________________________________ (Administered 24 hoursOral Administration before the PTH injection)______________________________________ Dose Serum Ca.sup.++Compound Tested (mg/kg) N (m mole/liter)______________________________________Normal Control -- 5 1.45 ± 0.01*Control -- 5 1.52 ± 0.02Compound of 100 mg 5 1.44 ± 0.02*Manufacture 300 mg 5 1.41 ± 0.01**Example 1______________________________________ Mean value ± S.E. *P <0.05, **P <0.01
TABLE 2(2)______________________________________ (Administered 72 hoursOral Administration before the PTH injection)______________________________________ Dose Serum Ca.sup.++Compound Tested (mg/kg) N (m mole/liter)______________________________________Normal Control -- 5 1.40 ± 0.01**Control -- 5 1.52 ± 0.02Compound of 30 mg 5 1.48 ± 0.02Example 8 100 mg 5 1.35 ± 0.02**Normal Control -- 5 1.42 ± 0.02*Control -- 5 1.54 ± 0.02Compound of 10 mg 5 1.52 ± 0.02Example 21 30 mg 5 1.36 ± 0.06** 100 mg 5 1.33 ± 0.04**Normal Control -- 5 1.43 ± 0.00Control -- 5 1.48 ± 0.02Compound of 30 mg 5 1.49 ± 0.00Example 23 100 mg 5 1.41 ± 0.02**Normal Control -- 5 1.40 ± 0.01*Control -- 5 1.49 ± 0.01Compound of 30 mg 5 1.44 ± 0.02Example 22 100 mg 5 1.28 ± 0.04**Compound of 30 mg 5 1.46 ± 0.02Example 28 100 mg 5 1.31 ± 0.04**Normal Control -- 5 1.46 ± 0.01Control -- 5 1.52 ± 0.02Compound of 30 mg 5 1.48 ± 0.01ManufactureExample 1 100 mg 5 1.16 ± 0.03**Normal Control -- 5 1.41 ± 0.02*Control -- 5 1.55 ± 0.01Compound of 30 mg 5 1.46 ± 0.02Manufacture 100 mg 5 1.16 ± 0.07**Example 2______________________________________ Mean value ± S.E. *P <0.05, **P <0.01
(2) EFFECT FOR INHIBITION OF BONE RESORPTION:
A left forelimb of a rat was immobilized by cutting the brachial nerve of the left forelimb. The inhibitory effect of the compound on the immobilization-induced atrophy of bone was demonstrated as mentioned below.
TEST METHOD:
Five-week Wistar rats were used for the experiment. The atrophy of bone was induced by reference to A. D. Kenny's report (Calcif, Tissue Int., 37, 126-133, 1985). Specifically, the plexus brachialis of the left forelimb of the animal (rat) was cut under thiopental anesthesia so that the left forelimb was immobilized. No treatment was imparted to the right forelimb (for control). Rats of a pseudooperation group were treated in the same manner as above except that the plexus brachialis was not cut. After two weeks, both the left and right humeri were collected. The soft connective tissue was removed off from the humeri, the humeri were fully fixed dehydrated and defatted with ethanol, and the dry weight of the respective humeri was measured. Afterwards, these were fired at 800° C. for 24 hours and the ashed weight was measured.
The compound was prepared in the same manner as in the above-mentioned Test Method (1) and was subcutaneously administered once a day for 14 days from the day of the operation, in the same manner as in the Test Method (1). For the control group and the pseudooperation group, only a physiological saline was injected in the same manner.
The results for each group were expressed in terms of means ±S.E. (standard error) and comparison was made among the groups by testing one-way analysis of variance. The significance level was taken at 5%.
RESULTS:
TABLE 3__________________________________________________________________________ Difference Difference of Bone of Bone Dose Weight Ash Content (mg/kg) N (mg) (a) (mg) (b)__________________________________________________________________________Pseudooperation -- 5 -0.4 ± 0.4** -0.4 ± 0.3**GroupControl Group -- 5 21.8 ± 2.2 14.7 ± 0.7Compound of 3 4 8.0 ± 1.0** 4.8 ± 0.5**Manufacture 10 5 3.2 ± 0.7** 1.7 ± 0.5**Example 1Pseudooperation -- 5 1.1 ± 3.0 0.4 ± 0.8GroupControl Group -- 5 13.6 ± 1.3 9.6 ± 0.9Compound of 1.0 5 4.8 ± 1.3** 3.0 ± 0.7**ManufactureExample 2__________________________________________________________________________Effect on Disuse Atrophy of Boneinduced by Neurectomy in Rats Left humerus .THorizBrace. Dry weight Ashed Ashed weightCompound Dose weight weight Dry weightTested (mg/kg) N (mg) (mg) %__________________________________________________________________________Subcutaneous Administration(2 weeks)Pseudooperation -- 5 120.6 ± 2.7** 66.6 ± 1.5 55.2 ± 0.1**GroupControl Group -- 5 96.6 ± 2.8 51.3 ± 1.4 55.3 ± 0.1Compound of 0.01 5 116.5 ± 1.5** 65.7 ± 0.9** 56.4 ± 0.2**Example 21 0.03 5 129.2 ± 1.0** 73.6 ± 0.7** 56.9 ± 0.2** 0.1 5 130.1 ± 3.2** 72.8 ± 1.8** 55.9 ± 0.4**Pseudooperation -- 5 109.8 ± 2.6** 61.6 ± 1.6** 56.1 ± 0.3**GroupControl Group -- 5 97.3 ± 2.4 52.9 ± 1.6 54.4 ± 0.5Compound of 0.1 5 113.9 ± 2.0** 64.9 ± 1.2** 56.9 ± 0.1**Manufacture 0.3 5 114.4 ± 2.6** 65.4 ± 1.6** 57.2 ± 0.3**Example 1 1.0 5 121.3 ± 2.1** 70.1 ± 1.1** 57.8 ± 0.4**Oral Administration(2 weeks)Pseudooperation -- 5 120.6 ± 2.7 66.6 ± 1.5** 55.2 ± 0.1**GroupControl Group -- 5 96.6 ± 2.8 51.3 ± 1.4 55.3 ± 0.1Compound of 3 5 113.0 ± 3.1 64.4 ± 2.3** 54.4 ± 0.2**Example 21 10 5 115.2 ± 4.0 67.0 ± 1.2** 56.0 ± 0.4** 30 5 118.7 ± 2.0 65.7 ± 0.9** 56.5 ± 0.2**Pseudooperation -- 5 120.5 ± 2.1** 64.7 ± 1.0** 53.7 ± 0.2**GroupControl Group -- 5 106.0 ± 1.9 54.8 ± 1.0 51.6 ± 0.4Compound of 10 5 102.8 ± 2.2 54.9 ± 1.3 53.4 ± 0.3**Manufacture 30 5 112.1 ± 1.4 61.0 ± 1.0** 54.4 ± 0.3**Example 1 100 5 123.9 ± 2.3** 68.9 ± 1.3** 55.6 ± 0.2**__________________________________________________________________________ Note: Mean value ± S.E. **P < 0.01 (a): (dry weight of nontreated humerus) - (dry weight of treated humerus) (b): (ashed weight of nontreated humerus) - (ashed weight of treated humerus)
(3) ANTARTHRITIC EFFECT:
The excellent prophylactic and therapeutic action of the compounds (I) of the present invention against arthritis was demonstrated and confirmed by the following test methods.
Specifically, for investigation of the anti-arthritic effect, experimental models of adjuvant arthritis which is resemble to rheumatoid arthritis in human were used in two test methods. In one method to test the therapeutic effect of the compounds, the compounds to be tested were administered to the animals already having the adjuvant arthritis. In the other method to test the prophylactic effect of the compounds, these were administered after the adjuvant administration, and the expression and progress of the resulting arthritis, if any, was observed.
The two tests for the therapeutic and the prophylactic effect are mentioned in detail hereunder.
EXPERIMENT (3)-1:
Therapeutic Effect on Adjuvant Arthritis in Rats.
0.1 ml of a suspension of dry dead cells of Mycobacterium butyricum as suspended in liquid paraffin in a proportion of 6 mg/ml was subcutaneously injected to male Lewis rats (7-week) in the tail. After 17 or 18 days, the thickness of the both hind paws was measured. One group comprising six rats in which the arthritis was noticeably observed was isolated. After the grouping day, the compound to be tested was subcutaneously or orally administered once a day for 14 days to the rats. Next day after the last administration, the thickness of the soles of the both hind legs was again measured.
EXPERIMENT (3)-II:
Prophylactic Effect on Adjuvant Arthritis in Rats.
0.05 ml of the suspension of dry dead bacilli of Mycobacterium butyricum as suspended in liquid paraffin in a proportion of 6 mg/ml was subcutaneously injected to male Lewis rats (6 to 7-week) in the left hind paw. After the adjuvant injection, the compound to be tested was administered to the rats once a day for 21 days. Next day after the last administration, the thickness of the both hind paws of the rats was measured.
For the Experiments (3)-I and (3)-II, the compounds of the present invention were dissolved, using sodium hydroxide and hydrochloric acid in physiological saline (pH 7.4), for subcutaneous administration, in such amount that the dose amounted to 2 ml/kg, and for oral administration, in distilled water (pH 7.4) so that the dose amounted to 5 ml/kg; and indometacin (as comparative drug) was suspended in 0.5% methyl cellulose solution so that the dose amounted to 5 ml/kg. Each rat was weighed at the first day of starting the administration of the compound to be tested and at the last day of the administration of the compound, and the difference of the weight there between (ΔB.W.) was obtained.
The results for each group were expressed in terms of mean ±S.E. (standard error) and comparison was made among the groups by testing by one-way analysis of variance. The significance level was taken at 5%.
TABLE 4______________________________________Experiment (3)-I Subcutaneous Administration Thickness of Paw (average Adminis- of right and Dose tration ΔB.W. left paws) (mg/kg) Route N (g) (× 0.01 mm)______________________________________Normal -- sc 6 57 ± 3** 658 ± 1**Control(physiologicalsalt solution)Arthritic -- sc 6 32 ± 1 1401 ± 32Control(physiologicalsalt solution)Indometacin 1 po 6 67 ± 4** 956 ± 32**Compound of 0.1 sc 6 40 ± 2 1258 ± 31**Manufacture 0.3 sc 6 50 ± 2** 1102 ± 36**Example 1 1.0 sc 6 56 ± 4** 956 ± 36** 3.0 sc 6 56 ± 1** 974 ± 32**______________________________________
TABLE 5__________________________________________________________________________Experiment (3)-IOral Administration Thickness of Paw (average Adminis- of right and Dose tration ΔB.W. left paws) (mg/kg) Route N (g) (× 0.01 mm)__________________________________________________________________________Normal Control -- po 6 41 ± 4 736 ± 5**(physiologicalsalt solution)Arthritic Control -- po 6 21 ± 2 1460 ± 32(physiologicalsalt solution)Indometacin 1 po 6 51 ± 4** 1044 ± 46**Compound of 100 po 6 50 ± 3** 1131 ± 36**ManufactureExample 1Normal Control -- po 6 51.5 ± 3.3** 747 ± 2**(physiologicalsalt solution)Arthritic Control -- po 6 24.2 ± 1.3 1435 ± 48(physiologicalsalt solution)Indometacin 1 po 6 58.2 ± 1.9** 931 ± 26**Compound of 10 po 6 29.7 ± 1.1 1317 ± 35Example 21 30 po 6 30.0 ± 1.1 1321 ± 35 100 po 6 29.7 ± 4.5 1119 ± 52**Compound of 10 po 6 23.3 ± 0.9 1435 ± 49Manufacture 30 po 6 32.8 ± 1.7 1296 ± 45*Example 1 100 po 6 43.3 ± 2.0** 1083 ± 36**__________________________________________________________________________
TABLE 6__________________________________________________________________________Experiment (3) IISubcutaneous Administration Admin- istra Thickness of Paw Dose tion ΔB.W. (× 0.01 mm) (mg/kg) Route N (g) Left Right__________________________________________________________________________Arthritic -- sc 6 230 ± 4 1451 ± 2.8 1298 ± 33Control(physiologicalsalt solution)Indometacin 1 po 6 261 ± 7* 1096 ± 41** 1028 ± 47**Compound of 0.1 sc 6 238 ± 2 1277 ± 19** 1279 ± 27Manufacture 0.3 sc 6 239 ± 2 1158 ± 12** 1107 ± 25**Example 1 1.0 sc 6 233 ± 3 1174 ± 14** 1110 ± 28**__________________________________________________________________________ *P < 0.05, **P < 0.01
The above-mentioned experimental results apparently demonstrate that the compound of the present invention had an inhibitory effect at least against to 0.01 mg/kg paw swelling by subcutaneous administration in the remedial experiment (Experiment (3)-I) and the ED 50 value of the said compound was 0.57 mg/kg. By oral administration, the said compound was also effective in an amount of 100 mg/kg. Further, in the prophylactic experiment (Experiment (3)-II), the compound was also confirmed to be effective by subcutaneous administration. Specifically, this had a significant inhibitory effect in the adjuvant-inoculated paw by subcutaneous administration of 0.1 mg/kg and in the opposite paw with no adjuvant by injection of 0.3 mg/kg.
(4) ACUTE TOXICITY TEXT:
The compound of Manufacture Example 1 was subcutaneously injected to rats in an amount of 10 mg/kg/day for continuous two weeks, and no rats died.
The compounds (I) of the present invention can be blended with any optional pharmaceutically acceptable carrier, vehicle, attenuant, etc. to be formed into powder, granules, tablets, capsules, pills, etc. for oral administration or into injection (for intro-articular injection, etc.), suppositories, inhalation, ointment, etc. for non-peroral administration. The amount of the dose of the compounds (I) of the present invention is, although varying in accordance with the administration route, patient's symptom, etc., generally form 10 mg/day/adult to 1 g/day/adult, preferably from 10 to 100 mg/day/adult, for oral administration, and from 0.1 to 100 mg/day/adult for non-oral administration.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following examples are intended to illustrate the present invention in more detail but not to limit it in any way. Manufacture of the raw material compound to be used in Examples is shown in Referential Example. Some of the raw material compounds were prepared in accordance with the methods described in "Industrial Chemistry" 66 (12), 1831 (1963) (S. Kishimoto) and Japanese Patent Publication No. 4887/62 (H. Kano et al.).
Manufacture of the known compounds included in the scope of the compounds (I) of the present invention is shown in Manufacture Examples.
REFERENCE EXAMPLE 1:
Raw Material Compound for Example 15
4.7 g of sodium metal was dissolved in 92 ml of ethanol. A mixture of 20 g of 2-heptanone and 26 g of diethyl oxalate was dropwise added thereto at 0° C. After the removing the ice bath, the reaction mixture was stirred at room temperature for 3 hours. After evaporation of the reaction mixture, 200 ml of water was added to the resulting syrup, and then an aqueous 10% hydrochloric acid was added with ice-cooling, the pH being adjusted to 1. After extraction with benzene (300 ml×3), the organic layer was washed with 100 ml of water, dried with Glauber's salt (Na 2 SO 4 ). And concentrated to give ethyl hexanoylpyruvate as a liquid (38 g).
A mixture of 38 g of ethyl hexanoylpyruvate in 190 ml of ethanol in the presence of 14.4 g of hydroxylamine hydrochloride and 16 g of sodium hydrogencarbonate was heated under reflux for 3 hours. After the reaction mixture was cooled to room temperature, the insoluble materials were separated by filtration, and the remaining filtrate was concentrated. The resulting residue was dissolved in chloroform (500 ml), which was washed with water, concentrated to give 5-pentyl-3-carboethoxyisoxazole as a liquid (36 g).
A mixture of 36 g of 5-pentyl-3-carboethoxyisoxazole in 105 ml of a concentrated aqueous ammonia was vigorously stirred overnight. The reaction mixture was filtered, and the resulting solid was washed with water and dried to obtain 20 g of 5-pentyl-3-carbamidoisoxazole.
Subsequently, 19 g of the thus obtained 3-carbamide was added to a solution of 77.5 ml of an aqueous 10% sodium hypochlorite containing 8.3 g of sodium hydroxide. The mixture was stirred for 2 hours at room temperature. The reaction mixture was dropped into 60 ml of a boiling water for 40 minutes, and then refluxed for further 40 minutes. The reaction mixture was rapidly cooled to give crystals. The crystals thus formed were filtered and washed with water to obtain 10 g of 3-amino-5-pentylisoxazole.
EXAMPLE 1: ##STR8##
A mixture of 4.9 g of 3-amino-5-methylisoxazole, 8.8 g of ethyl ortho-formate and 13.8 g of diethyl phosphite was heated at 150° C. with stirring for 40 minutes. The reaction mixture was cooled to room temperature and the product was purified on silica-gel column (eluent: 2% methanol-chloroform) to give 4.8 g of tetraethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as an oil.
The physico-chemical characteristics of this product are as follows:
(i) Mass Spectrum (FAB Mass): 385 (M+1)
(ii) Nuclear Magnetic Resonance (NMR) Spectrum: (in CDCl 3 )
______________________________________δ: 1.3 (12H, CH.sub.3 CH.sub.2 O × 4) 2.3 (3H, CH.sub.3) 4.0˜4.4 (8H, CH.sub.3 CH.sub.2 O × 4) 4.52 (1H, NHCH--) 5.60 (1H, H in isoxazole ring)______________________________________
EXAMPLE 2: ##STR9##
A mixture of 2.0 g of 3-amino-5-cyclopropyl-isoxazole, 3.0 g of ethyl ortho-formate and 9.1 g of diethyl phosphite was heated at 160° C. with stirring for 2.5 hours. The reaction mixture was cooled to room temperature and the product was purified on a silica gel column (eluent: 2% methanol-chloroform) to give 2.5 g of tetraethyl [(5-cyclopropyl-3-isoxazolyl)-amino]methylene-bis(phosphonate) as an oil.
The physico-chemical characteristics of this product are as follows:
(i) Pale Yellow Oil (at room temperature)
(ii) Mass Spectrum (FAB Mass): 411 (M+1), 365, 273
(iii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.84˜1.10 ##STR10## 1.34 ##STR11## 1.92 ##STR12## 2.04 ##STR13## 4.04˜4.40 ##STR14## 4.48 ##STR15## 5.48 ##STR16##______________________________________
In the same manner as Example 2, the following compounds were prepared.
EXAMPLE 3: ##STR17## (i) Yellow Oil (ii) Mass Spectrum (FAB Mass): 453 (M+1), 407, 315
(iii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.30 ##STR18## 1.20˜2.20 ##STR19## 1.84 ##STR20## 2.64 ##STR21## 4.04˜4.46 ##STR22## 4.50 ##STR23## 5.50 ##STR24##______________________________________
Starting Compound: 3-Amino-5-cyclohexylisoxazole
EXAMPLE 4: ##STR25## (i) Yellow Oil (ii) Mass Spectrum (FAB Mass): 413 (M+1), 367, 275
(iii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.96 ##STR26## 1.30 ##STR27## 1.68 ##STR28## 1.76 ##STR29## 2.59 ##STR30## 4.02˜4.46 ##STR31## 4.48 ##STR32## 5.54 ##STR33##______________________________________
Starting Compound 3-Amino-5-n-propylisoxazole
EXAMPLE 5: ##STR34## (i) Yellow Oil (ii) Mass Spectrum (FAB Mass): 447 (M+1), 401, 309
(iii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.30 ##STR35## 4.06˜4.44 ##STR36## 4.62 ##STR37## 6.10 ##STR38## 7.34˜7.82 ##STR39##______________________________________
Starting Compound: 3-Amino-5-phenylisoxazole
EXAMPLE 6: ##STR40##
A solution of 2.5 g of tetraethyl [(5-cyclopropyl-3-isoxazolyl)-amino]methylene-bis(phosphonate) in 25 ml of concentrated hydrochloric acid was heated under reflux for 3.5 hours. The reaction mixture was concentrated. Methanol and acetone were added to the concentrate to give 1.7 g of [(5-cyclopropyl-3-isoxazolyl)-amino]-methylene-bis(phosphonic acid) as a solid.
(i) m.p.: 176°-178° C.
(ii) Mass Spectrum (FAB Mass): 299 (M+1), 217
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 0.80˜1.16 ##STR41## 1.84˜2.12 ##STR42## 4.08 ##STR43## 5.82 ##STR44##______________________________________
(iv) Elementary Analysis (as C 7 H 12 N 2 O 7 P 2 ·0.5H 2 O):
______________________________________ C(%) H(%) N(%) P(%)______________________________________Calculated: 27.37 4.27 9.12 20.17Found: 27.14 4.02 9.05 20.09______________________________________
In the same manner as Example 6, the following compounds were prepared.
EXAMPLE 7: ##STR45## (i) m.p.: 208°-209° C. (ii) Mass Spectrum (FAB Mass): 341 (M+1), 259, 177
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 1.20˜2.12 ##STR46## 2.68 ##STR47## 4.06 ##STR48## 5.86 ##STR49##______________________________________
(iv) Elementary Analysis (as C 10 H 18 N 2 O 7 P 2 ·0.3H 2 O):
______________________________________ C(%) H(%) N(%) P(%)______________________________________Calculated: 34.74 5.42 8.11 17.92Found: 34.65 5.14 8.15 18.06______________________________________
EXAMPLE 8: ##STR50## (i) m.p.: 152°-153° C. (ii) Mass Spectrum (FAB Mass): 301 (M+1), 219
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 0.92 ##STR51## 1.66 ##STR52## 2.62 ##STR53## 4.12 ##STR54## 5.90 ##STR55##______________________________________
(iv) Elementary Analysis (as C 7 H 14 N 2 O 7 P 2 ·0.4H 2 O):
______________________________________ C(%) H(%) N(%) P(%)______________________________________Calculated: 27.36 4.85 9.11 20.16Found: 27.34 4.55 9.13 20.39______________________________________
EXAMPLE 9: ##STR56## (i) m.p.: 237°-238° C. (decomposition) (ii) Mass Spectrum (FAB Mass): 335 (M+1), 253
(iii) NMR Spectrum (in D 2 O with K 2 CO 3 ):
______________________________________δ: 3.96 ##STR57## 6.44 ##STR58## 7.44˜7.90 ##STR59##______________________________________
(iv) Elementary Analysis (as C 10 H 12 N 2 O 7 P 2 ):
______________________________________ C(%) H(%) N(%) P(%)______________________________________Calculated: 35.94 3.62 8.38 18.54Found: 36.09 3.79 8.12 18.85______________________________________
EXAMPLE 10: ##STR60##
A mixture of 2.2 g of 3-amino-5-ethylisoxazole, 3.4 g of ethyl ortho-formate and 8.1 g of diethyl phosphite was heated at 150°-155° C. with stirring for 45 minutes. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified on a silica gel column (eluent: 0.5-2% methanolchloroform) to give 5.7 g of [(5-ethyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as an oil.
The physico-chemical characteristics of this product are as follows:
(i) Mass Spectrum (FAB Mass): 399 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.1 ˜ 1.5 (15H, --OCH.sub.2 CH.sub.3 × 4, --CH.sub.2 CH.sub.3) 2.64 (2H, --CH.sub.2 CH.sub.3) 4.0 ˜ 4.4 (8H, --OCH.sub.2 CH.sub.3 × 4) 4.50 (1H, --NHCH--) 5.56 (1H, H in isoxazole ring)______________________________________
EXAMPLE 11: ##STR61##
6 g of tetraethyl [(5-methyl-3-isoxazolyl)amino]-methylene-bis(phosphonate) was dissolved in 60 ml of acetic anhydride and heated under reflux overnight. The reaction solution was concentrated under reduced pressure, and the resulting syrup was formed into a chloroform solution. This was washed with water and dried, and then the solvent was removed by distillation. The residue was purified on a silica gel column (eluent: 0.5-2% ethanolchloroform) to give 5.2 g of tetraethyl [N-acetyl(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as a pale yellow syrup.
This had the following physico-chemical property.
(i) Mass Spectrum (FAB Mass): 427 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.32 (12H, --OCH.sub.2 CH.sub.3 × 4) 2.12 (3H, --NCOCH.sub.3) 2.46 (3H, --CH.sub.3) 4.0 ˜ 4.4 (8H, --OCH.sub.2 CH.sub.3 × 4) 6.06 (1H, --NCH) 6.56 (1H, H in isoxazole ring)______________________________________
EXAMPLE 12: ##STR62##
Iodotrimethylsilane (2.68 ml) was added to an ice-cooled solution of 2 g of tetraethyl [N-acetyl(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 20 ml of carbon tetrachloride. Then the temperature was allowed to rise to room temperature, and the mixture was stirred for 1 hour. The reaction mixture was concentrated, methanol was then added, and the mixture was again concentrated. The residue thus obtained was washed with ether, hexane and acetone to give a solid which was recrystallized from acetone-hexane to give 0.5 g of [N-acetyl(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as crystals.
The physico-chemical characteristics of this product are as follows:
(i) Elementary Analysis (as C 7 H 12 N 2 O 8 P 2 ):
______________________________________ C(%) H(%) N(%)______________________________________Calculated: 26.77 3.85 8.92Found: 26.98 3.84 8.72______________________________________
(ii) Mass Spectrum (FAB Mass): 315 (M+1)
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 2.10 (3H, NCOCH.sub.3) 2.48 (3H, --CH.sub.3) 5.32 (1H, NCH) 6.50 (1H, H in isoxazole ring)______________________________________
EXAMPLE 13: ##STR63##
Iodotrimethylsilane (1.2 ml; 2 molar equivalents) was added dropwise to an ice-cooled solution of 1.6 g of tetraethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 16 ml of carbon tetrachloride. Then the temperature was allowed to rise to room temperature, and the mixture was stirred for 1 hour. The reaction mixture was concentrated, methanol was then added, and the mixture was again concentrated. The residue thus obtained was washed with hexane, and then dissolved in 0.1N aqueous sodium hydroxide, the pH being adjusted to 7. The solution was applied to an HP-20 resin column for purification (eluent: water) to give 0.2 g of disodium diethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as a solid.
The physico-chemical characteristics of this product are as follows:
(i) Elementary Analysis (as C 9 H 16 N 2 Na 2 O 7 P 2 ·H 2 O):
______________________________________ C (%) H (%) N (%)______________________________________Calculated: 27.71 4.65 7.18Found: 27.67 4.32 7.22______________________________________
(ii) Mass Spectrum (FAB Mass): 327 (M-1)
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 1.18 (6H, --OCH.sub.2 C .sub.-- H.sub.3 × 2) 2.30 (3H, --CH.sub.3) 3.8˜4.8 (4H, --OC .sub.-- H.sub.2 CH.sub.3 × 2) 3.96 (1H, --NHC .sub.-- H--) 5.82 (1H, H in isoxazole ring)______________________________________
EXAMPLE 14: ##STR64##
Iodotrimethylsilane (1.8 ml; 3 molar equivalents) was added dropwise to an ice-cold solution of 1.6 g of tetraethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 16 ml of carbon tetrachloride. Then the temperature was allowed to rise to room temperature, and the mixture was stirred for 1 hour. The reaction mixture was concentrated, methanol was then added, and the mixture was again concentrated. The residue thus obtained was washed with hexane, and dissolved in water. The solution was applied to an HP-20 resin column for purification (eluent: water) to give 0.27 g of ethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as a solid.
The physico-chemical characteristics of this product are as follows:
This had the following physico-chemical property.
(i) Elementary Analysis (as C 7 H 14 N 2 O 7 P 2 ·0.5H 2 O):
______________________________________ C(%) H(%) N(%)______________________________________Calculated: 27.17 4.85 9.06Found: 27.39 4.60 9.44______________________________________
(ii) Mass Spectrum (FAB Mass): 301 (M+1)
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 1.22 (3H, --OCH.sub.2 C .sub.-- H.sub.3) 2.30 (3H, --CH.sub.3) 3.8˜4.2 (2H, --OC .sub.-- H.sub.2 CH.sub.3) 4.12 (1H, --NHCH--) 5.88 (1H, H in isoxazole ring)______________________________________
EXAMPLE 15: ##STR65##
A mixture of 2 g of 3-amino-5-n-pentylisoxazole, 2.3 g of ethyl orthoformate and 7.2 g of diethyl phosphite was heated at 150° C. with stirring for 60 minutes. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified on a silicagel column (eluent: 0 to 3% methanol-chloroform) to give 3.2 g of tetraethyl [(5-n-pentyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as a pale yellow oil.
The physico-chemical characteristics of this product are as follows:
This had the following physico-chemical property.
(i) Mass Spectrum (FAB Mass): 441 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.2˜1.8 ##STR66## 2.6 ##STR67## 4.0˜4.4 ##STR68## 4.5 ##STR69## 5.5 (1H, H in isoxazole ring)______________________________________
In the same manner as Example 15, the following compounds were prepared.
EXAMPLE 16: ##STR70##
Physico-chemical property:
(i) Mass Spectrum (EI Mass): 454 (M)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.2˜1.8 ##STR71## 2.6 ##STR72## 4.0˜4.4 ##STR73## 4.5 ##STR74## 5.5 (1H, H in isoxazole ring)______________________________________
Starting Compound: 3-Amino-5-n-hexylisoxazole
EXAMPLE 17: ##STR75##
Physico-chemical property:
(i) Mass Spectrum (EI Mass): 468 (M)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.1˜1.8 ##STR76## 2.6 ##STR77## 4.0˜4.4 ##STR78## 4.5 ##STR79## 5.5 (1H, H in isoxazole ring)______________________________________
Starting compound: 3-Amino-5-n-heptylisoxazole
EXAMPLE 18: ##STR80##
Physico-chemical property:
(i) Mass Spectrum (FAB Mass): 483 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.2˜1.8 ##STR81## 2.6 ##STR82## 4.0˜4.4 ##STR83## 4.5 ##STR84## 5.5 (1H, H in isoxazole ring)______________________________________
Starting compound: 3-Amino-5-n-octylisoxazole
EXAMPLE 19: ##STR85##
Physico-chemical property:
(i) Mass Spectrum (FAB Mass): 441 (M+1)
(ii) NMR Spectrum
______________________________________δ: 0.9 (6H, (CH.sub.3).sub.2) 1.2˜1.7 ##STR86## 2.6 ##STR87## 4.0˜4.4 ##STR88## 4.5 ##STR89## 5.6 (1H, H in isoxazole ring)______________________________________
Starting compound: 3-Amino-5-isoamylisoxazole
EXAMPLE 20: ##STR90##
Physico-chemical property:
(i) Mass Spectrum (EI Mass): 504 (M)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.2˜1.4 ##STR91## 2.9 (3H, OMe) 3.8 (4H, CH.sub.2 CH.sub.2) 4.0˜4.4 ##STR92## 4.5 ##STR93## 5.5 (1H, H in isoxazole ring) 6.8, 7.1 (4H, H in benzene ring)______________________________________
Starting compound: 3-Amino-5-p-methoxyphenethylisoxazole
EXAMPLE 21: ##STR94##
A solution of 3 g of tetraethyl [(5-n-pentyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 30 ml of concentrated hydrochloric acid was heated under reflux for 3 hours. After the reaction mixture was concentrated, the solid obtained was washed with acetonitrile to give 1.8 g of [(5-n-pentyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as a solid.
This had the following physico-chemical property.
(i) Elementary Analysis (as C 9 H 18 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 32.94 5.53 8.54 18.88Found: 32.88 5.36 8.56 18.86______________________________________
(ii) Mass Spectrum (FAB Mass): 327 (M-1)
(iii) NMR Spectrum (in D 2 O with K 2 CO 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.3˜1.8 (6H, (CH.sub.2).sub.3) 2.6 ##STR95## 3.8 ##STR96## 5.8 ##STR97##______________________________________
In the same manner as Example 21, the following compounds were prepared.
EXAMPLE 22: ##STR98##
Physico-chemical property:
(i) m.p.: 238° C. (decomposition)
(ii) Elementary Analysis (as C 10 H 20 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 35.10 5.89 8.19 18.10Found: 35.38 5.72 8.11 17.84______________________________________
(iii) Mass Spectrum (FAB Mass): 343 (M+1)
EXAMPLE 23: ##STR99##
Physico-chemical property:
(i) m.p.: 205° C. (decomposition)
(ii) Elementary Analysis (as C 11 H 22 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 37.09 6.22 7.86 17.39Found: 37.09 6.15 7.83 17.28______________________________________
(iii) Mass Spectrum (FAB Mass): 357 (M+1)
EXAMPLE 24: ##STR100##
Physico-chemical property:
(i) m.p.: 225° C. (decomposition)
(ii) Elementary Analysis (as C 12 H 24 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%)______________________________________Calculated: 38.93 6.53 7.57Found: 38.93 6.51 7.64______________________________________
(iii) Mass Spectrum (FAB Mass): 371 (M+1)
EXAMPLE 25: ##STR101##
Physico-chemical property:
(i) m.p.: 196° C. (decomposition)
(ii) Elementary Analysis (as C 9 H 18 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 32.94 5.53 8.54 18.88Found: 32.66 5.50 8.66 18.72______________________________________
(iii) Mass Spectrum (FAB Mass): 329 (M+1)
EXAMPLE 26: ##STR102##
Physico-chemical property:
(i) m.p.: 265° C. (decomposition)
(ii) Elementary Analysis (as C 13 H 18 N 2 O 8 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 39.81 4.62 7.14 15.79Found: 39.69 4.46 7.19 15.71______________________________________
(iii) Mass Spectrum (FAB Mass): 392 (M+1)
EXAMPLE 27: ##STR103##
A mixture of 3 g of 3-amino-5-n-butylisoxazole, 3.7 g of ethyl orthoformate and 12 g of diethyl phosphite was heated at 150° C. with stirring for 60 minutes. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified on a silicagel column (eluent: 0 to 3% ethanol-chloroform) to give 5 g of tetraethyl [(5-n-butyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as a pale yellow oil.
The physico-chemical characteristics of this product are as follows:
(i) Mass Spectrum (FAB Mass): 247 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 0.9 (3H, CH.sub.3) 1.2˜1.8 ##STR104## 2.6 ##STR105## 4.0˜4.4 ##STR106## 4.5 ##STR107## 5.5 (1H, H in isoxazole ring)______________________________________
EXAMPLE 28: ##STR108##
A solution of 4.8 g of tetraethyl [(5-n-butyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 50 ml of concentrated hydrochloric acid was heated under reflux for 3 hours. After the reaction mixture was concentrated, the solid obtained was washed with acetonitrile to give 2.5 g of [(5-n-butyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as a solid.
This had the following physico-chemical property.
(i) m.p.: 200° C. (decomposition)
(ii) Elementary Analysis (as C 8 H 16 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 30.58 5.13 8.91 19.72Found: 30.28 4.84 8.95 19.52______________________________________
(iii) Mass Spectrum (FAB Mass): 315 (M+1)
EXAMPLE 29: ##STR109##
A mixture of 3.3 g of 3-amino-5-(4-methyl-3-ene)pentylisoxazole, 4.4 g of ethyl orthoformate and 20 g of diethyl phosphite was heated at 150° C. with stirring for 60 minutes. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified on a silicagel column (eluent: 0 to 3% methanol-chloroform) to give 3.6 g of tetraethyl [[5-(4-methyl-3-ene)pentyl-3-isoxazolyl]amino]methylene-bis(phosphonate) as a pale yellow oil.
The physico-chemical characteristics of this product are as follows:
(i) Mass Spectrum (EI Mass): 452 (M)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 1.6˜1.7 ##STR110## 5.6 (1H, H in isoxazole ring)______________________________________
In the same manner as Example 29, the following compounds were produced.
EXAMPLE 30: ##STR111##
Physico-chemical property:
(i) Mass Spectrum (EI Mass): 472 (M)
(ii) NMR Spectrum:
______________________________________δ: 5.9 (1H,H in isoxazole ring) 6.7˜7.5 (1H,H based on styrene)______________________________________
Starting compound: 3-Amino-5-styrylisoxazole
EXAMPLE 31: ##STR112##
Iodotrimethylsilane (6.2 g) was added dropwise to an ice-cold solution of 3.5 g of tetraethyl [[5-(4-methyl-3-ene)pentyl-3-isoxazolyl]amino]methylene-bis(phosphonate) in 35 ml of carbon tetrachloride. Then the temperature was allowed to rise to room temperature, and the mixture was stirred for 1 hour. The reaction mixture was concentrated, methanol was then added, and the mixture was again concentrated. The residue thus obtained was washed with acetone and acetonitrile to give 1.8 g of [[5-(4-methyl-3-ene)pentyl-3-isoxazolyl]amino]methylene-bis(phosphonic acid) as a solid.
The physico-chemical characteristics of this product are as follows:
This has the following physico-chemical property.
(i) m.p.: 213° C. (decomposition)
(ii) Elementary Analysis (as C 10 H 18 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 35.30 5.33 8.23 18.21Found: 35.19 5.23 8.30 18.05______________________________________
(iii) Mass Spectrum (FAB Mass): 341 (M+1)
In the same manner as Example 31, the following compounds were prepared.
EXAMPLE 32: ##STR113##
Physico-chemical property:
(i) m.p.: 287° C. (decomposition)
(ii) Elementary Analysis (as C 12 H 14 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%) P (%)______________________________________Calculated: 40.01 3.92 7.78 17.20Found: 39.73 3.96 7.61 17.46______________________________________
(iii) Mass Spectrum (FAB Mass): 459 (M-1)
EXAMPLE 33: ##STR114##
A mixture of 2.9 g of 3-amino-4-methylisoxazole, 5.7 g of ethyl orthoformate and 20.4 g of diethyl phosphite was heated at 160° C. with stirring for 3 hours. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified on a silicagel column (eluent: chloroform-ethyl acetate) to give 3.2 g of tetraethyl [(4-methyl-3-isoxazolyl]amino]methylene-bis(phosphonate) as a solid.
m.p.: 68°-69° C.
EXAMPLE 34: ##STR115##
To an ice-cold solution of 9.8 g of 3-amino-5-methylisoxazole in dichloromethane (98 ml) was added dropwise 40 ml of a mixture of formic acid/acetic anhydride (5:3). Then the mixture was stirred overnight at room temperature. The reaction mixture was concentrated, and the solid obtained was washed with ether to give 10 g of 5-methylisoxazolyl-3-formamide.
A mixture of 9.8 ml of trimethyl phosphite and 1.3 ml of phosphorus trichloride was heated at 65° C. for 30 minutes. To this reaction mixture was added 1 g of 5-methylisoxazolyl-3-formamide, and the mixture was stirred at that temperature for 1 hour. The reaction mixture was concentrate and subjected to purification on a silica gel column (eluent: chloroform-methanol) to give 0.9 g of tetramethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) as crystals.
The physico-chemical characteristics of this product are as follows:
(i) Mass Spectrum (FAB Mass): 329 (M+1)
(ii) NMR Spectrum (in CDCl 3 ):
______________________________________δ: 2.30 ##STR116## 3.8˜4.0 (12H, MeO × 4) 4.64 (1H, C .sub.--HNH) 5.60 ##STR117##______________________________________
In the same manner as Example 34, the compounds of Examples 2 to 5, 10, 15 to 20, 27, 29, 30 and 33 can also be prepared.
MANUFACTURE EXAMPLE 1: ##STR118##
Iodotrimethylsilane (7.1 ml) was added dropwise to an ice-cold solution of 4.8 g of tetraethyl [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 90 ml of carbon tetrachloride. Then the temperature was allowed to rise to room temperature, and the mixture was stirred for 1 hour. The reaction mixture was concentrated, methanol was then added, and the mixture was again concentrated. The solid thus obtained was washed with a hot acetone to give 2.9 g of [(5-methyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as a colorless solid.
The physico-chemical characteristics of this product are as follows.
(i) Elementary Analysis (as C 5 H 10 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%)______________________________________Calculated: 22.07 3.70 10.30Found: 22.13 3.80 9.96______________________________________
(ii) Mass Spectrum (FAB Mass): 273 (M+1)
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 2.30 (3H, d, Me in isoxazole ring) 4.08 (1H, t, NHCH) 5.88 (1H, d, H in isoxazole ring)______________________________________
MANUFACTURE EXAMPLE 2: ##STR119##
A solution of 4.9 g of tetraethyl [(5-ethyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 46 ml of concentrated hydrochloric acid was heated under reflux for 3 hours. After the reaction mixture was concentrated, the solid obtained was washed with acetone to give 2.8 g of [(5-ethyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as a solid.
This had the following physico-chemical property:
(i) Elementary Analysis (as C 6 H 12 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%)______________________________________Calculated: 25.19 4.23 9.79Found: 24.89 4.30 9.55______________________________________
(ii) Mass Spectrum (FAB Mass): 287 (M+1)
(iii) NMR Spectrum (in D 2 O):
______________________________________δ: 1.20 (3H, --CH.sub.2 C .sub.--H.sub.3) 2.64 (2H, --CH.sub.2 CH.sub.3) 4.10 (1H, --NHCH--) 5.90 (1H, H is isoxazole ring)______________________________________
MANUFACTURE EXAMPLE 3: ##STR120##
A solution of 3.2 g of tetraethyl [(4-methyl-3-isoxazolyl)amino]methylene-bis(phosphonate) in 32 ml of concentrated hydrochloric acid was heated under reflux for 4 hours. After the reaction mixture was concentrated, the solid obtained was washed with a mixture of methanol-acetonitrile-acetone to give 1.8 g of [(4-methyl-3-isoxazolyl)amino]methylene-bis(phosphonic acid) as a solid.
(i) m.p.: 272°-274° C. (decomposition)
(ii) Elementary Analysis (as C 5 H 10 N 2 O 7 P 2 ):
______________________________________ C (%) H (%) N (%)______________________________________Calculated: 22.07 3.70 10.30Found: 21.90 3.70 9.99______________________________________
PRESCRIPTION EXAMPLE:
Examples for prescription of the compound of the present invention as a drug will be mentioned below.
(1) Tablet:
______________________________________Compound of Manufacture Example 1 5 mgLactose 119 mgCorn Starch 67 mgHydroxypropyl Cellulose 4 mgCalcium Carboxymethyl Cellulose 4 mgMagnesium Stearate 1 mgTotal 200 mg______________________________________
5 g of the compound of Manufacture Example 1, 119 g of lactose and 67 g of corn starch were uniformly blended, 40 ml of an aqueous 10% (w/w) hydroxypropyl cellulose solution was added thereto, and the resulting mixture was wet-granulated. The granules thus obtained were blended with 4 g of calcium carboxymethyl cellulose and 1 g of magnesium stearate, and the resulting mixture is formed into tablets, each having a weight of 200 mg/tablet.
(2) Capsule:
______________________________________Compound of Manufacture Example 1 5 mgCrystalline Cellulose 50 mgCrystalline lactose 144 mgMagnesium Stearate 1 mgTotal 200 mg______________________________________
The above-mentioned ingredients were blended each in an amount of 1000 times of the above-mentioned amount and encapsulant in gelatin capsules, each containing 200 mg of the mixture per one capsule.
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"Novel bisphosphonic acid derivatives, and a bone resorption-inhibitor and an anti-arthritis containing a bisphosphonic acid derivative represented by the formula (I): ##STR1## wherein R 2 represents a hydrogen atom, an alkyl group, etc.,
R 2 represents a hydrogen atom or a lower alkanoyl group,
R 3 , R 4 , R 5 and R 6 may be the same or different, each represents a hydrogen atom or lower alkyl group."
| 2
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CROSS REFERENCE TO RELATED APPLICATIONS:
[0001] This application is a continuation application of co-pending application Ser. No. 11/553,330, filed Oct. 26, 2006, now U.S. Pat. No. ______, the disclosure of which is incorporated herein in its entirety.
BACKGROUND
[0002] 1. Field of the Invention
[0003] This invention relates to the sorting of objects, and more particularly to the sorting of mass produced, customized objects.
[0004] 2. Description of the Related Art
[0005] Sorting devices are known for separately guiding finished parts to different discharge areas adjacent to tooling or packaging machines. Typically, sorting devices operate as a post-processing tool that is used to sort finished pieces.
[0006] Generally, finished pieces are identified on the basis of the quality of the material or the type of material. For example, only parts possessing a similar quality of material are selected and packaged together. The packaging station performs similar operations on similar parts. In most instances, parts having unique or customized features that must be packaged together are not readily accommodated. Presently, the sorting and packaging of unique, customized parts must be done manually to ensure accuracy.
[0007] Accordingly, there is a need to provide a simple and efficient sorting and selecting system that brings a variety of associated objects together during a production process with resulting improvements in efficiency and productivity.
SUMMARY
[0008] The present invention provides a system and associated method for sorting mass produced, customized objects.
[0009] In one aspect of the invention, a part sorting process is provided including loading a plurality of randomly presented parts; sorting at least one selected part of the randomly presented parts into a group of associated parts; and sequencing the group of associated parts.
[0010] In yet another aspect of the invention, a system is provided for sorting parts. The invention includes a system for receiving and continuously circulating a plurality of randomly presented parts. The invention also includes a sorting buffer for accumulating selected parts from the plurality of randomly presented parts in an assigned buffer location, and a sequencing system for sequencing the accumulated selected parts.
[0011] A more complete understanding of the invention can be obtained by reference to the following detailed description of the embodiments thereof in connection with the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings in which:
[0013] FIG. 1A is a flowchart of a sorting system process in accordance with an embodiment of the present invention;
[0014] FIG. 1B is a simplified illustration of a dental aligner on a carrier in accordance with an embodiment of the present invention;
[0015] FIG. 2 is a simplified illustration of components of a load cell of a sorting system in accordance with an embodiment of the present invention;
[0016] FIGS. 3A-3D are simplified illustrations of components of the load cell of FIG. 2 in accordance with an embodiment of the present invention;
[0017] FIG. 4 is a simplified illustration of an indexing table unloading parts and placing them on carriers in accordance with an embodiment of the present invention;
[0018] FIG. 5 is a simplified illustration of a reader in accordance with an embodiment of the present invention;
[0019] FIG. 6A is a simplified illustration of components of a sorting buffer cell in accordance with an embodiment of the present invention;
[0020] FIG. 6B is a simplified Illustration of the operation of a buffer conveyor associated with the sorting buffer cell in FIG. 6A in accordance with an embodiment of the present invention;
[0021] FIG. 7 is a simplified illustration of components of a puck sequencing cell in accordance with an embodiment of the present invention;
[0022] FIG. 8 is a simplified illustration of a storage cell in accordance with an embodiment of the present invention; and
[0023] FIG. 9 is a simplified illustration of a quality control station in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
[0024] In the detailed description of the invention that follows, the invention is described primarily in the context of a system and method for sorting mass produced customized dental appliances, such as dental aligners. It should be understood, however, that the system and processes of the present invention may be employed in the sorting of any of various types of items, work pieces or parts, such as prosthetic body parts, implantable hearing aids, eyeglass lenses and the like.
[0025] FIG. 1A is a flowchart representing manufacturing cells of a sorting system 100 in accordance with an embodiment of the present invention. In pre-processing cell 102 , if necessary, parts may undergo a pre-processing step in which the parts are cleaned, sanitized, or otherwise prepared for traversing sorting system 100 .
[0026] Load cell 104 represents a process for the introduction of a batch or plurality of items or parts that are manually (or alternatively, automatically) loaded into sorting system. 100 via a bulk supply pre-feeder mechanism. The pre-feeder mechanism delivers parts to a part distribution and circulation system, which includes a system of conveyors that distribute the parts over a conveyor for presentation to a vision system. In one embodiment, the quantity of parts delivered may be a metered quantity of the entire batch of parts delivered periodically to the part distribution and circulation system to avoid overwhelming the system.
[0027] The vision system, including a robot picker, identifies the part location and orientation, then picks up and places each part onto an indexing table at a loading position. In one embodiment, the robot picker in conjunction with the vision system selects only parts having a desired top/bottom up orientation and places them on the indexing table. In yet another embodiment, the robot picker in conjunction with the vision system selects a part and manipulates the part, if necessary, until the part has the desired orientation before placing the part onto the indexing table. For example, the robot picker may pick a part having a bottom up orientation and then rotate the part until it has a top up orientation before placing the part onto the indexing table.
[0028] Alternatively, as described in greater detail below, the robot picker may place a part on the indexing table without regard to the part's orientation. The indexing table then indexes to a vision station so that the part can be scanned for top/bottom orientation. Once the part orientation is determined, the indexing table then indexes to a reorientation station, which includes a mechanism capable of rotating the part, as required, to achieve a desired top/bottom up orientation.
[0029] Once properly oriented, the indexing table indexes to a ‘unique code’ read station so that a unique code of each part can be read and ultimately mapped to a particular corresponding part carrier or “puck.” After the indexing table indexes to an unload station, the properly oriented and identified parts are unloaded by a pick-and-place unit or the equivalent into the corresponding pucks.
[0030] In one embodiment, each puck may be identified by a radio frequency identification device (RFID). The puck's RFID and the unique code are “mapped” to each other and the data is stored in a database. Before exiting load cell 104 , each puck is scanned by a subsequent vision system to verify “part presence.”
[0031] The pucks are conveyed from load cell 104 to a sorting buffer cell 106 . Alternatively, the pucks may be conveyed to an exceptions handling cell 108 , which may include one or more manual quality assurance stations (QAS).
[0032] In one embodiment of sorting buffer cell 106 , the pucks travel to a walking beam past an RF reader or the equivalent. The RF reader identifies the unique code number and temporarily assigns the unique code to one of a number of buffer lanes. If the number of parts to be included in one group requires more than one lane, the group may be logically split among buffer lanes to assure that the parts are sequenced correctly. The walking beam advances pucks in a controlled motion to the head of the sorting buffer lanes. Once a puck gets to its assigned lane, the puck is pushed out of the path of the walking beam and into its assigned lane. Pucks are accumulated in their assigned lanes until all parts in the batch are sorted. When a lane is filled with a completed group or case of associated parts, the group is released to the unload section of sorting buffer cell 106 when space is available. Buffer lanes are then released one at a time from the unload section of sorting buffer cell 106 .
[0033] Routing system cell 110 includes a series of conveyors with merge and divert units routing pucks between the cells throughout sorting system 100 . For example, the conveyors rout pucks from load cell 104 to sorting buffer cell 106 or exceptions handling cell 108 and back to load cell 104 , from sorting buffer cell 106 to storage cell 112 and/or puck sequencing cell 114 , and from puck sequencing cell 114 to packaging cell 116 or to exceptions handling cell 108 and back to load ceil 104 . Note that exceptions handling cell 108 may include more than one QAS, thus parts that are routed to exceptions handling cell 108 during various stages of the sorting process may be routed to the QAS associated with that particular stage.
[0034] Incomplete groups are routed from sorting buffer cell 106 to the incomplete case storage cell 112 . In one embodiment, the pucks move via a conveyor, stop at an unloading station and are picked-and-placed on to a pallet. When the pallet is loaded it travels to an inserter/extractor (I/E) station. The pallet is transferred to the I/E via a standard lift and transfer. The I/E then moves the pallet to a shelf in a horizontal carousel for storage. When the last missing part or parts of a group arrives at incomplete case storage cell 112 , the I/E picks the pallets with the associated parts and places the pallets onto the conveyor for transport to a loading station. At the loading station, the group is completed and is then moved to puck sequencing cell 114 .
[0035] At puck sequencing cell 114 , the pucks are transferred to a walking beam and moved past a series of lanes. The lanes of the conveyor are assigned, for example, 1 through 50 and when each puck is in front of the proper lane it is transferred onto a stop/start take away conveyor. Once all pucks are transferred they are released by the conveyor where they then travel in the proper sequence to packaging cell 116 .
[0036] If a puck is marked “no read” at load cell 104 or sorting buffer cell 106 , the puck is diverted to exceptions handling cell 108 , which includes more than one QAS positioned throughout sorting system 100 . In one embodiment, the manual QAS includes an RF reader provided to read an ID tag disposed on the puck. A quality assurance computer terminal is used to allow an operator to manually enter an ID number of the puck and thus re-initialize the puck into sorting system 100 . The operator then releases the puck to be merged back into the main line ahead of sorting buffer cell 106 . The manual QAS also introduces direct batches of products that do not enter sorting system 100 through load cell 104 .
[0037] Generally, in one embodiment of the present invention, the mass produced, customized objects are dental appliances, referred to as a dental aligners, such as the dental aligner illustrated in FIG. 1B . Dental aligner 118 may be formed from a dental mold made from a computerized model representing digitally a patient's dental geometry and tooth configuration or, alternatively, from an impression made of a patient's teeth.
[0038] The computerized model of the patient's teeth may be digitally manipulated to portray a new tooth arrangement (i.e. an orthodontic prescription) and a mold may be produced to reflect each successive arrangement in the prescription. This may be repeated any number of times to derive a number of molds with differing tooth arrangements.
[0039] The series of computer models or digital data sets representing the dental geometries or orthodontic prescription associated with the series of molds is used to fabricate a series of dental aligners by disposing the dental molds in a thermoplastic fabrication machine. The series of dental aligners form a group of associated aligners that need to be sorted from other groups of associated aligners and properly sequenced before packaging.
[0040] In one exemplary embodiment, as shown in FIG. 1B , aligner 118 may be fabricated to fit within a 75 mm diameter, and have a weight less than. 8 ounces. Aligner 118 may be laser marked with patient information and aligner sequence with an upper or lower designation.
[0041] Dental aligner 118 may be of the type described, for example, in U.S. Patent Application Publication No. 2005/0082703, which is incorporated herein by reference.
1. Load Cell
[0042] FIG. 2 is a simplified illustration of load cell 104 of sorting system 100 in accordance with an embodiment of the present invention. In one embodiment, load cell 104 includes a bulk supply pre-feeder 202 , a part circulation system 204 , a robot loader 208 , including or working in conjunction with a vision system 210 , and an indexing table 214 .
[0043] In one operational embodiment, a batch of parts 201 , such as aligners 118 ( FIG. 1B ), are loaded into bulk supply pre-feeder 202 . In one embodiment, as many as approximately 500 aligners 118 may be fed into bulk supply pre-feeder 202 in one operation. In one embodiment, aligners 118 arrive at bulk supply pre-feeder 202 after pre-processing or a pre-treatment for example, after having been cleaned, tumbled and disinfected.
[0044] In one embodiment, part circulation system 204 includes a metering conveyor 216 , a vision belt conveyor 206 , a return conveyor 218 , and a return elevating bucket assembly 220 . Bulk supply pre-feeder 202 may dispense a portion of the batch of aligners 118 in metered quantities onto metering conveyor 216 based on a signal from a level sensor 203 mounted proximate to or on metering conveyor 216 . Level sensor 203 senses gaps between bunches of aligners 118 that have been dispensed on metering conveyor 216 . For example, when the gaps become larger than a predetermined size, bulk supply pre-feeder 202 is made to dispense more aligners 118 into the system. As described below, aligners 118 that are disposed onto metering conveyor 216 from the return elevating bucket assembly 220 also create a portion of the bunches of aligners.
[0045] An exemplary bulk supply pre-feeder 202 may be a three and a half (3-V2) cubic foot pre-feeder, which is available as Farason Model GF-3.6, from Farason Corporation of Pennsylvania.
[0046] In one embodiment, to ensure that aligners 118 are distributed evenly onto vision belt conveyor 206 and are separated in a single layer, one or more rotating paddlewheels 222 with pliable spokes are mounted adjacent the end of metering conveyor 216 and the beginning of vision belt conveyor 206 . The pliable spokes may be mounted on a horizontal axle or, alternatively, on one more vertical spindles. Paddlewheels 222 , receive aligners 118 , such that the pliable spokes separate aligners 118 to keep aligners 118 from grouping in large clumps onto vision belt conveyor 206 . This increases the number of “pickable” parts dispersed onto vision belt conveyor 206 .
[0047] Alternatively, parts 201 can be delivered directly from bulk supply pre-feeder 202 onto vision belt conveyor 206 . In this alternative embodiment, bulk supply pre-feeder 202 may include a funnel shaped dispenser that allows parts 201 to be dispensed only along a single vertical plane, thus ensuring that the parts are dispersed in a separated manner.
[0048] Paddlewheels 222 distribute or spread aligners 118 over vision belt conveyor 206 for presentation to robot loader 208 in combination with a vision system 210 (hereinafter, in combination, “robot system 212 ”). As described below, aligners 118 are picked up from vision belt conveyor 206 and placed onto indexing table 214 by robot system 212 . A suitable type of robot system 212 is available as an Adept Cobra 800 Scara Robot with Adept Vision.
[0049] Aligners 118 not removed by robot system 212 fall off vision belt conveyor 206 and return to metering conveyor 216 via the return conveyor 218 and return elevating bucket assembly 220 so that aligners 118 can be circulated and thus represented to robot system 212 .
[0050] In operation, returning aligners 118 are discharged off the end of return conveyor 218 into return elevating bucket 224 . The bucket cycles may be based on a level sensor 226 mounted in return elevating bucket 224 , which indicates when enough parts (e.g. aligners) have been collected for return to metering conveyor 216 . In one embodiment, return elevating bucket 224 elevates aligners 118 (as shown in phantom) and dispenses them onto metering conveyor 216 , which may be mounted directly overhead and parallel to vision belt conveyor 206 and return conveyor 218 . Metering conveyor 216 is cycled on and off to meter aligners 118 onto vision belt conveyor 206 . In one embodiment, parts not unidentifiable by robot system 212 are rejected into a manual removal hopper 230 at the end of the operation for manual identification at a manual QAS.
[0051] Robot system 212 identifies the location and orientation of part 201 on vision belt conveyor 206 , picks up and places each part 201 onto indexing table 214 at the loading position.
[0052] When no pickable parts are available to be processed from the current batch of aligners 118 , the cycle for the batch is considered complete. The machine may automatically switch to “cleanout,” which means bucket 224 remains in an. elevated location proximate to metering conveyor 116 . Any remaining rogue parts 201 (i.e. aligners 118 ) then exit the back of the machine into manual removal hopper 230 for manual retrieval.
[0053] An exemplary type of part circulation system 204 , including a metering conveyor, a vision conveyor, a return conveyor, and a return elevating bucket assembly, is available as Farason Model SRFF-30 FaraFeeder, from Farason Corporation of Pennsylvania.
[0054] As shown in FIG. 3A , indexing table 214 includes part holders 302 , which are designed shaped and configured to receive and hold parts 201 . In one embodiment, part holder 302 may be designed and shaped to hold and receive aligners 118 .
[0055] As shown in FIG. 3B , indexing table 214 may receive aligners 118 in any top-up or top-down orientation. Accordingly, to ensure that aligners 118 axe in an acceptable orientation, indexing table 214 indexes to a vision station 304 so that aligners 118 may be scanned for top-up or to down orientation. In operation, vision station 304 identifies the top-up or top-down orientation of aligner 118 .
[0056] As shown in FIG, 3 C, if it has been determined that aligner 118 is not in a desired orientation, when indexing table 214 indexes to reorientation station 306 , at least one orienting device 308 is employed to manipulate aligner 118 , as required, to achieve the desired orientation in holder 302 . For example, orienting device 308 grips aligner 118 having the top-down, orientation and removes it from holder 302 . Indexing table 214 continues to rotate the same holder 302 to the next incremental position. Simultaneously orienting device 308 rotates aligner 118 180° to achieve a top-up orientation. Orienting device 308 then replaces aligner 118 back into its same holder 302 .
[0057] As shown in FIG. 3D , indexing table 214 then indexes to a ‘code’ read station 310 . Code read station 310 includes a vision system 316 including a processor or computer. Vision system 316 reads an identification mark preformed on aligner 118 , such as a laser code. The computer is used to access the vision system software for initial setup of the code read or for re-programming.
[0058] In operation, vision system 316 identifies aligner 118 and maps the aligner to a carrier 402 , (hereinafter puck 402 , see FIGS. 1B and 4 ) used to ferry aligner 118 through the remaining sorting process. In one embodiment, each puck 402 is identified using an ID system, such as that which uses a small RFID for identification and tracking purposes. An RFID tagging system includes the tag, a read/write device, and a host system application, for data collection, processing, and transmission. An RFID tag may include a chip, memory and an antenna.
[0059] As shown in FIG. 4 , after an aligner 118 has been identified and mapped to puck 402 at code read station 310 ( FIG. 3D ), indexing table 214 moves to an ‘unload’ station where pick and place unit 404 , for example, a robot arm with a vacuum end arm tool, unloads aligner 118 , and places aligner 118 into puck 402 , which is being conveyed on conveyor 406 . Pick and place unit 404 may be designed to unload any volume of parts, for example, two at a time.
[0060] “No reads” from vision system 316 may occur from time to time due to an illegible code on part 201 . If this occurs, vision system 316 sends a “no read” signal to a manual quality control station. The RFID tag on puck 402 to be mapped to the unidentified part 201 is marked with a “no read” bit and routed to the manual quality control station for identification.
2. Sorting Buffer Cell
[0061] As previously described, pucks 402 including parts 201 are conveyed from load cell 104 to sorting buffer cell 106 or, in the case of the ‘no reads’, to exceptions handling cell 108 . Sorting buffer cell 106 is used to group parts 201 into predetermined groups. Thus, the randomly loaded parts 201 that enter load cell 104 are placed into predetermined groups as desired.
[0062] In one embodiment, as shown in FIGS. 5 and 6A , sorting buffer cell 106 includes a conveyor 502 , a reader 504 , such as an RF reader or the equivalent, and a walking beam 600 . In operation, pucks 402 travel on conveyor 502 past reader 504 to walking beam 600 . Reader 504 identifies puck 402 , which includes the unique part 201 , as part of a specific grouping of parts 201 . For example, in one embodiment, part 201 is aligner 118 having a unique shape and size. Aligner 118 may be one of a group of aligners representing a full prescription of aligners 118 for use with a single patient. Thus, as reader 504 identifies pucks 402 including aligners 118 as belonging to the predetermined prescription, processing capabilities associated with reader 504 cause pucks 402 to be temporarily assigned to one of a number of buffer lanes 604 ( FIG. 6A ) designated for aligners 118 for the predetermined prescription. Thus, assignment of buffer lanes 604 corresponds with the desired grouping. Thus, each new “case”, “group” or “prescription” to enter walking beam 600 has a new buffer lane 604 assigned. Buffer lanes 604 are assigned to cases in a logical order. If the size of the grouping requires more than one buffer lane 604 , the order is logically split among buffer lanes 604 . For example, if a case exceeds 50 aligners 118 , the case is assigned two buffer lanes 604 and pucks 402 are separated according to case or prescription number.
[0063] As shown in FIG. 6A , in operation, walking beam 600 , includes a buffer conveyor 602 , buffer lanes 604 and pushers 606 . In operation, after reader 504 ( FIG. 5 ) reads the ID, such as the RFID tag on puck 402 , puck 402 is conveyed to buffer conveyor 602 . In one embodiment, buffer conveyor 602 may be equipped with a motor and encoders (not shown.) so that each revolution of the motor equals one puck move or step.
[0064] In operation, as shown, in FIG. 6B , to advance pucks ( 1 , 2 , from in front of corresponding buffer lanes (A, B, C) to in front of corresponding buffer lanes (B, C, D), buffer conveyor 602 moves one increment to the right casing pucks ( 1 , 2 , 3 ) to move one position. Buffer conveyor 602 then moves back away from pucks ( 1 , 2 , 3 ) and then to the left. Once back in its original position, buffer conveyor 602 moves forward to once again surround pucks ( 1 , 2 , 3 ). Pucks 402 are advanced in this controlled stepping motion so that each puck 402 may be paused at the head of each new buffer lane 604 before being moved to the head of the next buffer lane 604 .
[0065] Once puck 402 has reached the head of its assigned buffer lane 604 , puck 402 is pushed, while paused, out of the path of buffer conveyor 602 . Puck 402 is pushed using pushers 606 into sorting buffer lanes 604 . In one embodiment, pushers 606 may be pneumatically or hydraulically activated pistons. Alternatively, pucks 402 may be pushed into buffer lanes 604 using a robotic picker or a burst of air and the like.
[0066] Accordingly, pucks 402 accumulate in their assigned buffer lanes 604 until all aligners 118 entering load cell 104 are sorted into their associated groups. In one embodiment, when a buffer lane 604 is filled with a completed group, such as a full prescription of aligners 118 , the group may be released to the unload section of sorting buffer cell 106 . In one embodiment, buffer lanes 604 may be about 35 feet long and 4 feet wide and may have a belt speed for moving pucks 402 down the lane of about 60 ft/minute. Buffer lanes 604 also may include a series of release gates (not shown) for allowing the removal of a group of pucks 402 . Buffer lanes 604 are released one at a time from the unload section of sorting buffer cell 106 to puck sequencing cell 114 .
[0067] In one embodiment, the gross production rate for sorting buffer cell 106 may be about 60 parts per minute. In addition, sorting buffer cell 106 may include up to 30 buffer lanes 604 , which may hold up to 50 pucks 402 , yielding an overall capacity of 3000 pucks 402 . In addition, sorting buffer cell 106 may also have a downstream capacity equal to that of the upstream capacity.
[0068] In the event that reader 504 ( FIG. 5 ) is unable to read an RFID tag, the unidentified puck 402 may be routed to the manual quality control station where an operator may need to manually re-enter the unidentified puck into the system. If the operator manually re-enters the unidentified puck into the system before the batch has completed its cycle, the puck is sent to the proper buffer lane 604 . Subsequently, the completed group of pucks is directed to puck sequencing cell 114 .
3. Puck Sequencing Cell
[0069] After aligners 118 are grouped into buffer lanes 604 , they are next placed in a predetermined sequence. As illustrated in FIG. 7 , puck sequencing cell 114 includes sequencing walking beam 702 and stop/start take away conveyor 706 , which may be running at 60 ft/min. Prior to entering puck sequencing cell 114 , pucks 402 index past an RFID reader similar to that shown in FIG. 5 . The reader reads the RFID tag associated with puck 402 and places the value in a moving register. Pucks 402 are then indexed to the corresponding sequencing lane 704 . Sequencing walking beam 702 may be equipped with a motor and an encoder (not shown) so that each revolution of the motor equals one puck move followed by a pause in the same manner as described above with regard to FIGS. 6A and 6B . Each time the pucks 402 move, the RFID number is moved accordingly in the register.
[0070] Once puck 402 has reached its assigned position, puck 402 is pushed using pushers 708 during the pause out of the path of sequencing walking beam 702 and onto start/stop take away conveyor 706 into an assigned lane 704 . This process repeats until the maximum number of parts is in their correct positions in lanes 704 . Once it has been verified that all pucks 402 have made it to the proper positions, puck sequencing cell 114 releases the group of parts 201 to packaging cell 116 .
[0071] In one example, aligners 118 in pucks 402 are to be placed in a sequence numbered 1 -N for clarity. Pucks 402 are conveyed and transferred to sequencing walking beam 702 and moved past sequencing lanes 704 . Sequencing lanes 704 of stop/start take away conveyor 706 are assigned 1 through N lanes 704 , for example, 1 - 50 . As puck 402 is positioned by sequencing walking beam 702 in front of the proper sequencing lane 704 , puck 402 with aligner 118 is transferred onto the stop/start take away conveyor 706 . Once all pucks 402 are transferred, which means that aligners 118 for a particular prescription are positioned in the desired number sequence, pucks 402 are released by conveyor 706 and are moved in the desired sequence to packaging cell 116 for further processing. Sequencing walking beam 702 and transfer designs may be identical to those used in walking beam 600 of sorting buffer cell 106 .
[0072] In one embodiment, puck sequencing cell 114 may operate at a rate of 45 PPM and may be able to buffer a maximum of 50 aligners 118 .
[0073] Referring again to FIGS. 5 and 6A , it may happen that a puck 402 holding aligner 118 is not identified by reader 504 ( FIG. 5 ) and may need to be re-circulated. Meanwhile, the group of identified pucks 402 continues to be held in a particular buffer lane 604 until all associated aligners 118 of a particular group are gathered in the designated buffer lanes 604 . In one embodiment, after a default time has been reached, the incomplete group of identified pucks 402 may be diverted to an incomplete case storage cell 112 .
4. Incomplete Case Storage Cell
[0074] Incomplete groups or cases 801 of parts 201 are routed from sorting buffer cell 106 to incomplete case storage cell 112 (hereinafter “storage cell 112 ”). As shown in FIG. 8 , pucks 402 move via a conveyor 803 , to an unloading station 816 and are picked-and-placed via a pick-and-place mechanism 802 to a pallet 804 . When pallet 804 is loaded it travels to a standard Inserter/Extractor (I/E) unit 808 . In one embodiment, I/E unit 808 causes pallet 804 to move to a shelf 810 in a horizontal carousel 812 for storage. When the last missing aligners 118 of an associated group 801 makes it to storage cell 112 , I/E unit 808 picks pallet 804 with the associated aligners 118 and places pallets 804 onto a conveyor for transport to a loading station. At the loading station, the group is completed. The group of pucks 402 , now completed, is moved to puck sequencing cell 114 .
[0075] In one operational embodiment, incomplete cases 801 , which are identified at sorting buffer cell 106 , are routed to storage cell 112 via conveyor system 803 . Pucks 402 , including aligners 118 , stop at a loading/unloading station 816 where a maximum of four pucks 402 are picked and placed using pick-and-place mechanism 802 onto pallet 804 . In this embodiment, a maximum of 16 pucks 402 are held on a 4×4 pallet 804 with a maximum of 4 different cases or groups 801 stored on each pallet 804 .
[0076] Pallet 804 moves via a conveyor 807 to I/E unit 808 . I/E unit 808 vertically moves pallet 804 to access particular shelves 810 located within carousel bins 814 in horizontal carousel 812 for storage.
[0077] When the last missing aligner 118 of a particular case 801 moves to storage cell 112 , the system reverses the storage process and removes the proper pucks 402 (i.e. pallets) for the particular case 801 . Pallets 804 housing the remaining aligners 118 are removed from horizontal carousel 812 using I/E unit 808 and are placed back on conveyor 807 . Pallets 804 are then transported to the loading/unloading location 816 . Pucks 402 are picked and placed back onto main conveyor 803 and held until all aligners 118 for that case 801 are once again present. After all pucks 402 are in position and ease 801 is full, case 801 is released to puck sequencing cell 114 .
[0078] In one operational embodiment, storage cell 112 may operate at a rate of 4 pallets per minute or up to 64 pucks per minute if all 16 places on each pallet are full.
[0079] Storage cell 112 handles incomplete cases 801 and stores them until such time that it has been verified that all parts 201 have arrived. In one embodiment, cases 801 may be resolved within 24 hours. In one embodiment, a query may be made for a list of aligners 118 stored in storage cell 112 , which may be sorted by “time in”.
[0080] In one embodiment, it may be possible to get a “no pick” from the pick and place mechanism 802 either from conveyor 803 to pallet 804 or from pallet 804 to the conveyor. If this occurs, pick-and-place mechanism 802 , after placing pucks 402 it has already picked, goes back to the “no pick” position and re-picks the missing puck 402 .
5. Exceptions Handling Cell
[0081] If a puck 402 is marked “no read” at load cell 104 or sorting buffer cell 106 , the non-read puck 402 is diverted to exceptions handling cell 108 , which includes one or more manual quality control stations 900 . Manual quality control station 900 may include an RF reader 902 provided to read the RFID tag on puck 402 . Manual quality control station 900 may also include a computer terminal 904 that allows an operator to manually enter the code number of puck 402 and aligner 118 and thus initialize it in the system. The operator may release the puck 402 and so it may be merged back into the main line ahead of sorting buffer cell 106 . If the operator can enter the information before the current batch of aligners 118 has been transferred to the discharge end of sorting buffer cell 106 then it can be sent to the proper buffer lane 604 ( FIG. 6A ) just as if puck 402 had come from load cell 104 . If, however, the operator cannot enter aligner 118 in time, puck 402 is sent through sorting buffer cell 106 to storage cell 112 . Alternatively, manual quality control station 900 can also introduce direct batches of parts that do not enter the sorting system through load cell 104 .
[0082] In accordance with the present invention, each cell of the present invention includes routing capabilities that are well known in the art. Routing system 110 includes, for example, a series of conveyors with merge and divert units routing pucks 402 throughout sorting system 100 . Conveyors and conveying techniques are used to rout pucks 402 from the load cell to the sorting buffer cell or to the manual quality control station and back to the load cell, from the sorting buffer cell to the incomplete case storage cell and/or the puck sequencing cells, and from the puck sequencing cells to the packaging cell or to the manual quality control station and back to the load cell.
[0083] In one operational embodiment, routing of pucks 402 is done using a plurality of multiple conveyors and part conveying techniques, with merge and divert units. In one example, with no intention to limit the invention, a first conveyor routs pucks from load cell 104 to sorting buffer cell 106 or exceptions handling cell 108 and back to load cell 104 . The first conveyor includes merge and divert units to allow “no read” pucks to go to the manual quality control station. A second conveyor routs pucks 402 from sorting buffer cell 106 to incomplete case storage cell 112 and/or puck sequencing cell 114 . The second conveyor includes a plurality of merge and divert units. A first divert unit allows a puck 402 to go to one of two puck sequencing cells and a second divert unit allows pucks 402 to go to incomplete case storage cell 112 . A third conveyor routs pucks 402 from puck sequencing cell 114 to packaging ceil 116 or to exceptions handling cell 108 and back to load cell 104 . A third conveyor may include two merge units and one divert unit. The divert unit allows pucks 402 to go to either the load cell 104 or a second manual quality control station. The conveyors may ran at any appropriate speed, for example, at a speed of 60 feet per minute allowing for a puck throughput rate of at least 60 parts per minute on each conveyor. Conveyors and conveying techniques are well known and are available from, for example, FlexLink Systems, Inc. of Allentown, Pa.
[0084] While the present invention has been shown and described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
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A system and associated method is provided for sorting parts, which includes a conveyor system for receiving and circulating a plurality of randomly presented parts, a sorting buffer for accumulating selected parts from the plurality of randomly presented parts in an assigned buffer location, and a sequencing system for sequencing the accumulated selected parts.
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BACKGROUND OF THE INVENTION
The present invention relates generally to operations performed in conjunction with a subterranean well and, in an embodiment described herein, more particularly provides a valve used to control actuation of a tool positioned within the well and associated methods.
It is well known in the art to actuate a tool positioned within a subterranean well in response to hydrostatic pressure in the well. For example, U.S. Pat. No. 5,492,173 discloses a tool which includes an activation mechanism responsive to such hydrostatic pressure. The disclosure of that patent is incorporated herein by this reference.
The activation mechanism causes power to be supplied to a control circuit when the hydrostatic pressure reaches a predetermined amount. Thereafter, as the tool is lowered in the well, a timer determines when the power will be supplied to a motor in order to set a lock or plug within the well at an appropriate location. An accelerometer may also be utilized to reset the timer as the tool is displaced in the well, so that the lock or plug is not inadvertently set before the tool has arrived at the appropriate location.
Where the accelerometer is not utilized, the timer is set before the tool enters the well. This timer setting is based on an estimate of the time required to lower the tool to the appropriate location within the well. Unfortunately, this estimate may be incorrect, perhaps due to unforeseen difficulties in lowering the tool in the well, in which case it is likely that the lock or plug will be set prior to reaching the appropriate location. For example, an obstruction may be present in the wellbore or a portion of the wellbore may be deviated from vertical sufficiently far to impede lowering of the tool therein.
Of course, it is well known to displace a tool through a deviated portion of a well by attaching the tool to tubing, such as coiled tubing, and essentially push the tool through the wellbore. However, the use of tubing for this, or another, purpose presents other problems in actuating the tool. For example, it is generally considered uneconomical to perform a trial run with the tubing in order to gain an accurate estimate of the time required to lower the tool to the appropriate location for setting the lock or plug. Therefore, the timer setting estimate may be based on conjecture alone. As another example, if it is desired to utilize the accelerometer to periodically reset the timer as the tool is being lowered in the well, the tubing will typically not accelerate or decelerate at a sufficient level required to excite the accelerometer, due to the mass of the tubing.
Additionally, calculations of hydrostatic pressure in a well are frequently inaccurate. Such inaccuracies may occur due to human error, inaccurate measurement of fluid weight, inaccurate measurement of well deviation, inaccurate measurement of true vertical depth, etc. Since it is the hydrostatic pressure which has been utilized in the past to begin operation of the timer, such inaccuracies also affect the location at which the lock or plug is set by the tool.
The above circumstances may also apply to other tools which rely on fluid pressure within a well for their actuation. For example, in some cases firing heads utilized with perforating guns, setting tools, tubing cutters, etc. utilize fluid pressure for their actuation. Other tools, which do not presently rely on fluid pressure for their actuation for one or more of the above reasons, could be actuated by fluid pressure if the above problems could be resolved satisfactorily.
From the foregoing, it can be seen that it would be quite desirable to provide a means of actuating a tool or accomplishing another objective which does not require a predetermined hydrostatic pressure for its operation, but which actuates the tool or accomplishes its objective in response to an event which may be predictably controlled from the earth's surface. It is accordingly an object of the present invention to provide such an apparatus and associated methods of using the apparatus.
SUMMARY OF THE INVENTION
In carrying out the principles of the present invention, in accordance with an embodiment thereof, a valve is provided which is responsive to a fluid pressure differential controllable from the earth's surface, utilization of which does not require precise calculation of hydrostatic pressure within a well. The valve is suitable for use in conjunction with a tool conveyed into the well by tubing attached thereto. Methods of actuating the tool are also provided.
In broad terms, a valve is provided by the present invention, which is operatively interconnectable to two pressure regions of a subterranean well. Where a tubing string is positioned in the well, the pressure regions may correspond to the interior and exterior of the tubing. The valve includes a member that has two surface areas formed thereon. Each of the surface areas is in fluid communication with a corresponding one of the pressure regions. The member displaces when fluid pressure in one of the pressure regions is greater than fluid pressure in the other pressure region by a predetermined amount. Displacement of the member causes a chamber of the valve to be placed in fluid communication with one of the pressure regions.
In another aspect of the present invention, a valve is provided which is operatively positionable within a subterranean well having a tubing string disposed therein. The valve includes a housing, first and second fluid passages, a chamber and a member displaceable relative to the housing. The housing is sealingly connectable to the tubing string, thereby placing the first fluid passage in fluid communication with the interior of the tubing string and placing the second fluid passage in fluid communication with an annulus formed between the tubing string and the wellbore. The member is displaceable, in response to a difference between fluid pressures in the first and second fluid passages, from one position in which the chamber is isolated from the second fluid passage to another position in which the chamber is in fluid communication with the second fluid passage.
In yet another aspect of the present invention, apparatus is provided which is operatively positionable within a subterranean wellbore. The apparatus includes a switch disposed within a first chamber and a piston reciprocably disposed between the first chamber and another, second, chamber. The piston is displaceable to engage the switch in response to a difference in pressure between the two chambers. A valve is interconnected to the second chamber. The valve opens to place the second chamber in fluid communication with fluid pressure within the well. Alternatively, the switch may be an explosive device, in which case the piston causes detonation of the explosive device in response to a difference in pressure between the chambers.
In still another aspect of the present invention, a method is provided for communicating pressure to a chamber, which method may be utilized to actuate a tool. A valve is interconnected with a tubing string to which the chamber is also connected. The valve is placed in fluid communication with the interior and exterior of the tubing string, and with the chamber. Fluid pressure is applied to the interior of the tubing string to create a predetermined differential pressure from the interior to the exterior of the tubing string. The valve is then opened in response to the predetermined differential pressure, thereby communicating fluid pressure to the chamber. When used to actuate the tool, a piston may be displaced in response to the fluid pressure entering the chamber, thereby causing the piston to engage a structure positioned in another chamber within the tool.
The present invention permits operations to be performed in subterranean wells with greater precision, economy and efficiency. These and other features, advantages, benefits and objects of the present invention will become apparent to one of ordinary skill in the art upon careful consideration of the detailed description of a representative embodiment of the invention hereinbelow and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 (Related Art) is schematicized view of a pressure activated tool for use in a subterranean well;
FIG. 2 is a cross-sectional view of a pressure activated switch valve embodying principles of the present invention and associated apparatus operatively interconnected with the tool of FIG. 1;
FIGS. 3A-3B are enlarged cross-sectional views of the pressure activated switch valve of FIG. 2 operatively interconnected to the tool of FIG. 1, the valve being shown in a closed configuration thereof in FIG. 3A and the valve being shown in an open configuration thereof in FIG. 3B; and
FIG. 4 is an enlarged cross-sectional view of the valve of FIG. 2 operatively interconnected to a perforating gun firing head.
DETAILED DESCRIPTION
Representatively and schematically illustrated in FIG. 1 is a tool 10 similar to that described in the incorporated U.S. Pat. No. 5,492,173. Specifically, FIG. 1 shows various devices used to control activation of a motor 12 within the tool 10. In general, the devices are interposed between a power source 14 and the motor 12, in order to control when the motor will be activated in the tool described in the incorporated patent, activation of the motor 12 is utilized to set a plug or lock (not shown) at a particular desired location within a subterranean well.
A piston 16 is axially reciprocably and sealingly disposed within a cylinder 18 of the tool 10. An upper volume 20 within the cylinder 18 above the piston 16 is exposed to hydrostatic pressure within the well. Thus, as the tool 10 is lowered into the well, fluid pressure in the upper volume 20 gradually increases.
A lower volume 22 within the cylinder 18 below the piston 16 contains atmospheric pressure. A compression spring 24 is disposed within the lower volume 22 and exerts an upwardly biasing force on the piston 16. Therefore, the hydrostatic pressure in the upper volume 20 must exceed a combination of atmospheric pressure and the biasing force of the spring 24 in order to downwardly displace the piston 16 relative to the cylinder 18.
Operatively interconnected to the piston 16, and also disposed within atmospheric pressure, is a switch 26. The position of the switch 26 (i.e., whether open or closed) determines whether power is supplied from the power source 14 to a control circuit 28. The switch 26 is closed when the piston 16 displaces downwardly relative to the cylinder 18, and the switch is opened when the piston 16 is displaced upwardly relative to the cylinder by the spring 24. It will be readily appreciated by one of ordinary skill in the art that a predetermined hydrostatic pressure must be present in the volume 20 for the switch 26 to be closed, and for power to be supplied to the control circuit 28.
The control circuit 28 includes a timer 30 and an accelerometer 32. The timer 30 is of the type which counts down from a set time period, at which time the timer conducts and supplies power to the motor 12. The time period may be set based upon an estimate, for example, of the time required to properly position the tool 10 within the well. This time period must be set before the tool 10 enters the well.
As an alternative to setting the time period based on an estimate of the time required to position the tool 10 within the well, the accelerometer 32 may be utilized to periodically reset the timer 30 whenever the tool accelerates or decelerates (e.g., as the tool is being lowered in the well). In that case, the time period for which the timer 30 is set corresponds to the amount of time after the tool 10 has stopped (no longer accelerates or decelerates), at which it is desired to set the plug or lock in the well. If run on wireline or slickline, the tool 10 may be conveniently stopped periodically during its descent into the well by merely applying a brake on the wireline or slickline reel, to thereby ensure that the accelerometer 32 resets the timer 30, so that the plug or lock is not set prematurely. However, when run on coiled tubing, or another type of tubing string, the mass of the tubing may prevent sufficient acceleration or deceleration needed to reset the timer 30, and the tubing may not be so easily or conveniently stopped periodically.
Note that the upper volume 20 is open to a wellbore 34 of the well surrounding the cylinder 18. This wellbore 34 is the source of the hydrostatic pressure used to displace the piston 16. When run on wireline or slickline, the wellbore 34 is also the only pressure region available for displacing the piston 16. The fluid pressure in the wellbore 34 may be altered at the earth's surface by, for example, pumping into the wellbore to increase the pressure therein, but it will be readily appreciated that any such added pressure is cumulative to the hydrostatic pressure, and so any inaccuracies in calculating the hydrostatic pressure are not removed or changed by adding pressure thereto. Thus, even though fluid pressure in the wellbore 34 may be altered from the earth's surface, it cannot be more accurately controlled than the hydrostatic pressure.
Referring additionally now to FIG. 2, apparatus 40 is representatively illustrated which embodies principles of the present invention. In the following description of the apparatus 40 and other apparatus and methods described herein, directional terms, such as "above", "below", "upper", "lower", etc., are used for convenience in referring to the accompanying drawings. Additionally, it is to be understood that the various embodiments of the present invention described herein may be utilized in various orientations, such as inclined, inverted, horizontal, vertical, etc., without departing from the principles of the present invention.
The apparatus 40 is conveyed into a wellbore 42 by tubing, such as coiled tubing 44, extending to the earth's surface. However, it is to be clearly understood that other forms of conveyance may be utilized without departing from the principles of the present invention. It will be readily appreciated that, by using a tubing string 44 to convey the apparatus 40, two pressure regions are available for use in operating the apparatus, namely, the interior 46 of the tubing 44, and the annulus 48 radially between the apparatus and the wellbore 42.
The apparatus 40 is sealingly attached to the tubing 44, such that the tubing interior 46 is in fluid communication with an internal fluid passage 50 extending axially within the apparatus. As shown in FIG. 2, initially the fluid passage 50 is pressure equalized with the annulus 48. This pressure equalization is provided by a pair of orifices 52 formed radially through a shuttle 54 of a conventional circulating valve 56. It is to be understood that it is not necessary to provide the circulating valve 56 for use with the apparatus 40, but that the applicant prefers its use, since it permits the tubing 44 to fill with fluid as it is lowered into the well. Other devices, such as a conventional flow diverter valve, etc., may be used in place of the circulating valve 56 without departing from the principles of the present invention. A suitable circulating valve is Halliburton part no. 698.10150, and a suitable flow diverter valve is Halliburton part no. 698.19035, both of which are manufactured by, and available from, Halliburton Company of Duncan, Okla.
To close the valve 56 and thereby provide fluid isolation between the interior 46 of the tubing 44 and the annulus 48, fluid is pumped from the earth's surface, through the interior of the tubing, outward through the orifices 52 and into the annulus 48. As the fluid passes through the orifices 52, the fluid experiences a pressure drop, and so the fluid pressure in the interior 46 becomes greater than the pressure in the annulus 48. A greater rate of fluid flow produces a correspondingly greater pressure differential.
When the pressure differential is sufficiently great to overcome the upwardly biasing force of a compression spring 58 within the valve 56, the shuttle 54 displaces axially downward and closes off the orifices 52. At this point, a pressure increase will be observed at the earth's surface and no further pressure differential need be applied. Only a minimum amount of pressure differential need be maintained to keep the orifices 52 closed, for example, approximately 100 psid.
A valve 60 is sealingly attached to the circulating valve 56 and is in fluid communication with the fluid passage 50. Attached below the valve 60 is a tool 62, which is similar in many respects to the tool 10 previously described. Specifically, in one respect, the tool 62 includes a piston 64 which may be displaced to engage a structure within the tool, in order to activate the tool. The valve 60 is utilized to control fluid communication with a chamber 66 to which the piston 64 is exposed, in order to control activation of the tool 62.
The valve 60 is in fluid communication with the interior 46 of the tubing 44, and with the annulus 48. In an important aspect of the present invention, the valve 60 opens to permit fluid communication with the chamber 66 when a predetermined pressure differential exists between the interior 46 and the annulus 48. It will be readily appreciated that this pressure differential is easily and accurately controllable from the earth's surface at any time. It will also be readily appreciated that this method of activating the tool 62 does not require reliance on any estimates of time, or on movements of the tool and its means of conveyance. Additionally, this method permits an operator to remove the tool 62 from the well without any danger that it will be activated as it is being retrieved.
Referring additionally now to FIG. 3A, the apparatus 40 is representatively illustrated separated from the circulating valve 56 and tubing 44 for illustrative clarity. FIG. 3A is also somewhat enlarged as compared to FIG. 2, so that details of the valve 60 and tool 62 may be more clearly shown and described.
The piston 64 is axially upwardly biased by a compression spring 68. An axially spaced apart set of circumferential seals 70, 72 are carried externally on the piston 64. The lower seal 72 is sealingly received in a central axial seal bore 74 formed in a top sub 76 of the tool 62. The seal 72 isolates the chamber 66 from an atmospheric chamber 78 within the tool 62.
It will be readily appreciated that if fluid pressure in the upper chamber 66 is sufficiently greater than fluid pressure in the lower chamber 78 to overcome the biasing force of the spring 68, the piston 64 will be downwardly displaced relative to the top sub 76. Initially, in the configuration shown in FIG. 3A, both of the chambers 66, 78 are at atmospheric pressure, and the piston 64 is upwardly biased by the spring 68 into contact with a sleeve 80 of the valve 60. When, however, the valve 60 is opened, the upper chamber 66 will be placed in fluid communication with the annulus 48, thereby causing axially downward displacement of the piston 64, provided sufficient fluid pressure exists in the annulus to compress the spring 68.
Attached to the piston 64, and extending downwardly therefrom, is a generally tubular spring retainer 82. The spring retainer 82 radially outwardly surrounds a compression spring 84, which exerts an axially downwardly biasing force on a generally rod shaped plunger 86. An external shoulder formed on the plunger 86 engages an internal shoulder formed on the spring retainer 82 to prevent removal of the plunger from within the spring retainer.
When the piston 64 is axially downwardly displaced, the spring retainer 82, spring 84 and plunger 86 are displaced therewith. Eventually, the plunger 86 will contact a structure, such as a switch 88, disposed within the tool 62. It may now be appreciated that the spring 84 lessens the impact of the plunger 86 on the switch 88 and, when maintained in contact therewith, exerts an approximately constant biasing force thereon. However, it is to be clearly understood that it is not necessary for the spring retainer 82, spring 84 and plunger 86 to be provided in the tool 62 according to the principles of the present invention, since, depending upon the structure to be engaged, it may be desirable to extend the piston 64 downwardly and have the piston engage the structure directly. It is also to be understood that the structure may be other than the switch 88 without departing from the principles of the present invention.
At this point it may be seen that the tool 10 shown in FIG. 1 and generally described above may be used for the tool 62 shown in FIG. 3A. In that case, the piston 64 may correspond to the piston 16, the spring 68 may correspond to the spring 24, the chamber 66 may correspond to the chamber 20, the chamber 78 may correspond to the chamber 22, the switch 88 may correspond to the switch 26, etc. Thus, when the valve 60 is opened, the piston 64 may engage the switch 88 (via the plunger 86) to close it and supply power to the control circuit 28. Alternatively, since opening of the valve 60 may be accurately controlled from the earth's surface, as will be described more fully hereinbelow, the switch 88 may be interconnected directly between the power source 14 and the motor 12, so that the motor is powered immediately upon opening of the valve.
The valve 60 is maintained in its closed configuration as shown in FIG. 3A by a shear pin 90 installed radially through a sidewall portion of the sleeve 80 and a member 92 axially reciprocably and sealingly disposed within the sleeve. In its upwardly disposed position relative to the sleeve 80, as shown in FIG. 3A, the member 92 prevents fluid communication between the annulus 48 and the chamber 66, and the valve 60 is closed. However, when the member 92 is displaced to its downwardly disposed position relative to the sleeve 80 (see FIG. 3B), such fluid communication is permitted, and the valve 60 is open.
The member 92 carries three axially spaced apart circumferential seals 94, 96, 98 externally thereon. The upper seal 94 is sealingly received in an upper bore 100 formed internally on the sleeve 80. The lower seals 96, 98 are sealingly received in a lower bore 102 formed internally on the sleeve 80, with the seals axially straddling a fluid passage 104 formed radially through the sleeve.
The fluid passage 104 is in fluid communication with the chamber 66 via an opening 106 formed through the sleeve 80 below the bore 102. However, the fluid passage 104 is isolated from fluid communication with the annulus 48 by the seals 96, 98, and by a circumferential seal 108 carried externally on the sleeve 80. The seal 108 sealingly engages a bore 110 formed internally on a generally tubular housing 112 radially outwardly surrounding the sleeve 80. The housing 112 is configured for sealing attachment to the tubing 44 or circulating valve 56.
The seal 108 and another circumferential seal 114 carried externally on the sleeve 80 axially straddle a fluid passage 116 formed radially through the housing 112. The fluid passage 116 is in fluid communication with one or more circumferentially spaced apart fluid passages 118 (only one of which is visible in FIG. 3A) formed radially through the sleeve 80, a series of circumferentially spaced apart fluid passages 120 formed radially through the member 92, an axially extending fluid passage 122 formed in the member and axially spaced apart fluid passages 124, 126 formed radially through the member.
It will be readily appreciated by one of ordinary skill in the art that if the fluid pressure in the fluid passage 50 is equal to the fluid pressure in the annulus 48, the member 92 is balanced, that is, the member is not biased axially upward or downward thereby. This is due to the fact that an upper surface area of the member 92 exposed to fluid pressure in the fluid passage 50 is equal to a lower surface area of the member exposed to fluid pressure in the annulus 48. These surface areas correspond to the area of the bore 100 sealingly engaged by the seal 94. If, however, additional fluid pressure is applied to the fluid passage 50, such as by circulating fluid from the earth's surface, through the tubing 44 and radially outward through the orifices 52, the member 92 will be downwardly biased by the difference between the fluid pressure in the fluid passage 50 and the fluid pressure in the annulus 48.
If sufficient additional fluid pressure is applied to the fluid passage 50, for example, by closing the circulating valve 56 as described above and continuing to apply fluid pressure to the interior 46 of the tubing 44, the downwardly biasing force on the member 92 produced by the differential pressure between the fluid passage 50 and the annulus 48 will eventually shear the shear pin 90 and permit the member to downwardly displace relative to the sleeve 80. Thus, by appropriately sizing the shear pin 90, or by installing an appropriate number of the shear pins when assembling the valve 60, the operator may select the differential pressure at which the shear pin 90 shears. The applicant prefers that the shear pin 90 shear when the fluid pressure in the fluid passage 50 exceeds the fluid pressure in the annulus 48 by approximately 600 psi, but it is to be understood that any predetermined differential pressure may be used without departing from the principles of the present invention.
Note that an upper end 128 of the member 92 extends axially outward from the sleeve 80. The end 128 is exposed to, and extends somewhat into, the fluid passage 50. As will be more fully described hereinbelow, a weighted bar or other object may be dropped through the interior 46 of the tubing 44 from the earth's surface to impact the end 128 and shear the shear pin 90, as an alternate method of downwardly displacing the member 92 and opening the valve 60. It is, thus, a distinct advantage of the apparatus 40 that it may activated using no less than two independent methods, each of which is predictably, controllably and conveniently performed from the earth's surface.
Referring additionally now to FIG. 3B, the apparatus 40 is representatively illustrated with the valve 60 open and the tool 62 activated thereby. The member 92 is in its downwardly disposed position relative to the sleeve 80, so that the seals 96, 98 no longer axially straddle the fluid passage 104. Consequently, the fluid passage 104 is now in fluid communication with the annulus 48 via the fluid passages 126, 122, 124, 118 and 116.
Fluid pressure in the annulus 48 has entered the chamber 66 and caused axially downward displacement of the piston 64. The upper seal 70 now sealingly engages an inclined shoulder 130 internally formed on the top sub 76, preventing further downward displacement of the piston 64. The plunger 86 has downwardly displaced with the piston 64 and has engaged the switch 88.
The shear pin 90 is sheared, a predetermined differential pressure between the fluid passage 50 and the annulus 48 having been achieved. Alternatively, the shear pin 90 may have been sheared by applying sufficient force to the end 128 of the member 92 by, for example, impacting it with a weighted object.
It is to be clearly understood that fluid pressures within the well, other than that in the annulus 48, may be placed in fluid communication with the chamber 66 without departing from the principles of the present invention. For example, the fluid passage 10, may be appropriately positioned so that fluid communication with the fluid passage 50 is permitted when the member 92 is displaced to open the valve 60. In that manner, the tool 62 may be activated with fluid pressure in the interior 46 of the tubing 44, instead of fluid pressure in the annulus 48. Additionally, alternative differential pressures may be utilized to open the valve 60. For example, fluid pressure in the annulus 48 greater than fluid pressure in the fluid passage 50 may be utilized to open the valve 60 by appropriate reconfiguration of the various seals and fluid passages therein.
Referring additionally now to FIG. 4, an alternate construction of the apparatus 40 is representatively illustrated. As shown in FIG. 4, the tool 62 includes an explosive device, such as an initiator 132 and detonating cord 134, in the atmospheric chamber 78. The initiator 132 and detonating cord 134 may be of the type commonly used in firing heads for perforating guns, tubing cutters, setting tools, etc. Thus, the tool 62 as shown in FIG. 4 may be a firing head or other tool in which it is desired to activate or detonate an explosive device. It will, therefore, be readily appreciated that the apparatus 40, and the valve 60 apart therefrom, may be used for a variety of applications, other than those specifically described herein, without departing from the principles of the present invention.
Note that the plunger 86 has a generally conical shaped end 136 for engagement with the initiator 132, the plunger operating as a firing pin as shown in FIG. 4. Since it is at times preferable for a firing pin to engage an explosive device with maximum impact to ensure detonation thereof, the tool 62 may be provided without the spring retainer 82, spring 84 and plunger 86, the end 136 instead being formed on a downwardly extending portion of the piston 64. In that manner, the piston 64 would impact the initiator 132 directly.
The valve 60, as shown in FIG. 4, has been downwardly displaced relative to the housing 112 by a weighted bar 138. The bar 138 has been dropped from the earth's surface, through the interior 46 of the tubing 44, into the fluid passage 50 and into contact with the upper end 128 of the member 92. This contact (or impact) has sheared the shear pin 90 and permitted the member 92 to displace downwardly. Thus, it is not necessary to achieve a differential pressure between the two pressure regions, the fluid passage 50 and the annulus 48, for operation of the valve 60 according to the principles of the present invention.
Of course, modifications, additions, substitutions, deletions and other changes may be made to the valve 60, the overall apparatus 40 and the methods described herein. Some of these possible changes have been described above and many others would be obvious to a person of ordinary skill in the art. These changes are contemplated by the principles of the present invention, even though only a few specific embodiments of the present invention have been described. Accordingly, the foregoing detailed description is to be clearly understood as being given by way of illustration and example only, the spirit and scope of the present invention being limited solely by the appended claims.
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A pressure activated valve and associated methods of using same provide increased functionality and convenience in actuating a tool operatively positioned within a subterranean well. In a described embodiment, a switch valve is utilized to control actuation of a downhole power unit. The switch valve is configured to cause actuation of a switch within the downhole power unit in response to a differential fluid pressure. The differential fluid pressure is created by applying pressure to the interior of a tubing string to which the valve is attached.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 12/986,908, filed Jan. 7, 2011. The contents of said application are hereby incorporated in their entirety by reference.
FIELD OF THE INVENTION
[0002] This invention relates to a ceiling fan having a single fan blade having an integral central portion which functions as a motor housing.
BACKGROUND OF THE INVENTION
[0003] Ceiling fans typically include a motor having a rotating flange which rotates about an axis that is collinear with a downrod by which the fan is attached to the ceiling. The fan motor is typically encased in a motor housing which wraps about the motor while leaving partial access to the rotating flange. Such partial access to the rotating flange is required so that the fan blades may be attached to the rotating flange. The requirement of a partial access often leads to an increase in the heat, vibration and noise into the surrounding environment. Furthermore, a partial access may subject the internal components to premature failure in environments that are high in salinity, humidity, or dust (e.g., due to rusting, corrosion, or seizing). Commercially available ceiling fans include numerous examples in which the fan blades are attached to the rotating flange by use of blade irons. Other known ceiling fans use means for attaching the fan blades directly to the rotating flange without the use of blade irons.
[0004] In both types of known ceiling fans, the motor, including the motor housing, is first suspended from the ceiling. The ceiling fan installer may then attach the blade irons, either separately or in a blade iron and blade combination. Alternatively, the ceiling fan installer may attach the fan blades directly to the rotating flange. In any event, the ceiling fan installer must work in an uncomfortable position, generally screwing fasteners into the rotating flange from underneath the ceiling fan motor to install multiple numbers of ceiling fan blade irons and/or blade combinations.
[0005] Further, both types of known ceiling fans require multiples of fan blade irons and blade combinations. This often leads to fasteners such as screws wearing out or corroding over time, thus potentially causing a safety hazard as a fan blade can become detached from the rest of the ceiling fan during use. This is also true for other mechanisms or devices other than screws used to secure fan blades to the ceiling fan. For example, U.S. Pat. No. 6,149,388 discloses the use of a collar having recessed sectors and protrusions to prevent disengagement from the ceiling fan Like other fan blade irons, the collar system is also subject to wearing out and corrosion over time.
[0006] The requirement for multiples of fan blade irons and blade combinations also leads to an imbalance of the entire ceiling fan during operation, and the ceiling fan must often be adjusted by the use of fan blade weights of various measures. This can be a time-consuming process for the ceiling fan installer to properly correct the imbalance. U.S. Pat. No. 6,364,612 discloses the use of springs fitted onto the vanes (e.g., fan blade irons) to absorb the swinging force of the ceiling fan to correct the imbalance. However, use over a period of time will eventually cause such springs to wear out and result in the ceiling fan operating in an imbalanced state.
[0007] In addition, the use of motor housings to conceal the fan motor results in a need to mold or otherwise manufacture an additional item(s) and in additional assembly time for the manufacturer and/or ceiling fan installer. Use of additional items can increase materials having differing weights and densities. These differences can result in an unbalanced or imbalanced ceiling fan during operation as described above, thus necessitating the use of fan blade weights. These needs may result in additional expenditure of resources such as time, materials, and cost.
SUMMARY OF THE INVENTION
[0008] A first aspect of the invention provides a ceiling fan comprising a motor having a rotating flange; a single integrally formed fan blade comprising two substantially equally weighted wing portions disposed opposite each other and a center portion disposed between and integrally formed with the two wing portions and having passageway therethrough, wherein the passageway is sized such that the fan motor fits at least partially within the passageway; and means for attaching the center portion of the fan blade to the rotating flange of the motor. In some embodiments, the wing portions present substantially equal air movement and balanced rotation.
[0009] In one specific embodiment, the ceiling fan further comprises a light kit disposed below the passageway. In some embodiments, the ceiling fan further includes a cap disposed above the passageway.
[0010] In certain embodiments, the wing portions of the fan blade each exhibit a twist.
[0011] In some embodiments of the invention, the means for attaching the center portion of the fan blade to the rotating flange of the motor comprises a plurality of fastener openings and a plurality of alignment indentations on the rotating flange; a ring comprising a plurality of fastener openings and a plurality of alignment posts, wherein the fastener openings of the ring align with the fastener openings of the rotating flange and the alignment posts of the ring mate with the alignment indentations of the rotating flange wherein the ring further comprises means to attach the center portion of the fan blade with the ring.
[0012] In some embodiments of the invention, the center portion of the fan blade further comprises a plurality of extensions extending radially inwardly wherein each extension includes a fastener opening.
[0013] Yet another aspect of the invention provides a ceiling fan comprising a motor having a rotating flange; a single integrally formed fan blade comprising two substantially equally weighted wing portions disposed opposite each other and a center portion disposed between and integrally formed with the two wing portions and having a passageway therethrough, wherein the passageway is sized such that the fan motor fits at least partially within the passageway; and means for attaching the center portion of the fan blade to the rotating flange of the motor.
[0014] Yet another aspect of the invention provides a ceiling fan comprising a motor having a rotating flange; a single integrally formed fan blade comprising two substantially equally weighted wing portions disposed opposite each other and a center portion disposed between and integrally formed with the two wing portions and having a passageway therethrough, wherein the passageway is sized such that the fan motor fits at least partially within the passageway; means for attaching the center portion of the fan blade to the rotating flange of the motor; and a light kit.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a perspective view of a first embodiment of a single-blade ceiling fan of the invention.
[0016] FIG. 2 is a perspective view of a first embodiment of a fan motor useful in the invention.
[0017] FIG. 3 is a perspective view of the fan motor of FIG. 2 in combination with an attachment ring.
[0018] FIG. 4 is an elevated perspective view of a first embodiment of a single integrated ceiling fan blade useful in the invention.
[0019] FIG. 5 is an elevated perspective view of the central portion of the fan blade shown in FIG. 4 .
[0020] FIG. 6 is an elevated perspective view of the central portion of the fan blade of FIG. 4 attached to the fan motor and attachment ring combination shown in FIG. 3 .
[0021] FIG. 7 is an elevated perspective view of an embodiment of an attachment ring useful in the invention.
[0022] FIG. 8 is a perspective view of a portion of the bottom side of the attachment ring shown in FIG. 7 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] FIG. 1 illustrates a first embodiment of the inventive ceiling fan 1 . The embodiment illustrated in FIG. 1 includes a single integrally formed fan blade 10 . The single integrally formed fan blade 10 includes two opposing wing portions 12 a and 12 b and a center portion 14 . Center portion 14 partially encloses the fan motor (not shown in FIG. 1 ). A light kit 16 is attached to the ceiling fan and is located below the center portion 14 . In alternative embodiments, a cover plate (not shown) may be used in lieu of a light kit. A downrod 18 suspends the ceiling fan 1 from the ceiling. Any of a number of known ceiling connectors may be used to suspend the downrod 18 from a ceiling junction box or electrical connection point. The downrod defines an axis of rotation about which the fan motor rotates. Wing portions 12 a and 12 b extend radially outward from the axis of rotation. In the embodiment shown in FIG. 1 , the wing portions 12 a and 12 b exhibit a twist, or change in blade angle of attack, along the length of the wing portions 12 a and 12 b. The twist shown in FIG. 1 , however, is illustrative and not limiting of the invention. Alternative twists, sizes, and shapes of wing portions 12 a and 12 b are contemplated in this invention, provided that wing portions 12 a and 12 b are substantially equally weighted and configured to present substantially balanced air movement and rotation. For example, in one alternative embodiment, wing portions 12 a and 12 b may be flat, exhibiting no twist. Referring still to FIG. 1 , placed above center portion 14 is a cap 20 .
[0024] FIG. 4 illustrates fan blade 10 . As seen in FIG. 4 , the center portion 14 of fan blade 10 includes a top layer 14 a and a bottom layer 14 b. Layer 14 a extends upwardly from the top surface of fan blade 10 and layer 14 b extends downwardly from the bottom of fan blade 10 . Center portion 14 further includes an open passageway 22 , the height of which is defined by the distance between layers 14 a and 14 b. Passageway 22 is formed by a circular opening in layer 14 a which lies apart from and over a circular opening in layer 14 b. In preferred embodiments, the height of passageway 22 is sufficient to substantially enclose a fan motor. FIG. 5 illustrates the center portion 14 of fan blade 10 . Extending radially inward to passageway 22 from layer 14 a are projections 24 . Projections 24 include fastener openings 26 . As shown in FIG. 6 , screws 28 (or other appropriate fasteners) may be passed through fastener openings 26 to attach fan blade 10 onto a fan motor 30 or attachment ring 32 which is, in turn, attached to fan motor 30 . In some embodiments of the inventive ceiling fan, the entire fan blade 10 is made of a top and a bottom surface joined along all edges except at the interior edges of passageway 22 . In other embodiments, wing portions 12 a and 12 b may be formed from a single ply or layer of material to which a second ply is bonded at the center portion 14 permitting the formation of passageway 22 .
[0025] FIG. 7 illustrate an attachment ring 32 which may be used in certain embodiments of the invention. FIG. 7 is an elevated perspective view showing the top surface of the ring having a number of spaced holes 34 of varying size and configuration. FIG. 2 illustrates a fan motor 30 having a rotating flange 36 which also includes a plurality of fastener openings 38 configured to receive screws or other appropriate fasteners. Rotating flange 36 further includes guide indentations 40 configured to receive guide posts (not shown in FIG. 2 .) FIG. 8 illustrates a portion of a bottom side of ring 32 . The bottom side of ring 32 includes guide posts 42 configured to interconnect with guide indentations 40 on rotating flange 36 . FIG. 3 illustrates a fan motor 30 having a rotating flange 36 onto which ring 32 has been attached.
[0026] Referring again to FIG. 6 , a fan motor 10 having a rotating flange (not visible in FIG. 6 ) onto which ring 32 has been attached is shown. Further shown in FIG. 6 is the attachment of fan blade 10 onto ring 32 (and thereby the rotating flange) by threading a screw 28 through each fastener opening 26 into an appropriate opening in ring 32 . In alternative embodiments, fan blade 10 may be attached directly to rotating flange 36 without the use of a ring. Although screws 28 are illustrated as attaching fan blade 10 to ring 32 , it will be understood that other means for such attachment may be used. For example, center portion 14 could include downwardly projecting, contractable clips that would interlock with interlocking receiving members on the rotating flange or ring. In yet other embodiments, the means for attaching the center portion 14 of fan blade 10 onto the rotating flange, either directly or by attachment to a ring, may include hook and loop fasteners, adhesives, such as epoxy, rivets, cotter pins, and magnets. Once attached, fan blade 10 will rotate with the rotation of rotating flange 26 .
[0027] In the embodiment shown in FIG. 6 , a cap may be placed over the passageway 22 . An example of a cap 44 having a conelike shape is shown in FIG. 9 . In alternative embodiments, cap 44 may have other shapes, such as a hemispheroid, ovoid, or polyhedral.
[0028] The illustrated embodiments show the fan blade attachment means attaching to an upper surface of the rotating flange. However, in alternative embodiments, the fan blade attachment means may attach to a bottom and/or side surface of the rotating flange.
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A ceiling fan including a motor having a rotating flange; a single integrally formed fan blade, wherein the fan blade includes two substantially equally weighted wing portions disposed opposite each other; and a center portion disposed between and integrally formed with the two wing portions and having a passageway therethrough, wherein the passageway is sized such that the fan motor fits at least partially within the passageway; and means for attaching the center portion of the fan blade to the rotating flange of the motor is provided.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Patent Application Ser. No. 61/435,737 entitled “HIGH SWIRL AIR CAP,” filed on Jan. 24, 2011, which is herein incorporated by reference in its entirety for all purposes.
BACKGROUND
This section is intended to introduce the reader to various aspects of art that may be related to various aspects of the present system and techniques, which are described and/or claimed below. This discussion is believed to be helpful in providing the reader with background information to facilitate a better understanding of the various aspects of the present disclosure. Accordingly, it should be understood that these statements are to be read in this light, and not as admissions of prior art.
The invention relates generally to spray systems and, more particularly, to industrial spray coating systems for applying coatings of paint, stain, and the like. Spray coating devices are used to apply a spray coating to a wide variety of product types and materials, such as wood and metal. The spray coating fluids used for each different industrial application may have much different fluid characteristics and desired coating properties. For example, wood coating fluids (e.g., stains) are generally viscous fluids, which may have significant particulate/ligaments throughout the fluid. Existing spray coating devices, such as air atomizing spray guns, are often unable to breakup such particulate/ligaments to produce a desired coating. That is, the spray coatings that result from insufficient atomization usually have an undesirably inconsistent appearance, which may be characterized by mottling and various other inconsistencies in textures, colors, and overall appearance.
BRIEF DESCRIPTION
The present embodiments may provide improved atomization in spray devices to reduce the incidence of such undesirable particulates and/or ligaments. For example, in one embodiment, a system is provided that includes a spray coating device. The spray coating device has a liquid passage extending to a liquid outlet configured to output a liquid flow, and an air passage extending to a plurality of air outlets configured to output an air flow. The plurality of air outlets is angled to swirl the air flow.
In another embodiment, a system is provided with a spray head component having a plurality of air outlets. The plurality of air outlets has a plurality of air flow axes, wherein the plurality of air outlets is configured to output an air flow along the plurality of air flow axes. The plurality of air outlets is arranged at least partially around a liquid flow axis, and the plurality of air outlets is angled inwardly toward the liquid flow axis without intersecting the liquid flow axis.
In a further embodiment, a system is provided with a spray head component having a central surface with a central opening configured to allow output of a liquid flow along a liquid flow axis. The spray head component also includes a plurality of air atomization outlets disposed about the central opening along the central surface, and a first air horn protruding from the central surface at a first offset distance from the central opening. The first air horn has a first inner surface that curves circumferentially about the liquid flow axis, and the first inner surface has at least one first air shaping outlet. The spray head component also includes a second air horn protruding from the central surface at a second offset distance from the central opening. The second air horn includes a second inner surface that curves circumferentially about the liquid flow axis, and the second inner surface has at least one second air shaping outlet.
DRAWINGS
These and other features, aspects, and advantages of the present invention will become better understood when the following detailed description is read with reference to the accompanying drawings in which like characters represent like parts throughout the drawings, wherein:
FIG. 1 is a plan view of an embodiment of a spray coating device having a spray head component configured to create air swirl for fluid atomization;
FIG. 2 is a cross-sectional side view of the spray coating device of FIG. 1 illustrating various features for creating and shaping a spray coating;
FIG. 3 is a partial cross-sectional side view of an embodiment of the spray head component of FIGS. 1 and 2 taken within line 3 - 3 ;
FIG. 4 is an exploded perspective view of an embodiment of the spray head component of FIGS. 1-3 and separately illustrating embodiments of an air cap, a nozzle, and a pintle assembly of the spray head component;
FIG. 5 is a front axial view of an embodiment of a front face of the air cap taken along line 5 - 5 of FIG. 3 , illustrating an air swirl created by a plurality of angled openings of the face;
FIG. 6 is a front axial view of the air cap taken along line 6 - 6 of FIG. 3 ;
FIG. 7 is a partial cross-sectional view of an embodiment of an air horn of the spray head component taken along line 7 - 7 of FIG. 4 ;
FIG. 8 is a partial cross-sectional view of another embodiment of an air horn of the spray head component taken along line 7 - 7 of FIG. 4 ;
FIG. 9 is a cross-sectional side view of the spray coating device of FIG. 1 illustrating an embodiment of an air cap having a removable liquid nozzle; and
FIG. 10 is an exploded perspective view of an embodiment of the spray head component of FIGS. 1 and 9 and separately illustrating embodiments of an air cap, a nozzle, and a fluid seat of the spray head component.
DETAILED DESCRIPTION
One or more specific embodiments of the present invention will be described below. In an effort to provide a concise description of these embodiments, all features of an actual implementation may not be described in the specification. It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions must be made to achieve the developers' specific goals, such as compliance with system-related and business-related constraints, which may vary from one implementation to another. Moreover, it should be appreciated that such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure.
FIG. 1 illustrates an embodiment of a spray coating device 10 that may incorporate various spray-shaping and atomization features in accordance with the presently contemplated embodiments. In the illustrated embodiment, the device 10 includes a spray head component 12 coupled to a body 14 of the spray coating device 10 . The spray head component 12 generally includes features for creating swirl in an air flow, as represented by arrows 16 . The swirled air flow 16 includes a first directional swirl 18 and a second directional swirl 20 . The first directional swirl 18 and the second directional flow 20 may be created by a plurality of angled orifices of the spray head component 12 , as will be discussed in detail below with respect to FIGS. 2-6 . The first directional swirl 18 is created to improve atomization of a liquid flow 22 that is ejected from the spray coating device 10 along a liquid flow axis 24 . The first directional swirl 18 may induce some amount of swirling of the liquid flow 22 , which may cause a conical or vortical-shaped fluid ejection that diverges from the liquid flow axis 24 . To compensate for such induced swirl, and to create a regular spray shape, the second directional swirl 20 , which rotates in an opposing relationship to the first swirl direction 18 with respect to the liquid flow axis 24 , flattens the ejected fluid into a flat spray pattern.
It should be noted that the spray head component 12 in accordance with the present embodiments is presented in the context of a combination with the spray coating device 10 to facilitate discussion, and that the discussion of the spray coating device 10 and its components is not intended to limit the scope of the present approaches to air swirling to facilitate fluid atomization and spray shaping. Indeed, the spray head component 12 is combinable with a wide variety of spray coating devices including less than or more features than those presently disclosed. Therefore, keeping the operation of the spray head component 12 in mind, the spray coating device 10 also includes features that facilitate handling and spray triggering by a user, interface with various fluid sources (e.g., paint, water, lacquer, or other liquid coating sources, air sources, and so forth), fluid pressure adjustment, and storage, to name a few.
Specifically, in the illustrated embodiment, the spray coating device 10 includes a handle 26 to facilitate use of the spray coating device 10 by a user. The handle 26 is configured to allow gripping by the user's hand, and is disposed proximate a trigger 28 to allow the user to grip and trigger the spray coating device 10 as needed. The trigger 28 is generally configured to allow the liquid flow 22 to be ejected from the device 10 and also to allow air to flow through the spray head component 12 to form the swirled air flow 16 . As an example, the trigger 28 may be coupled to one or more valves that are internal to the spray coating device 10 , as will be discussed in further detail with respect to FIG. 2 . The trigger 28 is coupled to the body 14 of the device 10 at a pivot joint 30 , which hinges the trigger 28 to allow rotational movement when the user pulls the trigger 28 towards the handle 26 and when the trigger 28 is released.
As noted above, the device 10 also includes a liquid adjustment assembly 32 for adjusting liquid flow through the device 10 and an air adjustment assembly 34 for adjusting air flow through the device 10 . The liquid adjustment assembly 32 may be coupled to the body 14 of the device 10 by a suitable connection, such as a press-fit, an interference fit, a snap fit, threads, and so on. The liquid adjustment assembly 32 , as illustrated, may include a fluid valve adjuster 36 that is configured to move a fluid needle valve 38 between positions to vary fluid flow within the body 14 of the device 10 . Similarly, the air adjustment assembly 34 may be coupled to the body 14 via press-fit, an interference fit, a snap fit, threads, and so on. The air adjustment assembly 34 also includes an air valve adjuster 40 that is configured to move an air needle between positions to vary an air flow through the body 14 of the device 10 , as will be discussed in further detail below with respect to FIG. 2 . The device 10 also includes a fluid inlet coupling 42 for receiving liquid from a liquid source, as well as an air inlet coupling 44 for receiving air (e.g., compressed air) from an air source. When not in use or between sprayings, the device 10 may be stored (e.g., hung) using hook 46 .
FIG. 2 is a cross-sectional side view of the spray coating device 10 illustrating various internal features that result in the production of the swirled air flow 16 and the liquid flow 22 that is atomized by the swirled air flow 16 . As illustrated, the spray coating device 10 includes the spray head component 12 coupled to the body 14 . The spray head component 12 includes a fluid delivery tip assembly 50 , which may be removably inserted into a receptacle 52 . For example, a plurality of different types of spray coating devices may be configured to receive and use the fluid delivery tip assembly 50 . The spray head component 12 also includes a spray formation assembly 54 coupled to the fluid delivery tip assembly 50 . The illustrated spray formation assembly 54 includes an air atomization cap 56 , which in some embodiments may be removably secured to the body 14 of the device 10 via a threaded retaining nut 58 . In other embodiments, the air atomization cap 56 may be secured to the body 14 via a snap fit, an interference fit, a press fit, bolts, clamps, and so forth.
The air atomization cap 56 includes a plurality of air outlets 60 disposed in a curved arrangement about the liquid flow axis 24 . The plurality of air outlets 60 are generally configured to atomize and/or shape the spray exiting the spray coating device 10 . The plurality of air outlets 60 includes a first plurality of air outlets 62 and a second plurality of air outlets 64 . The first plurality of air outlets 62 are configured to create the first directional swirl 18 ( FIG. 1 ) to atomize the liquid flow 22 as the device 10 is activated (e.g., triggered). Embodiments of the first plurality of air outlets 62 are discussed in further detail below. The second plurality of air outlets 64 are disposed on air horns 66 that extend away from the body 14 of the spray coating device 14 and diverge away the liquid flow axis 24 . While the illustrated embodiment depicts the device 10 as including two air horns 66 , it should be noted that the number of air horns 66 may be increased or decreased, as will be discussed in further detail with respect to FIG. 4 . In accordance with presently contemplated embodiments, the second plurality of air outlets 64 are configured to generate the second directional swirl 20 discussed above with respect to FIG. 1 . The spray formation assembly 54 also may include other atomization mechanisms to provide a desired spray pattern and droplet distribution.
The body 14 of the spray coating device 12 includes a variety of controls and supply mechanisms for the spray head component 12 . As illustrated, the body 14 includes a fluid delivery assembly 68 having a fluid passage 70 extending from the fluid inlet coupling 42 to the fluid delivery tip assembly 50 . The fluid delivery assembly 68 also includes a fluid valve assembly 72 to control fluid flow through the fluid passage 70 and to the fluid delivery tip assembly 50 . The illustrated fluid valve assembly 72 includes the fluid needle valve 38 extending movably through the body 14 between the fluid delivery tip assembly 50 and the fluid valve adjuster 36 . The fluid needle valve 38 includes a tip portion 74 that protrudes into a removable nozzle and pintle assembly 76 . As will be discussed in further detail below, the nozzle and pintle assembly 76 includes features that, in conjunction with the tip portion 74 , control the flow of liquid through the fluid tip delivery assembly 50 . The fluid valve adjuster 36 is rotatably adjustable against a spring 78 disposed between a rear section 80 of the fluid needle valve 72 and an internal portion 82 of the fluid valve adjuster 36 . The fluid needle valve 72 is also coupled to the trigger 28 , such that the fluid needle valve 72 may be moved inwardly away from the fluid delivery tip assembly 50 as the trigger 28 is rotated in a first direction 84 (e.g., counterclockwise with respect to FIG. 2 ) about the pivot joint 30 . However, any suitable inwardly or outwardly openable valve assembly may be used within the scope of the presently contemplated embodiments. The fluid valve assembly 72 also may include a variety of packing and seal assemblies, such as packing assembly 86 , disposed between the fluid needle valve 72 and the body 14 .
An air supply assembly 88 is also disposed in the body 14 to facilitate atomization at the spray formation assembly 54 . The illustrated air supply assembly 88 extends from the air inlet coupling 44 to the air atomization cap 56 via air passages 90 and 92 . The air supply assembly 88 also includes a variety of seal assemblies, air valve assemblies, and air valve adjusters to maintain and regulate the air pressure and flow through the spray coating device 12 . For example, the illustrated air supply assembly 88 includes an air valve assembly 94 coupled to the trigger 28 , such that rotation of the trigger 28 about the pivot joint 30 (e.g., in the first direction 84 ) opens the air valve assembly 94 to allow air flow from the air passage 90 to the air passage 92 . The air supply assembly 88 also includes the air valve adjustor 40 coupled to an air needle 96 , such that the needle 96 is movable via rotation of the air valve adjustor 40 to regulate the air flow to the air atomization cap 56 . As illustrated, the trigger 28 is coupled to both the fluid valve assembly 72 and the air valve assembly 88 , such that fluid and air flow in concert to the spray head component 12 as the trigger 28 is pulled toward the handle 26 of the body 14 . The air and the liquid (e.g., liquid paint or other coating) may flow through the body 14 substantially simultaneously, or one fluid may flow through the body 14 prior to the flow of the other fluid, for example using timing features incorporated into the trigger 28 . For example, in one embodiment, the fluid may begin flowing through the body 14 prior to the flow of air. Indeed, any timing configuration of the trigger 28 may be utilized in accordance with the disclosed embodiments. As discussed in detail below, once engaged (e.g., triggered), the spray coating device 12 produces an atomized spray with a desired spray pattern and droplet distribution. Again, the illustrated spray coating device 12 , as discussed herein, is provided as one embodiment of the disclosed air swirl features. Any suitable type or configuration of a spraying device may benefit from providing an atomizing and/or spray shaping air swirl in accordance with the presently contemplated embodiments.
FIG. 3 is a partial cross-sectional side view of an embodiment of the spray head component of FIGS. 1 and 2 taken within line 3 - 3 . In particular, FIG. 3 illustrates various features of the spray head component 12 that are configured to produce an atomizing and spray-shaping air swirl. As illustrated, the needle 96 of the air supply assembly 88 ( FIG. 2 ) and the fluid needle valve 38 of the fluid valve assembly 72 are both partially open, such that air and fluid passes through the spray head component 12 to generate an atomized spray. Specifically, turning first to the features of the air supply assembly 88 , the air flows through an air passage 110 about the needle 96 as indicated by arrow 112 . The air then flows through the body 14 and into a central air passage 114 that diverges to a first set of air passages 116 and a second set of air passages 118 that lead to the first plurality of air holes 62 and the second plurality of air holes 64 , respectively. The air then exits the first and second plurality of air holes 62 , 64 to generate at least a first air flow, as depicted by arrows 120 , exiting the first plurality of air holes 62 , and a second air flow, depicted by arrows 122 exiting the second plurality of air holes 64 . In accordance with certain embodiments, the first air flow 120 generates the first directional air swirl 18 and the second air flow 122 generates the second directional air swirl 20 . The first directional swirl 18 , and thus the first air flow 120 , impinges on the liquid flow 22 radially inward and toward the liquid flow axis 24 at a first angle 121 . As an example, the first angle 121 may be between about 1° and about 65° relative to the axis 24 (e.g., 1°, 5°, 10°, 25°, 45°, 50°, 55°, or 65° from the axis 24 ) with respect to the oncoming liquid flow 22 . However, as discussed below, the first plurality of air holes 62 direct the first plurality of air flows 120 at an offset form the liquid flow axis 24 to generate the first directional swirl 18 . This results in swirling and atomization of the liquid flow 22 exiting the air atomization cap 56 (i.e., external to the spray coating device 10 ) to generate an atomized coating spray 124 . Because the first plurality of air holes 62 are angled so as to not intersect the liquid flow axis 24 , the atomized coating spray 124 may not be entirely flat (i.e., may be swirled). The second directional swirl 20 , and thus the second air flow 122 , impinges on the atomized coating spray 124 at a second angle 123 with respect to the liquid flow axis 24 . It should be noted that in some embodiments, the first and second angles 121 , 123 may be the same, while in other embodiments, the first and second angles 121 , 123 may be different. For example, the second angle 123 may be between about 1° and about 85° relative to and offset from the liquid flow axis 24 (e.g., 1°, 5°, 10°, 25°, 45°, 50°, 55°, 65°, 75°, or 85° from the axis 24 ) with respect to the oncoming atomized coating spray 124 . The second air flow 122 generates a flat coating spray 126 , as noted above, by swirling the second directional air flow 20 in an opposing relationship to the first swirled air flow 18 . However, in other embodiments, the second directional air flow 20 may be oriented in the same general direction as the first swirled air flow 18 . In some embodiments, the second air flow 122 may also provide further atomization of the atomized coating spray 124 .
Turning to the fluid flow through the device 10 , the fluid delivery tip assembly 50 includes the nozzle and pintle assembly 76 , which includes a sleeve 130 (e.g., a nozzle) disposed about a central member or pintle 132 . The illustrated pintle 132 includes a central fluid passage or preliminary chamber 134 , which leads to one or more restricted passageways or supply holes 136 . These supply holes 136 can have a variety of geometries, angles, numbers, and configurations (e.g., symmetrical or non-symmetrical) to adjust the velocity, direction, and flow rate of the fluid flowing through the fluid delivery tip assembly 50 . For example, in certain embodiments, the pintle 132 may have the supply holes 136 disposed symmetrically about the liquid flow axis 24 . In operation, when the needle valve 38 is open (i.e., the tip 74 is retracted away from an inner surface 137 of the nozzle and pintle assembly 76 ), a desired fluid (e.g., paint) flows through fluid passage 70 , about the needle valve 38 of the fluid valve assembly 72 , as indicated by arrows 138 . The fluid then flows into the central fluid passage or preliminary chamber 134 of the pintle 132 . As indicated by arrow 138 , the supply holes 136 then direct the fluid flow from the preliminary chamber 134 into a secondary chamber or throat 140 , which is defined as the space between a forward tip section 142 of the pintle 132 and an inner surface 144 of the sleeve 130 . The fluid flow 22 then exits the body 14 of the device 10 via a fluid tip exit 146 (e.g., a liquid outlet) of the nozzle and pintle assembly 76 along the fluid flow axis 24 .
In some embodiments, the sleeve 130 and the pintle 132 may have a configuration that results in a geometry of the throat 140 that diverges and converges toward the fluid tip exit 146 . During operation of such embodiments, these diverging and converging flow pathways may induce fluid mixing and breakup prior to air atomization and shaping by the air flows 120 and 122 . For example, successive diverging and converging flow passages can induce velocity changes in the fluid flow, thereby inducing fluid mixing, turbulence, and breakup of particulate that may be present in the liquid. Moreover, the fluid dynamics (e.g., viscosity, particulate concentration, and so on) of a given liquid may at least partially influence the particular configuration of the nozzle and pintle assembly 76 . Accordingly, the nozzle and pintle assembly 76 in accordance with presently contemplated embodiments is swappable (i.e., removable and replaceable) with other assemblies having differing sizes, shapes, and/or extents of the holes 136 and/or throat 140 to suit a particular coating application.
FIG. 4 is an exploded perspective view of an embodiment of the spray head component of FIGS. 1-3 and separately illustrating various components of the spray head component 12 . Specifically, the air cap 56 configured to produce the air swirls, the sleeve 130 , and the pintle 132 are illustrated as separated along the liquid flow axis 24 . In accordance with presently contemplated embodiments, the air cap 56 and the nozzle and pintle assembly 76 may be removable from the body 14 of the device 10 without special tools or equipment due to their facile manipulation with widely available tools (e.g., wrenches or pliers). Alternatively, in some embodiments, the air cap 56 and/or the nozzle and pintle assembly 76 may be removed by hand. Accordingly, the illustration of FIG. 4 depicts the separation of the components of the nozzle and pintle assembly 76 from the air cap 56 that may occur during cleaning or replacement operations. The air cap 56 , which is removable in addition to the nozzle and pintle assembly 76 , includes a central opening 150 oriented coaxially with the liquid outlet 146 of the sleeve 130 . This allows the liquid flow 22 to exit the device proximate and central to the plurality of first air holes 62 to facilitate atomization. In this way, the air flow is not collinear with the liquid flow, but rather impinges the liquid flow from a plurality of discrete locations (e.g., air holes 62 and 64 ) for atomization and spray shaping. The pintle 132 is illustrated as connected to a rear portion 152 of the spray head component 12 , and has the forward tip section 142 aligned coaxially with the liquid outlet 146 of the sleeve 130 and the central opening 150 of the air cap 56 .
The pintle 132 , as noted above, includes the plurality of orifices 136 and the forward tip portion 142 that interfaces with the liquid outlet 146 of the sleeve 130 , both of which allow liquid to flow through the nozzle and pintle assembly 76 and out of the device 10 in a controlled manner. In the illustrated embodiment, the liquid outlet 146 is a circular opening, as opposed to an ellipsoidal opening (e.g., a cat-eye opening). However, the use of a cat-eye opening as the liquid outlet 146 is also contemplated herein. Additionally, the pintle 132 includes a rear section 154 having a nozzle portion 156 extending through at least a part of the body 14 of the device 10 . The nozzle portion 156 is also removable from the body 14 , for example, by pulling on the nozzle portion 156 in a direction away from the body 14 . The rear section 154 also includes a plurality of air holes 158 that direct air towards the first plurality of air holes 62 of the air cap 56 .
The sleeve 130 , as illustrated, includes a first cylindrical section 160 , a tapered section 162 , and a second cylindrical section 164 . The first cylindrical section 160 is generally configured to receive the nozzle portion 156 of the pintle 132 , for example to secure the pintle 132 within the air cap 56 and/or the body 14 of the spray coating device 10 . The first cylindrical section 160 tapers to the second cylindrical section 164 via the tapered section 162 , which generally has a frusto-conical shape to reduce the inner diameter of the sleeve 130 to form a suitable size for the throat 140 , which, as noted above, is defined as the cavity between the sleeve 130 (i.e., the second cylindrical section 164 ) and the forward tip portion 142 of the pintle 132 when the nozzle and pintle assembly 76 is assembled.
As noted above, the air cap 56 includes a plurality of air holes, specifically a first plurality of air holes 62 configured to produce the first directional air swirl 18 , and a second plurality of air holes 64 disposed on air horns 66 , the second plurality of air holes 64 being configured to produce the second directional air swirl 20 . Specifically, in the illustrated embodiment, the air cap 56 includes a first air horn 166 and a second air horn 168 protruding away from the body 14 of the device 10 and having respective second pluralities of air holes 64 . The first air horn 166 and the second air horn 168 are disposed at opposite diametrical extents of the air cap 56 and face one another. Specifically, the first air horn 166 includes a first inner surface 170 (e.g., a concave surface) that curves circumferentially about the liquid flow axis 24 of the central opening 150 , which may be considered the liquid opening of the air cap 56 . Similarly, the second air horn 168 includes a second inner surface 172 (e.g., a concave surface) that curves circumferentially about the liquid flow axis 24 of the central opening 150 . The second plurality of air outlets 64 is disposed on the curved first and second inner surfaces 170 , 172 . In accordance with certain presently contemplated embodiments, the curved geometry of the first and second inner surfaces 170 , 172 may facilitate interaction with and/or flattening of the swirling, atomized coating spray 124 . For example, the curved surfaces 170 , 172 help direct the second directional air swirl 20 radially inward towards the atomized coating spray 124 and against the first directional air swirl 18 .
The second plurality of air outlets 64 may be any size and/or shape to the extent that they are disposed on the respective inner surfaces of the air horns 66 . As will be appreciated with respect to the illustrated embodiment, the second plurality of air outlets 64 are angled relative to one another as a result of the concave shape of the surfaces on which they are disposed. However, as will be described in further detail with respect to FIG. 6 , each of the second plurality of air outlets 64 may be angled non-perpendicular relative to its respective surface and/or the liquid flow axis 24 . In other words, the air flow 122 ( FIG. 3 ) is not normal to the surface at each of the air outlets 64 . In this way, each of the second plurality of air outlets 64 is angled with respect to the direction of the atomized coating spray 124 (i.e., the liquid flow axis 24 ), as well as angled relative to their respective surfaces. As an example, the air outlets 64 may be angled by between about 1° and about 85° relative to and offset from the liquid flow axis 24 (e.g., 1°, 5°, 10°, 25°, 45°, 50°, 55°, 65°, 75°, or 85° from their respective surfaces and relative to the liquid flow axis 24 ). As such each of the second plurality of air outlets 64 may be considered as having a compound angular geometry.
In a similar manner to the second plurality of air outlets 64 , the first plurality of air outlets 62 each have a compound angular geometry, and are disposed on a central surface 174 of the air cap 56 . That is, each of the first plurality of air outlets 62 are angled relative to their respective surfaces as well as angled relative to the liquid flow axis 24 . As an example, the air outlets 64 may be angled by between about 1° and about 85° relative to and offset from the liquid flow axis 24 (e.g., 1°, 5°, 10°, 25°, 45°, 50°, 55°, 65°, 75°, or 85° from their respective surfaces and relative to the liquid flow axis 24 ). The compound angular geometry of the first plurality of air outlets 62 , in accordance with present embodiments, creates a swirling action of atomizing air, which facilitates particulate breakup as well as homogenization of the liquid flow 22 exiting the device 10 . FIG. 5 is a front axial view of an embodiment of the front surface 174 of the air cap 56 taken along line 5 - 5 of FIG. 3 .
In the illustrated embodiment, the first plurality of air outlets 62 has a plurality of air flow axes, represented generally as arrows 180 . The first plurality of air outlets 62 , as noted above, are each configured to output an air flow along their respective air flow axes 180 . In the illustrated embodiment, the first plurality of air outlets 62 is arranged symmetrically and circumferentially about the liquid flow axis 24 such that the first plurality of air outlets 62 completely surround the central opening 150 of the air cap 56 . In other embodiments, the first plurality of air outlets 62 may be arranged partially about the liquid flow axis 24 . In other words, the first plurality of air outlets 62 may or may not completely surround the central opening 150 . In accordance with certain presently contemplated embodiments, the first plurality of air outlets 62 is angled radially inward toward the liquid flow axis 24 without intersecting the liquid flow axis 24 .
For example, the respective air flow axes 180 of the first plurality of air outlets 62 do not align with the center of the central opening 150 , which corresponds to the liquid flow axis 24 . In this way, the air flow axes 180 each do not bisect the central opening 150 . Indeed, to allow the first plurality of air outlets 62 to swirl air, and therefore the liquid flow 22 , each of the first plurality of air outlets 62 is offset at an angle 182 from a radius 184 of the central opening 150 . The respective angles 182 of each of the first plurality of air outlets 62 may be the same, or may be different, and may vary between about 1° and 25° offset from radii aligning the liquid flow axis 24 and the respective centers 186 of each of the air outlets 62 . For example, the angle 182 may be about 1°, 5°, 10°, 11.5°, 15°, 20°, or 25°, or any angle in between. Moreover, while the first plurality of air outlets 62 is illustrated as including 12 air outlets, in other embodiments the first plurality of air outlets 62 may include 2, 4, 6, 8, 10, 14, or more outlets. Indeed, any number of air outlets 62 configured to produce a swirling effect on the liquid flow 22 as it exits the device 10 is presently contemplated.
While any number of the first plurality of air outlets 62 may be used in accordance with the presently contemplated embodiments, it should be noted that the size of each first plurality of air outlets 62 may at least partially determine a suitable number of the air outlets 62 , in addition to the angle 182 that is used for air swirling. While the first plurality of air outlets 62 may each have the same or different dimensions, as an example of certain embodiments, the diameter of each of the first plurality of air outlets 62 may be between about 0.005 inches (in) and about 0.05 in (e.g., about 0.01 in, 0.02 in, 0.03 in, 0.04 in, or 0.05 in). Indeed, the total atomization area for the first plurality of air outlets 62 may be between about 0.01 in 2 and 0.05 in 2 (e.g., about 0.005 in, 0.01 in 2 , 0.02 in 2 , 0.03 in 2 , 0.04 in 2 , or 0.05 in 2 ). For example, in one embodiment wherein the air cap 56 has 12 of the first air holes 62 , the area of atomization may be about 0.015 in 2 , with each of the air holes 62 having a diameter of about 0.039 in. It should be noted that while FIGS. 4-6 appear to present the air openings 62 in an ellipsoidal geometry, the orifices (the first plurality of holes 62 ) from which the atomizing air exits are indeed circular orifices when viewed from a perpendicular perspective with respect to the angled air flow 120 of each of the openings 62 .
FIG. 6 illustrates a front axial view of the air cap taken along line 6 - 6 of FIG. 3 . Referring to the air horns 66 and the relative size of the first plurality of air openings 62 compared to the second plurality of air openings 64 , the first plurality of air openings 62 may each be smaller than each of the second plurality of air openings 64 by about 5%, 10%, 15%, 25%, 50%, 75%, 100%, 150%, 200%, or more. In some embodiments, the particular size relationship between the first air openings 62 and the second air openings 64 may also be determined by the number of first openings 62 , the number of second openings 64 , as well as the desired area of atomizing air for the first openings 62 and the desired area of spray shaping air for the second openings 64 . For example, the total area of the first openings 62 may be about the same as the total area of the second openings 64 , or may be about 1%, 5%, 10%, 15%, 20%, 50%, 100%, or more, larger than the second openings 64 . In other embodiments, the second openings 64 may be about 1%, 5%, 10%, 15%, 20%, 50%, 100%, or more, larger than the first openings 62 .
In some embodiments, the size, shape, and extent of the second plurality of air openings 62 may be at least partially determined by the extent to which the air horns 66 surround the central opening 150 . As noted above, the second plurality of air outlets 64 may be any size and/or shape to the extent that they are disposed on the respective inner surfaces of the air horns 66 . In the illustrated embodiment, the first air horn 166 protrudes from the central surface 174 of the air cap 56 at a first offset distance 191 away from the center of the central opening 150 . The second air horn 168 also protrudes from the central surface 174 and is disposed at a second offset distance 193 away from the central opening 150 . The first offset distance and the second offset distance 191 , 193 may be substantially the same for both air horns 166 , 168 , and may be substantially continuous from the central opening to the air horns 166 , 168 due to their curved geometry. However, in other embodiments, the distances 191 , 193 may be different. The extent that each of the curved air horns 166 , 168 curve about the liquid flow axis 24 (or the central opening 150 ), as represented by arc 190 , may range from about 1° to about 180° (e.g., about 10° to about 160°, about 20° to about 140°, about 30° to about 100°, or about 40° to about 80°) around the circumference of the air cap 56 . In some embodiments, the arc 190 may be between about 25° to about 60° For example, the arc 190 may be 25°, 30°, 40°, 50°, 60°, or any angle in therein.
The extent of arc 190 , as well as the number, sizing, and angles of the second plurality of air outlets 64 may at least partially determine the manner in which the air flow 122 flattens the atomized coating spray 124 described above with respect to FIG. 2 . For example, in the illustrated embodiment, the first and second air horns 166 , 168 each include three air openings 192 that produce the air flow 122 along respective air flow axes, which is represented as arrows 194 . The air flow 122 , as noted above, produces swirled air that is countercurrent to the swirled air produced by the first plurality of air holes 62 . This results in the flattening effect described above, as well as additional atomization of the liquid.
Various configurations of air outlets of the air horns 66 may be further appreciated with respect to FIGS. 7 and 8 , which are partial cross-sectional views of embodiments of an air horn of the spray head component taken along line 7 - 7 of FIG. 4 . Specifically, FIG. 7 illustrates an embodiment of an air horn 200 having a curved inner surface 202 (e.g., a concave surface) with a pair of first spray shaping outlets 204 and a second spray shaping outlet 206 . As illustrated, the outlets 204 surround the outlet 206 . In accordance with the illustrated embodiment, the spray shaping outlets 204 , 206 are not aligned with respect to their respective distances 201 , 203 , 205 away from a lower portion 208 of the air horn 200 , which is generally aligned with the liquid opening 146 . However, in other embodiments, the spray shaping outlets 204 , 206 may be substantially aligned (i.e., have substantially the same distance 201 , 203 , 205 away from the lower portion 208 ).
In other configurations, the air outlets 64 of the air horns 66 may be replaced by one or more slots. FIG. 8 illustrates a partial cross-sectional view of another embodiment of an air horn of the spray head component taken along line 7 - 7 of FIG. 4 . Specifically, FIG. 8 depicts an air horn 210 having a spray shaping air slot 212 disposed on a curved inner surface 214 (e.g., a concave surface). In a similar manner to the arrangement of the air outlets 64 , 204 , and 206 described above, the air slot 212 extends in a crosswise direction 216 that is substantially parallel to the central surface 174 of the air cap 56 . In still further embodiments, the air horns 66 may include any number and/or combination of air slots and air openings having a variety of shapes and sizes. For example, the air openings on the air horns 66 may be ellipsoidal, rectangular, square, triangular, polygonal, and so on, with swirling occurring at least partially due to the curvature of the inner surfaces of the air horns 66 . Indeed, all such combinations are presently contemplated with respect to the formation of one or more swirled air flows to induce liquid atomization, or homogenization, or spray shaping, or any combination thereof.
As noted above, it may be desirable to incorporate feature that facilitate the use of the air cap configured to swirl air in conjunction with a variety of spray devices. For example, it may be desirable to provide an air cap in accordance with the presently contemplated embodiments that has the capability to receive a variety of geometries (e.g., shapes, and sizes) and configurations of valves, liquid outlets and internal flow patterns. One embodiment may include a relatively small liquid outlet for some spray coating applications (e.g., stains), while another embodiment may include a larger liquid outlet for other spray coating applications (e.g., epoxies), each of which may use different fluid seats. Accordingly, the disclosed embodiments provide interchangeable inserts configured for use with the air cap disclosed herein, which facilitates the use of different coating fluids.
With reference now to FIG. 9 , a side cross-sectional view of an embodiment of the spray coating device 10 is provided with the air cap 56 having a removable fluid tip and seat assembly 220 . The fluid tip and seat assembly 220 , in a general sense, may be varied to allow a user to vary the size of a liquid outlet 222 . For example, the fluid tip and seat assembly 220 includes a removable tip housing 224 configured to abut the air cap 56 , as will be discussed below. The tip housing 224 interfaces with a removable insert 226 , which is disposed within an inner circumference of the tip housing 224 and is placed in abutment with the same. Although the tip housing 224 and insert 226 are separate pieces in the illustrated embodiment, the housing 224 and insert 226 may be provided as a single piece in some embodiments.
The insert 226 may be a generally annular structure configured to be disposed within the tip housing 224 , and may extend through the tip housing 224 to a certain offset, or may be flush with the tip housing 224 . The insert 226 , proximate the center of its annular structure, includes the liquid outlet 222 . The liquid outlet 222 is generally an opening of the insert 226 having a geometry (e.g., shape and size) tailored to a particular application. For example, as discussed above, the liquid outlet 222 may have a diameter that at least partially depends on the fluid that will be utilized for a particular spray coating application (e.g., stains, paints, epoxies). The insert 226 also includes an inner surface 228 that begins at an inner extent of the insert 226 and tapers into the liquid outlet 222 . The tapered inner surface 228 is configured to interface with the liquid needle valve 74 , which provides adjustability of liquid flow through the fluid tip and seat assembly 220 . Moreover, the tapered inner surface 228 enables the insert 226 to be used in conjunction with a variety of liquid needle valves. Additionally, the tapered liquid needle valve 74 may be used in conjunction with similar inserts having a variety of sizes of the liquid outlet 222 . The fluid tip and seat assembly 220 also includes an annular member 230 disposed in abutment with the insert 226 . The annular member 230 may facilitate the interface of the fluid tip and seat assembly 220 with the nozzle portion 156 described above with respect to FIG. 4 .
FIG. 10 illustrates an exploded view of the components of the fluid tip and seat assembly 220 , each of the components being disposed along the liquid flow axis 24 . In the illustrated embodiment, the fluid tip and seat assembly 220 is exploded from the assembly 220 in an order of installation into the air cap 56 . For example, the air cap 56 may sequentially receive the tip housing 224 , the insert 226 , and the annular member 230 . The tip housing 224 can be made from any number of materials including stainless steel, tungsten carbide, delrin-type plastic, or any combination thereof. The tip housing 224 includes a forward tapered surface 232 having a frusto-conical shape extending from a first annular portion 234 . The tapered surface 232 opens to a central orifice 236 having a diameter 238 that facilitates an interface between the insert 226 and the tip housing 224 , as will be discussed below. The tip housing 224 also includes a second annular portion 240 disposed on an opposite side of the tip housing 224 from the tapered surface 232 . The second annular portion 240 includes a forward abutment surface 242 that abuts an inner surface 244 of the air cap 56 when the fluid tip and seat assembly 220 is placed into the air cap 56 . Moreover, the first annular portion 234 of the tip housing 224 has a diameter 246 that allows the forward portion of the tip housing 224 to extend through the central opening 150 of the air cap 56 while placing the forward abutment surface 242 against the inner surface 244 of the air cap 56 .
The insert 226 may be constructed from stainless steel, ultra high molecular weight (UHMW) or delrin plastic, tungsten carbide, or any combination thereof. The particular material or materials utilized for its construction may depend at least partially upon the particular coating application. For example, certain materials may be utilized for epoxies while others are used for paints or stains, and so on. The insert 226 includes a forward surface 248 , which is a curved surface in the illustrated embodiment. The forward surface 248 extends from a first annular portion 250 of the insert 226 , and has the liquid outlet 222 as a central opening. As noted above, the liquid outlet 222 may be varied by interchanging the insert 226 with another insert having a central opening of a different diameter. The forward surface 248 and the first annular portion 250 have a diameter 252 that allows the insert 226 to extend through the central opening 236 of the tip housing 224 . When the insert 226 is placed into the tip housing 224 , an abutment surface 254 of a second annular portion 256 of the insert 226 is placed against an inner surface 258 of the tip housing 224 , while the first annular portion 250 of the insert 226 extends through the central opening 236 of the tip housing 224 . As noted above, the insert 226 and the tip housing 224 , in some embodiments, may be a single piece.
The annular member 230 , as illustrated, includes a first abutment surface 260 that abuts a rear surface 262 of the second annular portion 256 of the insert 226 . A central orifice 264 of the annular member 230 allows a liquid needle valve, such as the needle valve 74 described above with respect to FIG. 9 , to extend from an interior of the spray device 10 and through the fluid tip and seat assembly 220 . The annular member 230 also has a rear abutment surface 266 that abuts against a nozzle portion, such as the nozzle portion 156 described above with respect to FIG. 9 . In an embodiment, the annular member 230 acts to seal the nozzle portion 156 against the fluid tip and seat assembly 220 to prevent fluid leakage. In this regard, the annular member 230 may be constructed from any material that is able to seal the nozzle portion 156 against the fluid tip and seat assembly 220 , for example synthetic and/or natural rubbers, plastics, ceramics, sintered materials, porous materials, malleable or soft metals, and so on.
While only certain features of the invention have been illustrated and described herein, many modifications and changes will occur to those skilled in the art. It is, therefore, to be understood that the appended claims are intended to cover all such modifications and changes as fall within the true spirit of the invention.
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The present disclosure relates generally to spray systems and, more particularly, to industrial spray coating systems for applying coatings of paint, stain, and the like. Specifically, the disclosed embodiments relate to a spray gun an air cap configured to produce air swirl. For example, in an embodiment, a system is provided that includes a spray coating device. The spray coating device has a liquid passage extending to a liquid outlet configured to output a liquid flow and an air passage extending to a plurality of air outlets configured to output an air flow. The plurality of air outlets is angled to swirl the air flow.
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BACKGROUND OF THE INVENTION
1. FIELD OF INVENTION
This invention pertains to a detector used for sensing cracks in an elongated web, and in particular, to a detector for detecting the size and shape of edge cracks in a paper web in a papermaking process.
2. BRIEF DESCRIPTION OF THE PRIOR ART
Most paper today is made in a continuous sheet on large papermaking machines from a web which undergoes several processing steps. The web is usually 20 feet wide or greater and is made in a continuous manner at very high speeds of, for example, 3000 ft/min. Because the profitability of papermaking machines is directly related to their continuous operation, interruption of full production is extremely costly and, therefore, factors which cause such interruptions are studied intensely to reduce such incidents to a minimum. One factor which results in the interruption of the papermaking machine is a crosswise tear in the paper web. Whenever such a tear occurs the papermaking machine must be shut down totally or partly until the problem is resolved. One cause of these tears are cracks formed at the web edges as the web travels through the machine. While often minor cracks can be tolerated with no problems, larger cracks can propagate across the sheet to form a tear.
Therefore, it is important to monitor cracks on the web edges and to analyze their formation and behavior in a papermaking machine to control web tearing. A better understanding of crack formation and propagation would also lead to improved preventive maintenance and emergency procedures. In fact, numerous devices are known for detecting cracks in moving elongated webs for such purposes. For example, devices are known which scan the web material in the direction of its width to find cracks as taught in U.S. Pat. No. 4,160,913 to Brenholdt, U.S. Pat. No. 4,247,204 to Merlen et al., U.S. Pat. No. 4,335,316 to Glanz et al. and U.S. Pat. No. 4,791,304 to Iida. Other devices are also known which detect tears and holes as well as web edges using stationary light transmission/detection systems. In these systems, light is transmitted toward the web material and is detected by detectors on the other side of the web material when the light is allowed to pass through the web material by cracks or holes therein. For example, such devices are taught in U.S. Pat. No. 2,735,329 to Meunier (sheet metal), U.S. Pat. No. 4,559,451 to Curl, U.S. Pat. No. 4,652,124 to Bowen et al. U.S. Pat. No. 4,680,806 to Bolza Schunemann, U.S. Pat. No. 4,709,157 to Shimizu et al., U.S. Pat. No. 4,728,800 to Surka and U.S. Pat. No. 4,788,442 to Sabater et al.
The above-mentioned devices detect tears in fabric webs which are relatively thick and move at relatively slow running speeds. Until now, because of the high speed of papermaking machines and the resultant flutter of the edges of the light weight paper sheets, it has been very difficult to sense and monitor edge cracks properly. Moreover, such systems do not determine the size and shape or direction of cracks in such a manner that tears in the web can be more accurately predicted. The present invention is designed to improve performance by determining the size and the shape of cracks in the web even in the presence of sheet flutter.
SUMMARY OF THE INVENTION
In view of the above, the most important objective of the present invention is to provide a detector which can be used to sense edge cracks in a paper web accurately even in the presence of significant machine disturbances such as sheet edge flutter and sheet edge lateral movement.
A further objective is to provide a detector which is relatively small which can be moved easily along the sheet edge from one part of a papermaking machine to another. This capability is very important in case it is necessary to identify and fix the machine sections which generate edge cracks
Another objective of the invention is to keep the device operating at high humidity and temperature conditions, such as in a paper machine dryer, where ambient conditions can be up to 200° F. at near saturating humidity. Yet another objective of the invention is to provide a detector which can be easily interfaced with a personal computer to ensure the system portability. The amount of data collected must be minimized since it is restricted by the data processing rate of the personal computer.
A further objective of the present invention is to provide an edge detector in which the crack dimensions such as width and length of an edge crack and the crack shape can be determined from a single measurement. Crack widths and lengths are defined as the dimensions of the crack openings along the machine direction and the cross-machine direction, respectively. Cracks can adopt various shapes depending on the general orientation such as slanting toward or against the sheet running direction or both to have a crooked slope, and by detecting such shapes, those cracks with shapes more likely to cause a tear can be determined.
Yet another objective is to provide an edge crack detector which requires minimum data processing, thereby obviating the need for high-speed and expensive processors which are not appropriate for portable equipment.
A yet further objective of the present invention is to provide an edge crack detector which can function without the need for tracking or compensating for lateral drifts or flutter of the paper web.
As known to those skilled in the art, the paper web formed in a papermaking machine is generally subject to two kinds of extraneous movements: flutter and lateral drift. Flutter refers to a three dimensional movement of the web similar to the movement of a flag in a breeze. Lateral drift refers to the movement of the web transverse to the machine direction. An edge crack detector deployed along a papermaking line must be able to detect the edge movement caused by either flutter or lateral drift. It is desired to eliminate such problems from the edge determination.
Briefly, a detector for sensing edge cracks constructed in accordance with this invention consists of an array of light emitters preferably in the infrared region and a matching array of IR-sensitive receivers for detecting the light. The emitters and receivers are positioned on the opposite sides of the web so that only the light transmitted through the cracks is detected by the receivers The receivers are spaced laterally in the cross-machine direction from the web edge and are oriented so that each generates a signal related to the width of the crack at a particular distance from the edge of the web. The signals from the receivers are then fed to a signal processor for determining the crack's dimensions and shape. Tracking means are also provided to detect and compensate for the lateral drift. In accordance with the invention, the tracking means may be implemented by manipulating the signals received in the signal processor.
By way of example, crack shape can be monitored by the addition of a parameter, the delay time D. The light transmitting/detecting first channel which is triggered is set to have a value of D equal to zero. Other channels have values of D greater than zero depending on the order of activation. In accordance with the invention a combination of the values of crack widths P and delay times D can be used by the signal processor to recreate the crack size and shape.
A method to detect the web edge in accordance with a preferred embodiment of the invention is to activate the IR-emitters in a preselected sequence and to feed the output of the receiver into the signal processor to detect sources which are blocked from the receiver by the web. In this manner, the instantaneous position of the web edge is obtained, including the profiles of edge cracks. Analog or digital filters may also be used to eliminate the effects of flutter or lateral drift.
Other objectives and advantages of the invention shall become apparent from the detailed description of the invention.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 shows a schematic diagram of a preferred embodiment of a portable edge crack detector constructed in accordance with this invention;
FIG. 2 shows an isometric view of the IR transmitters and receivers of FIG. 1 used for crack detection;
FIG. 3 shows an isometric view of a device for calibrating the detector of FIG. 1;
FIG. 4 shows a typical response curve by one pair of sensors for a crack detected by the apparatus of FIG. 1;
FIG. 5 is a diagram of data input to the program of the invention for calculating and displaying crack dimension and shape;
FIGS. 6-8 shows typical formats of the displayed output; and
FIGS. 9,10 (a)and 10(b) illustrate flow charts of the system for collecting and processing data on crack dimensions, shapes, and edge detection in accordance with the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates a portable edge crack detector 10 constructed in accordance with this invention, including a plurality of sources of light 12 which respectively direct infrared light toward a plurality of infrared light sensors 14 across a paper web 16 moving at high speed in the direction indicated by arrow A so that at least some of the light may be blocked by the web. Light sensor 14 has an output schematically indicated by line 18 which is fed to a signal processor 20. The signal processor 20 analyzes this output 18 to detect the physical dimensions, such as the width, length, and shape of edge cracks on web 16 in accordance with the techniques of the invention. This information may be stored in a memory 22 and/or displayed on a display device 24. The display device 24 may be for example, a printer, a plotter, or a video display.
As shown in more detail in FIG. 2, web 16 runs in a papermaking machine in direction A with its edge 26 disposed between light sources 12 and light sensors 14. The edge 26 may have a crack 28 which typically has an irregular shape with a maximum length indicated by the letter L and a maximum width W. Light source 12 includes one or more IR crack detection transmitters 30 generating light in the range of 7.5-9 μm wavelength. This range is selected because frequently the air adjacent to the web has a very high humidity. Humid air is relatively transparent to IR light at this frequency so that it will not affect significantly the measurements made by the edge crack detector 10 of the invention.
The light detection transmitters 30 direct the IR light toward the light sensor 14 which preferably consists of one or more IR crack detection receivers 32. Each crack detection transmitter 30 and receiver 32 includes a plurality of needle tip fiber optic cables 34 with a diameter smaller than 1/16" as shown for respectively transmitting and receiving the IR light for crack detection. The tips of the fiber optic cables 34 are preferably in parallel and spaced about 0.25 inches apart. The receivers 32 cooperate with the transmitters 30 so that each receiver 32 monitors the width of an edge crack at a predetermined distance from the edge 26. Thus, the first crack detection receiver 32 may monitor the width of the gap about 0.125 inches from the edge, the second receiver may monitor the width of the gap at 0.375 inches from the edge and so on. Thus, by correlating the information from the individual receivers 32, a two-dimensional composite profile of the edge crack may be obtained. The number of receivers 32 to be used is determined by the maximum size of the cracks that are to be monitored. A system of this type is described in abandoned U.S. Pat. application Ser. No. 07/550,406, filed Jul. 10, 1990, by the present inventor, the contents of which are hereby incorporated by reference in their entirety.
As shown in FIG. 2, for a maximum crack length of 4.0"16 pairs of receiver-emitter fiber optic cables 34 may be needed. The receivers 32 and the transmitters 30 may both be, for example IR sensors F7M available from Scientific Technologies Inc. that have been modified to have response time reduced to 0.1 ms. Each of these sensors includes a source of light as well as a light detector connected to the fiber optics cables 34 having the characteristics and configurations described above. Also, the fiber optic cables are preferably of sufficient length to isolate the electric components from high ambient temperature and humidity.
The only elements of the detector described above which must be situated in the vicinity of the web are the compact fiber optics strands 34 used for conditioning the light sources and the received lights as shown in FIG. 2. These elements are relatively small and can withstand even the high temperature and humidity conditions of the paper machine along a papermaking line. Thus, the detection is portable along the papermaking line.
The response of pairs of IR transmitter/receivers made by different manufacturers may vary somewhat and, therefore, it may be necessary to calibrate them. A device 36 for calibrating a crack detection transmitter 30 and a crack detection receiver 32 is shown in FIG. 3. The device consists of a shaft 38 for rotating a thin wheel 40 as indicated by arrow B. A notch 42 is made in the wheel by making two parallel cuts substantially in the radial direction at a preselected spacing S apart and removing the material therebetween. The wheel is rotated at a high speed so that the notch 42 has a linear velocity equal to the speed of the web 16 in the papermaking machine. The transmitter 30 and receiver 32 are positioned across from each other close to the perimeter of the wheel 40, with the wheel 40 disposed in between. As shown in FIG. 3, the receiver is positioned with its slit extending perpendicularly to the notch 42. As the wheel 40 rotates, the light from the crack detection transmitter 30 is blocked from the crack detection receiver 32 except at the notch 42. The signal from the receiver is recorded, and the wheel 40 is changed for a different wheel having a notch with a different spacing S. Different wheels may be made with the spacing increasing in steps from 1/16 inch to 1.50 inches. A typical curve of the digital signal generated by the receiver for a notch is shown in FIG. 4 wherein the vertical axis indicates the signal voltage and the horizontal axis indicates time. It was found that the elapsed time between points C and D is proportional to the width of the notch 42. Thus, the device in FIG. 3 can be used to generate a calibration standard for an edge crack detector. This standard then may be used to determine the width of a crack from the signals generated by a receiver. Based on the response time of the detector, a maximum sensitivity of about 1/8 inches in crack width dimension at a web speed of 3000 ft/min. may be possible.
During operation of the circuit of the invention, a counter of signal processor 20 is used to track the outputs of sensors 14 for determining the size and shape of cracks 28 in the web 16. At the time a sensor 14 is activated, an internal clock of the counter is reset to zero. Between points C and D of FIG. 4, the counter is activated and counts up or down to register only the time interval between on and off, which corresponds to the crack width W indicated by that sensor channel. The time interval is coded by the count values (P values) as shown in FIG. 5. The amount of memory required per channel to store this data is only about 10 bytes or about 160 bytes for an array of 16 channels. This low memory requirement is an important feature to make the total system portable since any standard personal computer can be used to process the resulting data.
Since the sensor response time is tuned to 0.1 ms, the sensor resolution for the width W is the distance the web travels in 0.2 ms, or enough time to turn the sensor ON then OFF. For a web speed of 3000 fpm, the sensor resolution has been confirmed to be about 0.125".
The crack length L in the direction along the width (transverse to the moving direction) of the web 16 is equivalent to the number of channels that are triggered multiplied by 0.25" which is the distance in a preferred embodiment between two adjacent sensor channels. The crack length is thus measured by an increment of 0.25" in FIG. 5.
Crack shape can be monitored in accordance with the invention by the addition of a third parameter, the delay time D, as illustrated in FIG. 5. As shown, the first detector channel which is triggered is set to have a value of D equal to zero. Other channels have values of D greater than zero depending on the order of activation. These values are determined by processor 20 and stored for display on display device 24. A combination of the values of Ps and Ds can be used to recreate the crack size and shape as illustrated in FIGS. 6, 7 and 8, where the horizontal axis represents the output of each detector and thus represents crack length, while the vertical axis incorporates crack width W and delay D to display the crack size and shape.
Another feature of the invention is to detect the presence of a web edge. This is possible simply using processor 20 by assigning negative values for any channels detecting crack widths greater than 10 feet. Since such a crack is nonexisting, it is determined that the web edge lateral movement is being detected rather than an edge crack. The web edge position can therefore be determined by counting the number of channels with negative values. This technique can thus be used to detect lateral movement of the web 16. Also, as described in the aforementioned abandoned U.S. application Ser. No. 07/550,406, analog or digital filters may also be used to eliminate the effects of flutter or lateral drift.
A recording time is also used in accordance with the invention to represent the minimum amount of time that must elapse between the end of one event and the beginning of the next event, where the events occur when a crack activates at least one of the sensor channels. The recording time allows the signal processor 20 adequate time to capture the data from an event and write it to memory (disk) 22. The recording time is enforced in hardware and is dictated by the speed of the microprocessor of the signal processor 20.
Gap time, on the other hand, as used herein, is designed by software so that a typical sheet edge movement or fluttering is neglected but not an actual edge crack. This is possible since the movement or fluttering of a sheet edge position is much more frequent than the occurrance of cracks. Thus, if only one channel is activated more than once during the gap time, it is assumed to be caused by the fluttering or wandering of the sheet edge, not by an edge crack. Gap time is therefore determined by the operator, who sets the value based on experimental data of flutter and the sheet edge guiding system. The gap time is generally longer than the recording time.
As used herein, a time-out period is the maximum allowable time that an event can be recorded. It is designed so that the individual detectors can distinguish between an edge crack and the occasion when the sensor is off the edge and therefore is on continuously. The time-out period is set in software to determine the position of the edge and can be controlled by the software. Generally, the event time is longer than the gap time but shorter than the time-out period.
The flow chart diagrams summarizing the functioning of signal processor 20 for calculating the crack size and shape in accordance with the above-mentioned technique can be found with reference to FIGS. 9 and 10. For the purposes of this description, sensor numbering is assumed to start with 0 at the outermost sensor and end with 16 at the innermost sensor, where it is assumed that the preferred embodiment comprises 16 sensors. Only the first seven sensors (0-6) need to be used to detect the sheet edge, for it is assumed that the total lateral displacement due to sheet wandering amounts to only 1.5 inches in the direction transverse to the moving direction of the web.
In a preferred embodiment of the invention, a counter/timer board having at least 40 counters is used. Counters 1 and 2 are cascaded to form a 32-bit time stamp counter. The time stamp indicates the time, in 0.1 msec increments, from the start of data recording. The time stamp counter runs continuously and will count for almost 5 days before reaching the maximum value (2 32 ) before wrapping around to zero. Counters 3 and 4 are used to compare the time out-period with a duration of an event. Counters 3 and 4 begin to count down from a value for the time-out period programmed by the operator, and if it reaches zero before an event is over, it terminates the event and considers it invalid. This technique is used to prevent indefinitely long events which correspond to sheet breaks or when a sheet edge wanders out of view of a sensor. The time-out period therefore must be set to cover the maximum detectable crack width period.
Counters 5 and 6 are for gauging the duration and the delay time of a signal of sensor 0, while counters 7 and 8 gauge the duration and the delay of sensor 1, counters 9-10 are for sensor 2, and so on, until counters 35-36, which are provided for sensor 15. Each sensor covers 0.25 inch of sheet width so that a maximum crack length of 4 inches can be monitored. Of course, the range for crack length can be increased by adding more sensor channels.
The algorithm for crack dimension and shape detection in accordance with the invention starts by asking the user for information such as the desired time-out period, gap time values, file names, and the like. The system then creates a disk file for output at step 100 and programs the counter/timer boards by programming the time stamp counter at step 102 and the time-out counter at step 104. The system then installs the interrupt routine at step 106. The interrupt routine will be described in detail below with respect to FIG. 10.
The system then waits for events to occur. The events are handled by the interrupt routine which will be described below with respect to FIG. 10. The system of FIG. 9 thus monitors the interrupt at step 108 to determine when the interrupt is done. However, if the user presses an input key at step 110 before the interrupt is completed, the interrupt is disabled at step 112, the disk file is closed at step 114 and the algorithm is exited at step 116. On the other hand, when an event occurs, the interrupt routine decides whether the event is valid, and if so, data is displayed on the screen and written to the log file for later evaluation. However, if not, the program displays a column of -1, which symbolizes an invalid event. The program then waits for the next event to occur.
The algorithm of FIG. 9 communicates with the interrupt routine of FIG. 10 through an array of bits The first element of the array is used as a return flag which the interrupt routine of FIG. 10 sets to nonzeros after each event, and the algorithm of FIG. 9 sets it to zero after capturing the data before continuing with the next task. Bit 9 is set by the interrupt routine to force the flag to nonzeros, while bit 8 is set if the event ends due to a time-out. Bits 0-6 are set to the states of sensor 0-6 at the end of each events and these states are used to indicate the edge position. The remaining elements of the array are used for temporary storing of the crack width and delay time values of each channel until the completion of an event.
After processing of the interrupt routine of FIG. 10, the program of FIG. 9 first checks if a time-out occurred at step 118. If sod the event is immediately declared invalid and the paper edge is defined as the position of the highest numbered sensor which is still activated at the end of the event. The resulting values are then displayed on the display device 24 at step 120. However, if it is determined at step 118 that no time-out occurred during processing of the interrupt routine, the event counter is incremented at step 122 and the time stamp value is checked. If the event ends after the gap time, the event is valid. However, if the event ends before the gap time, the algorithm checks the number of sensors involved in the event. If only one sensor channel is involved, that sensor channel is determined to be riding on the sheet edge, where sheet fluttering makes the sensor flicker. The event is declared invalid since no crack is involved. On the other hand, if more than one sensor channel is activated, then it is determined that a crack must be passing by, and accordingly, the event is declared to be valid.
If the event is valid, the algorithm calculates the edge positions based on the order of the channels being activated (FIG. 5). It then checks all the counter values. Some counters might have zero values if the crack width at the sensor channel is zero. In such a case, the program will set the corresponding delay time, which is a function of the degree of slanting of the crack, also to zero. The algorithm will then set all crack width and delay time to -1 for any sensor channel which is off the edge of the paper. This provides a simple visual and logical way to indicate the edge position. A value of -1 indicates that the sensor is off the edge. Finally, the algorithm of FIG. 9 increments the event counter at step 122, calculates the time stamp at step 124 and then determines whether any of the channels along the edge (channel 0-6) are disabled at step 126.
If none of these channels is disabled, the crack width and delay time values are displayed on the display screen at step 128. However, if any one of these channels is disabled, at step 130 the crack width and delay time of the disabled channel are set to -1 as noted above before the crack width and delay time values are displayed on the screen at step 128. The system then checks at step 132 whether any of the pulse widths are equal to zero, and if so, at step 134 the delay is set to zero for any channel whose pulse width is equal to zero. The system then writes all data to the log file at step 136 and then waits for the next event.
The interrupt routine of FIG. 10 is activated at step 200 at the end of each event or a two second time out. As illustrated in FIG. 10 (a), an interrupt is issued at step 202, and if it is determined at step 204 that the interrupts are not enabled, the interrupt request is cleared at step 206, the interrupts are reenabled at step 208, and the system returns from the interrupt at step 210. However, if it is determined at step 204 that the interrupts are enabled, it is then determined at step 212 whether the program is busy. If the program is busy, the return flag is set to a maximum value of 256 at step 214, and the interrupts are reenabled at step 208 before the system returns from the interrupt at step 210. However, if the program is determined not to be busy at step 212, the system first latches the time stamp counter to get a time log for the event at step 216. The system then gets the current states of sensors 0-6 at step 218 for use in edge detection. The system then saves the contents of all crack width and delay times of each sensor and latches the value of the time out counter at step 220 and clears the interrupt request on the counter/timer board at step 222.
As illustrated in FIG. 10 (b), the interrupt routine next determines at step 224 whether a time out has occurred. This is indicated by the state of the output of counter 4. If the output of counter 4 is zero, it is determined that a time out occurred, and the interrupt routine communicates this fact to the program by setting bit 8 to 1 in the return flag at step 226. Otherwise, the value of bit 8 is set to zero. If a time out occurred, it is then determined at step 228 whether any of channels 0-6 are still active. If so, any active channels are disabled at step 230 until it is determined at step 232 that all of the channels are inactive. The crack width and delay time values are then stored in the array of the interrupt routine at step 234. However, if it is determined at step 224 that no time out occurred, it is determined at step 236 whether any of the channels 0-6 are inactive, and if so, any inactive channel is enabled at step 238. The counter values for crack width and the delay time values are then stored in the array of the interrupt routine at step 234.
The interrupt routine of FIG. 10 then performs housekeeping functions. Namely, it sets bit 9 in the return flag to nonzeros, updates the return flags on the states of sensors 0-6, reprograms all counters except the time stamp counter, and resets the external sensor conditioning circuit in steps 240-248. The interrupts are then reenabled at step 208 and the interrupt is exited at step 210. The crack width and delay time values can thus be formed into an image and displayed on the display screen at step 128 and stored to disk at step 136 of FIG. 9 as described above. For example, images of the type illustrated in FIGS. 6-8 will be displayed so that the severity of the crack may be determined.
Signal processor 20 may be programmed to take all values of Ps, Ds, and the number of activated channels to redisplay the crack dimensions and shapes. Preferably, signal processor 20 is capable of sorting the sensor outputs to rank cracks according to size, time of occurrence, and frequency of occurrence. Some simple statistics such as mean and standard deviation preferably can also be performed in accordance with conventional techniques
Obviously, numerous modifications may be made to the invention by those skilled in the art without departing from its scope as defined in the appended claims. For example, the technique of the invention may be used to detect imperfections in fabric webs.
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A detector for detecting edge cracks in the web in a papermaking machine includes a plurality of light sources for directing light at the web and a plurality of light sensors for receiving the light through the cracks for generating a plurality of signals indicative of the dimensions and shape of the crack. The size and shape of the cracks are determined from the sensor outputs by a processor and preferably displayed on a suitable display. Crack shapes are determined by introducing a delay parameter which relates the output for each detector channel to the time a first detector channel is triggered. In particular, the first detector channel which is triggered is given a delay value of zero, while other channels are given delay values greater than zero depending on the order of activation. The signal acquisition and analysis are designed to be compatible with a personal computer so as to ensure the system's portability. The device also includes the use of fiber optics and quick response infrared sensors to meet the high resolution and high temperature conditions for crack detection in a papermaking machine, for example. Plural light sources and sensors detect an edge of a moving paper web when a sensor detects light on at least two different occasions during a gap time of duration such that light detection may be assured to be caused by sheet flutter or wander rather than edge cracks.
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RELATED U.S. APPLICATION DATA
The present application is a continuation of U.S. patent application Ser. No. 10/011,204, filed Nov. 8, 2001 now abandoned; which is a continuation of U.S. patent application Ser. No. 08/700,530, filed Oct. 23, 1996, now U.S. Pat. No. 6,316,186, which is the U.S. National Stage of International Application No. PCT/GB95/00521 Mar. 10, 1995. The entire disclosure of each of the aforementioned applications is incorporated by reference in the present application.
FIELD OF THE INVENTION
The present invention relates to binding assays using binding agents with tail groups, and in particular binding agents having oligonucleotide tail groups. These binding assays are useful in determining the concentration of analytes in liquid samples.
BACKGROUND OF THE INVENTION
It is known to measure the concentration of an analyte, such as a drug or hormone, in a liquid sample by contacting the liquid sample with a binding agent immobilised on a solid support, the binding agent having binding sites specific for the analyte, separating the binding agent having analyte bound to it and measuring a value representative of the fraction of the binding sites of the binding agent that are occupied by the analyte. Typically, the concentration of the analyte in the liquid sample can then be determined by comparing the value representative of the fraction of the binding sites occupied by analyte against values obtained from a series of standard solutions containing known concentrations of analyte.
In the past, the measurement of the fraction of the binding sites occupied has usually been carried out by back-titration with a labelled developing reagent using either so-called competitive or non-competitive methods.
In the competitive method, the binding agent having analyte bound to it is back-titrated, either simultaneously or sequentially, with a labelled developing agent, which is typically a labelled version of the analyte or an anti-idiotypic antibody capable of recognising empty binding sites of the binding agent. The developing agent can be said to compete for the binding sites on the binding agent with the analyte whose concentration is being measured.
The fraction of the binding sites which become occupied with the labelled analyte can then be related to the concentration of the analyte as described above.
In the non-competitive method, the binding agent having analyte bound to it is back-titrated with a labelled developing agent capable of binding to either the bound analyte or to the occupied binding sites on the binding agent. The fraction of the binding sites occupied by analyte can then be measured by detecting the presence of the labelled developing agent and, just as with competitive assays, related to the concentration of the analyte in the liquid sample as described above.
In both competitive and non-competitive methods, the developing agent is labelled with a marker to allow the developing agent to be detected. A variety of markers have been used in the past, for example radioactive isotopes, enzymes, chemiluminescent markers and fluorescent markers.
In the field of immunoassay, competitive assays have in general been carried out in accordance with design principles enunciated by Berson and Yalow, for instance in “Methods in Investigative and Diagnostic Endocrinology” (1973), pages 111-116. Berson and Yalow proposed that in the performance of competitive immunoassays, maximum sensitivity is achieved when an amount of binding agent is used to bind approximately 30-50% of a low concentration of the analyte to be detected. In non-competitive immunoassays, maximum sensitivity is generally thought to be achieved by using sufficient binding agent to bind close to 100% of the analyte in the liquid sample. However, in both cases immunoassays designed in accordance with these widely-accepted precepts require the volume of the sample to be known and the amount of binding agent used to be accurately known or known to be constant.
In International Patent Application WO 84/01031, I disclosed that the concentration of an analyte in a liquid sample can be measured by contacting the liquid sample with a small amount of binding agent having binding sites specific for the analyte. In this “ambient analyte” method, provided the amount of binding agent is small enough to have only an insignificant effect on the concentration of the analyte in the liquid sample, it is found that the fraction of the binding sites on the binding agent occupied by the analyte is effectively independent of the volume of the sample.
This approach is further refined in EP 304,202 which discloses that the sensitivity and ease of development in the assays in WO 84/01031 are improved by using an amount of binding agent less than 0.1V/K moles located on a small area (or “microspot”) on a solid support, where V is the violume of the sample and K is the affinity constant of the binding agent for the analyte. In both of these references, the fraction of the binding sites occupied by the analyte is measured using either a competitive or non-competitive technique as described above.
SUMMARY OF THE INVENTION
There is continuing need to develop binding assays which have enhanced kinetics to allow assays to be carried out more quickly and easily. In addition, it would be desirable to provide a binding assay which the user of the assay can easily customise for the detection of different groups of analytes.
Accordingly, in a first aspect, the present invention provides a method of determining the concentrations of analytes in a liquid sample comprising:
(a) immobilising one or more capture agents on a solid support, each capture agent being capable of specifically binding a given binding agent; (b) contacting the liquid sample with one or more binding agents, each binding agent having binding sites specific for a given analyte so that a fraction of the binding sites become occupied by the analyte, and a tail group adapted to bind to a corresponding capture agent; (c) contacting the liquid sample, either simultaneously or sequentially with the step (b), with the immobilised capture agents so that the binding agents become bound to their respective capture agents; and (d) determining the fraction of the binding sites of a binding agent occupied by analyte to determine the concentration of the analyte in the liquid samples.
Accordingly, the present invention provides an assay in which the binding of the analytes takes place in the liquid phase, rather than at a surface of a solid substrate. This enhances the kinetics of the reaction between analyte and binding agent.
Thus, in one embodiment, contacting the liquid sample with the binding and capture agents simultaneously allows the assay to be carried out in a single step, eg using a single reaction vessel. Alternatively, sequential contact of the binding agent(s) and capture agent(s) may be preferred, especially where the liquid is serum or blood, and non-specific binding is an important source of error. In these cases, the binding agent can be first contacted with the liquid sample in a first vessel and then the sample transferred to a second vessel to allow the capture agent to bind the binding agent to the solid support.
In a second aspect, the present invention provides a method of immobilising one or more binding agents on a support, each binding agent having binding sites specific for a given analyte and a tail group adapted to bind to a capture agent, comprising:
(a) immobilising one or more capture agents on a support each capture agent being capable of binding to the tail group of a given binding agent and, (b) contacting the binding agents with the support having the capture agents immobilised thereon so that the binding agents become specifically bound to their respective capture agents through their tail groups.
The above method can additionally comprise the step of attaching the tail groups to the binding agents prior to exposing them to the capture agents immobilised on the support.
Thus, it is possible for the user of the assay to customise binding agents for use in determining the concentration of different groups of analytes and using the customised binding agents in conjunction with a universal support having capture agents immobilised on it, to which the binding agents can individually bind by virtue of their tail groups.
In this aspect of the invention, the assay is carried out by exposing the support to a liquid sample after the binding agent(s) has or have become bound to the capture agent(s).
In either aspect, the present invention provides an assay in which the binding agent is indirectly linked to capture agent immobilised on the substrate via the tail group.
Preferably, the capture agent is an oligonucleotide sequence which can hybridise to a complementary sequence comprising the tail group of the binding agent. The oligonucleotides acting as capture agent or tail of the binding agent are sufficiently long to provide strong and specific hybridisation under the stringency conditions used in the assay. Typically, complementary oligonucleotides of at least about 8 or 9 nucleotides in length are used. In a preferred embodiment, the oligonucleotides are preferably between 8 and 30 bases, more preferably between 16 and 20 bases, in length. However, the use of very long polynucleotides is not preferred as these can lead to a reduction in the specificity of binding different capture agents or to self hybridise, forming hairpin loops (double stranded regions). However, a suitable length and sequence of oligonucleotide for a set of assay conditions can readily be determined by those skilled in the art.
Conveniently, the binding agent is an antibody having binding sites specific for an analyte. Accordingly, when the capture agent on the support is exposed to the liquid phase binding agent, the binding agent becomes bound to the solid support. Alternatively, where the analyte is a nucleic acid sequence, the binding agent can be an oligonucleotide. Thus, in this embodiment, the binding agent has a first sequence capable of hybridising to the analyte and a second sequence acting as the tail group.
Preferably, a small amount of binding agent is used in accordance with the assays disclosed in WO 84/01031 or EP 304,202, so that the volume of the liquid sample need not be known. Thus, the amount of binding agent should be sufficiently small so that it does not significantly affect the ambient concentration of the analyte in the liquid sample. Typically, the use of an amount of binding agent which binds less than 5% of the analyte is preferred. However, the use of a smaller amount of binding agent, eg to bind 2% or 1% of the analyte, further reduces the disturbance to the ambient concentration of the analyte and helps to minimise the error in determining the analyte concentration.
Where the assay is conducted in accordance with EP 304,202 using less than 0.1V/K moles of binding agent, the affinity constant (K) for the binding of analyte to binding agent is measured in accordance with normal practice. This means the value of the affinity constant used to determine how much binding agent constitutes 0.1V/K moles is the value that is obtained under the conditions (eg reactants, time of incubation, pH, temperature etc) that are used in the assay.
Preferably, each capture agent is used in excess to bind substantially all of a given binding agent. This maximises the assay sensitivity and ensures that when the amount of binding agent used needs to be known or known to be constant, the user of the assay can be confident that substantially all of a binding agent used in an assay becomes bound to its capture agent on the support.
Preferably, molecules of capture agent are immobilised on a support at discrete locations, eg as microspots. This allows the concentration of a plurality of different analytes to be simultaneously determined using a plurality of different capture agents at a series of locations on the support. Where the capture agent(s) is or are immobilised as microspots, the sensitivity of the assay can be improved immobilising the capture agent at high density, thereby improving the signal-to-noise ratio (see for example our co-pending application PCT/GB94/02814). Assuming sample volumes of the order of 0.1-1.0 ml, the microspots preferably have an area less than 1 mm 2 and a final surface density of binding agent between 1000 and 100000 molecules/μm 2 .
Alternatively, a given capture agent can be immobilised on a support at a plurality of locations so that a series of measurements of the concentration of an analyte can be made simultaneously.
Preferably, the fraction of the binding sites occupied by the analyte is detected using developing agents in a competitive and/or non-competitive method as described above. The developing agents are capable of binding to occupied or unoccupied binding sites of the binding agent or to bound analyte and are labelled to enable bound developing agent to be detected. Preferably, the developing agents are labelled antibodies.
The markers can be radioactive isotopes, enzymes, chemiluminescent markers or fluorescent markers. The use of fluorescent dye markers is especially preferred as the fluorescent dyes can be selected to provide fluorescence of an appropriate colour range (excitation and emission wavelength) for detection. Fluorescent dyes include coumarin, fluorescein, rhodamine and Texas Red. Fluorescent dye molecules having prolonged fluorescent periods can be used, thereby allowing time-resolved fluorescence to be used to measure the strength of the fluorescent signal after background fluorescence has decayed. Latex microspheres containing fluorescent or other markers, or bearing them on their surface can also be employed in this context. The signals from the markers can be measured using a laser scanning confocal microscope.
Alternatively, other high specific activity labels such as chemiluminescent labels can be used. In the case of chemiluminescent labels, the signals from different chemilumiscent labels used to mark binding agent or developing agent can be simultaneously detected using, for example a charge-coupled device (CCD).
The binding agent (or a proportion of it) can conveniently be labelled, eg with a fluorophor. In accordance with the method set out in EP 271,974, this means that it is not necessary for the user of the assay to know the amount of binding agent or to know that it is constant. This is because the ratio of the signals from the binding agent and the signal indicating the fraction of the binding sites of the binding agent occupied by analyte is dependent on the fraction of the sites of the binding agent occupied by the analyte, but is independent of the total amount of binding agent present.
Alternatively, if the user of the assay knows the volume of the sample, a larger amount of binding agent can be used so that the assay is not operating under ambient analyte conditions. This allows the concentration of the analyte to be determined using one label on the developing agent and either knowing the amount of binding agent is constant or labelling it with a second marker so that the amount is known.
In a variant of this approach (described in our co-pending application PCT/GB94/02813), two labelled developing agents can be used, a first capable of specifically binding to unoccupied binding sites of the binding agent and a second capable of binding to occupied binding sites or bound analyte. Thus, the signal from either marker is representative of the fraction of the binding sites occupied by analyte, while the sum of the signals is representative of the total amount of binding agent used.
This method can also avoid the necessity of knowing that a constant amount of binding agent is used as variations in the amount of binding agent immobilised can readily be corrected for. Under these circumstances, the sample volume v must either be known or constant. This can be seen from the following formula show how the signals from two labelled developing agents relates to the concentration of analyte in a sample.
Let the signal emitted by the label marking the developing agent directed against occupied binding agent binding sites be given by S o ,
and the signal emitted by the label marking the developing agent directed against unoccupied binding agent binding sites be given by S u ,
and let the constants relating the respective signals to occupied and unoccupied sites be ε o and ε u respectively, and K=the effective equilibrium constant governing the reaction between the analyte and binding agent.
Then, if the analyte concentration in a sample is given by Y,
Y =( S o /ε o )[ε u /( KS u )+1 /v]
Assuming v is known, this equation contains two unknown constants, ε o and ε u /K. By determining the signals S o and S u for a series of known analyte concentrations, these constants can be determined, and unknown analyte concentrations estimated from corresponding determinations of S o and S u . Thus, the assay need not work under ambient analyte conditions.
Under ambient analyte conditions, the term 1/v becomes negligible, and S o /S u is proportional to the ambient analyte concentration.
In a first kit aspect, the present invention provides a kit for determining the concentrations of one or more analytes in a liquid sample in a method as described above, the kit comprising:
(a) a solid substrate having attached thereto at a plurality of locations capture agent capable of specifically binding a binding agent; (b) one or more binding agents, each binding agent having binding sites specific for an analyte, and a tail group adapted to bind one or more capture agents; and (c) one or more developing agents having markers capable of binding to occupied binding agent binding sites or analyte bound to binding agent or unoccupied binding agent binding sites.
In a second kit aspect, the present invention provides a kit for customising an assay for the determination of the concentration of one or more analytes comprising:
(a) one or more tail groups, each tail group being for attachment to a binding agent; (b) a solid substrate having attached thereto at a plurality of locations one or more capture agents capable of specifically binding to a tail group; wherein the user of the assay attaches the tail groups to the binding agents, thereby providing binding agents which can be used in conjunction with the solid substrate to which the capture agents are attached in a method as described above.
DESCRIPTION OF THE DRAWINGS
A preferred embodiment of the present invention will now be described with reference to the accompanying schematic drawings in which:
FIG. 1 shows an assay to detect two analytes in a liquid sample using two species of capture agent and two species of binding agent, the capture agent immobilised at two microspots;
FIG. 2 shows the assay of FIG. 1 in which the capture agent has become bound to the binding agent;
FIG. 3 shows a non-competitive method of determining the occupancy of the binding agent using a second labelled antibody; and,
FIG. 4 shows a graph of signal plotted against TSH concentration from the experimental example below.
DETAILED DESCRIPTION
FIGS. 1 to 3 show a binding assay in which two species of binding agent 2 , 4 having binding sites specific for different analytes 6 , 8 are used. Each binding agent 2 , 4 comprises an antibody 10 , 14 provided with an oligonucleotide tail group 12 , 16 . The oligonucleotide tail groups have different nucleotide sequences, the sequences being complementary to one of the sequences of capture agents 18 , 20 , immobilised on a solid support 22 in the form of microspots. In this example, the oligonucleotides are 8 nucleotides long.
In the assay, the two analytes 6 , 8 in the sample are exposed to binding agents 2 , 4 so that a fraction of the analytes 6 , 8 become bound to the antibodies 10 , 14 . As this reaction occurs in the liquid phase, the kinetics of the reaction between the antibodies 10 , 14 and the analytes (antigens) 6 , 8 are optimised.
Simultaneously or sequentially with the initial antibody/analyte reaction, the liquid sample and binding agent are exposed to the solid support 22 having capture agents 18 , 20 immobilised on it. This allows the nucleotide sequences 12 , 16 of the binding agents 2 , 4 to bind to the complementary sequences of the capture agents 18 , 20 immobilised on the support 22 . This is shown in FIG. 2 . However, the capture agents 16 , 18 are generally used in excess to ensure that substantially all the binding agent 10 , 14 is bound to the support 22 . Thus, in FIGS. 2 and 3 , one molecule of capture agent 28 is left unoccupied.
The fraction of the binding sites of the binding agents 2 , 4 can then be determined using a conventional back-titration technique. Thus, in FIG. 3 labelled antibodies 24 , 26 are used in a non-competitive technique to mark the presence of occupied binding agents 2 , 4 respectively. As the antibodies 24 , 26 are labelled with markers (not shown) a fraction of the binding sites of the binding agents 2 , 4 can then be determined. This in turn allows the concentration of the analytes in the liquid sample to be found, eg by reference to results obtained using a series of solutions of known analyte concentration.
The assay shown in FIGS. 1 to 3 can be adapted to measure the concentration of any pair of analytes using the same solid support 22 having capture agents 18 , 20 immobilised on it. This can be done by providing binding agent suitable for binding an analyte with an oligonucleotide tail group 12 , 16 so that the binding agents will specifically bind to one of the microspots 18 , 20 . Thus, it is envisaged that the user of the assay will be able to customise his or her binding agent for use with a universal array of microspots.
EXAMPLE
Reagents:
1) Mouse IgG (monoclonal anti-TSH) from the Scottish Antibody Production Unit (SAPU).
2) Rabbit IgG, goat anti-mouse IgG (whole molecule) and goat anti-rabbit IgG (whole molecule) antibodies from Sigma.
3) Sulfate FLUOSPHERES (colored and fluorescent latex microspheres), 0.1 μm diameter, yellow/green fluorescent (ex 490; em 515 nm) and Sulfate FLUOSPHERES (colored and fluorescent latex microspheres), 0.1 μm diameter, red fluorescent (ex 580; em 605 nm) from Molecular Probes.
4) Oligonucleotides from Oswell DNA Service:
a) CACACACACACACACACA (SEQ ID NO: 1) with 5′-biotin modification (poly-CA) b) GTGTGTGTGTGTGTGTGT (SEQ ID NO: 2) with 5′-phosphorothioate modification (poly-GT) c) GAGAGAGAGAGAGAGAGA (SEQ ID NO: 3) with 5′-biotin modification (poly-GA) d) CTCTCTCTCTCTCTCTCT (SEQ ID NO: 4) with 5′-phosphorothioate modification (poly-CT)
5) Sulfo-LC-SPDP {sulfosuccinimidyl 6-[3′-(2-pyridyldithio)-propionamido]hexanoate} from Pierce.
6) PD10 columns and Sephadex G200 from Pharmacia.
7) RIA grade Bovine Serum Albumin (BSA), TWEEN20 (surfactant), sodium azide, di-sodium hydrogen orthophosphate anhydrous, sodium di-hydrogen orthophosphate, EDTA and TRIZMA (agent for stabilizing acid-alkaline balance in liquids) from Sigma.
8) Avidin DX from Vector Laboratories
9) CENTRICON-30 (filtering and concentrating unit) and CENTRIPREP-30 (filtering and concentrating unit) concentrators from Amicon.
10) Thyroid stimulating hormone (TSH) from NIH USA
Adsorption of Anti-Mouse IgG and Anti-Rabbit IgG Antibodies to Sulfate FluoSpheres
1) A 0.5 ml aliquot of 2% (10 mg), 0.1 μm yellow/green FLUOSPHERES (colored and fluorescent latex microspheres) was added to 2 mg of goat anti-mouse IgG antibody dissolved in 0.5 ml 0.1M phosphate buffer, pH7.4. A 0.5 ml aliquot of 2% (10 mg), 0.1 μm red FLUOSPHERES (colored and fluorescent latex microspheres) was added to 2 mg of goat anti-rabbit IgG antibody dissolved in 0.5 ml 0.1M phosphate buffer, pH7.4. Both preparations were shaken overnight at room temperature.
2) The two preparations were centrifuged for 10 min at 8° C. in a MSE High-Spin 21 Ultra-centrifuge.
3) Each pellet was dispersed in 2 ml of 1% BSA in phosphate buffer, shaken for 1 hour at room temperature and centrifuged as above.
4) Each pellet was dispersed in 2 ml of 0.5% TWEEN20 (surfactant) in phosphate buffer, shaken for 30 min at room temperature and centrifuged as above.
5) Each pellet was dispersed in 2 ml of phosphate buffer and centrifuged as above.
6) Each pellet was dispersed in 2 ml of phosphate buffer and centrifuged as above.
7) Each pellet was dispersed in 2 ml of 1% BSA containing 0.1% sodium azide and stored at 4° C.
Conjugation of Mouse Monoclonal IgG and Rabbit IgG to Oligonucleotides
1) 3 mg of sulpho-LC-SPDP was added to 4.6 mg of mouse anti-TSH monoclonal or rabbit IgG dissolved in 1 ml of PBS/EDTA and shaken for 30 min at room temperature.
2) The activated antibodies were separated from unreacted SPDP on PD10 columns. The samples were eluted with PBS/EDTA and 0.5 ml fractions collected.
3) The fractions from the first peak containing the activated antibody were pooled and concentrated using a Centricon-30 concentrator to approximately 10 μl.
4) 100 nM of 5′-phosphorothioate modified poly-GT oligonucleotide was added to 14.8 nM of the activated mouse monoclonal IgG. 58.3 nM of 5′-phosphorothioate modified poly-CT oligonucleotide was added to 8.7 nM of the activated rabbit IgG. Both preparations were made up to 1 ml with PBS/EDTA and shaken overnight at room temperature.
5) The oligonucleotide conjugated mouse and rabbit IgG preparations were separated from unreacted oligonucleotides on a SEPHADEX G200 (chromatographic medium column (1.5 ×45 cm). The samples were eluted with PBS/EDTA and 2 ml fractions collected.
6) The fractions from the first peak containing the oligonucleotide conjugated antibody were pooled and concentrated using a CENTRIPEP-30, (filtering and concentrating unit) concentrator to approximately 500 μg/ml and stored at 4° C.
To Demonstrate that a Mixture of Oligonucleotide-Conjugated Antibodies Would Hybridize Only with Complementary Oligonucleotide Deposited on a Solid-Phase as Microspots
1) Dynatech black MICROFLUOR microtitre wells were coated with 50 μl of avidin-DX in 0.1M bicarbonate buffer, pH 8.5 and at a concentration of 5 μg/ml for 5 min at room temperature.
2) After washing with 0.1M phosphate buffer, the avidin coated microtitre wells were blocked with 200 μl of 1% BSA for 1 hour at room temperature and washed again with the same buffer and dried.
3) A 0.25 μl droplet of each of the two 51-biotin modified poly-CA and poly-GA oligonucleotides in 0.1% BSA and at a concentration of 0.025 nM/ml were deposited on opposite sides of avidin coated microtitre wells and allowed to react for 30 min under a moist atmosphere. The droplets were then aspirated and the microtitre wells washed with phosphate buffer.
4) A 50 μl aliquot of Tris-HCI assay buffer containing 0.25 μg/ml each of the poly-GT-conjugated mouse monoclonal IgG and poly-CT-conjugated rabbit IgG was added to all but the control microtitre wells (50 μl of assay buffer containing unconjugated mouse and rabbit IgG was added to the control wells instead), shaken for 1 hour under a moist atmosphere and washed with phosphate buffer containing 0.05% Tween20.
5) A 200 μl aliquot of Tris-HCI assay buffer containing 0.3 μg/ml goat anti-mouse IgG antibody conjugated yellow-green FLUOSPHERES (colored and fluorescent latex microspheres) and 0.6 μg/ml goat anti-rabbit IgG antibody conjugated red FLUOSPHERES (colored and fluorescent latex microspheres) was added to all microtitre wells, shaken for 1 hour at room temperature, washed with phosphate TWEEN20 (surfactant) buffer and scanned with a confocal laser scanning microscope equipped with an Argon/Krypton laser.
Results Excitation: 488DF10 Emission: 525DF35 Yellow/Green Sample Signal Control 13.3 ± 0.5 Avidin - - - B-Poly-CA - - - Poly-GT-Mouse 100.9 ± 10.9 IgG microspot Avidin - - - B-Poly-GA - - - Poly-CT-Rabbit 16.9 ± 0.3 IgG microspot Excitation: 568DF10 Emission: 585EFLP Sample Red Signal Control 22.0 ± 0.2 Avidin - - - B-Poly-CA - - - Poly-GT-Mouse 24.0 ± 0.4 IgG microspot Avidin - - - B-Poly-GA - - - Poly-CT-Rabbit 99.8 ± 2.7 IgG microspot
Conclusions
(1) The poly-GT oligonucleotide tagged mouse IgG hybridized only with complementary biotinylated poly-CA but not non-complementary biotinylated poly-GA oligonucleotide microspots deposited on the same microtitre well.
(2) The poly-CT oligonucleotide tagged rabbit IgG hybridized only with complementary biotinylated poly-GA but not non-complementary biotinylated poly-CA oligonucleotide microspots deposited on the same microtitre well.
To Demonstrate Antigen Binding of the Oligonucleotide Tagged Antibody Microspots
1) Dynatech black MICROFLUOR microtitre wells were coated with 50 μl of avidin-DX in 0.1M bicarbonate buffer, pH 8.5 and at a concentration of 5 μg/ml for 5 min at room temperature.
2) After washing with 0.01M phosphate buffer, the avidin coated microtitre wells were blocked with 200 μl of 1% BSA for 1 hour at room temperature and washed again with the same buffer and dried.
3) A 0.25 droplet of 5′-biotin modified poly-CA oligonucleotide in 0.1% BSA and at a concentration of 0.025 nM/ml was deposited on each of the avidin coated microtitre wells and allowed to react for 30 min under a moist atmosphere. The droplets were then aspirated and the microtitre wells washed with phosphate buffer.
4) A 50 μl aliquot of Tris-HCI assay buffer containing 0.25 μg/ml of the poly-GT-conjugated anti-TSH mouse monoclonal IgG was added to the microtitre wells, shaken for 1 hour under a moist atmosphere and washed with phosphate buffer containing 0.05% TWEEN20 (surfactant).
5) A 200 μl aliquot of TSH standards in Tris-HCI assay buffer (0, 0.1, 0.3 & 1.0 μU/ml) was added to triplicate wells and incubated for 1 hour at room temperature and washed with phosphate-Tween20 buffer.
6) A 200 μl aliquot of 50 μg/ml anti-TSH developing antibody conjugated yellow/green sulfate FLUOSPHERES (colored and fluorescent latex microspheres) was added to all microtitre wells, shaken for 1 hour at room temperature, washed with phosphate TWEEN20 (surfactant) buffer and scanned with a confocal laser scanning microscope equipped with an Argon/Krypton laser.
RESULTS AND CONCLUSION
The poly-GT oligonucleotide tagged anti-TSH mouse monoclonal IgG was fully functional as demonstrated by the successful generation of a standard curve when it was used as binding antibody deposited on the solid-phase via biotinylated complementary poly-CA oligonucleotide coupled to avidin coated microtitre wells (see FIG. 4 ).
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The present invention discloses methods and kits for the determination of the concentration of one or more analytes in a liquid sample using capture agents immobilised on a solid support and binding agents for binding the analyte(s), the binding agents having tail groups capable of binding to the respective capture agent. Preferably, the capture agents and binding agents are complementary oligonucleotides, and the capture agents are immobilised in the form of microspots. The use of the tail groups and capture agents can allow the binding of the analyte(s) to the binding agent(s) to take place in solution, rather than at a surface, improving the kinetics associated with this process. In addition, the user of the assay can customise any suitable binding agents for use with a universal support, by attaching tail groups them.
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BACKGROUND OF THE INVENTION
The present invention is directed to a support or holder for a portable appliance and in particular for a hand-held electrical hair dryer.
Portable hand-held electrical hair dryers are well known and have gained widespread popularity for both home and professional use in the styling and drying of a person's hair. The hair dryer usually includes a casing having a handle portion and a main housing portion which houses a heater, motor and fan assembly. In use the fan is operated by the motor to draw air into the housing through the heater and then outwardly of the housing through a suitable air discharge orifice.
Although these hair dryers are not large items, they are of a configuration which usually prevents ready storage thereof when not in use. Since the dryer is frequently used it must be readily available to the user and therefore various storage stands or holders have been provided in the past for storing the dryers to accomplish these ends. Further in certain of these stands operation of the dryer is permitted while the dryer is in a stored position so that the user's hands are free for other purposes such as combing or brushing the hair while it is being dried.
In general the prior art holders provide for stands having cradles for receiving the handle or other portion of the hair dryer casing. Although these known stands have proven acceptable for the intended uses, various problems are found in known devices for utilization of the devices both for storing the dryer when not in use yet still maintaining the desirable feature of allowing for operation of the dryer while in the stored position.
It is an object of the present invention to provide a novel holder or support for a portable electrical hair dryer.
Another object is to provide a holder having novel means for maintaining the dryer in stored position and allowing for operation thereof in a plurality of positions in the stored position.
A still further object is to provide a novel holder having novel means for maintaining and locking the hair dryer in stored position which includes means for ready release thereof from the holder.
A further object is to provide a novel holder of relatively few parts thereby allowing for a reduction in manufacturing costs both in labor and material.
SUMMARY OF THE INVENTION
The present invention contemplates a holder for a hair dryer which includes a support member adapted for mounting on a wall surface. An appliance receiving or gripping portion extends from the base of the support and is provided with a grip for receiving and positioning the handle of the dryer. Retractable detent means are provided in the support with actuating means provided for moving the detent means into and out of engagement with the handle to releasably lock and unlock the handle within the gripping portion.
The above and other objects and advantages of the present invention will appear more fully hereinafter from a consideration of the detailed description which follows taken together with the accompanying drawing wherein one embodiment of the invention is illustrated.
DESCRIPTION OF THE DRAWINGS
In the drawing:
FIG. 1 is a perspective view of a support member incorporating one embodiment of the present invention and illustrates a hair dryer appliance mounted therein;
FIG. 2 is a front elevational view of the support of FIG. 1 and shows the support inverted from the position of FIG. 1;
FIG. 3 is a sectional view taken on the line 3--3 of FIG. 2;
FIG. 4 is a sectional view taken on the line 4--4 of FIG. 4; and
FIG. 5 is a rear elevational view of the support.
DETAILED DESCRIPTION
Referring now to the drawing for a more detailed description of the present invention a holder incorporating one embodiment thereof is generally indicated by the reference numeral 10 in FIG. 1.
A hair dryer 12 is shown in broken line outline form in FIG. 1 and is provided with a handle portion 14 disposed within a tubular shaped receiving or grip portion 15 of holder 10. Hair dryer 12 may be of a usual type which includes within the casing a motor, fan and heater assembly for discharging heated air through discharge orifice 16 when the hair dryer is connected to a suitable electrical outlet via connecting cord 17.
Holder 10 is made of premolded plastic material and includes a rectangular shaped base 19 from which projects a hollow extension portion 20. Grip portion 15 of holder 10 is formed at one end of extension 20 and comprises a pair of arcuate shaped arms 22 and 24 conforming to the outer cylindrical surface of handle 14 of hair dryer 12. An opening or slot 25 is provided in grip portion 15 between the ends of arms 22 and 24 to permit passage therebetween of power connecting cord 17 when dryer 12 is removed or deposited in gripping portion 15.
Upper and lower metal wall mounting plates 26 and 27 are secured to the rear of base 19 by means of screws 28 fitted into threaded bosses (not shown) formed in base 19. A plurality of keyhole shaped openings 30 are formed in plates 26 and 27 for permitting the mounting of holder 10 to a wall surface either in a vertical (FIG. 2) or horizontal position in accordance with the needs of the user.
As mentioned it is a feature of the present invention to provide novel means for maintaining hair dryer 12 in holder 10. To this end a rectangular slide plate 31 is disposed within extension 20 with the spaced side marginal portions 32 and 33 thereof disposed in spaced guide channels 34-35 provided on the inner wall surface of extension 20. A pair of detent arms 36 and 37 (FIGS. 3 and 4) depend from the end of plate 31 and project through openings 38 and 39 in the walls of gripping portion 15. Resilient detenting pads 40 are secured to the ends of detent arms 36 and 37 to engage the surface of handle 14 of hair dryer 12 to frictionally detent handle 14 within grip portion 15.
Actuating means for moving plate 31 and detent arms 36 and 37 out of engagement with handle 14 include an actuating button 42 rotatably mounted on wall 43 of extension 20 by means of a peripheral recess 44 seated on the surface of wall 43 about opening 45 therein. A drive shaft 46 located eccentrically on button 42 depends therefrom through opening 45 into driving engagement in opening 47 of slide plate 31.
In use of holder 10 with holder 10 mounted on a wall surface and with detent arms 36 and 37 in the retracted position shown in FIG. 4, handle 14 of hair dryer 12 is placed in grip position 15 after first passing electrical connecting cord 17 through slot 25. The handle 14 may then be rotated to any desired position in grip 15 to present the heated air orifice 16 of hair dryer 12 at a desired angle by the user.
The user then rotates button 42 to move slide plate 31 in the direction of arrow A in FIG. 4 through drive shaft 46. Plate 31 is moved in guide channels 34-35 together with detent arms 36 and 37 to place pads 40 in detenting frictional engagement with handle 14 locking the latter to holder 10. If desired hair dryer 12 may then be operated through a suitable electrical power connection through cord 17 in mounted position in holder 10. To release handle 14 from grip 15 button 42 is rotated in an opposite direction thereby releasing detent pads 40 from handle 14 whereby hair dryer 10 may be withdrawn from holder 10.
It will be apparent from the foregoing description that the novel holder has many advantages in use. One advantage among others is the fact that the holder may be mounted in varied positions on a wall and the air discharge outlet of the dryer set at a desired angle for operation while in mounted position in gripping portion 15 by rotation of handle 14 and then locking the handle at the desired angular position by means of the described detent means.
Although one embodiment of the present invention has been illustrated and described in detail, it is to be expressly understood that the invention is not limited thereto. Various changes can be made in the design and arrangement of parts without departing from the spirit and scope of the invention as the same will now be understood by those skilled in the art.
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A storage or holder device for an electrical appliance such as a hair dryer adapted for mounting on a wall surface and having an appliance gripping portion for receiving the handle of the appliance and further including selectively releasably detenting means within said holder and operable externally thereof for locking the appliance to the holder.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
Not Applicable
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
Not Applicable
BACKGROUND OF THE INVENTION
This invention relates to construction of cementitious structures. In particular, the invention relates to a system and method for using inserts and a coating for architecturally finishing seams between roof panels of cementitious materials.
Cementitious roof panels, specifically Autoclaved Aerated Concrete (“AAC”) roof panels, have been used for many years. There are many advantages of cementitious roof panels: durability, no rot nor decay, and strength. AAC roof panels additionally have insulation value due to their mass and the fact that they are aerated.
Applying a thin coating over AAC roof panels to weatherproof the roof has disadvantages. A primary disadvantage is that it is aesthetically undesirable because panel seam joints are difficult to repair. Moreover, even if the panel seam joints are repaired, the resulting large, smooth monotonous roof surface is unbecoming.
In the background art, these problems of using AAC roof panels have been solved by using expensive secondary roofing materials to weatherproof the roof. Normally, a pressure treated furring strip board is attached to AAC roof panels and then plywood sheets are nailed to the furring strips. A weatherproof asphalt paper is then stapled over the wood decking. Finally, a finished roofing system, such as asphalt shingles, etc. is installed. This approach to weatherproofing ACC roofs is accomplished at greater expense and labor than is necessary to weatherproof conventional wood roofs. Additionally, the asphalt shingles and other materials need to be replaced after about fifteen years so there is great amount of pollution in landfills, etc. There is a strong need for an environmentally friendly, permanent roof system.
It is usually cost prohibitive to add more expensive types of roofing, e.g., standing seam steel roofing, to an AAC roof. Moreover, standing seam steel roofs have an enormous amount of embodied energy and use valuable steel that would be better used for other purposes.
The finishing of the interior surface of AAC roof panels requires that sheetrock or thick plaster be applied in order to produce an architecturally acceptable interior finish. The panels are normally installed horizontally, spanning from one interior load-bearing wall to another. The (first) lowest panel is placed initially and secured and then the subsequent panels are installed by resting them on the first panel. The panels are normally not installed vertically (from fascia to ridge line) due to the butt ends not having a place to rest, and the difficulty of aligning the butt ends to produce a uniform (flush) exposed edge. Therefore the background art's added labor and materials required to construct a habitat employing AAC roof panels were excessive to extent the inherit advantages of ACC could not be appreciated.
For the reasons presented above, background art cementitious roof panel systems have been covered with conventional roofing materials at great additional labor, waste of materials and cost. The applicant's disclosures of roof coating, gravity fed gutters and panel fascia have provided an environmentally-friendly and cost-effective weather proofing system. There is a very strong need for environmentally-friendly roofing materials for AAC structures that exhibit a low quantity of embodied energy that are aesthetically attractive so consumers will be motivated to purchase them.
There is a very strong need for manufacturing and construction processes wherein all the inherent advantages of AAC roof panels can be economically actualized. The optimum solution is for a simplified and economical field installation of a superior product that also would be architecturally appealing.
The background art is characterized by U.S. Pat. Nos. 7,104,020; and 7,204,060 and by U.S. Patent Application Nos. 2001/0045070; 2002/0078659; 2002/0174606; 2006/0003144; and 2007/0056223; the disclosures of which patents and published patent applications are incorporated by reference as if fully set forth herein. In the background art, AAC roof panels are installed horizontally to avoid the problems inherent in installing cementitious roof panels vertically. Background art structures that incorporated vertical roof panels are simple single ridge roofs. There are no examples of economically-viable, vertically-installed, cementitious roof panels on a roof with multiple hips and valleys. Background art AAC roof systems lack the architectural, aesthetic advantages of other roofing systems. Also the smooth roofs have problems of mortar in seams creating additional work to eliminate noticeable surface irregularities. Standing seam steel roofs have an enormous amount of embodied energy and use valuable steel that would be better used for other purposes.
BRIEF SUMMARY OF THE INVENTION
The purpose of preferred embodiments of the invention is to provide a coating and/or an insert that simulates standing seam for a cementitious roof. One advantage of preferred embodiments of the invention is that the use of the insert makes finishing the roof easier. Another advantage of preferred embodiments of the invention is that is a more aesthetically pleasing roof is produced. One object of preferred embodiments of the invention is to provide a cementitious roof system that emulates a standing seam steel roof. In a preferred embodiment, the invention is incorporated into structures disclosed by the applicant in U.S. Pat. No. 7,204,060 and by U.S. Patent Application Publication Nos. 2002/0078659; 2002/0174606; 2007/0056223; the disclosures of which patents and published patent applications are incorporated by reference as if fully set forth herein.
In a preferred embodiment, the invention is a manufacturing process and construction methodology that produces a finished roof that economically actualizes all the inherit advantages of AAC roof panels in an architecturally appealing design. This embodiment, in combination with the teachings of the applicant's other patent applications enables AAC roof panels to be installed vertically. By installing a simple insert into the seams between the panels alleviates and remedies the problem of unsightly seams and transforms them to be architectural advantageous and aesthetically appealing simulated standing seams.
In the background art, AAC roof panels are normally installed horizontally, spanning from interior load bearing wall to load bearing wall. The first (lower) panel is placed and secured and then the subsequent panels are installed by resting them on the first panel. The panels are normally not installed vertically (with their seams in a plane that is perpendicular to the exterior walls) due to the butt ends not having a place to rest, the difficulty of aligning the ends for an exposed uniform flush end. Therefore, in the background art, the additional labor and materials required to construct a habitat employing AAC roof panels were excessive to extent that the inherit advantages of ACC could not be appreciated.
In a preferred embodiment, the invention is a complimentary architectural component that is vertically aligned and inserted into joints between cementitious roof panels or cementitious wall panels. This embodiment concerns making a cementitious roof look like a standing seam steel roof by inserting protruding pieces in the roof panel joints that run from the fascia to the ridge, preferably on two-foot centers. The inserts render the joints between the cementitious panels easier to finish as well as producing a superior but less expensive and more environmentally friendly roof system that appears to be a very expensive standing seam steel roof that wastes the Earth's resources.
Using the disclosed inserts with the disclosed coatings, allows for a coating to be applied without labor intensive and costly joint finishing. Without the disclosed inserts being installed in the seams, each joint would have to be sanded smooth so that no imperfections would show through the thin roof coating. Moreover, without the use of the disclosed inserts an ugly and boring roof profile is produced.
In another preferred embodiment, the invention is a coating for the exposed surfaces of cementitious roof panels and associated seam inserts. Preferably, the coating is a combination of two primary components: a powder (A) and a water-based liquid (B). The primary components are preferably mixed together at a strict weight ratio of 60 percent A and 40 percent B. The combination is a water-based liquid roof weatherproofing material that is vapor permeable. It may be tinted various colors, may be applied in a single coat, and is capable of adhering granules to the surface being coated. The roofing disclosed herein is water based, environmentally friendly and never has to be removed as do asphalt shingles, etc. Instead of replacing this roofing material, one simply has to apply a new coating of the disclosed coating material.
In this preferred embodiment, a batch of the coating combination is made by combining about 55 pounds of powder A with about 22 pounds of liquid B. Powder A is preferably comprised of Portland cement in the range of about 40 percent to about 60 percent by weight and a crystalline quartz silica in the range of about 40 percent to about 60 percent by weight. The liquid is preferably comprised of an acrylic polymer dispersion. Preferably, the acrylic polymer dispersion constitutes 100 percent of the liquid. For example, the acrylic polymer dispersion is preferably Levelite Bonding Primary made by Elite of Atlanta, Ga. In a preferred embodiment, after the coating is applied, granules are added to the surface to protect it from ultraviolet (UV) rays, etc.
In a preferred embodiment, the invention is a method for installing a roofing system on a structure, said method comprising: installing a plurality of cementitious roof panels adjacent to one another to produce a roof surface having a plurality of substantially vertical oriented seams; placing a cementitious seam insert in each seam and attaching each said seam insert to the adjacent cementitious roof panels; and coating said cementitious roof panels and said cementitious seam inserts with a coating. Preferably, said plurality of cementitious roof panels comprises two autoclaved aerated roof panels. Preferably, each said seam insert comprises a body that comprises a rigid cementitious board. Preferably, each said seam insert further comprises shoulders that are fixed to said body. Preferably, said shoulders are provided with channels adjacent to their connections to said body. Preferably, said body has a plurality of transverse holes. Preferably, the structure has a ridgeline and an eave or integrated gutter system said substantially vertical seams and said seam inserts run from adjacent to said ridgeline to adjacent said eave or integrated gutter system, thereby producing a roof that requires no further finishing and resembles a standing seam steel roof. Preferably, the method further comprises: cutting a groove or slot in each panel; and installing a seam insert in each groove or slot; thereby creating a standing seam look. Preferably, the method further comprises: cutting or forming an integrated gutter system into said cementitious roof panels. Preferably, the method further comprises: cutting or notching an integrated gutter system into said seam inserts.
In another preferred embodiment, the invention is a system for installing (or manufacturing and installing) a roofing system on a structure, said system comprising: means for installing a plurality of cementitious roof panels adjacent to one another to produce a roof surface having a plurality of substantially vertical oriented seams (e.g., the equipment required to manufacture, lift and place the panels, such as mixers, molds, cranes, forklifts, etc.); means for placing a cementitious seam insert in each seam and attaching each said seam insert to the adjacent cementitious roof panels (e.g., the equipment required to manufacture, lift, place and attach the seam inserts, such as mixers, molds, presses, cranes, forklifts, mortar, etc.); and means for coating said cementitious roof panels and said cementitious seam inserts with a coating (e.g., the equipment required to manufacture and apply the coating, such as mixers, brushes, trowels, etc.). Preferably, said plurality of cementitious roof panels comprises two autoclaved aerated roof panels. Preferably, each said seam insert comprises a body that comprises a rigid cementitious board. Preferably, each said seam insert further comprises shoulders that are fixed to said body. Preferably, said shoulders are provided with channels adjacent to their connections to said body. Preferably, said body has a plurality of transverse holes. Preferably, the structure has a ridgeline and an eave or integrated gutter system said substantially vertical seams and said seam inserts run from adjacent to said ridgeline to adjacent said eave or integrated gutter system, thereby producing a roof that requires no further finishing and resembles a standing seam steel roof. Preferably, the system further comprises: means for cutting a groove or slot in each panel (e.g., conventional cutting equipment for cementitious materials, such as saws, etc.); and means for installing a seam insert in each groove or slot (e.g., the equipment required to manufacture, lift, place and attach the seam insert, such as mixers, molds, presses, cranes, forklifts, mortar, etc.); thereby creating a standing seam look. Preferably, the system of further comprises: means for cutting or forming an integrated gutter system into said cementitious roof panels (e.g., convention equipment for cutting and sealing AAC, such as saws, coatings, brushes, etc.). Preferably, the system further comprises: means for cutting or notching an integrated gutter system into said seam inserts (e.g., convention equipment for cutting and sealing cementitious material, such as saws. etc.).
In another preferred embodiment, the invention is a roofing system for a structure having a ridgeline and an eave, said roofing system comprising: a plurality of cementitious roof panels that are installed substantially adjacent to one another and extend from the ridgeline to the eave to produce a surface having a plurality of substantially vertical oriented seams; a plurality of cementitious seam inserts, each cementitious seam insert having a first portion that is situated within each seam and that is attached to the adjacent cementitious roof panels and a second portion that protrudes from said surface; and a coating that is applied to said surface of said cementitious roof panels and to said second portion of said cementitious seam inserts.
In another preferred embodiment, the invention is a roofing system comprising: a plurality of cementitious roof panels having exposed surfaces that are separated by a plurality of substantially vertical oriented seams; a plurality of cementitious seam inserts, each cementitious seam insert having a first portion that is attached to the adjacent cementitious roof panels and a second portion that protrudes from said surface; and a coating that is applied to said exposed surfaces of said cementitious roof panels and to said second portion of said cementitious seam inserts. Preferably, said coating comprises a combination of two primary components: a powder and a water-based liquid. Preferably, said primary components have a weight ratio of about 60 percent powder and about 40 percent water-based liquid. Preferably, said powder is comprised of Portland cement in the range of about 40 percent to about 60 percent by weight and a crystalline quartz silica in the range of about 40 percent to about 60 percent by weight and said liquid is an acrylic polymer dispersion.
In another embodiment, the invention is a roofing system or a structure having a roof system produced according to a method disclosed herein. In another embodiment, the invention is a method for installing a roofing system on a structure, said method comprising: a step for installing a plurality of cementitious roof panels adjacent to one another to produce a roof surface having a plurality of substantially vertical oriented seams; a step for placing a cementitious seam insert in each seam and attaching each said seam insert to the adjacent cementitious roof panels; and a step coating said cementitious roof panels and said cementitious seam inserts with a coating; wherein said plurality of cementitious roof panels comprises two autoclaved aerated roof panels; wherein each said seam insert comprises a body that comprises a rigid cementitious board; wherein each said seam insert further comprises shoulders that are fixed to said body; wherein said shoulders are provided with channels adjacent to their connections to said body; wherein said body has a plurality of transverse holes; and wherein the structure has a ridgeline and an eave or integrated gutter system said substantially vertical seams and said seam inserts run from adjacent to said ridgeline to adjacent said eave or integrated gutter system, thereby producing a roof that requires no further finishing and resembles a standing seam steel roof.
Further aspects of the invention will become apparent from consideration of the drawings and the ensuing description of preferred embodiments of the invention. A person skilled in the art will realize that other embodiments of the invention are possible and that the details of the invention can be modified in a number of respects, all without departing from the concept. Thus, the following drawings and description are to be regarded as illustrative in nature and not restrictive.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The features of the invention will be better understood by reference to the accompanying drawings which illustrate presently preferred embodiments of the invention. In the drawings:
FIG. 1 is a perspective view of a preferred embodiment of a standing seam AAC roof.
FIG. 2 is an elevation view of a preferred embodiment of a standing seam AAC roof.
FIG. 3A is a perspective view of a first embodiment of the seam insert of a preferred embodiment of the invention. The seam inset is shown inserted into a seam between two AAC roof panels. The near roof panel is not shown for clarity.
FIG. 3B is a perspective view of second embodiment of the seam insert of a preferred embodiment of the invention. The seam inset is shown inserted into a seam between two AAC roof panels. The near roof panel is not shown for clarity.
FIG. 4 is a perspective view of the embodiment of the seam insert of FIG. 3B showing the channels in the shoulders of the embodiment.
FIG. 5 presents a cross section view of installed roof panels with seam inserts installed in seams and in a slot cut into the middle roof panel. In this embodiment, the roof panels and seam inserts are coated with a coating material.
FIG. 6 is a perspective view of the standing seam roof in accordance with a preferred embodiment of the invention. In this embodiment, the roof has hips and valleys.
The following reference numerals are used to indicate the parts and environment of the invention on the drawings:
10 standing seam AAC roof 12 seam inserts, inserts 14 AAC roof panels, roof panels 16 integrated gutter system, integrated gutter 18 fascia water deflection system, fascia 20 holes 22 mortar 24 panel seam 25 body 26 shoulders, transverse shoulders 28 channel 30 coating, coating material, roofing coating material 32 slot 34 first portion 36 second portion
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1 , a preferred embodiment of standing seam AAC roof 10 is presented. In this embodiment, one of a plurality of seam inserts 12 is mortared into the seam between each pair of ACC roof panels 14 . Preferably, each of the seam inserts 12 is comprised of body 25 comprising a rigid cementitious board.
Referring to FIG. 2 , an elevation view of standing seam AAC roof 10 of FIG. 1 is presented. In this embodiment, each seam insert 12 terminates above integrated gutter 16 and fascia 18 . Thus, this embodiment incorporates the integrated, gravity-fed gutter system and the fascia water deflection system disclosed at column 20, lines 39-57 of U.S. Pat. No. 7,204,060. The integrated gutter system and the fascia water deflection system are also disclosed in FIGS. 1, 2A, 2B, 2C, and 2D of U.S. patent application Ser. No. 11/123,635, the disclosure of which patent application is incorporated by reference as if fully set forth herein. In an alternative embodiment, the integrated gutter system is cut or formed into roof panels 14 before or after they are installed. In another alternative embodiment, the integrated gutter system is cut or formed into seam inserts 12 before or after they are formed. In this embodiment, a notch is provided in each seam insert 12 through which the gutter passes.
Referring to FIGS. 3A and 3B , a first (simple) embodiment and a second (complex) embodiment of one of the seam inserts 12 are illustrated. In both of these embodiments, seam inserts 12 are preferably comprised of body 25 that is made of a cementitious material. Holes 20 in tower vertical half of the body 25 of each of the inserts 12 are preferably provided to allow the mortar 22 in each panel seam 24 to embed each of the inserts 12 into the panel seam 24 and lock it into place. Preferably, after inserts 12 are installed and mortar 22 has set, coating 30 is applied to the exposed surfaces of installed roof panels 14 and inserts 12 .
Referring to FIG. 4 , transverse shoulders 26 are shown extending from the sides of the body 25 of each of the inserts 12 . The presence of shoulders 26 enable workers to easily maintain a consistent height at which each of the inserts 12 protrudes out of each panel seam 24 . Shoulders 26 are preferably provided with recessed channel 28 that locks roofing coating material 30 into the channels 28 when roofing coating material 30 cures. Channels 28 also provide an anchor area for the coating as it extends over the top of each of the seam inserts 12 . It is preferred that coating 30 completely cover and coat the inserts 12 as well as the panels 14 because weathering is expected to prevent the inserts 12 from color matching the coating 30 over time.
Referring to FIG. 5 , a cross section view of installed roof panels 14 with seam inserts 12 installed in seams 24 and in slot 32 that is cut down the middle roof panel. In this embodiment, roof panels 14 and seam inserts 12 are coated with coating material 30 . With panels 14 aligned in parallel, when mortar 22 is applied, inserts 12 make a clean joint that requires no other finishing work before coating material 30 is applied.
In an alternative embodiment (not shown), each of the seam inserts 12 is provided with shoulders 26 and a second portion 36 , but is not provided with a first portion 36 . In this embodiment, inserts 12 have the shape of an inverted capital T. In this embodiment, inserts 12 are attached to the exposed surface of panels 14 over seams 24 with an adhesive or with mortar before being coating with coating 30 .
Referring to FIG. 6 , a perspective view of a structure with a standing seam roof 10 is presented. In this embodiment, roof 10 has hips and valleys. In this embodiment, a simple cementitious board insert 12 is inserted into seams 24 and then roof coating 30 is applied to all materials (panels 14 and inserts 12 ) simultaneously. In this way, a roof system is produced that hides joints with no other finishing. The seam inserts can be coated with the roof at same time as the roof panels, producing one constant seamless roof coating system. Preferred embodiments of the invention produce a roof that has inserts in the vertically-oriented gaps or seams between roof panels, the gaps or seams being located in planes that are oriented substantially perpendicular to the outside walls of the structure.
Many variations of the invention will occur to those skilled in the art. Some variations include a simple insert. Other variations call for a complex insert. All such variations are intended to be within the scope and spirit of the invention.
Although some embodiments are shown to include certain features, the applicant specifically contemplates that any feature disclosed herein may be used together or in combination with any other feature on any embodiment of the invention. It is also contemplated that any feature may be specifically excluded from any embodiment of the invention.
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A system and method for installing a roofing system on a structure, said system comprising: means for installing a plurality of cementitious roof panels adjacent to one another to produce a roof surface having a plurality of substantially vertical oriented seams; means for placing a cementitious seam insert in each seam and attaching each said seam insert to the adjacent cementitious roof panels; and means for coating said cementitious roof panels and said cementitious seam inserts with a coating.
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TECHNICAL FIELD
This invention relates generally to sewing machines, and, more specifically, to sewing machines having apparatus to ensure a seam is sewn having a correct width.
BACKGROUND
Sewing machines wherein the instant invention finds exemplary application include industrial sewing machines used to form edge seams. Such machines may incorporate a feedback sensor to ensure proper positioning of material being sewn. A light-based sensor arrangement used in certain commercial sewing machines has a light sensor that is positionable to track a location of an edge of material while the material is being sewn. The sensor can be adjusted to trigger when the sewn seam becomes too wide, occluding the sensor beam. When such a condition occurs, the sensor triggers to turn off the sewing machine. Unfortunately, however, the momentum of the sewing machine causes additional stitches to be sewn in the material before the needle can be brought to a halt. Consequently, from about one to perhaps several inches of noncompliant seam will be sewn as the machine slows down. Generally, the noncompliant portion of the seam must, at a minimum, be picked apart for re-stitching at a correct width. The entire seam may need to be undone, and the seam started from a beginning, for aesthetic or other reasons. In some cases, the noncompliant seam may ruin the article in which the seam is being sewn, causing the article to be scrapped.
Certain available sewing machines have an edge guide to space a sewing machine needle from a material's sewn edge. Such guides are adjustable mechanically, for example, by turning a threaded shaft, but such adjustment is limited to an initial set-up for seam size. A seam may be sewn by an operator with such a machine by pressing material into engagement with the guide surface simultaneously with pushing slightly in a direction to feed material into the machine needle. No adjustability in guide location is contemplated when a seam is being sewn.
SUMMARY OF THE INVENTION
The invention provides a device automatically to adjust a seam size while sewing the seam in a sewing machine. The invention can be embodied as a clamping foot for a sewing machine. The clamping foot includes an inside foot adapted for attachment to the sewing machine, and an outside foot suspended in transversely adjustable relation from the inside foot. A biasing element is typically arranged to bias the outside foot in an outside direction from the inside foot. The clamping foot may be used in combination with an edge guide operable to assist in feeding material into sewing engagement with a sewing machine on which the clamping foot is attached. Usually, a transducer is affixed between the sewing machine and the edge guide. The transducer transversely displaces the edge guide to control a seam size. A sensor is positioned to validate a seam size and provide a signal in a feedback loop to control the transducer. A stop mechanism may be used to limit a maximum transverse displacement of the outside foot in an inside direction.
These features, advantages, and alternative aspects of the present invention will be apparent to those skilled in the art from a consideration of the following detailed description taken in combination with the accompanying drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
In the drawings, which illustrate what is currently considered to be the best mode for carrying out the invention:
FIG. 1 is a front and side view in perspective, from an above and outside position, of an embodiment according to the invention.
FIG. 2 is a front and side view in perspective, from an above and inside position, of a portion of the embodiment of FIG. 1 .
FIG. 3 is a perspective view, from a below and inside position, of the embodiment of FIG. 2 .
FIG. 4 is a rear and side view in perspective, from a below and inside position, of the embodiment of FIG. 2 .
FIG. 5 is a close-up front and side view in perspective, from an above and outside position, of a portion of the embodiment in FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made to the drawings in which the various elements of the invention will be given numerical designations and in which the invention will be discussed so as to enable one skilled in the art to make and use the invention. It is to be understood that the following description is only exemplary of the principles of the present invention, and should not be viewed as narrowing the claims which follow.
The invention relates to sewing seams in material. The invention will typically be described from the reference point of material being sewn. That is, directions are described from the material's perspective. An outside direction may be characterized by a vector pointing from the material toward an edge, typically the edge being sewn. Similarly, an inside direction may be characterized by a vector oppositely directed from an outside direction. Outboard, or outside, are typically used as relative locations and may indicate being located away from the material, or simply more toward such location than a reference location. A seam size is defined as the distance from a closest edge of the material to the stitches forming the seam.
The principal working components of a currently preferred embodiment of the invention, generally indicated at 10 , are illustrated in FIG. 1 . The seam adjustment device 10 includes an edge guide 102 , a sensor, generally indicated at 110 , and a displacement transducer, generally indicated at 120 . A seam adjuster 10 also desirably includes an outside foot, generally indicated at 125 , adapted to accommodate a transverse displacement. Certain of these components can conveniently be carried on a slide plate 127 for installation on a commercial sewing machine.
Edge guide 102 can function as a brace element against which material to be sewn is placed by a sewing machine operator. Typically, a small amount of outwardly directed pressure is exerted by the operator on the material to maintain the material against the edge guide 102 . As the material is sewn, the seamed edge passes past sensor 110 which validates the correct seam size. Edge guide 102 may be transversely located to position the guide surface a desired distance transverse and outboard to a sewing needle and at the correct distance to form a desired seam size. The edge guide 102 is configured and arranged for its position, relative to a sewing needle, to be adjusted by transducer 120 . Automated adjustment of a position of the edge guide 102 is controlled by a feedback loop based upon seam size.
Illustrated sensor 110 includes light-based sending unit 130 and a light receiving unit 133 . As illustrated, light carried by pipe 135 passes through sending unit 130 , is scattered, refracted, and reflected, with a portion being subsequently received by receiving unit 133 . The return signal from unit 133 is carried by light pipe 137 and is used to operate switch 139 .
When the sewn edge is in compliance for size, switch 139 is typically in an open configuration. When the seam goes out of compliance, because sensor 110 indicates the seam is too wide, switch 139 closes, and sends an adjustment signal through cable 142 to adjust the seam width. Cable 142 may carry the adjustment signal to a power supply 145 to boost the signal subsequently sent to a control switch, generally indicated at 149 . However, the boost from a power supply 145 may not be required in certain embodiments of a seam adjuster 10 . In the latter case, the signal may be sent from switch 139 directly to operate a transducer to adjust seam size.
As illustrated in FIG. 1, the boosted signal is transmitted from power supply 145 through cable 152 to operate valve 155 . When valve 155 is opened, a fluid is permitted to flow through line 157 and operate displacement transducer 120 . Fluid is typically supplied from a fluid source 161 and brought to a convenient location on, or near, a sewing machine through supply line 163 . A currently preferred fluid is compressed air, although hydraulic fluids are also operable. The illustrated displacement transducer 120 is an air driven piston 170 . The invention is not limited to use of such piston type displacement transducers. Alternative transducers within contemplation to adjust a position of edge guide 102 nonexclusively include individually or in combination: linear motors, rack and gear linkages, single and multibar linkages, cams, cams and followers, DC motors, stepper motors, and any other workable arrangement to convert some form of energy into a transverse displacement of the edge guide 102 .
FIGS. 2-5 illustrate certain operational details of the invention. A stationary clamping foot 175 of a commercially available sewing machine is modified to have an independent inside foot 177 and an outside foot 179 . In accordance with conventional sewing machines, stationary foot 175 operates to hold the material being sewn in clamped engagement with the slide plate 127 . Walking foot 183 , in combination with a feed mechanism located under the material (not shown), operates to feed material past needle 185 for stitching.
With reference now to FIG. 4, outside foot 179 desirably is adapted for transverse displacement toward and away from needle 185 . One way to accommodate such transverse motion is achieved by suspending outside foot 179 from inside foot 177 with a suspension mechanism, generally indicated at 189 . Alternatively, an outside foot 179 may be suspended from other portions of a sewing machine. As illustrated, suspension mechanism 189 includes a rail 193 which is arranged in sliding capture through inside foot 177 . Rail 193 can be adapted, as illustrated, to form a forward protruding lever portion to assist in positioning an outside foot 179 . Other conformations of suspension systems are within contemplation, nonexclusively including sliding journalled elements, dovetail joints, pivoting rods, and multibar linkages.
One or more biasing elements, such as spring 195 , are typically included to bias outside foot 179 in an outboard direction. Outside foot 179 may then be placed into engagement with surface 196 of edge guide 102 when adjusting a sewing machine to sew a given seam size. However, outside foot 179 does not necessarily have to be in engagement with surface 196 for the invention to be operable. Outside foot 179 functions to maintain material in a substantially flat orientation between edge guide 102 and a needle 185 . A transverse displacement of edge guide 102 therefore moves the material by a corresponding amount to adjust a seam size. It is within contemplation for outside foot 179 to be replaceable with alternative outside feet which are either wider or more narrow than illustrated. Wide feet 179 may be more appropriate when sewing wide seams, and narrow feet 179 may be more appropriate when sewing narrow seams.
A stop mechanism, such as screw 197 , may be arranged to limit a transverse displacement of outside foot 179 in an inside direction. As illustrated, end 199 of screw 197 is spaced apart from inside surface 201 of outside foot 179 . Stop mechanism 197 desirably is adjustable to provide a range in maximum inward displacement values for outside foot 179 .
FIG. 5 illustrates certain distance relationships in one embodiment of the invention. When setting up a sewing machine to sew a seam, edge guide 102 is positioned at a distance D 1 from a centerline of needle 185 . D 1 therefore corresponds to the seam size. Outside foot 179 has a width D 2 , leaving a space between it and walking foot 183 indicated by D 3 . Stop 197 is set to limit displacement of outside foot 179 , by a distance less than D 3 , to prevent contact between outside foot 179 and walking foot 183 . Typically, stop 197 is set to limit an inward displacement of edge guide 102 to a minimum value determined to be sufficient to make a seam size correction, “steering” the material back into seam size compliance. Such “steering” displacement is typically less than the distance indicated by D 3 . Factors affecting a steering displacement include the material type, thickness, weight, and texture. A steering displacement may be generally set at a certain percentage of a seam size. A steering displacement may also be determined by a maximum amount of travel permitted by the displacement stroke of an edge guide 102 . A transducer 120 may be provided having an adjustable stroke, or a stop mechanism may be set to operate on the edge guide 102 directly.
The position of a sensor 110 is desirably adjustable to locate the sensing zone 205 at a distance transverse to a sewing machine needle 185 corresponding to the desired seam size. As with the edge guide 102 , a component's position may be maintained by tightening bolts 207 or 209 subsequent to moving the component into its desired position. A position may be measured relative to a sewing needle 185 by use of a tape measure, or other measuring device. It is also within contemplation for a vernier scale to be incorporated into a slide plate 127 to assist in adjusting a sewing machine for a desired seam size. Other calibrated mechanisms to adjust an edge guide or sensor 110 to a position may include rotating dials or mechanisms adapted to provide audible or mechanical feedback (e.g., “click”) at discrete intervals.
It is preferable for the sensing zone 205 of a sensor 110 to be positioned in stitched proximity and fairly close to the needle 185 . That is, the sensor 110 is usually positioned to observe (for feedback) a portion of material in which a seam has just been stitched. A close location to the needle 185 provides feedback of seam size in time to effect a correction in such size before creating scrap, or requiring shutdown of the sewing machine.
It is within contemplation to use alternative sensor arrangements, other than illustrated in the figures, for seam size feedback. For example, a single light-based sensor may be self-contained to provide both sending and receiving functions. Other alternative sensors within contemplation include capacitive sensors, direct displacement transducers, other laser or LED-based sensors, sensing arrays, or any other sensor capable of indicating the location of an edge of sewn material. A pair of sensors may be used in harmony, with one sensor observing the stitches, and another simultaneously observing the finished edge to create a pair of signals having information with which a seam size may be calculated, and the information used in a feedback loop. A proportional control and feedback also can be employed to operate the invention. In such a case, larger displacement is applied in correspondence with an increased error in seam size.
While the invention has been described in particular with reference to certain illustrated embodiments, such is not intended to limit the scope of the invention. The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiments are to be considered in all respects only as illustrative and not restrictive. The scope of the invention is, therefore, indicated by the appended claims rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
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An improved sewing machine is disclosed for making consistent edge seams. The improvement automatically adjusts a width of a sewn seam based upon feedback from a sensor which detects a position of a sewn edge. Feedback from the sensor causes a transverse adjustment in the position of an edge guide. An outside foot of the sewing machine may be suspended on a biased linkage to permit its transverse displacement when making an adjustment to a seam width.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This patent application is a Continuation application of U.S. patent application Ser. No. 14/651,809 filed on Jun. 12, 2015, which claims priority to the International Application No. PCT/EP2013/076547 filed on Dec. 13, 2013 and claims benefit of European Patent Application Serial No. 12197192.3, filed on Dec. 14, 2012, the contents of which are incorporated by reference herein in their entirety.
TECHNICAL FIELD OF THE INVENTION
[0002] The present invention relates to the field of drugs for regenerative treatments, in particular for regeneration of muscle cells and mitigation of programmed cell death in human cells of various origins.
INCORPORATION-BY-REFERENCE OF MATERIALS FILED ON COMPACT DISC
[0003] The present application includes a Sequence Listing which has been submitted in ASCII format via EFS-Web and is hereby incorporated by reference in its entirety. Said ASCII copy, created on Dec. 13, 2013 is named SONN1037CON_SeqList and is 2 kilobytes in size.
BACKGROUND OF THE INVENTION
[0004] Predominant diseases characterized by a lack of regeneration of cells or deregulated apoptosis are sarcopenia and cachexia. The etiology of sarcopenia is multifactorial but still poorly understood while the sequelae of this phenomenon, i.e. loss of independence and metabolic complications, represent a major public health problem. The most evident metabolic explanation for muscle decline in elderly people is an imbalance between protein synthesis and breakdown rates but other causes like disproportionately increased rate of programmed cell death (apoptosis), neurodegenerative processes, reduction in anabolic hormone productions or sensitivity such as insulin, growth and sex hormones, dysregulation of cytokine secretions, modification in the response to inflammatory events, inadequate nutritional intakes and sedentary lifestyle are involved. A multimodal approach combining nutrition, exercise, hormones, specific anabolic drugs may be treatment regimens for limiting the development of sarcopenia with aging. However, all therapy approaches have severe disadvantages, for instance hormones and anabolic drugs often have severe side effects. A consensus definition of sarcopenia is disclosed in von Haehling et al., J Cachexia Sarcopenia Muscle (2010) 1:129-133.
[0005] Sarcopenia and lack of physical activity are connected. However, physical activity alone cannot prevent sarcopenia completely. Treatment strategies of sarcopenia are unsatisfying. The most common therapies are application of hormones that interact with muscle growth such as testosterone. Unfortunately, it has been shown that treatment with testosterone may induce a variety of side effects such as cardiovascular diseases or cancer.
[0006] Sarcopenia is usually seen in elderly people, but can also be observed in young adults, like dementia. The prevalence of sarcopenia in 60-70 year old people is 5-11%, whereby in people over 80 years it is 11-50%. It is estimated that 200 million people will suffer from this syndrome over the next 30 years (Cruz-Jentoft A., Age and Ageing 2010, 39).
[0007] Not only people with age-related sarcopenia are affected, but also patients being bedridden, having tumors or people without physical activity have a marked decrease of muscle tissue. The enormous costs for the health care system for these patients together with the fast increase of the aging population and concomitantly the increase of age-related sarcopenia demands an efficient therapy for sarcopenia.
[0008] Cachexia is defined as physical wasting with loss of muscle mass and weight that is caused by disease. It is common for elderly individuals who have disease to exhibit cachexia. Additionally, muscle mass loss is characteristic of the conditions of frailty and sarcopenia. Physical frailty is a condition that results from reduced strength, reduced gait velocity, reduced physical activity, weight loss, and exhaustion. Sarcopenia and frailty could be classified as cachectic conditions because they are associated with muscle mass loss.
[0009] Apoptosis describes the so called programmed cell death, which is an active process by which cells get destructed. This destruction undergoes some characteristic morphological changes, like chromatin condensation, cell shrinkage, membrane blebbing, and formation of apoptotic bodies. It is known, that the cells in the adult body are in a perfect balance between cell division and controlled cell death. There are different events where apoptosis occurs, e.g. in the formation of fingers and toes in the human embryonic development or when cells are degenerated, nonfunctional and/or potentially dangerous to the animal.
[0010] Apoptosis is characterized by a controlled sequence of events. The first sign is condensation of chromatin, DNA-fragmentation, expression of proteolytic enzymes and finally cell destruction. These biochemical and morphological changes can be measured with different methods, whereat it is very important to choose examination methods, which are able to distinguish between apoptosis and necrosis, because some of them just detect cell death in general.
[0011] Available evidence suggests that targeting myonuclear apoptosis provides novel and effective therapeutic tools to combat sarcopenia (Marzetti E. et al. (2012) Gerontology 58/2:99-106). Since loss of muscle cell mass is a serious problem for elderly people it would be of great importance to provide a therapy that regains muscle strength for these patients. Muscle cell loss is also known as sarcopenia. There is currently no satisfying therapy for this disease and induction of muscle cell growth might lead to a new and innovative therapy for sarcopenia. Muscle cell loss results from an imbalance between cell division and controlled cell death (apoptosis).
[0012] It is a goal to find suitable pharmaceutical agents and methods to stimulate cell growth and/or reduce apoptosis for the treatment of various wasting diseases.
SUMMARY OF THE INVENTION
[0013] The present invention provides SERF2 as novel pharmaceutical agent for such treatments. In a first aspect, the present invention provides SERF2, a nucleic acid encoding said SERF2 or a cell expressing SERF2 for use as a medicament. In a related aspect the invention provides SERF2, a nucleic acid encoding said SERF2 or a cell expressing SERF2 for use in treating or preventing an atrophy disease or condition or for cell regenerative therapy or for increasing cellular growth in a patient.
[0014] Also provided is an in vivo or in vitro method of increasing the proliferation of stem cells or progenitor cells or reducing the rate of apoptosis of said cells, comprising administration of SERF2 or SERF2 encoding nucleic acids to said cells.
[0015] In a fourth aspect the invention provides a pharmaceutical composition comprising SERF2 or SERF2 encoding nucleic acids. Such a composition may comprise a pharmaceutically acceptable carrier or stabilizer.
[0016] As is apparent, all of these aspects are related to each other, are equivalent and all preferred embodiments relate to each one of these aspects equally. The subject matter of the present invention is further defined in the claims.
[0017] SERF2 (Small EDRK-rich factor 2) is a protein with a known sequence, see e.g. Swiss-Prot Database P84101 (human), P84102 (mouse) or NCBI Database NP_001018118 (human protein), NP_035484 (mouse protein), NM_001018108 (human nucleotide), NM_011354 (mouse nucleotide). Isoforms are deposited under database accession numbers NP_001018118.1, NP_001186804.1, NP_001186805.1, NP_001186806.1 and NP_001186807.1. In the past, it has also been referred to as H4F5rel (H4F5 related—SERF2 shares 69% sequence identity with H4F5, Scharf et al. nature genetics 20, 1998: 83-86). SERF2 is further disclosed in US 2007/042392 A1 (as SEQ ID NO: 1143, EBI database acc. No. AGI32189) and in WO 2000/55351 A1 (as SEQ ID NO: 1054, EBI database acc. No. AAB53514), both incorporated herein by reference. SERF2 is further disclosed in Van Ham Tjakko J et al., Cell, Vol. 142, No. 4 (2010), 601-612 and NCBI database acc no. AAC63516).
[0018] In the past, there have been different results on the functional capabilities of SERF homologue proteins. Some papers report a toxic role through aggregation of amyloidogenic proteins (e.g. van Ham et al. Cell 142, 2010: 601-612) while other reports describe a protective role via deposition of toxic proteins in inclusion bodies. It is important to appreciate that fibrillar aggregates of aggregation-prone proteins as described by van Ham et al. are a hallmark of neurodegenerative disorders only.
[0019] Several neurodegenerative diseases are associated with an expanded trinucleotide sequence CAG in genes. Since CAG codes for the amino acid glutamine, these disorders are collectively known as polyglutamine diseases. Although the genes (and proteins) involved in different polyglutamine diseases have little in common, the disorders they cause follow a strikingly similar course: If the length of the expansion exceeds a critical value of 35-40, the greater the number of glutamine repeats in a protein, the earlier the onset of disease and the more severe the symptoms. This fact suggests that abnormally long glutamine tracts render their host protein toxic to nerve cells, and all polyglutamine diseases are hypothesized to progress via common molecular mechanisms. One possible mechanism of cell death is that the abnormally long sequence of glutamines acquires a shape that prevents the host protein from folding into its proper shape. Polyglutamine (polyQ) diseases are classified as conformational neurodegenerative diseases, like Alzheimer and Parkinson diseases, and they are caused by proteins with an abnormally expanded polyQ stretch.
[0020] Using computer models of polyglutamine, it was shown that if, and only if, the length of polyglutamine repeats is longer than the critical value found in disease, it acquires a specific shape called a β-helix. The longer the glutamine tract length, the higher the propensity to form β-helices. Expansion of polyglutamine (polyQ) tracts in proteins results in protein aggregation and is associated with cell death in neurodegenerative diseases. Disease age of onset is correlated with the polyQ insert length above a critical value of 35-40 glutamines. The aggregation kinetics of isolated polyQ peptides in vitro also shows a similar critical-length dependence. By using computer simulations of isolated polyQ peptides, it was shown that a mechanism of aggregation is the conformational transition in a single polyQ peptide chain from random coil to a parallel β-helix. This transition occurs selectively in peptides longer than 37 glutamines. The production of the apparent toxic species—soluble oligomers—and their subsequent ability to cause neuronal injury depends on the precision of an intramembranous proteolytic cleavage. Some oligomeric species are small and soluble enough to diffuse readily through the brain parenchyma and affect synaptic structure and function and, ultimately, neuronal survival.
[0021] In a series of experiments, van Ham et al. (supra) tried to identify modifier of aggregation (MOAG-4/SERF as a regulator of age-related proteotoxicity in C. elegans . The authors found that depending on the number of glutamine residues (<40 residues), protein aggregation can be detected and is reduced when they introduced a point mutation in MOAG-4. However, life span was not influenced in these animals. The members of the SERF protein family seem to have similar functions as MOAG-4. In addition, overexpression of SERF1/2 increased aggregation of mutant Huntington protein and cell death in mouse fibroblasts.
[0022] Despite these interesting findings, the results of this paper evoke a number of questions:
[0023] 1. Functional Studies in C. elegans often do not reflect the situation in humans or mammals, for instance recent results reveal a higher degree of species specificity among TCF proteins for coactivator interactions than for corepressor interactions, and uncover a basic difference between C. elegans and human TCF4 steady state nuclear levels. Another example is the dramatic difference between C. elegans and D. melanogaster unc-76 mutants on the one hand, which causes serious defects in the nervous system, and the mouse FEZ1 −/− knockout mice on the other, which show no morphological and no strong behavioral phenotype.
[0024] 2. There are reports in literature which describe a protective role for the SERF protein family rather than a toxic one.
[0025] 3. There is a marked difference in the AA-sequence between MOAG4 and SERF proteins (˜50%), therefore functional differences might be due to protein sequence differences.
[0026] 4. Most importantly, a highly artificial system is used. Only in cells transfected with 74 polyQ repeats, a situation that is never achieved in nature, aggregation takes place. In addition, aggregation is only seen with amyloidogenic proteins. Therefore, it remains to be seen if there is any natural function of MOAG4/SERF in the absence of exogenous proteins.
[0027] Nevertheless, in certain embodiments of the present invention the disease or condition to be treated is not one or more diseases or conditions selected from the groups of Alzheimer's disease, Parkinson's disease, Huntington's disease, or any polyglutamine diseases or any disease or condition caused by aggregation of amyloid fibers or of amyloidogenic proteins. In particular embodiments the disease or condition is not a disease or condition of the nervous system.
[0028] The results herein evidently show a protective and growth-supporting role of SERF2 in a variety of mammalian cell types. In several experiments it has been shown, that SERF2 induces proliferation in a variety of human cell lines. Beside cells of mesenchymal origin it also has effects on cells of the hematopoietic lineage and muscle cells, among others.
[0029] SERF2, as used herein relates to any SERF2 isoform or variant. In preferred embodiments SERF2 comprises or consists of an amino acid sequence as set forth in SEQ ID NO: 1, or an amino acid sequence that has at least 70% sequence identity with the sequence as set forth in SEQ ID NO: 1.
[0030] The term “sequence identity” refers to identity between two sequences, usually amino acid sequences, which can be determined by sequence alignment programs like BLAST, PSI-BLAST (www.ncbi.nlm.nih.gov/blast/) or ClustalW (www.ebi.ac.uk/clustalw/). These algorithms calculate the best match for the selected sequences, and line them up so that the identities, similarities and differences can be seen. The sequence identity to SEQ ID NO:1 is calculated to the entire sequence of SEQ ID NO: 1.
[0031] In preferred embodiments of the present invention the inventive SERF2 comprises or consists of a sequence with at least 70%, more preferred at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, at least 98% or even 100%, sequence identity with the sequence as set forth in SEQ ID NO: 1.
[0032] SERF2 can be a recombinant SERF2. Further preferred it is of the same origin as the patient but also SERF2 variants from other animals can be used. Preferably the patient is a mammal, especially a human or non-human animal, in particular a domestic animal, such as pig, rodents, or a primate. Preferably the SERF2 is human SERF2 or SERF2 from a non-human animal, in particular a domestic animal, such as pig, rodents, or a primate.
[0033] As used herein “comprising” is used in an open meaning, i.e. that the SERF2 of the present invention may have further amino acids or protein components. It may be a fusion protein. Such extended SERF2 proteins may have in preferred embodiments a limited size, e.g. up to 2000 amino acids, up to 1800 amino acids, up to 1600 amino acids, up to 1400 amino acids, up to 1200 amino acids, up to 1000 amino acids, up to 800 amino acids, up to 600 amino acids, up to 400 amino acids, up to 300 amino acids, up to 200 amino acids, or up to 160 amino acids. Of course the invention also relates to SERF2 proteins that consist of any one of said sequences comprised in the above mentioned embodiments. “Consisting” is used in a closed and sequence limiting meaning.
[0034] Alternatively (or in combination) to using SERF2 proteins it is also possible to use nucleic acids that encode the above mentioned SERF2 protein and its variants. Such a sequence is e.g. set forth in SEQ ID NO: 2, which encodes SEQ ID NO: 1.
[0035] Nucleic acids can be used to induce production of SERF2 in cells. Preferred formulations for nucleic acid delivery are e.g. liposomes, microemulsions, micelles or vesicles for controlled delivery. The cell may then produce and secrete SERF2 to provide a continuous production of the therapeutic agent.
[0036] Also provided is a cell that expresses SERF2 for the inventive uses. Such a cell preferably continuously secretes SERF2 to provide for the therapeutic effect. Such a cell can be any cell. In preferred embodiments the cell is not-immunogenic to the patient, e.g. it is a cell obtained from the patient that has been genetically engineered to recombinantly express SERF2. This modification of the cell can be performed in vitro or in vivo.
[0037] The previous and further detailed description relates to the SERF2 protein, the nucleic acid and the cells equally, in particular since the directly active therapeutic agent of the nucleic acid or the cell is also the expressed SERF2. All three embodiments are conterminously referred to as “SERF2” herein, wherein SERF2 protein is preferred since it is the directly acting agent.
[0038] The present invention provides in particular SERF2 for use in treating or preventing an atrophy disease or condition or for cell regenerative therapy.
[0039] “Preventing” as used herein does not require an absolute prevention in that a patient will never develop the diseases or conditions but it relates to a reduced risk in developing the disease or condition. It is a prophylactic treatment. Other forms of treatment occur after onset of the disease or condition, e.g. when a patient in need of a therapy has been identified. “Treating” does not mean that a disease or condition is completely cured. It may also refer to an improvement or amelioration of symptoms.
[0040] Atrophy is the general physiological process of reabsorption and breakdown of tissues, involving apoptosis on a cellular level. It is also termed as a partial loss of a part of the body. It can be caused by diseases or it can be a part of normal body development, such as during aging. In special embodiments, the atrophy is muscle atrophy, but other tissues may be affected and treated according to the invention as well. SERF2 achieves downregulation of myonuclear apoptosis, effective in maintaining muscle mass and function in late life and additionally stimulates cellular proliferation and development.
[0041] It essentially shifts the equilibrium between apoptosis and proliferation towards proliferation an regeneration. SERF2 decreases apoptosis and increases proliferation. Thus it can be used to treat cells or diseases with increased apoptosis and/or reduced proliferation or regeneration of cells. Thus in a preferred embodiment the atrophy treated according to the invention is associated with an increased apoptosis or reduced regeneration of cells. An atrophy might be a reduction of the mass of a certain tissue. Such a tissue can be a muscle (e.g. in sarcopenia), the skin (e.g. in medication- or age-caused skin thinning), a bone or an internal organ such as the liver, a tissue of the hematopoietic system, e.g. bone marrow, spleen, tonsils, lymph nodes.
[0042] In addition to treating atrophies, the invention can be used to increase cellular mass even when there is no shortcoming of a specific cell type. It can be used as a time-limited or extended therapy to increase a certain tissue mass. Such a tissue can e.g. be a muscle (e.g. for body building), the skin, a bone or an internal organ, such as the liver and tissues of the hematopoietic system, e.g. as mentioned above.
[0043] In preferred embodiments the treated atrophy is a reduction of cells selected from the group of muscle cells, in particular heart muscle cells or skeletal muscle cells or smooth muscle cells, a connective tissue cell, in particular a cell of connective tissue surrounding a muscle or a bone cell, epithelial cells, in particular blood vessel cells, and satellite cells, or bone cells (e.g. osteoblasts or osteoclasts).
[0044] The disease or condition to be treated or prevented can in special embodiments be selected from sarcopenia, cachexia, dystrophy, especially muscular dystrophy, hypoplasia, hypotonia, especially hypotonia after an operation, polymyositis, fibromyalgia, myotubular myopathy, metabolic diseases of the muscular system, Parkinson's, myasthenia gravis, cardiomyopathy, cardiomyocyte contractile dysfunction, skin aging. The inventive therapy can be for preventing muscle loss or muscle dystrophy after a time in a surgical cast or any other immobility, or any combination thereof. The disease or condition to be treated can be associated with insufficient angiogenesis. Diseases associated with insufficient angiogenesis are characterized by a loss in blood circulation and insufficient oxygen supply to a particular tissue (in particular the one of the tissues mentioned above to be treated in preferred embodiments). Diseases with insufficient angiogenesis are e.g. ischemic heart disease and conditions resulting due to anti-angiogenetic treatments, e.g. in therapies with antibodies that reduce or prevent blood vessel formation, e.g. in a therapy of macular degeneration, or in a therapy of cancer. A further disease or condition to be treated can be neutropenia, especially chemotherapy-induced neutropenia, which can be treated according to the invention by increasing proliferation or reducing apoptosis of cells of the hematopoietic system. Preferably hematopoietic stem cells are expanded in vivo or ex vivo and used to ameliorate symptoms in cancer treatments that would result in a reduction of blood cells. Of course also other stem cells, e.g. of any one of the tissues mentioned above, can be expanded using SERF2 according to the invention.
[0045] Somatic cells have both a limited lifetime and regeneration ability, which is especially evident during aging. Sarcopenia is defined as the degenerative loss of skeletal muscle and muscle strength in elderly people. Muscle loss causes a major disability of the elderly in everyday life, and leads to an enormous increase of healthcare cost. The risk of fall and fractures is enhanced and a loss of independence and live quality is evident. The reasons for the muscle loss are among others, proteolysis, lack of protein synthesis and muscle fat content. A mechanism for the loss of muscle cell mass is the decrease of satellite cells in skeletal muscle. Satellite cells are specialized cells located in the basal membrane of muscles and are crucial for muscle regeneration and growth of muscle tissue. The number of satellite cells decreases during age and is a reason for sarcopenia.
[0046] For the reason mentioned in the background section, new therapies to prevent apoptosis in muscle cells and to induce the formation of new muscle tissue are in great demand for treating sarcopenia and other diseases associated with cell loss.
[0047] In addition to the beneficial effects of SERF2 for muscle and satellite cells, it could be used for a variety of other cell types. The effect of SERF2 on hematopoietic cells (HC) is of utmost importance. It does protect these cell types from GF-deprived cell death and leads to prolonged survival. This is especially important in diseases where only small numbers of absolutely necessary cells are left (for instance during chemotherapy) or if rare cell types such as stem cells need to be expanded. Related to these effects, SERF2 can be used in vivo or in vitro to increase hematopoiesis or blood cell amounts, e.g. blood cell concentrations, in a subject. This may be of therapeutic or non-therapeutic use. Thus the present invention also relates to therapies to treat a blood cell deficiency or a subject in need of blood cell increase. The blood cells may be selected from erythrocytes (red blood cells), PBMCs, white blood cells, T cells, granulocytes and macrophages or monocytes.
[0048] Given the new results presented herein, that SERF2 exerts a proliferative and life-span enhancing effect on epithelial cells, SERF2 is well suited as a drug to prevent skin aging. Due to its relatively low molecular weight it could be packaged into liposomes and used as an efficient additive in medical care cosmetics. Thus SERF2 can also be used for cosmetic or therapeutic uses in the treatment of skin, to prevent or reduce aging effects.
[0049] Action of epithelial cells is particularly visible during angiogenesis. As shown herein, angiogenesis can be stimulated in vivo or in vitro by administering SERF2. Thus the present invention also provides for the use of SERF2 for stimulating angiogenesis. A patient with tissues with insufficient artery supply may be treated. The patient may have anoxic tissues that are treated by the present invention. The tissue with insufficient artery supply may also be acute or chronic, e.g. be in this state for at least 14 days, preferably at least 18 days, especially preferred at least 22 days, even more preferred at least 28 days, for at least 34 days, at least 40 days, at least 50 days or even at least 60 days. Thus, the present invention relates to a treatment of a patient who is in need of an induction of angiogenesis with SERF2, in particular in the tissue in need of such therapy. Preferably the therapy is topical.
[0050] SERF2 can be administered to a patient, e.g. the SERF2 protein or nucleic acid is administered directly by an adequate means to the patient's system or specific tissue.
[0051] Alternatively, cells of a patient are treated ex vivo with SERF2 and said cells are administered to said patient. SERF2 treated cells are activated for proliferation and can perform the necessary regenerative functions in vivo. The readministered administration is preferably topical, in particular to the tissue of origin of the cell (e.g. reapplying a muscle cell/muscular stem or progenitor cell such as satellite cells to a muscle). Preferred cells to be treated ex vivo and readministered is any kind of stem cell or progenitor cell, which generally have enhanced potential for proliferation and tissue regeneration.
[0052] The disease or condition to be treated according to the invention may be chronic or acute. “Chronic” in preferred embodiments relates to a disease or condition that exist for at least 14 days, preferably at least 18 days, especially preferred at least 22 days, even more preferred at least 28 days, within at least 34 days, at least 40 days, at least 50 days or even at least 60 days.
[0053] The present invention further relates to an in vitro or in vivo method of increasing the proliferation of stem cells, progenitor cells, epithelial cells, in particular epidermal skin cells, mesenchymal cells, in particular cardiomyocytes, satellite cells, skeletal muscle cells, hematopoietic cells, in particular hematopoietic stem cells or progenitor cells, or reducing the rate of apoptosis of said cells, comprising administration of SERF2 or SERF2 encoding nucleic acids to said cells. Hematopoietic cells may e.g. be cells or stem or progenitor cells of the bone marrow, spleen, tonsils or lymph nodes. Such an in vivo method can be suitable for one of the above mentioned therapies. In vitro methods can be used to proliferate cell cultures or in an ex vivo step for proliferating cells, which may then be reinserted into a patient in the course of a therapy.
[0054] Such cells are preferably selected from the group of muscle cells, in particular heart muscle cells or skeletal muscle cells or smooth muscle cells, a connective tissue cell, in particular a cell of connective tissue surrounding a muscle, and stem cells, progenitor cells, in particular satellite cells, hematopoietic cells, skeletal muscle cells, epithelial cells, in particular epidermal skin cells. The inventive SERF2 can be used to increase the mass of these cells in any tissue, e.g. to increase heart mass or volume. This increase can be used to treat a disease with an insufficiency of such cells, e.g. a muscle weakness, especially a hear muscle weakness, or for anabolic reasons. A particular preferred embodiment relates to the in vitro preparation of skin cells for an artificial skin, which cells or skin can be used in skin repair.
[0055] SERF2 (as always including proteins, nucleic acids or cells) can be administered in any way known in the art. Especially preferred forms of administration are topical administrations. Preferred topical administrations means are transdermal patches or by minipumps, which can continuously provide SERF2 on the site or tissue of need thereof. Of course, also a systemic administration is possible, to provide overall increased proliferative activity. In case of systemic administration—but also for topical forms of administration—SERF2 can be linked, e.g. fused, to a tissue homing molecule, such as a ligand of a surface receptor, specific for a selected kind of tissue. Such tissues can be selected from the above, e.g. muscle (heart, skeletal or smooth) cells, endothelial cells etc. Such a homing molecule allows tissue specific action of SERF2 with any kind of administration.
[0056] In preferred embodiments the administered SERF2 concentration is from 0.5 μg/ml to 1000 μg/ml, preferably 1 μg/ml to 800 μg/ml, especially preferred 2.5 μg/ml to 500 μg/ml, even more preferred 4 μg/ml to 300 μg/ml, most preferred 5 μg/ml to 100 μg/ml. These ranges have proved to be especially effective in the inventive therapy.
[0057] As shown in the examples, SERF2 can increase proliferation and/or reduce apoptosis of cells under stress, e.g. oxidative stress. Thus in a preferred embodiment the cells treated according to the invention are suffering from stress, in particular oxidative stress such as stress induced by reactive oxygen species including .OH.
[0058] The invention further relates to a pharmaceutical composition comprising SERF2 proteins or SERF2 encoding nucleic acids or the SERF2 expressing cells (all three embodiments conterminously referred to as “SERF2”, preferably SERF2 protein). Pharmaceutical compositions or formulations for therapeutic use may comprise a pharmaceutically acceptable diluent, carrier, solubilizer, emulsifier, preservative, stabilizer and/or adjuvant. The invention also provides for pharmaceutical compositions comprising a therapeutically effective amount of SERF2. The term “therapeutically effective amount” means an amount which provides a therapeutic effect for a specified condition and route of administration. The composition may be in a liquid or lyophilized form and comprises a diluent (Tris, acetate or phosphate buffers, NaCl) having various pH values and ionic strengths, solubilizer such as Tween or Polysorbate, carriers such as human serum albumin or gelatin, preservatives such as thimerosal or benzyl alcohol. Selection of a particular composition will depend upon a number of factors, including the condition being treated, the route of administration and the pharmacokinetic parameters desired.
[0059] Preferred formulations are formulations for topical administration. Especially preferred is a hydrogel, a patch, in particular a transdermal patch and a surgically inserted delivery means, such as a minipump. Also encompassed are compositions comprising SERF2 modified with water soluble polymers to increase solubility, stability, plasma half-life and bioavailability. Compositions may also comprise incorporation of SERF2 into liposomes, microemulsions, micelles, microparticles or vesicles for controlled delivery over an extended period of time.
[0060] In special embodiments SERF2 is provided with a carrier. The carrier is preferably selected from a gel, preferably a hy-drogel, or a wound dressing or a swab, optionally impregnated with a solution containing SERF2. Further carriers comprise carriers for slow-release which release the active agent combination as a longer effective application delayed or slower. Such a preparation with a corresponding carrier is especially suitable for topical and quick administration.
[0061] In particular, the present invention provides the pharmaceutical composition for use as a medicament, or for any one of the above described uses for SERF2.
[0062] The present invention will be further explained by the following figures and examples without being limited to theses specific aspects of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0063] FIG. 1 : Analysis of SERF2 after the second purification step (HIC column). Equal amounts of fractions 1-9 were loaded onto an SDS gel and subjected to western blot analysis. SERF2 (arrow) appears at appr. 13 kDa and is not retarded on the HIC column whereas impurities are retained. The higher apparent molecular weight is due to large amounts of positive charges (19 residues), which alters elution behavior of SERF2.
[0064] FIG. 2 : Effect of SERF2 on Proliferation of rat skeletal muscle cells (L6). 1×104 L6 cells were seeded per well containing 100 μl growth medium. Cells were incubated over night at +37° C., 5% v/v CO2 and humidified atmosphere. Prior performing the assay, viability of cells was checked under the microscope. Cells were washed three times with 100 μl DPBS per well. SERF2 was diluted μg/ml) in DMEM and 100 μl/well were added to the cells. Finally, cells were incubated at +37° C. for various time points. Subsequently 10 μl/well AlamarBlue™ reagent (Invitrogen) was added. Plates were incubated for one hour at +37° C. Fluorescence (Ex. 570 nm, Em. 585 nm) was measured using a Varioskan Flash multi-plate reader (Thermo Scientific). Obtained Data were evaluated using Microsoft Excel and Graph Pad Prism V4.
[0065] FIG. 3 : Effect of SERF2 on Proliferation of H9c2 cells is dose-dependent. Proliferation assay was performed essentially as in FIG. 2 . Incubation time was 24 hrs, added SERF2 concentrations ranged from 20 to 1.25 μg/ml.
[0066] FIG. 4 : Effect of SERF2 on Proliferation of mouse satellite cells (MuMa23/P13). Proliferation assay was performed essentially as in FIG. 2 . Incubation time was 24 hrs, added SERF2 concentrations were 20 and 4 μg/ml, respectively.
[0067] FIG. 5 : Kinetics of the Effect of SERF2 on Proliferation of rat cardiomyocytes (H9c2). Cells stimulated with SERF2 (green line) responded with proliferation and reached max. proliferation rate after 6 days. Proliferation assay was performed essentially as in FIG. 2 . Incubation times were 24, 48, 72 and 144 hrs, the SERF2 concentration added was 5 μg/ml.
[0068] FIG. 6 : Kinetics of the Effect of SERF2 on Proliferation of rat skeletal muscle cells (L6). Cells stimulated with SERF2 (green line) responded with proliferation and reached a max. proliferation rate after 6 days. Proliferation assay was performed essentially as in FIG. 2 . Incubation times were 24, 48, 72 and 144 hrs, the SERF2 concentration added was 5 μg/ml.
[0069] FIG. 7 : SERF2 protects a human epithelial cell line (A431) from H2O2-induced apoptosis. Experiments were performed in 6-well plates containing 5 ml cell culture medium (serum-free) per well and were seeded at a cell density of 1*106 cells/well and cultured overnight. On the next day 200 mM H2O2 or 200 mM H2O2 and SERF2 (5 μg/ml) was added to cultures. After 6 hours of incubation, the adherent cells were harvested, washed 3 times in PBS and dead cells were detected by trypan-blue staining using light microscopy. Shown is the percentage of dead cells.
[0070] FIG. 8 : SERF2 protects a human epithelial cell line (MCF-7) from H2O2-induced apoptosis. Experiments were performed in 6-well plates containing 5 ml cell culture medium (serum-free) per well and were seeded at a cell density of 1*106 cells/well and cultured overnight. On the next day 200 mM H2O2 or 200 mM H2O2 and SERF2 (5 μg/ml) was added to cultures. After 6 hours of incubation, the adherent cells were harvested, washed 3 times in PBS and dead cells were detected by trypan-blue staining using light microscopy. Shown is the percentage of dead cells.
[0071] FIG. 9 : SERF2 protects a human T-cell line (Jurkat) from H2O2-induced apoptosis. Experiments were performed in 6-well plates containing 5 ml cell culture medium (serum-free) per well and were seeded at a cell density of 1*106 cells/well and cultured overnight. On the next day 200 mM H2O2 (red bar) or 200 mM H2O2 and SERF2 (green bar; 5 μg/ml) was added to cultures. After 6 hours of incubation, the adherent cells were harvested, washed 3 times in PBS and dead cells were detected by trypan-blue staining using light microscopy. Shown is the percentage of dead cells.
[0072] FIG. 10 : SERF2 compensates for FCS and alleviates apoptosis in growth factor-dependent human myeloid cells. TF-1 cells were incubated under different culture conditions: FCS+GMC-SF (dark blue), serum-free medium+GM-CSF (5 μg/ml; pale blue), serum-free medium+GMC-SF+SERF2 (5 μg/ml; lime), serum-free medium+SERF2 (green) and serum-free medium only (red). After 9.5 hours culture supernatants were analyzed by an ELISA-technique for caspase-3 expression levels. Results are expressed as pNA in pmol/μl
[0073] FIG. 11 : SERF2 alleviates apoptosis in a human B cell line. 711-3 cells were incubated under different culture conditions: serum-free medium (dark blue), serum-free medium+SERF2 (5 μg/ml; lime) serum-free medium+SERF2+H2O2 (green) and serum-free medium+H2O2 (red). After 9.5 hours culture supernatants were analyzed by an ELISA-technique for caspase-3 expression levels. Results are expressed as pNA in pmol/μl.
[0074] FIGS. 12 a -12 c : Proangiogenic effect of SERF2 in CAM assays. To evaluate the pro-angiogenic properties of SERF2, 3 μg of A: PBS and C: SERF2 was applied per CAM. B: VEGF-A (0.5 μg/CAM) was used as positive control, PBS served as a negative control. New vessels were identified in VEGF and SERF2-treated CAMs. Treatment was performed on embryonic day 6 and 7. Angiogenic responses were evaluated microscopically. Pictures shown were taken for documentation on day 6.
[0075] FIG. 13 a : Changes in heart size in 7 dpf old zebrafish incubated with different doses of SERF2. FIG. 13 b : Changes in heart volume in 7 dpf old zebrafish incubated in different concentrations of SERF2 and erythropoietin (EPO). Significant differences to control animals are indicated by asterisks.
[0076] FIG. 14 : Changes in blood cell concentrations in zebrafish incubated in different doses of SERF2. Shown are mean values (blood cells/nl) and SEM. Asterisks indicate significant differences to control animals.
[0077] FIG. 15 : Changes in proliferation of endothelial cells of the caudal fin in 7 dpf or 15 dpf old zebrafish induced by different doses of SERF2 or EPO. Asterisk indicates significant differences to control animals.
[0078] FIGS. 16 a -16 b : Imaging of tail vasculature in 7 dpf zebrafish (top image=control, lower image=SERF2-treated). Magenta arrows indicate the dorsal artery, blue arrows the intersegmental vessels.
[0079] FIGS. 17 a -17 b : Detection of blood cells (green arrows) in 7 dpf zebrafish (top image=control, lower image=SERF2-treated). To determine blood cell concentration the number of detected cells were divided by vessel volume.
[0080] FIGS. 18 a -18 b : Apoptotic cells detected by TUNEL technology in gill, skeletal muscle and tail sections. From these experiments it is evident that the number of specifically stained cells in SERF2-treated animals is lower in different regions as compared to untreated animals.
DETAILED DESCRIPTION OF THE INVENTION
Examples
Example 1: Material & Methods
[0081] 1.1 SERF2—Cloning, Expression and Purification
[0082] SERF2 was identified by colony hybridisation with a AB4 cDNA library. The coding sequence of SERF2 is 180 bp, the length of the mature protein is 59 amino acids, the molecular weight 6899, the pI 10.44.
[0000]
SEQ ID NO 2:
atgacccgcggtaaccagcgtgagctcgcccgccagaagaatatgaaaaag
SEQ ID NO 1:
MTRGNQRELARQKNMKK
cagagcgactcggttaagggaaagcgccgagatgacgggctttctgctgcc
gcccgcaagcag
QSDSVKGKRRDDGLSAAARKQ
agggactcggagatcatgcagcagaagcagaaaaaggcaaacgagaagaag
gaggaacccaag
RDSEIMQQKQKKANEKKEEPK
tag-
[0083] SERF2 was cloned codon-optimized into pET28 vector (inferring Kanamycin resistance) at 5′Ncol and 3′XhoI site without tags. SERF2 was expressed in BL21 E. coli.
[0084] An overnight pre-culture was prepared from a glycerol stock in selective M9ZB Medium and incubated at 37° C., shaking at 220 rpm. The next day, the overnight pre-culture was diluted to OD600=0.1 and incubated at 37° C., shaking at 220 rpm until OD600=0.5. Subsequently, protein expression was induced with IPTG at a final concentration of 1 mM. The culture was then incubated for 4 hrs at 30° C., followed by an overnight incubation at room temperature, shaking at 220 rpm. Bacteria were harvested by centrifugation for 2 h at 2500 g.
[0085] 1.2 Purification of SERF2
[0086] For disruption, cells were resuspended in lysis buffer [75 ml/1 culture volume; 50 mM Na-phosphate pH 8, 300 mM NaCl, 0.2% Triton X-100] and subjected to three freeze/thaw cycles at −80° C. After the third thawing, 30 μg/1 DNAseI was added, and the lyzed cells were incubated at 37° C. for 30 minutes. Supernatant was collected by centrifugation for 2 hours at 2500 g.
[0087] For purification, the filtered lysate (0.22 μm) was loaded onto a SP-Sepharose column (70 ml CV) in 20 mMTris pH8.0 at a flow rate of 14 ml/min. Fractions were eluted by a linear gradient with 20 mM Tris/1M NaCl pH 8.0 recording protein at 214 nm. After isolating relevant fractions via silver stained SDS PAGE gel and western blotting, respectively, ammonium sulphate was slowly added to a final saturation of 30% stirred overnight. Subsequently, the salt-enriched SERF2 was ultrafiltered (0.22 μm) and subjected to a second purification via a Hi Trap Octyl-Sepharose FF column (25 ml CV) at a flow rate of 7 ml/min. Relevant fractions were identified via silver stain stained SDS PAGE gel and western blotting ( FIG. 1 ), pooled and dialysed against 20 mM Na-phosphate pH 7.4.
[0088] 1.3 Cell Culture
[0089] Rat derived embryonic cardiomyocytes H9c2 (ATTC CRL-1446) and embryonic skeletal muscle cells L6 (ATTC CRL-1458) were cultured in Dulbecco's Modified Eagle Medium high glucose (DMEM, Sigma Aldrich) containing 10% v/v fetal calf serum (FCS, PAA) and 1% v/v Penicillin/Streptamycin (Gibco). Cells were grown in 80 cm2 cell culture flasks (NUNC) using 15 ml growth medium. Both cell lines were incubated under humidified atmosphere at +37° C. and 5% v/v CO2. Cells were splitted when a confluency of approximately 90% was reached. Usually a splitting ratio of 1:5 or 1:10 was applied. For this purpose, supernatant was removed and cells were washed using 10 ml Dulbecco's Phosphate Buffered Saline (DPBS, Gibco). Cells were harvested by addition of 3 ml Trypsin/EDTA (Gibco) followed by an incubation of 5 to 10 min at +37° C. Successful detachment of cells was checked under the microscope (IMT-2, Olympus) and 7 ml growth medium were added. Cell number and viability were determined by trypanblue exclusion performed by using an automated cell analyzer (CEDEX, Innovatis). For this, 950 μl DPBS and 50μl cell-suspension were mixed and used for analysis.
[0090] Isolation of primary mouse satellite cells: Muscle tissue was taken from male ICR mice and minced by using scissors and a scalpel. Following incubation in protease solution (Sigma, St. Lois) for 1 h at 37° C., remaining tissue clumps were dissociated by vigorously pipetting and loaded onto a Percoll (Pharmacia) gradient (75%, 50%, 30%). After centrifugation for 20 min at 1250×g, cells were collected from the 2nd interphase (99% satellite cells), washed and cultured at a cell density of 1×105 cells/ml in 6-well plates. See also Danoviz ewt al. Methods Mol Biol. 2012; 798: 21-52.
[0091] Mammalian Cell Cultures:
[0092] Adherent cells: A431 are epidermoid carcinoma cells, MCF-7 cells are epithelial cells, ECV-304 was derived from a urinary bladder carcinoma.
[0093] Suspension cells: TF-1 cells originate from bone marrow of a patient with severe pancytopenia. These cells require medium supplemented with 5 ng/ml GM-CSF and differentiate into macrophages like cells. The Jurkat cell line was derived from the blood of a 14-year old boy with acute T-cell leukemia (ATCC). 711-3 is a human lymphoblastoid B-cell line.
[0094] 1.4 AlamarBlue™ Assay
[0095] Proliferation was measured using the AlamarBlue™ assay according to the manufacturer's protocol. Briefly, 1×104 cells were seeded per well containing 100μl growth medium. Cells were incubated over night at +37° C., 5% v/v CO2 and humidified atmosphere. Prior performing the assay, viability of cells was checked under the microscope. Usually cells reached 60% confluence. Cells were washed three times with 100μl DPBS per well. Peptides were diluted as desired (range 50 ng/ml to 20 μg/ml) in DMEM and 100 μl/well were added to the cells. Finally, cells were incubated at +37° C. for various time points depending on the type of experiment. Subsequently 10 μl/well AlamarBlue™ reagent (Invitrogen) was added. Plates were incubated for one hour at +37° C. Fluorescence (Ex. 570 nm, Em. 585 nm) was measured using a Varioskan Flash multi-plate reader (Thermo Scientific). Data were evaluated using Microsoft Excel and GraphPad Prism V4.
[0096] 1.5 Hen's Egg Test—Chorionallantoic Membrane (HET-CAM) Assay
[0097] Fertilized specific-pathogen free eggs (White leghorn) were obtained from BAXTER Biosciences (Vienna, Austria) on embryonic day 5 (E5). Eggs were disinfected on the surface using a towel soaked with Microzid (Schülke, Austria). A tiny hole was drilled and 3 ml albumen were removed using a syringe equipped with a 18G needle. Subsequently, the hole was covered with paraffin. To open the eggs, another hole was drilled on top. The egg shell was removed in this area using a pair of tweezers. The underlying membrane was removed resulting in the accessibility of the chorionallantoic membrane (CAM). This operational window was finally covered with sterile aluminum foil. Eggs were incubated at +37° C., 5% v/v CO2 and humidified atmosphere. On embryonic day 6 (E6), a plastic foil (outer diameter 12 mm, inner diameter of 3 mm) was washed three times with 70% v/v ethanol and three times with sterile Locke (0.15M NaCl, 5 mM KCl, 2 mM CaCl2, 2 mM NaHCO3) buffer. Finally, the plastic foil was laid onto the CAM. Selected peptides were diluted and applied onto the CAM on E6 by pipetting them in the middle of the plastic foil. Eggs were incubated at +37° C. until E8 or Ell depending on type of experiment. Pictures of the CAM were taken using a stereo microscope (StemiSV11, Zeiss, Germany) equipped with a digital camera (Coolpix990, Nikon, Japan) at defined time points. Angiogenic potential of tested peptides was evaluated microscopically at the end of the experiment.
[0098] 1.6 Staining Methods
[0099] Trypan Blue staining is one of the most commonly used methods to determine the cell viability using light microscopy. Trypan blue can only stain cells if their membrane is damaged. Viable cells do not take up the dye.
[0100] 1.7 Caspase 3—Specific ELISA
[0101] Caspase-3 is a member of the cysteine aspartic acid—specific protease family and is a marker of an early event in apoptosis. Caspase-3 expression was measured using a commercially available kit. Briefly, culture supernatants of cells undergoing apoptosis after different treatments were harvested and incubated with a substrate labeled with p-nitroaniline (pNA), which produces a yellow color when it is cleaved by caspase-3. The amount of produced yellow color is proportional to the caspase-3 activity, which can be determined by an ELISA reader at 405 nm (Promega). The assay was performed essentially as described by the manufacturer (instruction manual of CaspACE™ Assay System, Promega).
Example 2: Results
[0102] Recombinant SERF2 protein was cloned and expressed from a human cell line which resembles plasmacytoid dendritic cells. It has been shown that SERF2 both stimulated the proliferation of rat muscle cells and promotes angiogenesis. Therefore it is evident that SERF2 affects various human cells. A first experiment was set to find out, if SERF2 is able to stimulate proliferation of muscle cells and satellite cells.
[0103] 2.1 SERF2 Supports Proliferation of Skeletal Muscle Cells, Cardiomyocytes and Primary Satellite Cells
[0104] The aim of these experiments was to determine the proliferative effect of SERF2 on the rat embryonic cardiomyoblast cell line H9c2. Treatment was done for 24 h and an AlamarBlue™ assay performed as described in the methods section. Results obtained are shown in FIG. 3 . A similar set of experiments was performed on mouse satellite cells MuMa23/P1 Results obtained are shown in FIG. 4 . In both sets of experiments, treatment with human SERF2 resulted in a proliferative effect in a dose-dependent manner. This observation is similar to an experiment with L6 rat skeletal muscle cells ( FIG. 2 ). In these experiments both cell lines (L6 and H9c29) were treated once with SERF2. An AlamarBlue™ assay was performed daily until day six of incubation. The results of this experiment are shown in FIG. 5 and FIG. 6 respectively.
[0105] SERF2 exerted a proliferative effect on L6 rat skeletal muscle cells in a dose- and time-dependent manner. The maximum effect was observed after three to six days of incubation. A similar result was obtained when cardiomyoblasts (H9c2) cells were treated with SERF2. A proliferative effect was observed peaking at 5 μg/ml SERF2.
[0106] 2.2 SERF2 Exerts an Angiogenic Effect in Chicken CAM Assays
[0107] The HET-CAM assay enables the assessment of the angiogenic potential of substrates or cells. A suitable VEGF concentration was determined, which can be used as positive control. To achieve this, VEGF-A was applied onto the CAM of two eggs (100 ng/CAM abs.) once. Two eggs were left untreated and served as negative control. Treatment was performed on embryonic day 6 (E6). Angiogenic response was determined on Ell by light microscopy. Photographs of this experiment are shown in FIGS. 12 a - 12 c.
[0108] To evaluate the pro-angiogenic properties of SERF2, the protein was subjected to Het-CAM assay. An amount of 3 μg of PBS and SERF2 peptide was applied per CAM. VEGF-A (0.5 μg/CAM) was used as positive control, PBS served as negative control. Treatment was performed on embryonic day 6 and 7. All dilutions were stored at +4° C. in between and allowed to equilibrate to room temperature prior application. Angiogenic responses were evaluated microscopically on E7 as well as on E8. Each treatment was carried out in triplicates. Pictures were taken for documentation on these two days (see FIGS. 12 a -12 c ). As determined by manual count of newly formed vessels, SERF2 exerted a pro-angiogenic response in the Het-CAM assay.
[0109] 2.3 SERF2 Prevents Apoptosis in Human Cells
[0110] The question was asked whether SERF2 has an effect on growth factor depriviation- or stress-induced apoptosis. The experimental protocol included addition of Hydrogen peroxide (H2O2), which is known to cause cellular stress and consequently apoptotic death in doses below 200 μM (Cox A., Carcinogenesis. 2007, Vol. 28, 10). Furthermore apoptosis was induced by deprivation of granulocyte macrophage colony-stimulating factor (GM-CSF) in cultures of TF-1 cells. These cells are dependent on the presence of a growth factor which is absolutely necessary for growth and differentiation of TF-1 cells.
[0111] Results are shown in FIG. 7 (A431 cells—H2O2 assay), 8 (MCF-7 cells—H2O2 assay), 9 (Jurkat cells—H2O2 assay), 10 (TF-1 cells—growth factor assay) and 11 (711-3 cells—H2O2 assay).
[0112] In all experimental designs, the presence of SERF2 in cell cultures markedly reduced apoptosis. It is noteworthy that this effect was seen in cells of various origin, i.e. epithelial cells or cells of the myeloid or lymphoid lineage.
[0113] 2.4. In Vivo Effects of SERF2 in Zebrafish.
[0114] The zebrafish has become an important model to study vertebrate development, physiology, and human diseases. With respect to the circulatory system, the zebrafish not only has highly conserved pathways governing hematopoiesis, vasculogenesis and angiogenesis compared to mammals, it shares all major blood cell types with them. Therefore, the zebrafish is an excellent model organism in which to study vertebrate cardiovascular development. Largescale forward genetic screens have identified many zebrafish mutants modeling hereditary blood diseases, malignant hematologic disorders, developmental hematology, as well as altered heart development and cardiac function. Another advantage of the zebrafish model is that simple diffusion supplies oxygen to the embryo during the first ten days of development. Thus, embryos can survive and develop normally during this period with no heartbeat or circulating blood, which facilitates the study of the development of the circulatory system.
[0115] Given the tiny size of their larvae, several methods to calculate cardiovascular performance, angiogenetic processes, muscle function and integrity of motoneurons were developed over the last decade. We have used zebrafish for in vivo characterization of SERF2 using two application routes: 1) Injection of the native protein into the yolk sac of 3 day post fertilization (dpf) animals or 2) chronic incubation with the native protein to supply it via diffusion. The efficient uptake of the protein by both routes of administration allowed to investigate its effect on cardiac muscle growth, angiogenesis and apoptosis.
[0116] Method. SERF2 was administered by a) injection of the native protein into the yolk sac of 3 day post fertilization (dpf) animals and freshly fertilized eggs (2-8 cell stage) in various protein concentrations or chronic incubation with the native protein to supply it via diffusion. For in deep analysis of angiogenic effects flk-1 transgenic animals with gfp (green fluorescent protein) labelled endothelium were used. For all other experiments wildtype (wdt) animals were used.
[0117] Heart size was determined by measurement of end diastolic dimensions and calculation of end diastolic volume as described by Schwerte et al. (Schwerte et al. The Journal of Experimental Biology. 2003; 206(Pt 8):1299-1307).
[0118] Vascularization index. A cast of the vascular bed was obtained by accumulation of the shifting vectors of moving erythrocytes from a number of subsequent difference pictures, as described previously (by Schwerte et al., supra). In parallel to this flk-1 transgenic animals, which show green fluorescing endothelium, were imaged.
[0119] TUNEL assay for in situ staining of apoptotic cells Apoptotic. cells were detected by TUNEL technology using in situ Cell Death Detection Kit, Fluorescein (Roche Applied Science, Mannheim, Germany) according to the manufacturer's instructions.
[0120] Statistical Analysis. The acquired data statistically analyzed by using a two tailed students t-Test (Microsoft Excel) and significance was accepted when P<0.05. Data are presented as mean±S.E.M.
[0121] Conclusions. Treatment of zebrafish with SERF2 resulted in a significant increase of the animals heart volume. (see FIGS. 13 a & 13b). One of the most prominent findings was the high and significant increase in blood cell concentration by 50 to 100% compared to controls ( FIG. 14 ). Having in mind that this parameter is known from former studies to be more sensitive to physiological situations where increased oxygen delivery is needed, it may be a hint for increased vessel growth in later stages of zebrafish development than as already shown (Schwerte et al., supra). In vertebrates, blood vessels and blood cells have a common stem cell, the so called hemangioblast. It is known from the literature (Schwerte et al., supra) that the first response on hypoxia is an increased blood cell concentration before new vessels develop. From the physiological point of view this makes sense, because an increase in overall oxygen carrying capacity provides a faster response compared to newly developed vessels, which in turn have also to be filled with new blood and blood cells as well. Blood cell concentration is a central parameter in adjusting oxygen carrying capacity. In former studies it was shown that this parameter is more sensitive for physiological situations, where increased oxygen delivery is needed compared to vessel growth. At 7 dpf all but one treatment group show significantly increased blood cell concentrations. This increase was found in all drug delivery routes giving evidence that SERF2 can be delivered by both, incubation and uptake over the skin and injection and uptake over the gut ( FIGS. 15-17 ).
[0122] The reduced number of apoptotic cells in SERF2 treated animals reveals an obvious antiapoptotic effect of SERF2 in vivo ( FIGS. 18 a -18 b ).
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The present invention provides SERF2, a nucleic acid encoding said SERF2 or a cell expressing SERF2 for use as a medicament, in particular for use for use in treating or preventing an atrophy disease or condition or for increasing cellular growth in a patient such as sarcopenia, cachexia, dystrophy, hypoplasia, hypotonia, or muscle loss, as well as in vitro methods suitable for cell culture proliferation and pharmaceutical compositions.
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BACKGROUND OF THE INVENTION
The invention relates to a coupling device for elastic interconnection of a first and a second object.
A coupling device of this type is used, e.g., in vehicles in connection with mounting a wheel axle housing in a chassis of the vehicle, as disclosed, e.g., in U.S. Pat. No. 5,649,719.
If the coupling device's first contact device is securely connected to a central portion of the wheel axle housing, i.e. the first object, between and under two frame beams of the vehicle, and the second contact device is securely connected to a second end portion of two arms, whose first end portions are each rotatably connected to a frame beam, the object can be achieved that a movement of the wheel axle housing both in the vehicle's longitudinal direction and in the vehicle's horizontal transverse direction can substantially be prevented, while a relative movement of the wheel axle housing and the chassis in the height direction during a relative rotation or tilting of the chassis and the wheel axle housing at the linkage between the chassis and the first end portion of the arms, and a rolling of the wheel axle housing relative to the chassis are substantially possible.
The counteraction of the movement of the chassis in the vehicle's longitudinal direction and transverse direction depends on attempts being made hereby to compress portions of the rubber elastic material between the contact portions and on the rubber elastic material exerting substantial resistance against such a compression since it is virtually incompressible. However, the compression is not completely counteracted, since the material has a limited opportunity of escaping laterally at the material's free surfaces. The tilting is permitted since the rubber elastic portion is hereby mainly influenced only by a shearing stress and does not offer such great resistance against it.
FIG. 1 is a perspective view of such a known mounting of a wheel axle housing where a coupling device of the above-mentioned type is employed, with an exploded view of the components, and FIG. 2 illustrates a longitudinal section through the coupling device.
First end portions 6 , 8 of two arms 2 , 4 are each connected via respective screws 10 to the longitudinal frame beam 12 of a vehicle. The second end portions of the arms 2 , 4 converge at and are securely connected to a connecting piece 14 .
The connecting piece 14 is located above and in front of a wheel axle housing 16 . To the upper portion of this housing 16 , a bracket 20 with two arms 22 , 24 is attached by means of screws 18 .
The connecting piece 14 and the bracket 20 are interconnected by means of a coupling device 26 of the above-mentioned type by means of screws 27 , with the connecting piece 14 clasping the coupling device 26 .
As illustrated in FIG. 2 , the coupling device 26 comprises a sleeve-shaped device or rubber device 28 which is made of a rubber elastic material, and which has two conical end portions 30 , 32 , which are interconnected via an axial portion 34 .
Through the rubber device 28 there extends a first contact device 36 whose end portions have attachment areas 38 , 40 extending outwards past each end of the rubber device 28 and provided with holes 42 , 44 for the screws 27 . A central, extended portion or first contact portion 46 of the first contact device 36 extends radially outwards and is attached to the central portion 34 of the rubber device 28 .
Outside the rubber device 28 is mounted a second contact device comprising two annular contact portions or rings 48 , 50 , each of which abuts against an end portion 30 , 32 of the rubber device 28 .
The coupling device 26 is attached in a bore 52 which is provided in the connecting piece 14 , abutting against a shoulder 54 on one side and against a securing ring 56 on the other side.
Since the end portions 38 , 40 of the first contact device 36 project through and out of the rubber device 28 , taking up space radially, the radial measurement of the conical portions 30 , 32 of the rubber device 28 is consequently relatively small, with the result that these portions are not capable of appreciably counteracting a movement of the wheel axle housing 16 in the vehicle's transverse direction. This results in the vehicle having unsatisfactory driving characteristics.
Furthermore, the known coupling device is expensive and requires a great deal of space. Moreover, with the known device the wheel axle housing has to be located at a fixed height relative to the chassis when mounting the coupling device, resulting in a time-wasting assembly process.
Also U.S. Pat. No. 5,967,668 and U.S. Pat. No. 5,975,760 disclose coupling devices. None of these, however, show a specific arrangement of attachment area, rubber components and contact devices as in the coupling device according to the invention.
The object of the invention is to provide a coupling device of the above-mentioned type which is encumbered to a lesser extent by the above-mentioned disadvantages.
SUMMARY OF THE INVENTION
This object is achieved by a coupling device for elastic interconnection of a first and a second object, comprising
a device of a rubber elastic material, with two annular material portions, each of which extends round a longitudinal axis at an axial distance apart and with an inner and an outer, substantially conical side facing away from and towards the longitudinal axis towards respectively,
a first contact device which extends axially through the annular material portions and has first contact portions which are arranged to abut against respective inner sides of the material portions,
a second contact device with second portions which is arranged to abut against respective outer sides of the material portions,
where the first contact device has a first attachment area, whereby it can be attached to one of the objects.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described in greater detail with reference to the drawings.
FIGS. 1 and 2 illustrate a known coupling device.
FIG. 3 illustrate a first embodiment of a coupling device according to the invention and is a vertical longitudinal section through a vehicle along line III—III in FIG. 4 .
FIG. 4 illustrates a section along line IV—IV in FIG. 3 , through a coupling device according to the invention and adjacent portions of a vehicle.
FIGS. 5–7 illustrate other possible embodiments of the coupling device and are sections corresponding to that indicated by A in FIG. 4 , and through a second, third and fourth embodiment of the coupling device.
DETAILED DESCRIPTION OF THE INVENTION
As illustrated in FIGS. 3 and 4 , to a frame beam 60 of a vehicle there is attached via, e.g., a screw 62 , a first end portion 64 of an arm 66 of a pair of arms for mounting a wheel axle housing 82 . In a similar manner a second arm (not shown) of the pair of arms is attached to an opposite frame beam of the vehicle. From their first end portions 64 the arms extend backwards towards each other, and the second end portions of the arms 66 are securely interconnected via a connecting piece 68 ( FIG. 4 ). This connecting piece 68 is U-shaped, viewed from above, with two legs 70 , 72 which project backwards and have coaxial through-going bores 74 , 76 . In the radially internal surface of one bore 74 there is provided a radially inwardly open, circumferential groove 78 , and in the second bore 76 a shoulder 80 is provided in the radially internal surface portion.
On the wheel axle housing 82 there is provided an upwardly facing contact portion 84 with two upwardly open threaded holes. A hoop or curved piece 86 is arranged to be secured to the contact portion 84 by means of two screws 88 , 90 , which are screwed into their respective holes.
The arms' connecting piece 68 and the wheel axle housing 82 are interconnected via a coupling device 92 .
This coupling device 92 comprises a first contact device 94 in the form of a rotationally symmetrical axle with a longitudinal axis 95 . The contact device 94 comprises a first attachment area which is provided in the form of a central, circumferential, radially outwardly open groove or recess 96 , whose cross sectional shape is adapted to the cross sectional shape of the hoop 86 . This cross sectional shape is preferably radially inwardly tapering, and may be, for example, V-shaped or trapezoidal.
The first contact device 94 furthermore has two end portions or first contact portions 98 , 100 , whose surfaces 102 , 104 are provided in the form of conical surface portions tapering away from each other, where the longitudinal axes of the cones coincide with the longitudinal axis 95 .
The end portions 98 , 100 may have respective end journals 106 , 108 projecting away from each other and slightly out of the bores 74 , 76 .
The first contact device 94 abuts against and supports a device 110 of a rubber elastic material. This device 110 comprises two annular material portions or pieces 112 , 114 , each of which has a radially internal surface 116 , 118 and a radially external surface 120 , 122 in the form of coaxial conical surface portions.
Radially outside the rubber elastic device 110 there is provided a second contact device 140 comprising second contact portions, or more specifically a first ring 124 and a second ring 126 , each with a radially internal, conical surface 128 , 130 which is adapted to the external surface 120 , 122 of the material portions 112 , 114 , and a radially external, cylindrical surface 132 , 134 , whose diameter is adapted to the diameter of the bores 74 , 76 in the legs 70 , 72 of the connecting piece 68 .
The connecting device 92 can be secured to the legs 70 , 72 by the first ring 124 having a second attachment area 121 , which is arranged to abut against a lock ring 136 , which is inserted in the groove 78 of the leg 70 , and in the same way by the second ring 126 having a second attachment area 123 which is arranged to abut against the shoulder 80 of the leg 72 . The lock ring 136 can be brought into the groove 78 after the coupling device's rubber elastic material has been elastically compressed in the axial direction towards the right in FIG. 4 , the coupling device hereby leaning against the shoulder 80 . By this means it is ensured that the annular material portions 112 , 114 are secured without play between the first and the second contact devices.
Alternatively, in the bore 74 screw threads may be provided and the lock ring may have external threads whereby it can be screwed to forceful abutment against the first ring 124 of the second contact device 140 .
Furthermore, the coupling device 92 is fixed to the wheel axle housing 82 by the hoop 86 extending in the central groove 96 of the first contact device 94 and being secured thereto by means of the screws 88 , 90 which are screwed into the threaded holes of the wheel axle housing 82 .
Each of the annular material portions or pieces 112 , 114 may be constructed from several layers of rubber elastic material, between which are mounted corresponding conical reinforcing elements or rings 127 of a strong and rigid material, e.g. metal. The volume of the rubber elastic material which can be forced out or can swell out at free end surfaces of the rubber elastic material can thereby be reduced and the compression resistance of this material can increase, while maintaining the desired pliability of the material in relation to shearing forces. A metal ring corresponding to the reinforcing rings, can mark the radially internal end of the rubber elastic device 110 and be glued to the adjacent rubber elastic material.
The coupling device's components, i.e. the first contact device 94 , the rubber elastic device 110 and the second contact device 140 may be securely interconnected by means of, e.g., an adhesive or the like.
The first contact device 94 may be produced with or without end journals 106 , 108 , since the purpose thereof is to prevent a separation of the wheel axle housing and the connecting piece if the coupling device should fail.
It will therefore be understood that the rings 124 , 126 may extend all the way to the longitudinal axis of the first contact device. Thus the radial extent of the material portions 112 , 114 may be substantial, with the result that the portion of the connecting piece 68 which prevents a movement of the wheel axle housing in the vehicle's transverse direction and height direction is substantial, since an escape of rubber elastic material is largely prevented, while a deformation of this material as a result of shearing stresses becomes possible.
Even though there should be a need for end journals 106 , 108 , their diameter will be able to be much smaller than the diameter of the attachment areas 38 , 40 according to the prior art, since the end journals 106 , 108 act as an emergency device, which comes into force in the event of the destruction of the rubber elastic material device, and thus only require to be designed to withstand a load which occurs once.
It is stated above that the contact device of the coupling device comprises a first contact device or axle with a first attachment area which is provided in the form of a circumferential, radially outwardly open groove, wherein there may be inserted a radially internal portion of a hoop. As illustrated in FIG. 5 , a corresponding axle 94 ′ may instead have a first attachment area which is provided in the form of a central, radially outwardly projecting bead 144 , where a hoop 86 ′ corresponding to the hoop 86 may have a radially inwardly projecting groove 146 , which can be brought into engagement with the bead 144 in order to secure the axle 94 ′.
It will further be appreciated that a corresponding axle 94 ″ may have a cylindrical, central portion 148 and that, instead of a groove or a bead, a corresponding hoop 86 ″ may have a radially inwardly facing cylindrical portion 150 , which can be brought into abutment against the cylindrical portion 148 of the axle 94 ″, as illustrated in FIG. 6 . If the hoop 86 ″ is sufficiently firmly secured to the axle 94 ″, the object can be achieved that the frictional force which is exerted between these components is so great that a relative movement of the hoop 86 ″ and the axle 94 ″ is prevented.
Finally, an axle 94 ′″, as illustrated in FIG. 7 , may instead by attached to a wheel axle housing by means of, e.g., two screws (not shown) which extend through holes 150 , 152 in the shaft 94 ′″, and which can be screwed into threaded holes which are provided in the wheel axle housing (not shown).
A coupling device is described above for use in connection with a vehicle. It will be appreciated, however, that this coupling device may be employed in connection with any kind of device where there is a need for a corresponding relative movement of two objects, such as any other kind of transport means or other device. Even though it is stated above that the coupling device 92 connects the connecting piece 68 to the wheel axle housing 82 , it will therefore be understood that a coupling device according to the invention is generally arranged to connect two objects with each other in the above-described manner.
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A coupling device for elastic interconnection of, e.g., arms ( 66 ) which are linked to a frame ( 60 ) of the vehicle. The coupling device ( 92 ) substantially comprises two annular, conical portions ( 112, 114 ) of a rubber elastic material and an axle ( 94 ). A radially internal side of these annular material portions ( 112, 114 ) abuts against contact portions ( 98, 100 ) at the ends of the axle ( 94 ). The coupling device ( 92 ) further comprises two axially opposite rings ( 124, 126 ) which are arranged to abut against respective external sides of the annular material portions ( 112, 114 ). The axle ( 94 ) and the rings ( 124, 126 ) have attachment areas ( 96, 121 and 123 respectively), via which they can be attached to the wheel axle housing ( 82 ) and the frame ( 60 ) respectively. The attachment area ( 96 ) for the axle ( 94 ) is located between the first contact portions ( 98, 100 ).
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BACKGROUND OF THE INVENTION
[0001] Rigid endoscopes usually have an optical system consisting of an objective, an ocular and between them a relay lens system consisting of several relay sets. Because the objective and each relay set is producing an image which is turned up-side down, and because a standard endoscope should produce an upright image, usually an odd number of relay sets is used so that the image produced by the optical system is upright.
[0002] Generic relay sets, as shown in U.S. Pat. No. 4,676,606 and U.S. Pat. No. 4,693,568, have a symmetrical arrangement of lens units so that the relay set is consisting of two symmetric half sets.
[0003] Known relay sets have the disadvantage that they need highly complicated calculations to design a relay set with desired optical properties, i.e. with corrected lens aberrations. If a relay set is correctly designed, it has a fixed configuration and it is mass produced in this configuration to be used several times in an optical system.
[0004] The disadvantage of the relay set, according to the state of the art, is that according to its fixed configuration it also has a fixed overall length. This means that an optical system; at reasonable costs, can only be produced having a length that is a multiple (normally odd multiple) of the length of the relay set. If a standard resectoscope has three relay sets and a longer resectoscope is needed, it is necessary to use five relay sets so that the overall length of the ocular is almost double. If an only slightly elongated endoscope is needed, a relay set with a length other than the standard length is needed and has to be completely redesigned. Such a complete redesign of a relay set is extremely complicated and expensive.
BRIEF SUMMARY OF THE INVENTION
[0005] The objective of the present invention is to make the design of endoscope with different lengths easier and less expensive.
[0006] According to the invention, the lens units in each half set of the relay set and seen from the center are having the following refractive power (Positive and Negative in the following are called P and N): P,N,P,P. For the complete relay set this is P,P,N,P, (center), P,N,P,P. To make a relay set according to the state of the art with a new length, requires a complete recalculation of all distances of the lens units and also of the lens units themselves. Quite to the contrary, according to the invention a recalculation of the overall length of the relay set requires only finding new distances of the lens units. No changes with the lens units themselves are necessary. The correction of lens aberrations remains unaffected by the change of overall length. With the same set of lens units, using only different distances, a new overall length of the relay set can be achieved. Finding the correct placement of the lens units for a new overall length of the relay set is quite simple. For a given set of lens units simple formulas or curves can be given according to which all the places of the lens units for a desired overall length easily can be found. With the relay set according to the invention, therefore, it is an easy design step to change the overall length of the set. If an endoscope with a special overall length is needed, the invention allows for the simple design of relay sets of an appropriate length. The relay set according to the invention can be mixed in an optical system with conventional relay sets. If a given endoscope having three conventional relay sets each 60 mm long, has to be made 10 cm longer, one additional conventional relay set and one relay set according to the invention with a length of 40 mm can be added.
[0007] It is advantageous to have the corresponding lens units of the two half sets at symmetrical distances from the center. With this design the magnification of the lens unit is 1 as it is generally required.
[0008] Having the outer lenses in an asymmetrical position, the magnification is different from 1. The advantages of previous embodiments of the invention with respect to easy calculation of the overall length remain also with this embodiment.
[0009] It is advantageous to place a glass rod in the middle of the relay set. This is a well known measure to reduce the air length.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] In the drawings examples of the invention are schematically shown.
[0011] FIGS. 1 a - d show the arrangement of the lens units of a relay set in four different overall lengths;
[0012] FIGS. 2 a - c show the lens units of a relay set having the same length but three different magnifications;
[0013] FIG. 3 shows a conventional optical system with three conventional relay sets; and
[0014] FIGS. 4 a - c show an optical system having four conventional relay sets and one relay set according to the invention in three different lengths.
DETAILED DESCRIPTION OF THE INVENTION
[0015] FIGS. 1 a - d show relay sets according to the invention in different lengths.
[0016] In FIG. 1 a , a relay set 1 a is shown which, according to the invention, has two half sets 2 a and 2 b being symmetrically arranged with respect to the center of the relay set 1 which in the drawing is indicated by a center line 5 . From the center line 5 to the outside, the half set 2 a has lens units 3 a 1 , 3 a 2 , 3 a 3 and 3 a 4 . The half set 2 b has lens units 3 b 1 , 3 b 2 , 3 b 3 and 3 b 4 . The lenses of the pairs 3 a 1 - 3 b 1 , 3 a 2 - 3 b 2 , 3 a 3 - 3 b 3 and 3 a 4 - 3 b 4 are identical and are symmetrically placed with respect to the center line 5 . According to the invention, the refractive powers of the lens units are: 3 a 1 and 3 b 1 positive, 3 a 2 and 3 b 2 negative, 3 a 3 and 3 b 3 positive and 3 a 4 and 3 b 4 positive. This is indicated with the letters P and N underneath FIG. 1 a.
[0017] To the left and to the right of the relay set 1 a image planes 6 a and 6 b are shown. Because of its symmetrical arrangement, the relay set 1 is transporting an image from 6 a to 6 b or vice versa with the magnification 1 .
[0018] In FIG. 1 , the relay set 1 a is shown with a certain overall length.
[0019] In FIG. 1 b and in FIG. 1 c , relay sets 1 b and 1 c are shown having different overall lengths. As can be seen from FIG. 1 , for all three lens sets 1 a , 1 b and is exactly the same lens units are used. Only their relative distances from the center line 5 are varied. In all three configurations the magnification is 1. Only the overall length is different. Also the correction of lens aberrations remains the same. All major lens aberrations are sufficiently corrected.
[0020] If the relay set 1 a is correctly designed in one overall length as shown in FIG. 1 a , the variation of overall length is easily achieved. As can be seen from FIGS. 1 a to 1 c , the variation of lens positions follows simple relations.
[0021] The lens units 3 a 1 to 3 b 4 do not require any redesign. According to the invention, it is only necessary to have the lens units chosen with proper refractive power, namely 3 a 1 and 3 b 1 with positive power, 3 a 2 and 3 b 2 with negative power, 3 a 3 and 3 b 3 with positive power and 3 a 4 and 3 b 4 with positive power.
[0022] Following the before mentioned rule, the lens units can vary in shape from the embodiment shown in FIGS. 1 a to 1 c . Instead of the simple lenses shown in the drawing lens units of cemented type, composed of several different glasses can also be used.
[0023] FIG. 1 d shows an alternative relay set 1 d . The lenses 3 a 1 to 3 a 4 and 3 b 1 to 3 b 4 are the same as with 1 a . In the center gap between lenses 3 a 1 and 3 b 1 , a glass rod 7 with parallel end faces is placed in order to reduce in the big center gap between the half-sets 2 a and 2 b , the distance through which the light has to travel through air.
[0024] According to FIGS. 1 a to 1 d , the arrangement of lenses in the two half sets 2 a and 2 b is symmetrical with respect to the center line 5 . Due to this symmetrical arrangement of lens units the magnification of the relay sets 1 a to 1 c is 1 . An alternative possibility is shown in FIG. 2 .
[0025] FIG. 2 a shows a relay set 11 a having a similar design as relay set 1 a of FIG. 1 a . According to the invention, is the relay set 11 a again has a symmetrical arrangement of lens units with a sequence of refractive power P,N,P,P in each half set.
[0026] FIG. 2 b shows a relay set 11 b using exactly the same lens units as in relay set 11 a . As shown in FIG. 2 , the overall length of relay set 11 a and relay set 11 b are the same. But in the relay set 11 b , the outermost lenses 14 a and 14 b are shifted asymmetrically. Due to this asymmetrical arrangement of lenses the magnification is different. In this case it is 0.75.
[0027] FIG. 2 c shows relay set 11 c again having the same lenses as relay set 11 a . The outermost lenses 14 a and 14 b , as can be seen in FIG. 2 c , even more shifted asymmetrically as with lens unit 11 b . The overall length again is the same as that of the relay sets 11 a and 11 b . The magnification of the relay set 11 c is 0.5. It has to be remarked that in the examples shown in FIGS. 2 a to 2 c , the magnifications given as 1 for FIG. 2 a, 0.75 for FIG. 2 b and 0.5 for FIG. 2 c , are valid for rays passing the lens units from left to right. If the light goes from right to left the magnifications are 1 in FIG. 2 a, 1.33 for FIGS. 2 b and 2 for FIG. 2 c.
[0028] The relay sets 11 a , 11 b and 11 c of FIG. 2 have the same advantage as the lens unit 1 shown in FIG. 1 with respect to the possibility to easily change the overall length.
[0029] The relay sets shown in FIGS. 1 and 2 are used in rigid endoscopes as shown, for example, in FIG. 13 of U.S. Pat. No. 4,693,568. According to the standard design of rigid endoscopes, a rigid metal tube, not shown, is enclosing an optical system as shown in FIG. 3 .
[0030] The optical system of FIG. 3 is of a conventional design having an objective 20 , three relay sets 21 and an ocular 22 . The relay sets 21 are identical. They may be of any conventional design according to the state of the art as mentioned in the introduction. To keep the image upright, the number of relay sets 21 is odd.
[0031] If a longer endoscope is needed, additional relay sets can be added. This is shown in FIG. 4 a . To the right of the optical system, two additional relay sets are added. One of them is another conventional relay set 21 . The other one is a relay set 23 a designed according to the present invention, e.g. a relay set as shown in FIG. 1 or 2 . As can be seen from FIG. 4 a , the relay set 23 a is shorter than the relay set 21 so that a desired specific overall length of the endoscope results. As shown in FIGS. 4 b and 4 c , relay sets 23 b or 23 c of different lengths can replace 23 a so that any required overall length of the endoscope is possible.
[0032] Additionally, it is possible to replace any of the conventional relay sets 21 by a relay set 23 a , according to the present invention, so that the overall length of the endoscope can be adjusted to any required length. For special purposes, a relay set according to FIG. 2 , having a magnification smaller or bigger than 1, can be used.
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A relay set ( 1, 11, 23 ) for the optical system of a rigid endoscope, the optical system comprising an objective ( 20 ) at the distal end, an ocular ( 22 ) at the proximal end and between them a relay lens system consisting of several relay sets ( 1, 11, 21, 23 ), the relay set ( 1, 11, 23 ) consisting of two half sets ( 2 a , 2 b ) having the same lens units ( 3 a 1, 3 a 2, 3 a 3, 3 a 4; 3 b 1, 3 b 2, 3 b 3, 3 b 4 ) arranged in symmetrical sequence with respect to the center ( 5 ) of the set, wherein each half set ( 2 a , 2 b ) consists of four lens units ( 3 a 1, 3 a 2, 3 a 3, 3 a 4; 3 b 1, 3 b 2, 3 b 3, 3 b 4 ) having in the sequence of raising distance from the center ( 5 ) the refracting powers Positive, Negative, Positive, Positive (P, N, P, P).
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CROSS-REFERENCE TO RELATED PATENT APPLICATIONS
This application is a 371 National Stage of PCT Patent Application No. PCT/US2013/067051, filed Oct. 28, 2013, which claims priority to U.S. Provisional Application No. 61/716,769 filed Oct. 29, 2012, herein incorporated by reference in their entirety.
GOVERNMENT RIGHTS
This work was supported by the MRSEC Program of the National Science Foundation under Award Number DMR-0820341 and also by the National Science Foundation Grant ChE-0911460.
FIELD OF THE INVENTION
This invention is directed to compositions of matter, and also articles and methods of manufacture related to assembly of colloidal particles having specific directional bonding. More particularly the invention is directed to a method for making selectable colloidal analogues of atoms having valence characteristics, including forming colloidal particles with chemically functionalized patches which form specific directional bonds through non-covalent interactions.
BACKGROUND OF THE INVENTION
Self-assembly of colloidal particles is of great interest and importance due to its potential applications in many fields of use, such as for example, biomaterials, catalytic supports, atomic/molecular phase behavior study and photonics. The ability to design and assemble 3-dimensional structures from colloidal particles is limited by the absence of specific directional bonds. As a result, complex or low-coordination structures, common in atomic and molecular systems, are rare in the colloidal domain.
The past decade has seen an explosion in the kinds of colloidal particles that can be synthesized. A wide variety of new shapes have been made, from rods and cubes to clusters of spheres and dimpled particles and also other types of anisotropic particles including Janus particles, branched particle, triangles and polyhedrons. The self-assembly of such building blocks is largely controlled by their geometry, and thus, only a few relatively simple crystals have been made: face-centered and body-centered cubic crystals and variants. Colloidal alloys increase the diversity of structures, but many structures remain difficult or impossible to make. For example, the diamond lattice, predicted more than 20 years ago to have a full 3-dimensional photonic band gap, still cannot be made by colloidal self-assembly because it requires fourfold coordination. Without directional bonds, such low-coordination states are unstable.
In contrast to colloids, atoms and molecules control their assembly and packing through valence. In molecules like methane (CH 4 ), the valence orbitals of the carbon atom adopt sp 3 hybridization and form four equivalent C—H bonds in a tetrahedral arrangement. In the colloidal domain, the kinds of structures that could be made would vastly increase if particles with controlled symmetries and highly directional interactions were available. Consequently, what is needed are colloids with a form of “valence” characteristic which would advantageously resolve a wide variety of commercial needs heretofore not met.
SUMMARY OF THE INVENTION
The present invention concerns a general method for creating colloidal analogues of atoms with valence. Colloidal particles with chemically functionalized patches can be established to form highly specific and directional bonds. The “valences” of these new “colloidal atoms” possess virtually all the common symmetries—and some uncommon ones—characteristic of hybridized atomic orbitals, including without limitation, s, p, sp, sp 2 , sp 3 , sp 3 d, sp 3 d 2 , and sp 3 d 3 . In this methodology various patches (amidinated and carboxyl) can be applied to achieve these features wherein the chemical functionality of the patches is programmable and specific using synthetic organic or biological molecules and macromolecules with supramolecular interactions. For example, tri-block copolymers with metal coordination terminals, DNA with single-stranded “sticky ends” are functionalized on particle patches, thereby creating colloidal atoms from which different kinds of “colloidal molecules” can be assembled. Because the bonds between these new colloidal atoms are highly directional and fully controllable (length scale, strength and reversibility), they open up the possibility of building new low-coordinated open structures, both amorphous and crystalline, which is emerging as a key design feature for assembling colloids with photonic band gaps and also for achieving other “valence” sensitive structures. For example, tetravalent particles can form a three dimensional colloidal diamond lattice, and trivalent particles can form a two dimensional Kagome structure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a scheme illustrating the preparation of colloidal particles with functionalized patches (synthetic or biological molecules and macromolecules) with well-defined symmetries; a 4-patch particle is shown as an example. (1) a cluster of 4 polystyrene microspheres, prepared by a conventional method is swollen with styrene such that the extremities of the cluster, a tetrahedron in this case, protrude from the styrene droplet; (2) the styrene is then polymerized and the protrusions from the original cluster become patches with at least one of the surface properties: sulfonated, amidinated or carboxylated; (3) depending on the type of surface property, the patches are functionalized with small molecules, polymers, protein or oligonucleotides, using non-covalent and covalent coupling methods;
FIG. 2 a shows electron micrographs of colloidal clusters (amidinated particles are taken as an example), showing the particle configurations for clusters of n=1 to 7 microspheres; FIG. 2 b shows electron micrographs of amidinated patchy particles after encapsulation. The patches inherit the symmetries of their parent clusters; and FIG. 2 c shows confocal fluorescent images verifying the functionalization of DNA oligomers on patchy particles; the fluorescence comes from the dye-labeled streptavidin that links DNA with the patches. (Scale bar, 500 nm);
FIGS. 3 a -3 c show optical microscope bright-field images of sulfonated cluster tetramers before swelling ( FIG. 3 a ); swollen with styrene ( FIG. 3 b ) and after styrene is polymerized ( FIG. 3 c ). Purified particles are shown to demonstrate that clusters of the same order can be swollen by the same amount of styrene, leading to same configuration of the resulting patchy particles;
FIGS. 4 a and b show electron micrographs of patchy particles and that the sizes of patches can be adjusted by changing encapsulation conditions; FIG. 4 a in particular shows particles with relatively large patches which are fabricated when clusters are swollen with 1.0 mL of styrene monomer; primary spheres are 540 nm in diameter; FIG. 4 b shows under identical conditions of FIG. 4 a , but smaller patches are obtained when more monomer, 1.2 mL, is added; and FIG. 4 c shows smaller patches, relative to particle size, obtained using primary microspheres 850 nm in diameter; using larger particles facilitates observation under an optical microscope; divalent, trivalent and tetravalent particles from this batch are used in the colloidal molecule formation, and the monovalent particles are used in kinetics study (the arrow indicates decreasing patch size. Scale bars, 500 nm.);
FIGS. 5 a -5 c show the number distribution of the patchy particles and their separation with FIG. 5 a shows an electron micrograph of a mixture of amidinated patchy particles before they are separated by density gradient centrifugation; particles of the same order n have the same configuration and some of the higher order (n>7) particles are circled; their patch geometries extend beyond those of atomic orbitals. (Scale bar, 2 μm.); optical micrographs are shown in FIGS. 5 b and 5 c of test tubes containing patchy particle suspensions fractionated by density gradient centrifugation; and each white band represents a region of high concentration of identical patchy particles, wherein in FIG. 5 b patchy particles are fabricated from clusters using high shear, resulting in the formation of relatively more lower valence particles; eight bands are visible with the highest number being the monovalent patchy particles; in FIG. 5 c shows patchy particles fabricated from clusters using low shear; this results in the formation of a greater percentage of patchy particles with higher valence; twelve distinct bands corresponding to patchy particles, from monovalent to 12-valent, are visible, with the most pronounced band corresponding to trivalent patchy particles;
FIG. 6 a shows the small molecules and tri-block copolymer bearing —OHs anchoring groups as well as palladated pincer or pyridine as metal coordination groups; FIG. 6 b shows the scheme of palladated pincer-pyridine activation and ligand exchange' palladated pincer-Cl could be activated by addition of silver tetrafluoroborate in order to realize metal coordination with pyridine; a stronger ligand, triphenlyphosphine, can replace pyridine and bond to palladium;
FIGS. 7 a -7 d show the functionalization of the particle patches by esterification; in FIG. 7 a is shown a fluorescent microscopic image of carboxyl patchy particle after attachment of —OH dye molecules; FIG. 7 b shows fluorescence intensity measurements of 2-patch particles; the patch part has brighter fluorescence than that of the matrix; FIG. 7 c shows confocal fluorescence image of the dye labeled 2-patch particles showing that only the core clusters are visible; FIG. 7 d shows a schematic of the particle functionalization mechanism in THF;
FIGS. 8 a - f show bright field (left), confocal fluorescent (middle), and schematic images (right), of colloidal molecules self-assembled from patchy particles; FIG. 8 a shows complementary green and red monovalent particles form dumbbell-shaped AB type molecules. Supra-colloidal molecules AB 2 , AB 3 , and AB 4 are formed by mixing red monovalent with green; ( FIG. 8 b ) divalent; ( FIG. 8 c ) trivalent; and ( FIG. 8 d ) tetravalent particles; FIG. 8 e shows mixing complementary divalent particles, linear alternating polymer chain spontaneously assembles; FIG. 84 f shows when particles with bigger patches are used, cis-trans-like isomers can form; introducing more monovalent particles leads to ethylene-like colloidal molecules. (Scale bars, 2 μm);
FIGS. 9 a and b show schematic images and snapshots from movies with step-by-step reactions between colloidal atoms; bent arrows point from the colloidal atom to the site where it is going to attach; straight arrows indicate time sequence; FIG. 9 a also shows monovalent particles attaching to tetravalent particle, one by one, forming an AB 4 type colloidal molecule; and FIG. 9 b shows complementary divalent particles polymerizing into a linear chain structure. (Scale bar, 2 μm);
FIGS. 10 a -10 c show the self-assembly and dissociation of pincer and pyridine functionalized divalent particles triggered by addition of AgBF 4 and triphenylphosphine; FIGS. 10 a, b and c (left panel) show bright field images and FIG. 10 d right panel shows the schematic images of stepwise interactions of 10 a - 10 c.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In one preferred embodiment the fabrication and functionalization of patchy particles is summarized in FIG. 1 . Specifically, the fabrication can begin with preparing cross linked polystyrene microspheres (with at least one of amidinated, carboxylated or sulfonated surface functionality); and these microspheres are preferably micrometer or sub-micrometer in diameter. Small clusters of these microspheres can be assembled using a conventional emulsion-evaporation method. This process produces so-called “minimal-moment” clusters with reproducible symmetries and configurations: for example, some such symmetries include without limitation spheres, dumbbells, triangles, tetrahedra, triangular dipyramids, octahedra, and pentagonal dipyramids, for clusters of n=1 to 7 particles (see FIG. 2 a for amidinated clusters as a specific example).
Patchy particles are formed from the clusters preferably using a two-stage swelling process followed by polymerization. First, a low-molecular weight, water-insoluble organic compound (1-chlorodecane) is introduced into the colloidal clusters that are suspended in water with surfactant (sodium dodecyl sulfate, SDS). Adding a small amount of acetone to the suspension aids in the transport of the 1-chlorodecane into the colloidal clusters. Subsequent stripping of the acetone from the solution traps the 1-chlorodecane in the polymer clusters. An oil-soluble initiator, such as, benzoyl peroxide (BPO) (or Azobisisobutyronitrile, AIBN) and 1,2-dichloroethane, are introduced which dissolves the initiator and is miscible with 1-chlorodecane. The clusters are then swollen by a styrene monomer. The 1-chlorodecane which has been introduced earlier acts as an osmotic swelling agent that increases the amount of monomer that can be absorbed by the clusters. Since each cluster of a given number of particles contains the same amount of swelling agent, chemical equilibrium assures that different clusters of the same size all swell by about the same amount, with the total amount of swelling controlled by the quantity of added monomer. The bright-field optical images of clusters and styrene swollen clusters are shown in FIGS. 3 a and b , sulfonated particles are chosen as a specific example.
After swelling, the styrene is polymerized by thermally degrading the initiator previously introduced into each cluster ( FIG. 3 c ). Swelling is controlled so that the extremities of the original clusters are not encapsulated, but are left as patches. Clusters of the same order n are encapsulated to the same extent, leading to uniform patch configurations. Using initiators such as BPO ensures that there are no functional groups introduced, so the surface created by swelling the clusters—the “anti-patch” surface—is chemically inert and different from the patches. Only the patches have the amidinated, carboxylated or sulfonated functional groups. As can be seen in FIG. 2 b , the particles have distinct patches; and their morphology is well characterized by SEM.
Patch size is controlled during the swelling process by adjusting the amount of monomer that is introduced: the more monomer that is added, the smaller the patches are. FIGS. 4 a -4 c show that considerable variation in patch size can be achieved in this way. Small patches favor greater directionality, while larger patches permit multiple links per patch.
This method will provide samples containing large scalable quantities of particles having different “valence” (numbers of patches, FIG. 5 a ). Essentially all the starting colloidal particles are converted into particles with one or more such patches. Adjusting the emulsification conditions used when making the clusters changes the relative distribution of particles with different valence. Using a higher shear rate, for example, makes smaller emulsion droplets, which skews the distribution towards lower-valence particles. To fractionate the particles, we use density gradient centrifugation, obtaining up to twelve clear bands corresponding to particles with different valence (see FIGS. 5 b and c ). The Table below summarizes the fraction of particles obtained in each band for two different shearing conditions. For the lower shear preparation, each of the four upper bands, which correspond to particles with 1 to 4 patches, contains 108 to 109 identical particles. For the higher shear preparation, greater quantities are produced in the upper bands and lower quantities are produced in the lower bands. In most cases, conditions are used that produce the most 2-, 3- and 4-patch particles, which are most advantageous for making analogues of common molecules.
Table 1 shows the quantities of particles in the different bands. Density gradient centrifugation is used to fractionate the patchy particles. The fraction of identical particles obtained from a single centrifuge tube is shown in the Table. Fractions of 10%-20% correspond to 10 8 ˜10 9 particles in a single fractionation. Up to 3% of the particles appear in higher order bands comprising particles with 8-12 patches. The remainder of the particles, up to 20%, accumulates as sediment at the bottom of the centrifuge tube. This consists primarily of particles with 1 to 7 patches and can be recovered and purified by a second density gradient fractionation. These fractions were estimated from their number ratio relative to lower valence particles observed under a microscope.
TABLE 1
Number of patches
1
2
3
4
5
6
7
High shear
61%
15%
4%
1%
0.2%*
0.02%*
0.001%*
Low shear
7%
16%
25%
15%
8%
5%
3%
In a most preferred embodiment a key design feature of our method is the use of clusters as intermediates. The charged functional groups (sulfonated, amidinated and carboxylated) on the colloid surface are important to the patchy particle fabrication process. First, the positive/negative charge, along with the SDS surfactant, stabilizes the microspheres as well as the clusters by electrostatic repulsion. Moreover, when the clusters are swollen and encapsulated, the charges make the patches of the cluster more hydrophilic than the monomer-water interface, which is stabilized only by SDS. This difference in interfacial energies leads to finite contact angles and well-defined patches. Also, the clusters' diversity in particle number and symmetry, surface functionality are all translated directly to the number (1, 2, 3-patches etc.) and symmetry (linear, triangular, tetrahedral, etc.) and the functionality (amidinated, carboxylated, and sulfonated) of the particle patches. Examples 1-3 provided hereinafter illustrate preparation of amidinated, carboxylated and sulfonated patchy particles, respectively.
In another aspect of the invention patchy particle functionalization can be carried out as described hereinafter. For example, patchy particles can be site-specifically functionalized due to the presence of amidine or carboxylic acid groups on the patch surface. Site-specific functionalization the particle patches with small molecules, synthetic polymers and biological materials bearing recognition units (“RU” hereinafter) will enable the directional interactions required for particular self-assembled structures. Either a covalent or non-covalent, or a strategy combing both can be employed.
The amidinated patches can be functionalized with biotin, to which DNA with single-stranded “sticky” ends is attached using a biotin-streptavidin-biotin linkage. Sulfo-NHS-Biotin (Biotinamidohexanoic acid 3-sulfo-N-hydroxysuccinimide ester sodium salt), is a water-soluble biotin derivative which can be used to be attached to the patchy particles. This step is preferably carried out in buffer solution, (Phosphate-buffered saline, PBS, pH=7.42), where the N-hydroxysuccinimide ester (NHS) can react with amidine groups and covalently link the biotin to the patches. Triton X-100, a non-ionic surfactant, is used as well. This small molecules surfactant can absorb onto patchy particle surface and stabilize the particle by steric repulsion. However, they are short enough that the patches can still be functionalized with biotin.
The DNA oligomer is prepared separately and it has three parts. At the 5′ end, it has a biotin as an anchoring molecule and in the middle, a 49 base-pair double helix is present as a spacer. Finally, a single strand of 11 complementary or 8 palindrome base pairs is located at the 3′ terminus, forming the sticky end. Streptavidin acts as a connector to link the DNA to the patches. Specifically, in the preferred embodiment DNA is first mixed with streptavidin in a 1:1 ratio, to form a streptavidin-DNA complex. This complex is then mixed with the biotin-functionalized patchy particles, thus producing DNA-functionalized patchy particles. The streptavidin contains a fluorescence tag so that it can be visualized using confocal microscopy. The resulting product is shown in FIG. 2 c . Only the patches of the particle show fluorescence, indicating the streptavidin-DNA complex successfully coats the particle patches, and the amidine-NHS chemistry used for biotin functionalization performs as designed. This method efficiently produces DNA functionalized patchy particles. Meanwhile, biotin (small molecule) conjugated patchy particle and streptavidin (protein) conjugated patchy particles can be fabricated as intermediates, which are also very useful in colloidal assembly. An example of this methodology is provided hereinafter as Example 4.
In another aspect of the invention functionalization of carboxylated patchy particles is carried out under the assistance of a coupling reagent N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC). EDC is used to conjugate carboxylic acid with primary alcohol (—CH 2 OH) or amine (—CH 2 NH 2 ) in water and various organic solvents. In aqueous solution, patchy particles are functionalized with streptavidin or nucleotide with primary amine terminals by forming covalent amide bonds, which creates protein/nucleotide conjugated patchy particles.
In organic solvents, such as tetrahydrofuran (THF), synthetic small molecules and polymers bearing —OH groups are disposed on the patches by EDC coupling. A series of small molecules and polymers designed and synthesized for this purpose are listed in FIG. 6 a . These molecules and macromolecules have common features and consist of 3 parts, namely primary alcohol (—CH 2 OH) groups, an RU at the opposite end of the molecule and a spacer located therebetween.
The small molecules, sPincer and sPyridine were prepared by multiple step organic synthesis. The triblock copolymer pPincer was synthesized by ring-opening metathesis polymerization (“ROMP” hereinafter) of functional norbornene monomers sequentially using Grubbs 1 st catalyst. The length of the polymer and the ratio of different blocks (corresponding to the numbers for m, n, l in FIG. 6 a ) can be changed by varying the amount of Ruthenium catalyst and monomers. ROMP is a living polymerization methods including ATRP (atom transfer radical polymerization), RAFT (reversible addition-fragmentation chain-transfer polymerization) and NMP (nitroxide mediated radical polymerization) can also be employed by which the molecular weight, polydispersity and functionality of the resulting polymers can be well controlled.
There are three advantages when THF is used. First, supramolecular recognition units, such as hydrogen bonding and metal coordination, can achieve sufficient association strength in THF, which is needed to assemble the anisotropic particles into entropically unfavorable configurations. Second, the EDC coupling reaction can be carried out in organic solvent with ease and high yield. EDC decomposes in water gradually, while in organic solvent, it has much higher efficiency. Finally, if patchy particles with crosslinked matrix are used, although swollen, the shapes of the patchy particles are preserved in THF. FIGS. 7 a -7 d show an example of the successful covalent attachment of a fluorescence molecule on carboxylated patchy particle on the patches. Covalent functionalization can provide particles which are more stable under different conditions such as heat, solvent switching. The number and density of surface functionalization stay constant. Examples 5 and 6 provided hereinafter describe carboxyl patchy particle functionalization and use of an organic small polymer/triblock copolymer with RU, respectively.
In another aspect of the invention, self-assembly of patchy particles by directional non-covalent interactions can be accomplished. Bonding between particles occurs through patch-patch interactions, and thus the location and functionality of the patches can endow particles with bonding directionality and “valence.” Self-assembly of those patchy particles is realized by non-covalent interactions, i.e., hydrogen bonding and metal coordination and columbic interactions. Examples of DNA hybridization and palladated pincer-pyridine coordination are discussed below.
DNA is widely used for linking nanoparticles because DNA can be synthesized in a programmable manner with control over the length and sequences of functional groups, which, in turn, controls the specificity and the strength of interaction. DNA oligomers about a few to tens of nanometers in length provide short-range attractions compared to the size of the colloids, and thus enforce the directionality defined by the particle patches. Another advantage of using DNA is that the hybridization of the complementary strands is fully reversible, and the dissociation takes place within a narrow temperature range (T m ). Particle self-assembly can thus be manipulated simply by varying temperature and other parameters, such as salt concentration.
Following the strategy mentioned above, purified patchy particles can be formalized with complementary DNA strands, are labeled R and G, or with a palindrome strand, which are labeled P. R strands are designed to bind selectively to G strands and not to other R or P strands. Similarly, G strands bind only to R strands while P strands bind only to other P strands. To differentiate the particles under confocal microscope, red fluorescent (Alexa 647) streptavidin is used together with R particles, while green fluorescent (Alexa 488) streptavidin is used with G particles.
With this collection of DNA patchy particles, a variety of colloidal assemblies can be constructed that mimic molecules and macromolecules not only in geometry, but also in their “chemistry”. In those colloidal molecules, divalent, trivalent, and tetravalent particles act as central atoms and monovalent particles can act as ligands, forming several bonds around the central atoms. The interactions between the central atoms and the monovalent particles are highly directional and specific, as evidenced by the fluorescent images in FIG. 8 (middle panel), so that the geometry of the resulting colloidal molecule remains the same as the central atom. Illustrative Examples 7-12 are provided hereinafter.
On the other hand, palladated pincer-pyridine metal coordination is used for patchy particle assembly. The palladated pincer complex is a particularly useful molecular recognition unit because it has only one open coordination site accessible and can undergo fast and quantitative self-assembly with different ligands such as pyridine. Stronger ligand, such as triphenylphosphine can bind to the palladium and release pyridine ( FIG. 6 b ). The self-assembly of the particles can be triggered by simply adding AgBF 4 , and broken by adding another stronger ligand. This allows us to turn on and off the assembly easily. Also, incorporation of metals such as palladium into colloidal particles would bring electric and magnetic properties, thus creating multifunctional and smart materials. Illustrate Example 13 is provided hereinafter.
The self-assembly of colloidal atoms into molecules can be viewed as “colloidal reactions” or more generally as “supracolloidal chemistry”. Like conventional chemical reactions, colloidal particles with a particular morphology and binding capacity can be used as reagents, and mixed together stoichiometrically. For one example, 4 equivalents of monovalent and 1 equivalent of complementary tetravalent particles can be used to fabricate AB4 colloidal molecules. The colloidal molecule formation and divalent particle polymerization follows a stepwise kinetics. As shown in FIG. 9 a , the formation of an AB 4 molecule proceeds by the central tetravalent particle picking up monovalent particles, one at a time. In the case of divalent particle chain formation, the “polymerization” also follows a step-growth mechanism. FIG. 9 b illustrates how a polymer chain can be extended by adding divalent particles one by one at the end. Alternatively, two polymer chains can fuse into a longer chain.
The ability to design colloidal particles with directional interactions with a wide variety of well-controlled symmetries opens a new spectrum of structures for colloidal self-assembly, taking one beyond colloidal assemblies whose structures are defined primarily by repulsive interactions and colloidal shape. These colloidal particles with a designed “valence” feature can assemble, not only into molecular analogues, but also into other symmetries not available in molecular or crystalline systems. This versatility is demonstrated, for example, by the ability to construct colloidal phases of tetrahedrally coordinated glasses, diamond type crystal phases and “empty” liquids. Furthermore, the use of non-covalent interactions such as DNA hybridization for the attractive interactions between particle patches creates interactions that are both specific and reversible. These types of degrees of freedom and specificity mean that colloids with different properties, such as size, color, and chemical functionality, can be attached in well-defined sequences and orientations. For example, materials can include photonic crystals with programmed distributions of defects and 3-D electrically wired networks. By varying the temperature, concentration, and other reaction conditions, other new design principles can be developed and applied. These types of patchy colloids introduced herein expand the meaning of “colloidal chemistry” and bring us to a point where colloids can be assembled with as much complexity and selectivity as for most atoms and molecules and in some cases exceed the complexity and selectivity of atoms and molecules which are constrained by the laws of science that govern atomistic bonding.
In the following Examples section, various non-limiting examples illustrate a number of aspects of the invention.
EXAMPLES
Example 1
Typically, 10 mL of the amidinated cluster suspension (1% w/w, pH=2.93, 540 or 820 nm in diameter) was charged into a 50 mL 2-neck flask along with a magnetic stir bar. The flask was submerged in an oil bath and the temperature was set to 35° C. 1 mL of acetone was added and the suspension was stirred at 300 rpm. In a separated glass vial, 50 mg of benzoyl peroxide were dissolved in 0.63 mL of 1,2-dichloroethane. Then, 0.88 mL of 1-chlorodecane was added to the vial followed by the addition of 5 mL of an aqueous solution of 0.1% SDS. The resulting mixture was then vortexed to create an emulsion, from which 200 μL were added to the cluster suspension. The resulting mixture was stirred for 12 hours at 35° C. Then, the acetone was removed via evaporation under reduced pressure (30 mmHg). The flask was equipped with a condenser containing an oil bubbler at the top. Using a needle, nitrogen was bubbled through the suspension for 30 minutes. Then, 1 mL of styrene (with inhibitor removed) was added and allowed to swell the clusters. After 2 hours, the temperature was raised to 65° C. to initiate polymerization. The polymerization was allowed to take place for 14 hours. Then, the reaction was cooled to room temperature, which terminates the polymerization, yielding the desired patchy particles as a mixture.
Example 2
Typically, carboxylated cluster suspension (0.5% w/w, pH=9.5, 620 nm in diameter) was used. In the case of particles dispersed in organic solvents, 3% DVB are used together with styrene when the clusters are swollen. The rest of the fabrication condition is the same as that shown in Example 1.
Example 3
Typically, sulfonated cluster suspension (1%, pH=7.0, 850 nm) was used. The rest of the fabrication condition is the same as that shown in Example 1.
Example 4
Typically, 1 mg of sulfo-NHS-Biotin was charged into a dram vial containing a stir bar. 0.5 mL of patchy particles (particles fabricated in Example 1 are used) of interest was added to the vial and the suspension was allowed to stir for 12 hours. Biotin was used in large excess. Unreacted biotin was removed by washing the functionalized particles six times with an aqueous solution containing 10 mM PBS (pH:7.42, NaCl:100 mM) and 0.1% w/w Triton X-100. The 5′-biotin-DNA was mixed with streptavidin (Life tech., 0.5 mg/mL, green or red fluorescent labeled) in 1:1 molar ratio in a centrifuge tube and agitated for 1 hour. The resulting DNA-streptavidin complex was then attached to the biotin patchy particles. Typically, we added a 100 μL suspension of biotin patchy particles to 10 μL of the DNA-streptavidin complex and agitated the mixture for 3 hours at 25° C. The resulting particles were washed with and dispersed in an aqueous solution of PBS containing 1% w/w Pluronic F127 as surfactant. This dispersion can be stored at 4° C. and directly used for the self-assembly studies.
Example 5
Typically carboxylated patchy particles (100 μL, 0.1% w/w, dispersed in MES buffer, pH 6), 1 mg of EDC and 10 μL of streptavidin (Life tech., 0.5 mg/mL, green or red fluorescent labeled) were charged into a dram vial containing a stir bar. The suspension was allowed to stir for 12 h. After washing by centrifugation/redispersion in PBS containing 0.1 Triton-X100, streptavidin conjugated patchy particles were produced.
5′-biotin-DNA was mixed together with streptavidin patchy particle in PBS Triton solution, yielding DNA patchy particles.
Instead of using a streptavidin linker, DNA can also be attached to carboxylated patchy particles by EDC coupling. 5′-Amino-DNA (DNA with an amine group modified on the 5′ terminal) used. In this case, the DNA was linked to the particle by a covalent amide bond.
Example 6
Carboxylated patchy particles (fabricated in Example 2 with 3 crosslinking) are transferred and dispersed in THF. 10 μL of the particle suspension was charged in a dram vial along with a stir bar. 1 mg of EDC was added in the vial and the mixture was allowed to stir for 10 min. And then 1 mg of sPincer (or sPyridine, pPincer) was first dissolved in 10 μL of THF and then added into the vial. After overnight reaction, the particles are washing intensively in the THF by centrifugation/dispersion.
Example 7
From monovalent (1-patch) particles with complementary sticky ends, AB type colloidal molecules can be constructed. In FIG. 8 a (left), two monovalent particles stick together, forming colloidal dumbbells. In contrast to spherical particles uniformly coated with DNA, large aggregation does not occur, consistent with there being only one patch per particle. The confocal fluorescent image in FIG. 8 a (middle) confirms that DNA hybridization is the driving force for assembly by showing that only complementary R-G particle pairs are formed; no R-R or G-G pairs are observed. Such pairs are the colloidal analog of AB type molecules such as hydrogen chloride ( FIG. 8 a , right). Here, in contrast to hydrogen and chlorine, the sizes of the two atoms are the same, although they need not be. Patchy particles of different sizes can be fabricated and DNA bonds of various strengths can be used, so colloidal molecules of different size ratio and bond strength can be obtained.
Example 8
When G type divalent (2-patch) particles are mixed with R type monovalent particles, linear AB 2 type colloidal molecules are obtained, the colloidal analogues of molecules like carbon dioxide (CO 2 ), beryllium chloride (BeCl 2 ) and so on ( FIG. 8 b ).
Example 9
Triangle-like AB 3 ( FIG. 8 c ) and tetrahedron-like AB 4 ( FIG. 8 d ) colloidal molecules can be obtained using trivalent (3-patch) particles and tetravalent (4-patch) particles when they are put together with monovalent particles in a similar manner. Molecular analogues of the AB 3 colloidal molecules include boron trifluoride (BF 3 ) while analogues of AB 4 molecules are methane (CH 4 ) and carbon tetrachloride (CCl 4 ).
Example 10
Colloidal “alternating copolymer” chains can also be formed using complementary
colloidal divalent particles. FIG. 8 e shows a chain consisting of divalent particles while the accompanying fluorescent image shows that only G and R type particles bind to each other.
Example 11
Particles with bigger patches can also be used to build colloidal molecules and polymers. If the patches are big enough to accommodate more than one complementary particle, molecular isomers and branched polymers are obtained. FIG. 8 f shows that non-linear AB 2 type molecules are formed with conformational isomers that resemble the cis- and transconformation of a double bond. Such isomers may behave quite differently in diffusion, rotation and reactivity. If more monovalent particles are available, they can bind to the isomers and form an ethylene-like structure (see FIG. 8 f ). In the case of colloidal polymers of divalent particles, using particles with bigger patches leads to branched chains and crosslinked networks.
Example 12
Self-complementary palindrome strands can also be used for self-assembly of mono- and divalent particles. From monovalent particles, dumbbell A 2 type colloidal molecules can be constructed, such as H 2 , Cl 2 , etc. From divalent particles, homopolymers can be made. One can also envision trivalent, tetravalent, and palindrome particles of higher order that might assemble into extended open structures like a diamond lattice.
Example 13
Pyridine and pincer polymer functionalized divalent particles (fabricated in Example 6) were combined in equal portions. No particles assembly was observed immediately following the sample mixing. The metal coordination was triggered by adding silver tetrafluoroborate (AgBF 4 ) to the particle suspension. Ag(I) can activate the palladated pincer by removing the Cl, leaving the palladium one open coordinating site ( FIG. 6 b ). After the addition of AgBF 4 , the particle mixture was then agitated for 5 hours at room temperature. Control experiments were also set up while a single type of dimer was mixed with AgBF 4 and particles mixtures without AgBF 4 . After agitation, all samples were investigated in flat capillary tubes using inversed lens optical microscope. In the control set, the particles stayed stable and no aggregation is found. In sharp contrast, for the experimental set, most of the dimer particles aggregated and they formed daisy chains consisting of different number of particle within each chain. FIG. 10 b is snapshots of particle chains with different length. The number of particle per chain varied from 2 to 12 and some branched structures are observed. More importantly, oval shape particles linked together in a head to head configuration, suggesting the existence of the attraction interactions only between the patchy parts.
The foregoing description of embodiments of the present invention has been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the present invention to the precise form disclosed, and modifications and variations are possible in light of the above teachings or may be acquired from practice of the present invention. The embodiments were chosen and described in order to explain the principles of the present invention and its practical application to enable one skilled in the art to utilize the present invention in various embodiments, and with various modifications, as are suited to the particular use contemplated.
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A method for creating the colloidal analogs of atoms with valence: colloidal particles with chemically distinct surface patches that imitate hybridized atomic orbitals, including sp, sp2, sp3, sp3 d, sp3 d2 and sp3 d3. Functionalized with DNA with single-stranded sticky ends, patches on different particles can form highly directional bonds through programmable, specific and reversible DNA hybridization. These features allow the particles to self-assemble into ‘colloidal molecules’ with triangular, tetrahedral and other bonding symmetries, and should also give access to a rich variety of new microstructured colloidal materials.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application Ser. No. 60/756,847, filed Jan. 6, 2006, which is incorporated herein in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a rotary latch.
2. Description of Related Art
Rotary latches are well known in the art, providing a strong, compact latching mechanism for many applications. A rotary latch generally includes a housing portion fixed to a first structure having a U-shaped slot configured to receive a post fixed to an opposing structure. A C-shaped latch is pivotally attached within the housing and arranged to rotate from a latched position within and perpendicular to the U-shaped slot to an unlatched position. In the latched position, the C-shaped latch and the U-shaped notch overlap to define a central opening configured to hold the post. In the unlatched position, the C-shaped latch is rotated toward the opening of the U-shaped slot, allowing the post to move into or out of the U-shaped slot. The C-shaped latch usually includes a catch on its body in an opposing position to the opening of the “C” relative to the pivot point of the latch. The catch is configured to act in concert with a trip lever pivotally mounted within the housing. The C-shaped latch and the trip lever are generally spring-biased. The C-shaped latch is biased in an open position and the trip lever is biased in a locked position. When the C-shaped latch is moved into the closed position, the trip lever is biased to engage the catch, holding the C-shaped latch in the closed position. The C-shaped latch is released by rotating the trip lever until it disengages from the catch. A stud is usually mounted to the trip lever for attachment of a release cable. Because of the configuration of the trip lever having a fixed pivot axle, it is necessary to arrange the release cable in a very narrow approach angle to the stud, in order to be able to pivot the trip lever with a minimal force exerted on and by the release cable. In the known arrangement, the release cable is generally aligned parallel to the housing of the rotary latch. Deviations from the optimal attachment of the release cable to the stud, with a tangential positioning of the cable relative to the pivot axis of the trip lever, unnecessarily increase the force required to release the rotary latch. The mechanical advantage available in the trip lever can therefore be lost by suboptimal positioning of the cable. Also, in different applications, it becomes necessary to modify the configuration of the trip lever and the stud so that the release cable can even access the stud. This necessitates the manufacture and stocking of multiple configurations of rotary latch assemblies, dependent upon the variety of applications used in a particular assembly.
It would be advantageous to provide a rotary latch system that provides the maximum available mechanical advantage regardless of the exact alignment of the release cable relative to the pivot axis of the trip lever. It would further be advantageous to provide a rotary latch system that improves the accessibility of a release mechanism in different applications without requiring the physical modification of the rotary latch.
BRIEF SUMMARY OF THE INVENTION
A rotary latch for selectively locking a closure, such as a tonneau cover on a pickup truck bed or the swing-up window on a pickup truck cap, is provided with a spring loaded toggle release lever, or joystick. The joystick enables the rotary latch to be installed in any position with respect to a remote actuating handle because the joystick can be pushed or pulled in almost any direction to release the rotary latch.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The present invention will become more fully understood from the following detailed description and the accompanying drawings, wherein:
FIG. 1 is a side view of a pickup truck with a tonneau cover and a rotary latch with joystick according to the invention.
FIG. 2 is a partially broken sectional view of the rotary latch according to the invention, mounted on FIG. 1 pickup truck tailgate and tonneau cover, and substantially as taken on the line 2 - 2 of FIG. 3 .
FIG. 3 is a front view of the rotary latch of FIG. 2 .
FIG. 3A shows various means for actuating connection to the joystick of FIG. 3 and schematically illustrates the possibility of linking two (or more) latch mechanisms by means of their joysticks.
FIG. 3B shows a power actuator to joystick connector according to FIG. 3 .
FIG. 3C shows an unlatched position of parts of the FIG. 3 apparatus.
FIG. 4 is a pictorial view of the rotary latch of FIG. 3 .
FIG. 5 is a bottom view of the rotary latch of FIG. 3 .
FIG. 6 is a rear view of the rotary latch of FIG. 3 .
FIG. 6A is a fragment of FIG. 3 showing the joystick in central cross section.
FIG. 6B is a sectional view substantially taken on the line 6 B- 6 B of FIG. 6 .
FIG. 7 is an end view of the rotary latch of FIG. 3 .
FIG. 8 is an opposite end view of the rotary latch of FIG. 3 .
FIG. 8A is an exploded pictorial of a bracket for mounting the latch mechanism of FIGS. 1-8 .
FIG. 9 is an exploded pictorial view of the housing of the rotary latch of FIG. 3 .
FIG. 9A is a pictorial view of the latch member and latch release member of the rotary latch of FIG. 3 .
FIG. 10 is a side view similar to FIG. 6 , but with the rear housing portion mostly removed.
FIGS. 11A-11H depict the release sequence the main parts (only) of the rotary latch of FIG. 3 .
FIG. 12 is an end view of the free end of the joystick of the rotary latch of FIG. 3 .
DETAILED DESCRIPTION OF THE INVENTION
Certain terminology will be used in the following description for convenience in reference only and will not be limiting. The words “up”, “down”, “right” and left” will designate directions in the drawings to which reference is made. The words “in” and “out” will refer to directions toward and away from, respectively, the geometric center of the device and designated parts thereof. The words “proximal” and “distal” will refer to the orientation of an element with respect to the device. Such terminology will include derivatives and words of similar import.
FIG. 1 shows an application by way of example and not limitation, for the present invention. The invention is applicable in any enclosure requiring selective latching, and wherein the release of said latching can be accomplished by powered or manual actuation, electronically or mechanically, or by direct or remote control. In a motor vehicle 50 , e.g. a pickup truck, the present invention is applied for latching a door on a pickup truck cap or, as here shown, a tonneau cover 55 over a pickup truck bed cargo area 60 having a tailgate 65 . The tonneau cover 55 is movable between an open position (shown) and a closed position (shown in phantom). In the closed position, the tonneau cover 55 can be secured by a latch mechanism 100 releasably engaging a pin, or strike, 110 ( FIG. 2 ). The latch mechanism 100 is here indicated as being mounted on the tonneau cover 55 and the pin 110 on the tailgate 65 , respectively, but could on the tailgate 65 and tonneau cover 55 , respectively instead.
The latch mechanism 100 is attached to the inside of the tonneau cover 55 by a bracket 105 . A cooperating pin 110 is mounted to the tailgate 65 .
Referring further to FIGS. 3A-3C , the latch mechanism 100 includes a joystick 130 . The joystick 130 is spring biased into a rest position (vertical as shown in the drawings), and as will be further disclosed, displacement of the joystick 130 from such vertical position triggers unlatching of the latch mechanism 100 .
Referring now to FIGS. 5-10 , the latch mechanism 100 has a housing 140 formed of a left (in FIGS. 7-9 ) housing portion 145 and a right housing portion 150 .
The left ( FIG. 9 ) housing portion 145 comprises an elongate longitudinally extending sidewall 145 A having a laterally and endwardly facing notch 145 B, an elongate longitudinal flange 145 C extending widthwise perpendicularly from and following one length edge of the sidewall, a perpendicular first end flange 145 D at the notched end of the sidewall and adjacent one end of the elongate flange 145 C, a narrow step-like end wall 145 E extending widthwise perpendicularly from the other end of the sidewall to about half the width of the adjacent end of the elongate flange 145 C, an extension wall 145 F extending longitudinally from the free edge of the end wall 145 E in a plane parallel to the sidewall 145 A, and a narrow end flange 145 G extending from the free end of the extension wall generally parallel to and spaced from the step-like end wall 145 E.
The housing portion 150 is preferably substantially a mirror image of the housing portion 145 except as follows. The housing portion 150 comprises a longitudinally and widthwise extending flange 150 H at the longitudinally extending edge 150 J of its notch 150 B, but omits parts comparable to the longitudinal flange 145 C, first end flange 145 D and narrow end flange 145 G of the housing portion 145 .
The left and right housing portions are joined by a pair of swaged bushings 175 , 180 whose ends are fixedly received in respective apertures 155 , 165 and 160 , 170 in recessed portions of the sidewalls 145 A and 150 A. The swaged bushings 175 , 180 each have a threaded interior passage 185 for receiving a threaded fastener (e.g. screw) 190 , for securing the latch mechanism 100 to the bracket 105 and to an alignment plate 195 . In FIG. 3 , the bracket 105 is fixed to the tonneau cover 55 by bolt and nut units 194 . The left (in FIGS. 5 , 6 and 10 - 11 ) end of housing 140 defines a U-shaped channel, or notch, 198 for receiving the pin 110 .
The housing narrow end walls 145 E and 150 E space the housing extension walls 145 F and 150 F laterally inboard of the housing sidewalls 145 A and 150 A, at the width of the end flange 145 G. The extension walls 145 F and 150 F and end flange 145 G define the left (in FIGS. 5 and 6 ) end portion of the housing as a narrow (compared to the width of the housing at the sidewalls 145 and 150 ) nose 196 . The narrowed nose 196 allows mounting of the housing very close (e.g. almost abutting as in FIG. 5 ) the structure 65 (e.g. the truck tailgate) carrying the cooperating conventional pin 110 , even if the latter incorporates a radially projecting mounting flange, or the like, as indicated in the dotted line at 111 in FIG. 5 . Moreover, and as will be noted in FIG. 5 , since the narrowed nose 196 is spaced laterally inboard from both sidewalls 145 A and 150 A of the housing 140 , the housing 140 can be placed close to the pin supporting structure 65 , even with its orientation reversed, e.g. with its sidewall 150 A adjacent the pin supporting structure 65 , rather than its sidewall 145 A as in FIG. 5 . Thus, not only can the latch mechanism 100 be mounted in any desired orientation (e.g. joystick up, joystick down, joystick left, joystick right, housing length axis vertical or horizontal or sloped, but in any of those orientations, the housing 140 can be placed close to or spaced from the pin support structure 65 with which the latch mechanism 100 latchingly cooperates.
The mounting bracket 105 here includes a main body and a mounting flange 106 perpendicular thereto. Slots 107 and 108 in the main of the bracket 105 and in the flange 106 , respectively, allow adjustment of the location of the bracket 105 with respect to the adjacent side of the housing 140 and structure (e.g. the tonneau cover 55 of FIG. 1 ) on which the bracket is fixed.
To allow mounting of the housing 140 , in its contents, in any desired orientation, the bracket 105 may be fixed on either side of the housing 140 , e.g. either adjacent to the sidewall 150 A as seen in FIG. 8 , or to the opposite side wall 145 A. Moreover, with the mounting bracket 105 fixed to supporting structure (e.g. the FIG. 1 tonneau cover 55 ) by means of its mounting flange 106 ( FIG. 8 ), the housing 140 can be fixed in its joystick down orientation of FIG. 8 or reoriented with the joystick 130 up.
The alignment plate 195 ( FIG. 8A ) has through holes 195 A spaced from each other widthwise of the plate 195 at the same spacing as the slots 107 and the bracket and bushing holes 155 and 160 in the housing portion 145 and holes 165 and 170 in the housing portion 150 so as to coaxially align therewith. Aligned with the holes 195 A are a pair of upper lugs 195 B and a pair of lower lugs 195 C adjacent the top and bottom (in FIG. 8A ) edges of the alignment plate 195 . The lugs 195 B and 195 C protrude toward and are of width be snuggly received in the bracket slots 107 , as indicated in FIG. 8 . With the screws 190 loosened to adjust the position of the housing 140 along the length of the slots 107 , the adjustment plate 195 positively prevents one of the screws 195 from rising above the other and so prevents tilting of the housing 140 in a plane parallel to the adjustment plate 195 and main portion of the bracket 105 , i.e. maintains the top and bottom plates of the housing 140 perpendicular to the length axis of the slots 107 of the bracket 105 .
The latch mechanism 100 ( FIGS. 9A and 10 ) includes a rotating latch member 200 and a rotating latch release member 205 .
As shown in FIG. 10 , the latch member 200 and latch release member 205 are plate-like and pivotally mounted on the bushings 180 and 175 , respectively, which extend through corresponding holes 201 and 206 ( FIG. 9A ) therein.
The latch member 200 includes a C-shaped portion 235 to the left (in FIG. 10 ) of the bushing 180 and a tail portion 255 on the opposite side of the bushing 180 . The C-shaped portion 235 includes an inner arm 240 and an outer arm 245 . The inner arm 240 and the outer arm 245 define a U-shaped channel, or notch, 250 therebetween. The tail portion 255 has a shallow notch 215 in its lower ( FIG. 10 ) edge.
The close flanking of the C-shaped portion 235 ( FIG. 10 ) of the latch member 200 by the extension walls 145 F and 150 F of the housing portions 145 and 150 helps prevent the C-shaped portion 235 from bending or cocking out of its intended operating plane. Further, the bearing of the end flange 145 G on the extension wall 150 F (as seen in FIG. 5 ) helps rigidify the housing nose 196 .
The latch release member 205 includes a catch portion 260 . The catch portion 260 includes a step-like catch 265 and a shallow notch 230 . The catch 265 , as shown in FIGS. 9A-11 , is configured to engage the tail portion 255 of the latch member 200 . The latch release member 205 further includes a lever portion 270 . The lever portion 270 and catch portion 260 are on opposite sides of the bushing 180 . The lever portion 270 is formed as a flange perpendicular to the remainder of the latch release member 205 and comprises a leg 271 extending substantially tangentially beyond the bushing and terminating in a foot 272 extending parallel to the axis of the bushing hole 206 . The foot 272 here includes an aperture 275 .
A torsion-type latch spring 210 is also concentrically mounted on the bushing 180 , and at one end engages the notch 215 in the latch member 200 . The spring 210 at its other end bears against the end wall 220 of the housing 140 , thereby biasing the latch member 200 in a counterclockwise direction (as seen in FIG. 10 ). A second torsion-type spring 225 is mounted concentrically on the bushing 175 . The second spring 225 at one end engages the notch 230 in the latch release member 205 . The second spring 225 has its other end trapped behind the bushing 180 to bias the latch release 205 in a clockwise direction.
As shown in FIG. 6A , a rivet 280 protrudes through the longitudinal flange 145 C in alignment with the aperture 275 and thus secures a first end 285 of a coil compression spring 290 . The compression spring 290 passes through the aperture 275 and is received within a cavity 295 in the joystick 130 .
The joystick 130 includes a flat circular base portion, or annular flange, 300 ( FIG. 10 ), a necked-down (here convex or substantially frusto-conical) central portion 305 , and an elongate cylindrical arm portion 310 . The joystick 130 ( FIGS. 6A , 9 and 10 ) passes through a round aperture 315 in the flange 150 H of the right housing portion 150 . The flat circular base portion 300 of the joystick 130 is larger than the aperture 315 , so that the joystick 130 is retained within the housing 140 , with the base portion 300 bearing against an inner surface 316 of the flange 150 H of the housing 140 . The joystick 130 is biased into the aperture 315 by the compression spring 290 bearing between the base portion 300 of the joystick 130 and the longitudinal flange 145 C of the left housing portion 145 . The joystick central portion 305 tapers, from a diameter closely conforming to the aperture 315 , to the diameter of the cylindrical arm portion 310 . The profile of the outer wall 317 of the tapered central portion 305 can be linear or arcuate.
The compression spring 290 is partially compressed between the longitudinal flange 145 C ( FIG. 6A ) and the inboard end of the recess, or cavity, 295 in the inboard end of the joystick 130 , even in the relaxed (unactuated) position of the joystick shown. The rivet 280 is received in the first end 285 of the spring 290 to prevent the spring 290 from sliding sideways along the flange 145 C. The function of the rivet 280 can also be provided by forcible upsetting of the material of the flange 145 C in a position to retain the first end 285 of the spring 290 .
The joystick cylindrical arm portion 310 is hollow, having a threaded internal recess 320 . A pair of openings 322 , 325 pass transversely through the cylindrical arm portion 310 and the internal recess 320 . The threaded internal recess 320 is configured for receiving a connecting screw 330 ( FIG. 6A ). The cylindrical arm portion 310 further includes a pair of longitudinally spaced annular flanges 335 , 340 adjacent at its distal end 345 .
A given latch mechanism 100 may be used with one or more devices for unlatching same. As shown for example in FIG. 3 , the latch mechanism 100 is operable by a conventional power actuator 115 . As shown, the power actuator 115 is mounted in line with the latch mechanism 100 by a bracket 116 fixed to the tonneau cover 55 by nut and bolt units 117 (or by a bracket not shown carried by the latch mechanism 100 ). The power actuator 115 conventionally is electrically connected to a power source 120 (e.g. the vehicle battery not shown) and operated by a switch 125 . The switch 125 is conventionally capable of direct manual actuation or actuation by a conventional wireless remote control (not shown). The joystick 130 is connected to the power actuator 115 by a substantially rigid spring wire, push/pull connector, or “spring pull”, 135 ( FIG. 4 ). Due to the construction of the joystick 130 , displacement of the joystick 130 in any direction will actuate the latch mechanism 100 . Therefore, the joystick 130 need not be aligned with the latch mechanism 100 as shown. The power actuator 115 can be any type of mechanical or electrical actuator, or a hydraulic, magnetic, or pneumatic actuator. Furthermore, the actuator 115 need not be fixedly attached to the joystick 130 , but need only be positioned so as to displace the joystick 130 upon activation.
As shown in FIG. 3A , the spring pull 135 grips the cylindrical arm portion 310 of the joystick 130 between the flanges 335 , 340 . As a further example one or more conventional pullable release cables 350 , 355 ( FIG. 3A ) can be received through the openings 322 , 325 , and maintained therein by distal end plugs 360 , 365 fixed thereon. As a further example, a similar release cable, or a push rod 370 , having an eye 371 ( FIG. 6A ) can be fixed to the joystick 130 by a screw 330 .
In some instances, it may be desirable to provide more than one latch mechanism in a single installation of (e.g. tonneau cover pickup truck bed as in FIG. 1 ). For example, two could be located and spaced apart along the tailgate, or one might be provided on each side of the pickup truck bed. In such a dual installation, it may be desired to use a single powered or manual actuator to unlatch both latch mechanisms 100 . This can be done without any modification to the joysticks 130 of the dual latch mechanisms 100 . As seen for example in FIG. 3A , two joysticks 130 are spaced apart and linked by the cable 350 ,) the left (in FIG. 3A ) joystick 130 being connected through the wire member 135 to the power actuator 115 ( FIG. 3 ), and the other joystick being connected by a further cable 355 to another (e.g. manual) actuator of conventional type, not shown. In this way, actuation of one joystick 130 actuates the other so that both of the corresponding latch mechanisms 100 unlatch simultaneously.
Since axial pushing on the exposed end of the at rest joystick will also pivot the latch release member 205 and open the latch mechanism 100 , it is contemplated that screw 330 ( FIG. 6A ) may in some instances be substituted by a manually engageable push button, not shown, with the latch mechanism 100 being located so that such push button is reachable by a user either inside or outside the protected cavity (e.g. truck bed in FIG. 1 ).
Operation
The latch mechanism 100 has a latched position ( FIGS. 3 and 10 ), e.g. for latching the tonneau cover 55 in its closed, dotted line position on the pickup truck 50 .
As shown in FIG. 10 , the latch member 200 is held in a latched position against the bias of the spring 210 by the interference of the latch release member 205 , wherein the tail portion 255 of the latch member 200 is received within the catch 265 of the latch release member 205 .
Referring sequentially to FIGS. 11A-11H , the latched latch mechanism 100 is unlatched by axially depressing or pivotally deflecting the joystick 130 from its rest (here vertical) position shown in FIG. 11A . In this position, the latch member 200 is positioned such that the outer arm 245 of the C-shaped portion 235 appears perpendicular to the left end 196 of the housing 140 . The latch member 200 and the housing 140 thereby close the channel 198 and trap the pin 110 therein, such that the tonneaus cover (for example) is closed and latched.
The joystick 130 is then pivotally deflected e.g. by the power actuator 115 drawing on the spring pull 135 , by a manual actuator (not shown) pulling on a cable 350 , 355 , or in any other convenient way.
In FIG. 11B , the joystick 130 has been slightly pivotally deflected (to the right in FIG. 11B , though to the left or into or out of the page, or even axial deflection upward into the housing 140 would serve as well), forceably rotating the latch release member 205 slightly counterclockwise without yet releasing the latch member 200 . The joystick flat circular base portion 300 is slightly tilted away from the inner surface 316 of the housing 140 , while the frusto-conical portion 305 of the joystick 130 rides in the aperture 315 in the housing 140 .
In FIGS. 11C-11D , the joystick 130 is further deflected. The latch release member 205 is rotated further counterclockwise still without releasing the latch member 200 .
In FIG. 11E , the joystick 130 is fully deflected so that the latch release member 205 has been rotated sufficiently counterclockwise to clear the tail portion 255 of the latch member 200 . The latch member 200 is now free to rotate counterclockwise under the biasing force of the spring 210 .
In FIGS. 11F-11H , the latch member 200 , freed from latch release member 205 , sequentially rotates counterclockwise towards its unlatched position. In FIG. 11H , the latch member 200 has rotated to its fully counterclockwise, fully open position. At any time in the FIG. 11F-11H sequence the joystick 130 can be released, so that the latch release member 205 is allowed to rotate clockwise under the bias of the spring 225 , to return both to their FIG. 11A rest position. As the latch member 200 rotates counterclockwise under the bias of its spring 210 , the inner arm 240 of latch member 200 effectively pushes the latch mechanism 100 and pin 110 away from each other. The user is thus free to open the tonneau cover 55 to its FIG. 1 solid line position.
In the preferred embodiment shown, and as seen for example in FIG. 10 , during actuation the joystick base portion 300 bears at diametrically opposed points on the housing flange 150 H and on the foot 272 of the latch release member 205 to define a driven lever arm. On the other hand, the free end of the joystick, as at a point between the flanges 335 and 340 , may be connected to an actuator (for example the power actuator 115 or one of the release cables 350 , 355 , or the like). The distance, between that connection point on the free end of the joystick and the mentioned point on the joystick base 300 bearing on the housing flange 150 H, defines a driving lever arm. The ratio of these two lever arms (e.g. 2 to 1) defines the mechanical advantage provided by the joystick.
Similarly, the distances from the rotative center of the latch release lever 205 (the axis of swaged bushing 175 ) to the point of contact of the foot 272 with the joystick base 300 above mentioned and to the point of engagement of the step-like catch 265 with the portion 255 of the latch member 200 , define corresponding driving and driven lever arms of the latch release member 205 . For example in the embodiment shown, the ratio of such lever arms is approximately 2 to 1, the latch release member 205 thus providing a mechanical advantage of approximately 2 to 1.
Thus, the joystick and catch release member, taken together would, in this example, thus provide a combined mechanical advantage of approximately 4 to 1.
Moreover, the distances from the pivot axis of the latch member 200 (the central axis of its swaged bushing 180 ) to the point of contact of its tail portion 255 with the step-like catch 265 of the latch release member 205 and to the point of contact of the spring 210 with the shallow notch 215 , again defines driving and driven lever arms, which in the embodiment shown are the length ratio of about 3/2.
Thus, in this particular example, there is a total mechanical advantage of about 6 to 1 from the joystick free end to pin 110 . The FIG. 1 tonneau cover 55 may have substantial weight. To release the latch mechanism 100 requires the tonneau cover mounted inner arm 240 to push downward on the pin 110 with sufficient force to cause the bushing 180 and housing 140 and bracket 105 to lift the tonneau cover 55 out of its normally closed, latched position shown in dotted line in FIG. 1 . Thus, the latch member spring 210 has to be strong enough to forcibly pivot the latch lever 200 , from its FIG. 11F position through its FIG. 11G position and into its fully opened FIG. 11H position, to lift the heavy tonneau cover 55 . However, that same strong spring 210 , in the latch mechanism closed position of FIGS. 10 and 11 A strongly holds the tail portion 255 against the step-like catch 265 , so as to strongly resist the opening rotation of the latch release lever 205 above discussed as to FIGS. 11B-11D . Again, the distance, from the point of contact of the tail portion 255 of the latch member 200 with the step-like catch 265 of the latch release member 205 , ( FIGS. 10 and 11A ) to the point of contact of the spring 210 with the edge of the spring 210 with the edge of the notch 215 in the latch member 200 , is here in the approximate ratio of 1 to 1. Accordingly, the combined mechanical advantage available to overcome the force of the spring 210 by actuation of the joystick 130 is hereabout 6 to 1. Accordingly, if a 40 pound force is required to lift the tonneau cover 55 to complete the laterally sequence from FIG. 11F through 11H , only about ⅙ that force (e.g. 7 pounds) need be applied to the end of the free end of the joystick 130 to open the latch mechanism 100 . Accordingly, it becomes possible to actuate the joystick 130 by relatively low force means, for example a conventional low cost power actuator 115 , even with a relatively heavy tonneau cover, and without need for the user to attempt to assist the unlatching process by manually lifting the tonneau cover. In short, even a relatively heavy tonneau cover 55 will pop open as the end result of the unlatching process shown in the FIG. 11A-11H sequence.
Vehicle users will occasionally load their pickup beds high enough that the user must exert downward pressure on the tonneau cover 55 to enable the pin 110 and latch lever 200 to assume their FIG. 10 latched positions. In that instance, after latching, the user stops pressing downward on the tonneau cover 55 and moves away to other activity, but the overweight load in the pickup bed is still pressing the tonneau cover upward away from the pickup truck bed, and hence urges the latch mechanism 100 upward with respect to the pin 110 , i.e. adding to the counterclockwise (in FIG. 10 ) force of the spring 210 and hence pushing the tail portion 255 even harder against the step-like catch 265 to further resist counterclockwise, unlatching rotation of the latch release member 205 . Thus, the substantial mechanical advantage provided by the inventive joystick 130 and latch release 205 allows this added resistance to latching to be overcome with a relatively light force applied to the joystick 130 manually, by cables, or by the power actuator 115 .
The power actuator 115 and other means (e.g. cables 350 / 365 of FIG. 3B actuate the joystick independently of each other, i.e. the power actuator actuates the joystick when the cables are slack and the cables actuate the joystick when the actuator is not powered. The latch mechanism 100 can be initially installed without the power actuator and, at some later time, the user can add a power actuator.
Should a person accidentally become trapped in the FIG. 1 pickup truck bed with the tonneau cover 55 latch closed, the inventive latch mechanism 100 provides a safety advantage in that it enables relatively easy escape. More particularly, the joystick 130 stands proud from the housing 140 to a substantial extent and so is relatively easy to find, even in the dark. Also, the joystick 130 requires only a very low activating force (in view of the substantial mechanical advantage of the latch mechanism 100 ), and pushing or pulling the joystick in a wide range of directions causes the latch mechanism 100 to unlatch.
The joystick 130 is free to rotate about its length (vertical in FIGS. 6 and 6A ) axis to orient the diametral through holes 322 and 325 in any desired direction on a plane perpendicular to the longitudinal axis of the joystick, so as to accommodate the actuators (e.g. cables 350 and/or 355 ( FIG. 3B )) approaching the joystick from virtually any direction.
While the invention has been described in the specification and illustrated in the drawings with reference to preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention as defined in the claims. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to particular embodiments illustrated by the drawings and described in the specification as the best mode presently contemplated for carrying out this invention, but that the invention will include any embodiments falling within the scope of the appended claims.
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A rotary latch for selectively locking a closure, such as a tonneau cover, is provided with a joystick or toggle release lever. The joystick release lever enables the rotary latch to be installed in any position with respect to a remote handle because the joystick can be pulled in any direction, 360 degrees, to release the rotary latch. The joystick includes a trapped base supporting a spherical portion that is nested in a circular opening in the housing of the latch. The joystick is spring loaded, and is movable about its central axis in any direction, causing the base to pivot against the inside of the housing. The base of the joystick is positioned over a spring-loaded catch locking the rotary latch. As the base of the joystick rotates against the inside of the housing, it depresses the spring-loaded catch, releasing the rotary latch.
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CROSS-REFERENCE FOR RELATED APPLICATIONS
[0001] This application is a continuation of and claims priority to U.S. application Ser. No. 09/448,701, filed Nov. 24, 1999, the contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates generally to a tubular implantable prosthesis including a stent and graft composite structure used to repair and/or replace or otherwise treat a body vessel. More particularly, the present invention relates to a stent-graft composite device including a radially expandable stent employing natural or bioengineered spider silk or its derivatives as a covering.
BACKGROUND OF THE INVENTION
[0003] Employment of various implantable tubular prostheses in medical applications is well known for the treatment of a wide array of vascular and other diseases. Such tubular prostheses are used extensively to repair, replace or otherwise hold open blocked or occluded body lumens such as those found in the human vasculature.
[0004] One type of prosthesis which is especially useful in maintaining the patency of a blocked or occluded vessel is commonly referred to as a stent. A stent is a generally longitudinal tubular device formed of biocompatible material which is useful in the treatment of stenosis, strictures or aneurysms in body vessels such as blood vessels. These devices are implanted within a vessel to reinforce collapsing, partially occluded, weakened or abnormally dilated sections thereof. Stents are typically employed after angioplasty of a blood vessel to prevent re-stenosis of the diseased vessel. While stents are most notably used in blood vessels, stents may also be implanted in other body vessels such as the urogenital tract and bile duct.
[0005] Stents are generally radially expandable tubular structures which are implanted intraluminally within the vessel and deployed at the occluded location. A common feature of stent construction is the inclusion of an elongate tubular configuration having open spaces therethrough which permit radial expansion of the stent. This configuration allows the stent to be flexibly inserted through curved vessels and further allows the stent to be radially compressed for intraluminal catheter implantation. Flexibility is a particularly desirable feature in stent construction as it allows the stent to conform to the bends in a vessel.
[0006] Once properly positioned adjacent the damaged vessel, the stent is radially expanded so as to support and reinforce the vessel. Radial expansion of the stent may be accomplished by inflation of a balloon attached to the catheter, or the stent may be of the self-expanding variety which will radially expand once deployed. Structures which have been used as intraluminal vascular grafts have included coiled stainless steel springs; helically wound coil springs manufactured from a heat-sensitive material; and expanding stainless steel stents formed of stainless steel wire in a zig-zag pattern. Examples of various stent configurations are shown in U.S. Pat. No. 4,503,569 to Dotter; U.S. Pat. No. 4,733,665 to Palmaz; U.S. Pat. No. 4,856,561 to Hillstead; U.S. Pat. No. 4,580,568 to Gianturco; U.S. Pat. No. 4,732,152 to Wallsten and U.S. Pat. No. 4,886,062 to Wiktor.
[0007] Another implantable prosthesis which is commonly used in the vascular system is a vascular graft. Grafts are elongate tubular members typically used to repair, replace or support damaged portions of a diseased vessel. Grafts exhibit sufficient blood tightness to permit the graft to serve as a substitute conduit for the damaged vessel area.
[0008] The most important features of a graft are porosity, compliance and biodegradability. A graft should be microporous to provide a stable anchorage for vascular cells and stimulate tissue ingrowth and cell endothelialization therealong. Porosity is an essential component for functional synthetic vascular prostheses and plays an important part in their long-term patency. Grafts which are impermeable to blood after the time of implantation do not permit the subsequent ingrowth of cells which is necessary for uniform and satisfactory bonding of the internal lining of a prosthesis.
[0009] In addition, the graft should be compliant to stimulate ingrowing tissue and form a new elastic component of a vascular or other lumen. Poor compliance is one of the most important factors responsible for the poor performance of synthetic vascular grafts. Poor compliance prevents the reconstruction of narrow lumens by causing occlusions in the replacement prosthesis. A mismatch in compliance between the lumen and the graft results not only in high shear stress, but also in turbulent blood flow with local stagnation.
[0010] The graft may also be biodegradable so that the ingrowing tissue can take over the function of the graft. This improves the patency of the graft and promotes long term healing.
[0011] Vascular grafts may be fabricated from a multitude of materials, such as synthetic textile materials and fluoropolymers (i.e. expanded polytetrafluoroethylene (ePTFE)) and polyolefinic material such as polyethylene and polypropylene. Nylon is often used, but polyester is chosen more frequently because of its good mechanical and chemical properties. Polyester is the most commonly used because it is available in a wide range of linear densities and its low moisture absorption also gives good resistance to fast deterioration. Polyurethane is another polymer especially used for its elasticity. Graft material selection is not limited to those materials listed above, but may include others that are conducive to the biocompatibility, distensibility and microporosity requirements of endovascular applications.
[0012] If the graft is thin enough and has adequate flexibility, it may be collapsed and inserted into a body vessel at a location within the body having diameter smaller than that of the intended repair site. An intraluminal delivery device, such as a balloon catheter, is then used to position the graft within the body and expand the diameter of the graft therein to conform with the diameter of the vessel. In this manner, the graft provides a new blood contacting surface within the vessel lumen. An example of a graft device as described herein is provided in commonly assigned U.S. Pat. No. 5,800,512 to Lentz et al.
[0013] Composite stent-graft devices employing tubular structures are also known wherein a stent is provided with one or both of a polymeric cover disposed at least partially about the exterior surface of the stent and a polymeric liner disposed about the interior surface of the stent.
[0014] These composite devices have the beneficial aspects of a stent, which is used to hold open a blocked or occluded vessel, and also a graft which is used to replace or repair a damaged vessel. Several types of stent-graft utilize fibrous grafts having porosity conducive to tissue ingrowth and elasticity conducive to expansion and contraction within a fluid environment. Often, fibers of various materials are used, alone or in combination, to form graft structures that accentuate the positive effects of stents on their vascular environment. Use of fibers obviates the need to shape and mold a device into its ultimate working configuration, and many fibers have proven to be biocompatible with vascular tissues.
[0015] Several types of stent-graft devices are known in the art. Examples of such stent-graft composite devices are shown in U.S. Pat. No. 5,476,506 to Lunn; U.S. Pat. No. 5,591,199 to Porter et al.; U.S. Pat. No. 5,591,223 to Lock et al.; and U.S. Pat. No. 5,607,463 to Schwartz et al.
[0016] The procedures which utilize the above disclosed devices obviate the need for major surgical intervention and reduce the risks associated with such procedures. While such composite devices are particularly beneficial due to the thinness at which they may be formed and the radial strength which they exhibit, the devices may suffer from a lack of biocompatibility in long-term applications, such as those in which therapeutic drugs are to be delivered over an extended period of time. Thus, it may be difficult to maintain an endovascular device having graft materials formed from polymeric materials that induce inflammatory responses in native vessels.
[0017] Reduction of implantation-related inflammation can be effected by selection of graft materials that are inherently more biocompatible than those heretofore employed in stent-graft devices. Conventional graft materials such as PET polyester and nylon have high solubility factors which indicate that the material is prone to higher rates of solubilization within native vessels and therefore more prone to inflammatory responses. Such responses can translate in swelling of the surrounding vessel and impeded blood flow therethrough as a result thereof. Inflammations can further lead to tissue ingrowth at the periphery of the prosthesis, further impeding blood flow and defeating the purpose of the stent-graft device to not only maintain the patency of the vessel, but also assist in the healing of surrounding tissue.
[0018] Biological or bioengineered silk material, on the other hand, exhibits desirable characteristics which inhibit the inflammatory responses observed with other conventional polymeric materials used in stent-graft applications. Woven silk material possesses a smooth surface which does not interfere with the inherent hemodynamic properties of blood flow. Biological silks also have natural elastic properties that increase endoprosthetic distensibility over conventional stent-graft materials.
[0019] Biological silks are typically derived from silkworms. Fibers produced by silkworms can be easily fabricated into cloth, however, the strength and toughness of silkworm silk is relatively low. Because silkworm fibers are too fine for commercial use, between 3 and 10 strands are used at a time to achieve a silk strand of required diameter for weaving.
[0020] Spider silk, however, demonstrates superior mechanical properties which make it desirable in use for various medical applications, including stent-graft endoprostheses. The combined high tensile strength (4×10 9 N/m 2 ) and elasticity (35%) of major ampullate spider silk (also known as “dragline” silk) translates into a toughness that is superior to all man-made or natural fibers, including silkworm strands. The silk is thus five times stronger than steel, yet 30% more flexible than nylon and can absorb three times the impact force without breaking than Kevlar.
[0021] An orb web, the typical spider web, is constructed of several different silk types, each composed primarily of protein. These silks vary in their mechanical properties over a very wide range of tensile strength and elasticity. The best studied silk is dragline silk from Nephila clavipes , also known as the golden orb weaving spider. This one spider can synthesize as many as six types of silk, each having slightly different mechanical properties. Dragline silk is a semicrystalline polymer which, besides forming the dragline, is used to form the frame of the web. The material must perform functions such as absorbing the energy of a flying insect so that the prey neither breaks nor bounces off of the trap. Dragline silk must also support the weight of a rapelling spider. Dragline silk is stronger than a steel cable of the same diameter.
[0022] In addition, dragline silk is the only silk that has the ability to supercontract. Wetting of unrestrained fibers of dragline silk at room temperature causes the fibers to contract to about 60% of their relaxed dry length. In synthetic fibers, such supercontraction occurs only at extreme temperatures or in harsh solvents. Supercontraction of dragline fibers is accompanied by a decrease in tensile strength and an increase in elongation before breaking. Unlike synthetic fibers, however, the mechanical properties of the dragline fiber return to their original values once dried and re-stretched.
[0023] Furthermore, dragline silk is also non-allergenic, making it very desirable for medical applications. Single strands are only 1/20,000 of an inch across apiece, and the diameter of the fiber ranges from 0.1 to 8μ, depending upon the type of silk. Spider silk is a soluble fluid in the aqueous environment of the spider's abdomen, but it is an insoluble solid after it exits the spider's body. Insolubility is a major factor in a web's durability which can translate into an increased lifespan for endoprosthetic devices.
[0024] Synthetic genes can be designed to encode analogs of the silk proteins to produce biosilk. Use of recombinant DNA technology enables bacteria to produce and customize the silk proteins which form silk substances. Silk-like protein polymers can also be implemented, such as ProNectin F (a trademark of Protein Polymer Technologies of San Diego, Calif.). Such polymers mimic the molecular structure of natural silk and incorporate properties of human proteins. They can be processed in films and bond with different types of cells in native tissue.
[0025] The following table presents a comparison of extensibility and tensile strength of three spider silks of Nephila clavipes :
Silk Extension Tensile Strength Major ampullate (dragline) 35% 400 kpsi Minor ampullate 5 100 Flagelliform 200 100
[0026] Thus, endoprosthetic devices which employ spider silk and derivatives thereof (i.e. biosilk, combinations of silk/biosilk with other well-known polymeric graft materials) would not only retain their shape better, but also remain more flexible. In addition, because the proteins which form the silk substances comprise a biological material, they integrate more effectively in the human body.
[0027] Accordingly, it is desirable to implement a biosilk material, either naturally occurring or genetically engineered, in a stent-graft device which exhibits sufficient radial strength to permit the composite device to accommodate a radially expandable stent and yet improves biocompatibility with a vascular site into which implantation occurs. It is further desirable to provide an expandable tubular stent which exhibits sufficient radial strength to permit the stent to maintain patency in an occluded vessel and yet prevent reoccurrence of occlusions in a passageway by providing an expandable tubular stent of generally open, cylindrical configuration that utilizes silk material. Such a device prevents inflammation of lumen passageways due to incompatibility with graft material and assists in the healing of diseased lumen tissue by enabling extended elution of therapeutic substances therefrom.
SUMMARY OF THE INVENTION
[0028] It is an advantage of the present invention to provide an improved tubular stent-graft composite device.
[0029] It is another advantage of the present invention to provide an easily manufactured stent-graft device which reduces tissue inflammation due to implantation of the device within vascular tissue.
[0030] It is yet another advantage of the present invention to provide a stent-graft composite device having the dual function of structural support for a radially expandable stent and absorption and release of therapeutic agents.
[0031] It is a further advantage of the present invention to utilize biological silk substances as graft coverings to assist blood flow and reduce inflammatory reactions in stent-graft endoprostheses.
[0032] The present invention provides a stent-graft composite intraluminal prosthesis comprising an elongate radially adjustable tubular stent, defining opposed interior and exterior stent surfaces and a polymeric stent sheath covering at least the exterior surface of the stent. The stent can include a plurality of open spaces extending between the opposed exterior and interior surfaces so as to permit said radial adjustability. The stent has a polymeric material on its exterior surface, its interior surface, in interstitial relationship with the stent or any combination of the above. The polymer is preferably selected from the group of polymeric materials consisting of biological or genetically engineered spider silks, such as those derived from Nephila clavipes . If separate sheaths are placed on both the exterior and interior surfaces of the stent, the sheaths are secured to one another through said open spaces, such as by lamination, suturing or adhesion. One of the sheaths may comprise a tubular structure fabricated from a conventional polymeric graft material, such as polyester or nylon. In the alternative, either tubular sheath may include a combination of biological or bioengineered spider silk with polymeric fibers.
[0033] A method of making a stent-graft endovascular prosthesis of the present invention is also disclosed. The disclosed method includes providing an elongated radially adjustable tubular stent, defining opposed interior and exterior stent surfaces. A tubular silk structure is disposed about at least one of an exterior and luminal surface of the stent and secured thereto. Securement is effected preferably by sutures, however, when both the exterior and luminal stent surfaces are to be covered, the silk structures may be secured through the open spaces of the stent as described hereinabove. If separate sheaths are placed on both the exterior and interior surfaces of the stent, the sheaths are secured to one another through said open spaces, such as by sutures also made from a spider silk or derivative thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 is a perspective view of a preferred embodiment of a tubular stent-graft prosthesis of the present invention.
[0035] FIG. 2 is a perspective view of one embodiment of a stent which may be used in a stent-graft composite prosthesis of the present invention.
[0036] FIG. 3 shows a side view of a tubular stent-graft prosthesis of FIG. 1 having sutures therein.
[0037] FIG. 4 shows a cross-section of a preferred embodiment of the tubular stent-graft prosthesis of the present invention taken along line a-a of FIG. 3 .
[0038] FIG. 5 shows a schematic of a polymeric film on a mandrel prior to affixing a stent thereon.
[0039] FIG. 6 shows a schematic of the film and mandrel of FIG. 5 after placement of a stent thereover.
[0040] FIG. 7 shows a cross-section of the stent and polymer combination of FIG. 6 after removal from the mandrel, taken along line b-b.
[0041] FIG. 8 shows a cross-section of the stent and polymer combination of FIG. 7 having a tubular silk structure disposed about an exterior surface thereof.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0042] In the present invention, a tubular stent-graft prosthesis is provided which incorporates a tubular radially adjustable stent having a polymeric covering over an exterior and/or luminal surface thereof. The preferred covering is formed from biological or genetically engineered silk fibers such as those derived from spiders, or from fibers incorporating said silk and a polymeric graft material therein. Silk is a preferred covering because it is very biocompatible, has a smooth surface finish and has natural elastic properties that increase its distensibility over conventional stent-graft materials. The silk is employed as graft material for a stent wherein the material can be applied luminally, externally or laminated to the stent. The covering can either be flush with the ends of the stent or centered mid-stent, allowing a portion of the stent to remain uncovered. The covering can be secured to the stent using sutures, preferably also formed of silk.
[0043] Now referring to the figures, where like elements are identically numbered, FIG. 1 shows a preferred embodiment of a tubular stent-graft prosthesis 10 of the present invention. Prosthesis 10 includes a tubular radially expandable stent 12 having a sheath 14 on at least an exterior surface thereof. Sheath 14 includes a thin-walled material, preferably having a thickness between 0.005″-0.006″, inclusive. The sheath is made from a film or weave of silk or silk-like material such as spider dragline silks, bioengineered equivalents or combinations thereof (collectively referred to herein as “silk”) which are more biocompatible with vascular tissue than conventional graft materials. Silk material is selected because its remains insoluble in native vessels and therefore promotes a more biofriendly reaction when compared to current materials such as PET polyester and nylon. Currently utilized materials such as these exhibit a high solubility factor (10.7), resulting in an exacerbated inflammatory response in lumen tissue which in turn inhibits the effect of therapeutic substances placed thereon.
[0044] The silk material that is used in the device may have any of a variety of textures and finishes which promote endotheliazation. Such finishes includes smooth finishes that facilitate laminar blood flow and mesh-like material having improved porosity so as to promote endothelial lining/tissue growth. Blends of silk and polymers in the form of drawn fibers can also be used, as they exhibit an increased elastic modulus and moisture absorption factor which enables the prosthesis to thereby sustain tissue ingrowth thereon.
[0045] Although a wide variety of stents may be used, FIG. 2 shows a perspective view of one particular stent which may be employed in prosthesis 10 . The particular stent shown in FIG. 2 is more fully described in commonly assigned U.S. Pat. No. 5,575,816 to Rudnick, et al. Stent 12 is an intraluminally implantable stent formed of helically wound wire. Multiple windings 16 of a single metallic wire 17 , preferably composed of a temperature-sensitive material such as Nitinol, provide stent 12 with a generally elongate tubular configuration which is radially expandable after implantation in a body vessel. The multiple windings 16 of stent 12 define open spaces 20 throughout the tubular configuration and define a central open passage 21 therethrough between opposing extremities 12 a and 12 b . The helically wound wire configuration not only ensures patency and flexibility, but the open spaces also allow adhesion of tubular layers therethrough.
[0046] Although this particular stent construction is shown and described with reference to the present invention, various stent types and stent constructions may be employed in the present invention for the use anticipated herein. Among the various stents useful include, without limitation, self-expanding stent and balloon expandable stents. The stents may be capable of radially contracting as well, and in this sense can be best described as radially distensible or deformable. Self-expanding stents include those that have a spring-like action which causes the stent to radially expand or stents which expand due to the memory properties of the stent material for a particular configuration at a certain temperature. Nitinol is one material which has the ability to perform well while both in spring-like mode as in a memory mode based on temperature. Other materials are of course contemplated, such as stainless steel, platinum, gold, titanium and other biocompatible materials, as well as polymeric stents.
[0047] The configuration of the stent may also be chosen from a host of geometries. For example, wire stents can be fastened in a continuous helical pattern, with or without wave-like forms or zig-zags in the wire, to form a radially deformable stent. Individual rings or circular members can be linked together such as by struts, sutures, or interlacing or locking of the rings to form a tubular stent. Tubular stents useful in the present invention also include those formed by etching or cutting a pattern from a tube. Such stents are often referred to as slotted stents. Furthermore, stents may be formed by etching a pattern into a material or mold and depositing stent material in the pattern, such as by chemical vapor deposition or the like.
[0048] The fabrication of a composite device of the type shown in FIG. 1 can now be described. Prosthesis 10 is formed by providing a stent 12 with at least one silk tubular sheath 14 disposed circumferentially about an exterior surface thereof. As shown in FIG. 3 , the silk sheath can either be flush with the ends of the stent or centered mid-stent allowing a small amount (i.e. approximately 2-3 mm) of open stent on both the proximal and distal stent extremities 12 a and 12 b . The exposed portions may be desirable in certain applications to ensure securement of the prosthesis after deployment to a repair site.
[0049] The covering itself can be applied to the stent in three different orientations which are external, internal, or laminated to the stent. Silk fibers or films can be attached to stent platforms by suturing the material to the stent as shown in FIG. 3 . To suture the polymeric fiber or film to the stent, the preferred method is to use silk sutures 15 and attach sheath 14 to stent 12 at the sheath's distal and proximal ends. The number of sutures 15 that will hold the tubular silk material to the stent will depend on the stent diameter.
[0050] Sutures 15 can likewise be fabricated from spider silk, biosilk and derivatives or combinations thereof. Such sutures are one tenth the diameter of current silk sutures, reducing the amount of bleeding and scarring associated with surgical procedures. Although silk is the preferred suture material, other polymeric materials may be selected from the group consisting of absorbable (i.e., catgut, reconstituted collagen, polyglycolic acid) and nonabsorbable (i.e., silk, cotton and linen, polyester, polyamide, polypropylene and carbon fiber) materials. External factors that govern the selection of suture material include tissue type, temperature, pH, enzymes, lipids and bacteria.
[0051] As is evident from FIG. 4 , a cross section of prosthesis 10 reveals that sheath 14 circumferentially envelops the outer periphery of stent 12 . Although sheath 14 appears as a substantially complete tube that is slid over the stent while on the mandrel 22 , it is evident that the sheath may be a film or sheet having its opposing edges overlapped and secured to one another to form a tubular structure. It is anticipated that a luminal covering 14 a can be similarly affixed to stent 12 as heretofore described and as illustrated in FIG. 5 .
[0052] Sheaths 14 and 14 a can be simultaneously applied to stent 12 to provide a prosthesis having dual graft coverings. One or both of sheaths 14 and 14 a may be formed from a silk or silk derivative as described hereinabove. One of said sheaths may alternatively be formed form a polymeric material such as conventional PET polyester, nylon, polyethylene, polypropylene, polyurethane or combinations of any of these materials with one another or with the silk materials described herein. Referring to FIGS. 6 and 7 , a polymeric sheath can serve as a sheath 14 a that is provided on a mandrel 22 and has stent 12 affixed thereover. The mandrel and stent can then be placed into an oven for a time sufficient for sheath 14 a to be inextricably melted within the open spaces of stent 12 . Upon removal of the stent and sheath combination, a silk sheath 14 is placed thereover. A cross-section of this assembly is provided in FIG. 8 . It is evident that a polymeric sheath can easily be provided on an exterior surface of stent 12 as well, with a silk sheath on a luminal surface of the stent.
[0053] Either or both of the luminal and exterior surface sheaths 14 and 14 a may be provided with an adhesive thereon which permits adherence of the tubular structures to one another through the stent openings and simultaneously allows adherence of stent 12 to either or both of the structures. The adhesive may be a thermoplastic adhesive and more preferably, a thermoplastic fluoropolymer adhesive such as FEP. A suitable adhesive provides a substantially sealed tube without significantly reducing longitudinal and axial compliance.
[0054] The present prosthetic materials can also be implemented in an implantable vascular prosthesis or graft. “Vascular graft” can mean conventional and novel artificial grafts made of this material constructed in any shape including straight, tapered or bifurcated and which may or may not be reinforced with rings, spirals or other reinforcements and which may or may not have one or more expandable stents incorporated into the graft at one or both ends or along its length. The vascular graft of choice may be introduced into the vessel in any suitable way including, but not limited to, use of a dilator/sheath, placement of the graft upon a mandrel shaft and/or use of a long-nose forceps. The distal ends of the tubular graft and the mandrel shaft may be temporarily sutured together, or the distal end of the vascular graft may be sutured together over the mandrel to accommodate unitary displacement into a vessel, for example, through a sheath after the dilator has been removed. One or both ends of the vascular graft may be sutured or surgically stapled in position on the treated vessel to prevent undesired displacement or partial or complete collapse under vascular pressure.
[0055] Where the graft is expandable and in tubular or sleeve form, the diametrical size of the graft may be enlarged in contiguous relationship with the inside vascular surface via a balloon catheter. The tubular graft itself may comprise a biologically inert or biologically active anti-stenotic coating applied directly to the treated area of the remaining vascular inner surface to define a lumen of sufficient blood flow capacity. The graft, once correctly positioned and contiguous with the interior vascular wall, is usually inherently secure against inadvertent migration within the vessel due to friction and infiltration of weeping liquid accumulating on the inside artery wall. The length of the vascular graft preferably spans beyond the treated region of the vessel.
[0056] Additionally, the present invention prosthesis can be coated with hydrophilic or drug delivery type coatings which facilitate long-term healing of diseased vessels. The silk material can be loaded or coated with a therapeutic agent or drug, including, but not limited to, antiplatelets, antithrombins, anti-inflammatories, cytostatic and antiproliferative agents, for example, to reduce or prevent restenosis in the vessel being treated. The therapeutic agent or drug is preferably selected from the group of therapeutic agents or drugs consisting of sodium heparin, low molecular weight heparin, hirudin, prostacyclin and prostacyclin analogues, dextran, glycoprotein IIb/IIIa platelet membrane receptor antibody, recombinant hirudin, thrombin inhibitor, calcium channel blockers, colchicine, fibroblast growth factor antagonists, fish oil, omega 3-fatty acid, histamine antagonists, HMG-CoA reductase inhibitor, methotrexate, monoclonal antibodies, nitroprusside, phosphodiesterase inhibitors, prostaglandin inhibitor, seramin, serotonin blockers, steroids, thioprotease inhibitors, triazolopyrimidine and other PDGF antagonists, alpha-interferon and genetically engineered epithelial cells, and combinations thereof. While the foregoing therapeutic agents have been used to prevent or treat restenosis and thrombosis, they are provided by way of example and are not meant to be limiting, as other therapeutic drugs may be developed which are equally applicable for use with the present invention.
[0057] The stent-graft prosthesis of the present invention features a variety of characteristics to make its widespread application efficacious, such as easy handling, suturability, capacity for uniform mass production, shelf storage, repeated sterilization and availability in appropriate sizes. Although various changes and modifications can be made to the present invention, it is intended that all such changes and modifications come within the scope of the invention as set forth in the following claims.
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A stent-graft composite intraluminal prosthesis comprises an elongate radially adjustable tubular stent, defining opposed exterior and luminal stent surfaces and a polymeric stent sheath covering at least the exterior surface thereof. The stent can include a plurality of open spaces extending between the opposed exterior and interior surfaces so as to permit said radial adjustability. The stent has a polymeric material on its exterior surface, its interior surface, in interstitial relationship with the stent or any combination of the above. The polymer is preferably selected from the group of polymeric materials consisting of biological or genetically engineered spider silks, such as those derived from Nephila clavipes . The silk includes bioengineered spider silks as well as silk-like polymers manufactured using human proteins and blends of such silks with commonly used polymeric graft materials. If separate sheaths are placed on both the exterior and interior surfaces of the stent, the sheaths are secured to one another through said open spaces, such as by lamination, suturing or adhesion.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a combustor, particularly to a gas turbine combustor in which additional air can be supplied by a bypass passage.
2. Description of the Related Art
In general, a gas turbine combustor is disposed between a compressor and a turbine. Fuel F is supplied to a gas turbine combustor through a fuel supplying passage of a nozzle portion in the gas turbine combustor. Compressed air A compressed by the compressor is supplied to a casing of the gas turbine combustor and, then enters the nozzle portion through an inlet portion of the nozzle portion and is supplied to the combustor through a swirler. Thus, the compressed air A and the fuel F are mixed and burned in the combustor. High temperature gas produced by combustion of the compressed air A and the fuel F is discharged from the combustor through a tail portion thereof to drive the turbine provided on the downstream side of the gas turbine combustor in the direction of air flow.
A bypass passage having a bypass valve is provided on one side of the combustor tail portion. When the output of the turbine varies, the bypass valve is opened and closed so that the compressed air A in the casing is supplied to the combustor tail portion through the bypass passage from the inlet portion to an outlet portion thereof. Accordingly, additional compressed air A is supplied to the combustor tail portion so that the air-fuel ratio, i.e., the ratio of air to fuel in the gas turbine combustor can be maintained at an appropriate value.
However, the bypass passage is attached to only one side of the combustor in a known gas turbine combustor. Therefore, when additional compressed air A is supplied to the combustor tail portion through the bypass passage, the concentration of fuel in the combustor tail portion is locally decreased in the vicinity of the outlet of the bypass passage.
In general, when the ratio of combustion air to fuel is high, the flame becomes unstable due to lack of fuel. In addition, when the ratio of fuel to combustion air is high, NOx tends to easily occur. In other words, the flame tends to become unstable in the vicinity of the outlet of the bypass passage, and NOx tends to occur at the opposite side of the outlet, in a cross section of the combustor tail portion. Therefore, if the bypass valve is adjusted to maintain the air-fuel ratio at a substantially constant value, it is necessary for the additional compressed air passing through the bypass passage to be uniformly supplied to the combustor tail portion in the circumferential direction thereof.
The additional compressed air A is supplied to the combustor, particularly to the combustor tail portion via the outlet of the bypass passage, so that the temperature in the vicinity of the outlet is locally decreased, and unevenness of the temperature distribution occurs in a cross section of the combustor tail portion.
Accordingly, the object of the present invention is to provide a combustor in which the compressed air passing through the bypass passage is uniformly supplied into the combustor tail portion in the circumferential direction thereof, and unevenness of the temperature distribution in a cross section of the combustor tail portion is reduced.
SUMMARY OF THE INVENTION
According to an embodiment of the present invention, the present invention provides a combustor to burn fuel, comprising a bypass passage connected to one side of the combustor to supply air into the combustor; and an annular passage provided around the combustor and connected to the bypass passage, wherein air supplied through the bypass passage passes through the annular passage in the circumferential direction, and is uniformly supplied into the combustor in the circumferential direction thereof through an opening which connects the combustor and the annular passage.
Namely, according to the embodiment of the present invention, air passing through the bypass passage is uniformly supplied in the circumferential direction of the combustor and particularly to the combustor tail portion to thereby reduce unevenness of the temperature distribution in a cross section of the combustor tail portion.
These and other objects, features and advantages of the present invention will be more apparent in light of the detailed description of exemplary embodiments thereof as illustrated by the drawings.
BRIEF DESCRIPTION OF THE DRAWING
The present invention will be more clearly understood from the description as set below with reference to the accompanying drawings, wherein:
FIG. 1 is a sectional view of a known gas turbine combustor;
FIG. 2 is a side view of a combustor according to a first embodiment of the present invention;
FIG. 3 is a sectional view taken along the line X—X in FIG. 2 ;
FIG. 4 is a longitudinal partial sectional view of a combustor according to a first embodiment of the present invention;
FIG. 5 is a longitudinal partial sectional view of a combustor according to a second embodiment of the present invention;
FIG. 6 a is an enlarged schematic view of an overlapped portion of a first cylinder portion and a second cylinder portion in FIG. 5 ;
FIG. 6 b is an enlarged schematic view of an overlapped portion of a first cylinder portion and a second cylinder portion in FIG. 5 ;
FIG. 7 is a longitudinal partial sectional view of a combustor according to a third embodiment of the present invention;
FIG. 8 is a longitudinal partial sectional view of a combustor according to another embodiment;
FIG. 9 a is an enlarged schematic view of a supporting member in FIG. 8 .
FIG. 9 b is an enlarged schematic view of a supporting member in FIG. 8 .
FIG. 10 is a longitudinal partial sectional view of a combustor according to a forth embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Before proceeding to a detailed description of the preferred embodiments, a prior art will be described with reference to the accompanying drawings relating thereto for a clearer understanding of the difference between the prior art and the present invention.
FIG. 1 is a cross sectional view of a gas turbine combustor disclosed in a related art, for example, Japanese Unexamined Patent Publication (Kokai) No. 2000-130756. Such gas turbine combustor is disposed between a compressor and a turbine. Fuel F is supplied to a gas turbine combustor 100 through a fuel supplying passage 330 of a nozzle portion 300 in the gas turbine combustor 100 . Compressed air A compressed by a compressor 400 is supplied into a casing 800 of the gas turbine combustor 100 . The compressed air A enters the nozzle portion 300 through an inlet portion 350 of the nozzle portion 300 and is supplied into the combustor through a swirler 370 . Therefore, the compressed air A and the fuel F are mixed and burned in the combustor. High temperature gas produced by combustion of the compressed air A and the fuel F is discharged from the combustor through a tail portion thereof to drive a turbine (not shown) provided on the downstream side of the gas turbine combustor 100 in the direction of air flow.
A bypass passage 900 having a bypass valve 970 is provided on one side of the combustor tail portion 500 . When the output of the turbine varies, the bypass valve 970 is opened and closed so that the compressed air A in the casing 800 is supplied to the combustor tail portion 500 through the bypass passage 900 from an inlet portion 950 to an outlet portion 990 thereof. Accordingly, the additional compressed air A is supplied to the combustor tail portion 500 so that the air-fuel ratio, i.e., the ratio of air to fuel in the gas turbine combustor 100 can be maintained at an appropriate value.
An embodiment of the present invention will be described below with reference to accompanying drawings. In following drawings, the same members are designated by similar numerals.
FIG. 2 and FIG. 4 show a side view and a longitudinal partial sectional view of a combustor according to a first embodiment of the present invention, respectively. As shown in FIG. 4 , the fuel F is supplied to the gas turbine combustor 10 through a fuel supplying passage 33 provided in a nozzle 30 . The compressed air A compressed by a compressor (not shown) enters the nozzle 30 through the inlet portion 35 and is supplied into the gas turbine combustor 10 through a swirler 37 . The fuel F and the compressed air A are mixed and burned in the combustor.
A bypass passage 90 is connected to one side of a combustor tail portion 50 . The bypass passage 90 contains a bypass valve 97 (not shown). As shown in FIG. 2 , in the first embodiment, an annular passage containing member which contains an annular passage therein, i.e., an annular scroll 60 , is disposed between the combustor tail portion 50 and the bypass passage 90 . As shown in FIG. 3 which is a cross sectional view taken along the line X—X in FIG. 2 , an annular passage 61 extending in the circumferential direction is formed in the annular scroll 60 . The annular scroll 60 is provided on the outer peripheral portion of the combustor tail portion 50 substantially coaxially to the center axis of the combustor. As shown in FIG. 3 and FIG. 4 , a plurality of openings 51 are formed in a wall portion of the combustor tail portion 50 . In the first embodiment, the openings 51 formed in the wall portion of the combustor tail portion 50 are spaced at a substantially equal distance in the circumferential direction. Therefore, the bypass passage 90 and the annular scroll 60 are connected to each other via the outlet 99 , and the annular scroll 60 and the combustor tail portion 50 are connected to each other via the openings 51 .
When the output of a turbine (not shown) varies and a partial load is applied to the gas turbine combustor 10 , the bypass valve 97 is opened. Accordingly, additional compressed air A can be supplied from a casing 80 into the bypass passage 90 through the inlet portion 95 of the bypass passage 90 . As shown in FIG. 3 , the additional compressed air A enters the annular scroll 60 through the outlet portion 99 of the bypass passage 90 . The additional compressed air A enters the combustor tail portion 50 through the annular passage 61 of the annular scroll 60 and openings 51 formed in the wall portion of the combustor tail portion 50 . Therefore, the additional compressed air A is supplied substantially uniformly to the combustor, particularly to the combustor tail portion 50 , in the circumferential direction thereof. Accordingly, unevenness of the temperature distribution in the cross section of the combustor can be reduced when the partial load is applied. Slits can be formed on the wall portion of the combustor tail portion 50 in the circumferential direction thereof, in place of the openings 51 . In this case, the additional compressed air A can be more uniformly supplied into the combustor tail portion 50 .
FIG. 5 is a longitudinal partial sectional view of a combustor according to a second embodiment of the present invention. In the second embodiment, the combustor contains a first cylinder portion 53 and a second cylinder portion 54 . As shown in FIG. 5 , the first cylinder portion 53 and the second cylinder portion 54 are coaxially arranged and are partly overlapped with a predetermined space therebetween, so that an annular or cylindrical clearance 55 is formed between these cylinder portions. It is apparent from FIG. 5 that a superimposed portion 59 , in which these cylinder portions are overlapped, i.e., superimposed, is positioned in the annular scroll 60 . An upstream side end portion of the annular scroll 60 positioned on the upstream side in the flow direction of fuel F in the annular scroll 60 and a downstream side end portion of the annular scroll positioned on the downstream side are connected to the first cylinder portion 53 and the second cylinder portion 54 , respectively. Therefore, the additional compressed air A in the annular scroll 60 does not leak out.
Additional compressed air A entering from the bypass passage 90 into the annular scroll 60 passes along the inner wall of the combustor tail portion 50 via the annular passage 61 and the annular space 55 . Accordingly, a thin layer of a low-temperature airflow (a so-called cooling film) is formed along the inner wall of the combustor tail portion 50 , and then the combustor tail portion 50 is cooled by the low-temperature airflow layer (such a cooling method is called “film cooling”). An annular cooling film is formed because the space 55 is annular, and thus the combustor tail portion 50 can be uniformly cooled in the circumferential direction thereof. In other words, according to the second embodiment, additional compressed air passing through the bypass passage can be uniformly supplied to the combustor, particularly to the combustor tail portion in the circumferential direction thereof, and unevenness of the temperature distribution in a cross section of the combustor tail portion can be reduced.
FIG. 6 a and FIG. 6 b are schematic views of the superimposed portion 59 of the first cylinder portion 53 and the second cylinder portion 54 . In the second embodiment, as shown in FIG. 6 a , the first cylinder portion 53 and the second cylinder portion 54 are separate members, and define the annular space 55 . However, as shown in FIG. 6 b , the first cylinder portion 53 and the second cylinder portion 54 may be integrally formed as a single member, and a plurality of through holes 56 extending in the axial direction of the combustor tail portion 50 may be formed in the superimposed portion 59 . The through holes 56 are spaced at an equal distance in the circumferential direction. In this case, since the cooling film extends to a portion further downstream to that of the embodiment shown in FIG. 6 a , the combustor tail portion 50 can be cooled over a wider area.
FIG. 7 is a longitudinal partial sectional view of a third embodiment of a combustor according to the present invention. The combustor contains the first cylinder portion 53 and the second cylinder portion 54 . In the third embodiment, the superimposed portion 59 in which the first cylinder portion 53 and the second cylinder portion 54 are partially superimposed extends beyond the annular scroll 60 on the downstream side, in the flow direction of fluid, in the combustor. Additional compressed air A entering from the bypass passage 90 into the annular passage 61 of the annular scroll 60 enters the annular space 55 of the superimposed portion 59 . The additional compressed air A passes through the annular space 55 to thereby effectively cool the combustor, particularly the combustor tail portion 50 , by convection cooling. The combustor tail portion 50 can be cooled substantially uniformly in the circumferential direction over a wide area by convection cooling. In other words, according to the third embodiment, air passing through the bypass passage can be uniformly supplied in the circumferential direction of the combustor tail portion, and unevenness of the temperature distribution in the cross section of the combustor tail portion can be reduced over a wide area.
As a matter of course, as shown in FIG. 6 b , the first and second cylinder portions 53 , 54 are formed as a single member, and a plurality of through holes 56 may be formed in the superimposed portion 59 in place of the annular space 55 . In the above-described second embodiment, it is apparent that convection cooling is partially carried out in the superimposed portion 59 .
FIG. 8 is a longitudinal partial sectional view of another embodiment of a combustor according to the present invention. The combustor contains the first cylinder portion 53 and the second cylinder portion 54 . Similar to the above-described third embodiment, the annular space 55 is formed in the superimposed portion 59 in which the first cylinder portion 53 and the second cylinder portion 54 are partially superimposed. In this embodiment, a plurality of supporting members 57 are disposed between the first cylinder portion 53 and the second cylinder portion 54 and in the superimposed portion 59 . FIG. 9 a and FIG. 9 b are partially enlarged views of the first cylinder portion 53 having the supporting member 57 . In FIG. 9 a , a plurality of columnar supporting members 57 are spaced at an equal distance with each other on the outer wall of the first cylinder portion 53 . The inner wall of the second cylinder portion 54 is disposed on the top face of the supporting member 57 . However, for ease of understanding, the second cylinder portion 54 is omitted in FIG. 9 a and FIG. 9 b . The first cylinder portion 53 and the second cylinder portion 54 can be supported by the supporting members 57 , against combustion vibration caused during the operation of the combustor. Therefore, the annular space 55 can be maintained without being crushed by combustion vibration. Furthermore, the supporting member 57 can improve heat transferring between the first cylinder portion 53 and the second cylinder portion 54 . Thus, according to the embodiment, air passing through the bypass passage is uniformly supplied to the combustor, particularly to the combustor tail portion in the circumferential direction thereof, so that the unevenness of the temperature distribution in the cross section of the combustor tail portion can be reduced. As a matter of course, in the above-described second embodiment, the arrangement of the supporting member in the annular space 55 is included within the scope of protection of the present invention.
FIG. 10 is a longitudinal partial sectional view of a forth embodiment of a combustor according to the present invention. In the forth embodiment, a sleeve 70 is arranged substantially coaxially to the center axis of the combustor tail portion 50 , between the outer wall of the combustor tail portion 50 and the inner wall of the annular scroll 60 . Therefore, the sleeve 70 and the outer wall of combustor tail portion 50 are substantially parallel. The length in the axial direction of the sleeve 70 is substantially identical to that of the annular scroll 60 . As shown in FIG. 10 , a plurality of holes 71 are formed in the sleeve 70 . A plurality of openings 51 are formed in the combustor tail portion 50 within the annular scroll 60 . In the forth embodiment, the plural openings 51 and the plural holes 71 are disposed in a staggered configuration.
The additional compressed air A entering the annular scroll 60 through the bypass passage 90 passes through the annular passage 61 and the hole 71 of the sleeve 70 and impinges on the outer wall of the combustor tail portion 50 . The sleeve 70 and the combustor tail portion 50 are coaxial to each other, so that the additional compressed air A passing through the hole 71 of the sleeve 70 impinges substantially vertically on the outer wall of the combustor tail portion 50 . A cooling method in which fluid is vertically supplied onto the surface of the object to be cooled is called “impinge cooling” or “impingement cooling”. Then, the additional compressed air A enters the combustor tail portion 50 through the opening 51 of the combustor tail portion 50 .
In the forth embodiment, the additional compressed air passing through the bypass passage 90 is uniformly supplied to the combustor, particularly to the combustor tail portion in the circumferential direction thereof, so that unevenness of the temperature distribution in the cross section of the combustor tail portion can be reduced by impinge cooling. It is preferable that the opening 51 not be formed at a position of the combustor tail portion 50 corresponding to the hole 71 , since this improves the effect of impinge cooling. The sleeve 70 functions as an acoustic liner so that combustion vibration produced when the combustor is operated can be decreased.
As a matter of course, any combination of the embodiments described above to produce the combustor is included within the scope of the present invention. For example, to form an annular passage on the wall portion of the combustor without the annular scroll is within the scope of the present invention.
According to an embodiment of the present invention, the common effect can be obtained that the additional air passing through the bypass passage is supplied to the combustor, particularly to the combustor tail portion uniformly in the circumferential direction thereof, so that unevenness of the temperature distribution in a cross section of the combustor tail portion can be reduced.
According to another embodiment of the present invention, the effect can be obtained that the additional air can be further uniformly supplied from the bypass passage to the combustor, particularly to the combustor tail portion.
According to yet another embodiment of the present invention, the effect can be obtained that the combustor, particularly, the combustor tail portion, can be effectively cooled by a cooling film.
According to yet another embodiment of the present invention, the effect can be obtained that the combustor, particularly, the combustor tail portion, can be effectively cooled by convection cooling.
According to yet another embodiment of the present invention, the effect can be obtained that the supporting member is provided between the first cylinder portion and the second cylinder portion to support the same, and what can improve the heat transferring.
According to yet another embodiment of the present invention, the effect can be obtained that the combustor, particularly, the combustor tail portion, can be effectively cooled by impinge cooling, and the sleeve functions as an acoustic liner to reduce combustion vibration.
Although the invention has been shown and described with exemplary embodiments thereof, it should be understood by those skilled in the art that the foregoing and various other changes, omissions and additions may be made therein and thereto without departing from the spirit and scope of the invention.
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There is provided a combustor to burn fuel, comprising a bypass passage connected to one side of the combustor to supply air into the combustor; and an annular passage provided around the combustor and connected to the bypass passage, wherein air supplied through the bypass passage passes in the annular passage in the circumferential direction, and is uniformly supplied into the combustor in the circumferential direction thereof through an opening which connects the combustor and the annular passage. Accordingly, compressed air passing through the bypass passage can be supplied uniformly into a tail portion of the combustor, and unevenness of temperature distribution in a cross section of the combustor tail portion can be reduced.
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FIELD OF THE INVENTION
The present invention relates to an apparatus and process for cleaning foreign matter from fiber.
BACKGROUND OF THE INVENTION
In harvesting, seed cotton is stripped or picked from the plant, deposited in a trailer or other vehicle, and transported to a cotton gin. The cotton gin has apparatus for receiving the seed cotton, removing the seeds, cleaning the cotton fiber, and pressing the fiber into bales for transport to textile mills or compresses for further operation.
Prior to the present invention, trash or foreign matter in cotton fiber, or lint, presented significant problems to cotton producers and textile mills. High trash contents reduces the price the producer receives for the product. Efforts to further clean the fiber in the gin to reduce trash levels caused fiber damage by breaking and tangling the fiber. This fiber damage decreases the quality of the resulting yarn and cloth. The present invention performs the fiber cleaning needed by the producer for good returns without causing damage to the fiber which would reduce the quality of textiles made from the fiber.
U.S. Pat. No. 4,528,725 to Horn et al discloses a gin lint cleaner that utilizes a feed plate to direct the ginned fiber onto a downstream saw cylinder Horn et al then uses sharp-edged grid bars to further engage the ginned fiber with the downstream cylinder. The action of a second downstream saw cylinder and deflector remove the lint from the first cylinder and deposit the lint onto a second cylinder. Horn et al then uses round blunt bars, a seating bar, sharp-edged grid bars, a trash bar, and a combing bar. Between the feed plate, saw to saw interaction, and the combing bars, the ginned fiber is subject to considerable abrasion which tends to cause more fiber breakage. Therefore, there is still a need in the art for more efficient gin fiber cleaning which is capable of cleaning fiber with lower levels of fiber breakage and at lower energy costs.
SUMMARY OF THE INVENTION
In accordance with the present invention, there are provided fiber cleaning processes and apparatus which solve the problems identified above with regard to cleaning fiber. In describing the cylinders of the present invention, it will be understood that each cylinder rotates about an axis. Various bar devices are positioned adjacent and along the cylinders, parallel the axes.
The present invention combines the use of guiding means (including feed control bars) and flow deflecting means (including air control bars) to produce fiber cleaning that uses less power, breaks fewer fibers and results in less tangling of the fiber.
Doffing brush cylinders mechanically remove the ginned fiber from an upstream saw cylinder and transfers the fiber to the next downstream fiber cleaning saw cylinder, or in the case of the last downstream doffing brush cylinder, to a bale press. The transfer of ginned fiber takes place such that the flow of fiber changes direction at the pinch point between the upstream saw cylinder and the doffing brush cylinder. The pinch point is the point of contact of an upstream cylinder with the next downstream cylinder. The tangential speed of the outer periphery of the doffing brush cylinders is preferably set between 1.25 and 2 times the tangential speed of the outer periphery of the upstream saw cylinder.
As the ginned fiber is being rotated on the doffing brush cylinder and about to be transferred to a downstream cleaning saw cylinder the ginned fiber has a tendency to lift off the doffing brush cylinder before reaching the pinch point. Guiding means, including feed control bars, are provided by the present invention to help keep the ginned fiber on the doffing brush cylinder and guide the transfer of the ginned fiber from the doffing brush cylinder to the next downstream cleaning saw cylinder up to the pinch point.
Normally, entrained air along the outer periphery of the doffing brush cylinders continues to rotate beyond the pinch point of the downstream cleaning saw cylinder. The entrained air continues to flow to the point where the doffing brush cylinder again removes ginned fiber from an upstream saw cylinder. If fiber is allowed to travel with the entrained air back to the pinch point of the upstream saw cylinder and the doffing brush cylinder, the recirculated fiber increases the tangling of all the fiber, and thereby adversely affects the nep count of the fiber.
The present invention provides flow deflecting means including air control bars to deflect a substantial portion of the flow of entrained air from flowing around the doffing brush cylinder toward an upstream cleaning saw cylinder. By use of the air control bars, the entrained air will instead be deflected to flow counter rotationally around the next downstream cleaning saw cylinder. The air control bar is placed opposite the flow control bar between the pinch point of a doffing brush cylinder and a fiber cleaning saw cylinder on the non-fiber flow side of the pinch point.
In addition, an air control bar is placed immediately downstream of the point where the ginned fiber is removed from the last doffing brush cylinder and removed from the ginned fiber cleaning housing.
The specific nature of the invention, as well as other objects, uses, and advantages thereof, will clearly appear from the following description and from the accompanying drawings, which are not necessarily to scale.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a side elevation view of a preferred gin fiber cleaner of the present invention.
FIG. 2 is a large scale side view of a feed control bar of the present invention which has a substantially triangular cross-section with the hypotenuse being an arcuate surface which is parallel to the outer peripheral surface of the immediate upstream doffing brush cylinder.
FIG. 3 is a front view of a feed control bar of the present invention.
FIG. 4 is a side view of an air control bar of the present invention, shown in large scale.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In a typical cotton gin process flow, cotton is harvested in the field and transported to the location of a cotton gin building. The delivered cotton, which is sometimes referred to as seed cotton, contains foreign matter or trash, which may include stalks, stems, leaves, bark, and boll pieces. The foreign matter may also include small pebbles, dirt, sand, weeds, seeds and other trash which the harvesting equipment may have picked up.
The seed cotton is fed to one or more gin stand saw cylinders where the seeds are separated from the lint, or fiber cotton. The ginned cotton fiber still contains foreign matter after being processed by the gin stand cylinder. Therefore, the ginned cotton fiber is transported to a fiber cleaner, and from the fiber cleaner to a lint bale press (not shown).
FIG. 1 shows a preferred embodiment of a cotton fiber cleaner of the present invention. The figure shows a first ginning means for separating fiber and seed, including a gin housing having a gin saw cylinder 1 (i.e. gin stand cylinder), as well as fiber cleaning means including two fiber cleaning saw cylinders 3 and 5. The gin stand saw cylinder and two fiber cleaning saw cylinders are rotationally driven by a manner well known in the art, such as a motor connected by a drive belt to a drive pulley which is integrally attached to the cylinder.
For clarity, only the cotton fiber feed assembly is shown in FIG. 1. Likewise, much of the structure shown in FIG. 1, such as the sheet metal walls forming the trash disposal, and airflow control ducts and brackets for mounting are not shown. Those skilled in the art will be able to supply the necessary frame, covers, baffles, duct-work, mounting brackets and other omitted structure based on the disclosure herein and knowledge of the gin lint cleaning art.
With regard to the figures hereof, it will be understood that the arrows inside each cylinder represent the direction of rotation of that cylinder, and hence the direction of teeth or other structure attached thereon. Arrows outside the cylinders represent the direction of flow of trash and foreign matter or air flow, as appropriate. The flow of fiber is shown as a herringbone band on the outer periphery of the cylinders. Cylinders 1, 4 and 5 are rotating clockwise, while cylinders 2, 3 and 6 are rotating counter-clockwise as viewed in FIG. 1.
Cylinders 2, 4 and 6 are doffing brush cylinders which are part of fiber transporting or removing means. The doffing brush cylinders are preferably constructed as a solid spiral-wrapped brush. The doffing brush cylinders mechanically remove the ginned cotton fiber from the respective upstream saw cylinder 1, 3 and 5. The transfer of ginned cotton fiber takes place such that the flow of cotton fiber changes direction at the pinch point between an upstream cleaning saw cylinder and the next downstream doffing brush cylinder. The tangential speed of the outer periphery of the doffing brush cylinders is preferably between 1.25 and 2 times the tangential speed of the outer periphery of the respective upstream saw cylinder.
The fibers, which are attached to gin saw cylinder 1 after being separated from the seed (ginned), are doffed by doffing brush cylinder 2 at the pinch point between cylinders 1 and 2. The fibers exit the pinch point tangentially and proceed substantially in a straight line until impacting containment 9. The fibers continue on the surface of containment 9 and feed control bar 10 until engaged by the teeth of cleaning saw cylinder 3. The feed control bars 10 and 16 have an arcuate surface which is parallel to the outer peripheral surface of the doffing brush cylinders 2 and 4, respectively, adjacent to the pinch point. The feed control bars 10 and 16 are substantially triangular in cross-section with the hypotenuse of the triangle being the arcuate surface (FIG. 2). The feed control bars 10 and 16 extend substantially the entire length of the doffing brush and cleaning saw cylinders and are attached at each end to the gin housing (FIG. 3). The feed control bars 10 and 16 form a sharp point adjacent to the pinch point. The feed control bars 10 and 16 are placed as close as practical to the cleaning saw cylinders 3 and 5, respectively, as well as close as practical up to the pinch point between the doffing brush cylinder and the next downstream cleaning saw cylinder.
Normally, entrained air along the outer periphery of the doffing brush cylinder continues to rotate beyond the pinch point of the downstream cleaning saw cylinder. The entrained air continues to rotate along the outer periphery to the point where the doffing brush cylinder again removes ginned fiber from an upstream cylinder. It is believed that this entrained air promotes tangling of the fiber, thereby increasing the nep count.
In the present invention, flow deflecting means, including air control bars 11, 7 and 24, are used to deflect the flow of entrained air from continuing to flow around the doffing brush cylinder. Instead the air is deflected toward the next downstream cleaning saw cylinder. For example, the air control bar 11, located between doffing brush cylinder 2 and cleaning saw cylinder 3 deflects the flow of entrained air from continuing around doffing brush cylinder 2 to flowing in the annular space between cleaning saw cylinder 3, which is rotating in the opposite direction to the flow of deflected air, and containment 15 (FIG. 4). Air control bar 11 has an arcuate surface which is parallel to the outer peripheral surface of the next downstream cleaning saw cylinder.
The air control bar 11 prevents substantially all of the air from continuing to flow in the annular space between cylinder 2 and containment 12. Any air that does flow in the annular space between cylinder 2 and containment 12 is directed tangentially in a manner which does not alter the path of the fiber being doffed at the pinch point between cylinders 1 and 2. Eventually, most of the deflected air will be entrained around the outer periphery of doffing brush cylinder 4 (FIG. 1). The air control bar 17 has an arcuate surface which is substantially parallel to the outer peripheral surface of the doffing brush cylinder 4 adjacent to the pinch point. Containment 18 and fiber guide 14 prevent entrainment of trash which was previously thrown out. Fiber guide 14, which runs the length of doffing brush cylinder 4, prevents the doffing brush cylinder from contacting the fiber until the fiber is near the pinch point, thereby aiding in the doffing action. Air flow continues in the annular space between cleaning saw cylinder 5 and containment 22, and is entrained with the fiber between doffing brush cylinder 6 and containment 23. The entrained air exits the gin housing in lint flue 25. The air control bars 11, 17 and 24 are substantially triangular in cross-section with the hypotenuse of the triangle being the arcuate surface. The air control bars 11, 17 and 24 extend substantially the entire length of the doffing and cleaning cylinders. The air control bars 11 and 17 form a sharp point adjacent the pinch point. The air control bars 11, 17 and 24 are placed as close as practical to the doffing brush cylinder. The air control bars 11 and 17 are placed as close as practical up to the pinch point between the doffing brush cylinder and the downstream cleaning saw cylinder. The air control bars 11 and 17 are placed opposite the feed control bars 10 and 16 between the pinch point of the doffing brush cylinder and the fiber cleaning saw cylinder on the non-fiber flow side of the pinch point. Also, the arcuate surface of each of the air control bars 17 and 24 is parallel to the outer peripheral surface of the next upstream doffing brush. Both the feed control bars and the air control bars define: a first planar rectangular surface, a second planar rectangular surface oriented at approximately a right angle to the first surface, and an arcuate surface joined to both said first and second surfaces.
In addition, an air control bar 24 is placed downstream of the point where the ginned fiber is removed from the last doffing brush cylinder and removed from the gin housing. The air control bar 24 is placed such that it is immediately downstream of, and substantially mates with, the last downstream doffing brush cylinder.
Transferring and inverting the ginned fiber between two counter-rotating cleaning saw cylinders exposes both sides or surfaces of the ginned fiber to cleaning devices. For example, the cleaning bars 13 and 21 in FIG. 1, which are situated adjacent to the cleaning saw cylinders in the moting area, clean the side of the fiber facing away from the cleaning saw cylinder. The fiber is inverted during transfer from one cleaning saw cylinder to another, and additional cleaning takes place during transfer at the pinch point. Thus, in addition to providing more peripheral area for the use of cleaning devices, the use of two or more cleaning saw cylinders permits cleaning of both sides of the fiber. More peripheral area for cleaning is also available on gin cylinder 1 with cleaning bars 7 and 8.
Cleaning bars 13 and 21 are mounted to the housing and are parallel the axes, adjacent to the cleaning saw cylinders 3 and 5. The bars 13 and 21 have sharp edges parallel the cylinder axes. As the cleaning saw cylinders move the cotton fiber past the bars 13 and 21, the fiber is scrubbed against the edges. This disturbance of the fiber, in combination with centrifugal force and gravity, loosens foreign matter from the cotton fibers in the layer. The trash is then carried to a trash conveyor (not shown). The bars 13 and 21 are placed an effective distance from the cleaning saw cylinders. That is, at a distance which is effective for removing trash from the fiber, but not so close as to result in fiber damage.
Referring to FIG. 1, it may be seen that the pinch points are each radially separated by more than 180 degrees. This results in the staggered, or zig-zag arrangement of the cleaning and doffing brush cylinders. This staggered arrangement exposes more of the periphery of the cleaning saw cylinders in the path of the layer for the installation and utilization of cleaning devices such as the cleaning bars previously described.
It will be understood that additional fiber cleaning saw cylinders could be placed downstream of doffing brush cylinder 6 for additional cleaning capacity. In addition, for minimal cleaning capacity, the gin building housing could be constructed with only cylinders 1, 2, 3 and 4. However, in the preferred embodiment shown in FIG. 1, two fiber cleaning saw cylinders are used so that each side of the cotton fiber is cleaned once.
It will also be understood that the terms "upstream" or "downstream" are dependent upon the position of the referenced cylinder. The terms "upstream" and "downstream" are not restricted to the first or last cylinders, respectively.
Each of the fiber cleaning saw cylinders 3 and 5 have drive means connected thereto (not shown) for rotating the cylinders counter to each other. Each of the fiber cleaning saw cylinders has a plurality of saw teeth attached to and spaced over a surface thereof. An appropriate frame (not shown) supports the mounted cylinders and structure positioned thereabout.
The operation of the cotton gin of FIG. 1 is as follows. The cotton fiber enters the gin housing and is fed to the gin saw cylinder 1 (i.e. gin stand cylinder). The seed is separated from the fiber whereupon the ginned fiber is removed from the gin saw cylinder by counter rotating doffing brush cylinder 2. The ginned fiber is then transferred to a first fiber cleaning saw cylinder 3. Saw cylinder 3 is rotating in the same (counter-clockwise) direction as doffing brush cylinder 2. The ginned fiber thereby changes directions when it is transferred from doffing brush cylinder 2 to saw cylinder 3 at the pinch point. One side of the ginned fiber is then cleaned by cleaning bar 13 as the ginned fiber rotates past them. The ginned fiber is then removed and inverted from the first fiber cleaning saw cylinder 3 by a second counter rotating doffing brush cylinder 4. The ginned fiber is then transferred to a second fiber cleaning saw cylinder 5 at the pinch point between cylinders 4 and 5. Cylinder 5 is rotating in the same direction (clockwise) as doffing brush cylinder 4. Therefore, the ginned fiber changes direction as it is transferred from the second doffing brush cylinder 4 to the second fiber cleaning saw cylinder 5 at the pinch point. Containment 19 and adjustable fiber guide 20 prevent excess fiber loss. The other side of the ginned fiber is then cleaned by the cleaning bars 21 as the ginned fiber rotates past them. The ginned fiber is then removed from the second fiber cleaning saw cylinder 5 by third doffing brush cylinder 6. The cleaned ginned fiber is then removed from the third doffing brush cylinder 6 and removed to downstream baling apparatus via lint flue 25.
FIG. 3 is a front view of feed control bar 10 in relation to cleaning saw cylinder 3. The bar is attached to the gin housing by attachment means 30.
Various changes and modifications may be made in this invention, as may be apparent to those skilled in the art. Such changes and modifications are within the scope of this invention, as defined by the claims appended hereto.
INDEX OF ELEMENTS DESIGNATED BY A NUMERAL
1 gin saw cylinder
2 doffing brush cylinder
3 fiber cleaning saw cylinder
4 doffing brush cylinder
5 fiber cleaning saw cylinder
6 doffing brush cylinder
7 cleaning bar
8 cleaning bar
9 containment
10 feed control bar
11 air control bar
12 containment
13 cleaning bar
14 fiber guide
15 containment
16 feed control bar
17 air control bar
18 containment
19 containment
20 adjustable fiber guide
21 cleaning bar
22 containment
23 containment
24 air control bar
25 lint flue
30 attachment means
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A fiber cleaning utilizing an alternating series of cleaning saw cylinders and doffing brush cylinders. The doffing brush cylinders transfer ginned fiber from an upstream cleaning saw cylinder to the next downstream cleaning saw cylinder in such a way that the flow of the fiber changes direction at the pinch point between the upstream cleaning saw cylinder and the doffing brush cylinder. Guiding means including control bars are provided to help guide the ginned fiber from the doffing brush cylinder to the next downstream cleaning saw cylinder at the pinch point. Flow deflecting means including air control bars are provided to deflect a substantial portion of the flow of entrained air from flowing around the doffing brush cylinder.
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TECHNICAL FIELD
[0001] A piston-chamber combination comprising an elongate chamber which is bounded by an inner chamber wall and comprising a piston means in said chamber to be sealingly movable relative to said chamber at least between first and second longitudinal positions of said chamber, said chamber having cross-sections of different cross-sectional areas at the first and second longitudinal positions of said chamber and at least substantially continuously differing cross-sectional areas at intermediate longitudinal positions between the first and second longitudinal positions thereof, the cross-sectional area at the first longitudinal position being larger than the cross-sectional area at the second longitudinal position, said piston means being designed to adapt itself and said sealing means to said different cross-sectional areas of said chamber during the relative movements of said piston means from the first longitudinal position through said intermediate longitudinal positions to the second longitudinal position of said chamber, wherein the piston means comprises an elastically deformable container comprising a deformable material, wherein the piston means comprises an enclosed space communicating with the deformable container.
BACKGROUND OF THE INVENTION
[0002] EP 1179140 B1 discloses a piston chamber combination which comprises a container type piston, which is elastically deformable, communicating with an enclosed space 125 . Said space has a variable volume. In small constructions may it be not possible to ‘squeeze in’ functions which make the variability of said volume possible, and additionally may such constructions be expensive, in order to make these reliable.
[0003] EP 1384004 B1 discloses a container type piston wherein the piston is produced to have a production-size of the container in the stress-free and undeformed state thereof in which the circumferential length of the piston is approximately equivalent to the circumferential length of said chamber at said second longitudinal position, the container being expandable from its production size in a direction transversally with respect to the longitudinal direction of the chamber thereby providing for an expansion of the piston from the production size thereof during the relative movements of the piston from said second longitudinal position to said first longitudinal position. In order to expand from and return to said production size, it may be necessary to have an enclosed space in order to cope with the change of volume of the piston, in relation to the inner pressure of said piston. The small size of a construction and the complexity of the members making the variability possible makes it unlikely to have a reliable, long lasting and economical enclosed space, having a variable volume.
[0004] This invention was initiated with solutions for the problem of optimizing ergonomically the reading of a parameter such as pressure or temperature of a tyre by manual operation of a piston chamber combination, e.g. a floor pump. Current pressure gauges are positioned so far away from the user, that she or he needs to have a telescope or binoculars to enable a normal reading. As no user will use such view enhancers, many pressure gauges are being equipped with a manually rotatable pointer of a color, different from the pointer of the pressure gauge. The first mentioned pointer is pointing at the desired end pressure, and is set before the pumping session. Thereafter it is easier to assess on a distance of the difference in position of both pointers. The problem is, that end pressures of tyres normally differ from each other, and that the pointer needs to be set, mostly every time before starting the pumping. This is uncomfortable
[0005] The reason for all this, is that the pressure of a tyre in most current pumps is measured pneumatically in the hose of the pump. This prohibits the transmittal of the pneumatic information from the hose of the pump to another part of the piston-chamber combination, normally the chamber, closest to the user of the pump, due to the fact that there is a check valve between the pump and its hose, at least in high pressure pumps
[0006] A common used solution is using a wireless (=by means of electromagnetic waves) transmission for this transmittal. It normally however means the use of electronic parts, and specifically batteries or another electric source. This is expensive, resources demanding and change of batteries is uneasy to handle by a common user.
OBJECT OF THE INVENTION
[0007] The object is to provide solutions for a simple, reliable, long lasting and economical enclosed space, and for measuring a parameter.
SUMMARY OF THE INVENTION
[0008] This invention may optionally be used for a container type piston, which has an approximately constant size of the circumference of its transversal cross-section.
[0009] The piston may preferably be inflatable.
[0010] The wall of the piston may preferably comprise reinforcement means.
[0011] In a cross-section through the longitudinal direction, the container, when being positioned at the first longitudinal position of the chamber, may optionally have a first shape which is different from a second shape of the container when being positioned at the second longitudinal position of said chamber. At least part of the deformable material may be compressible and wherein the first shape may have an area being larger than an area of the second shape. The deformable material may at be least substantially incompressible.
[0012] The piston may comprising an elastically deformable container, the container comprising an elastically deformable wall, and inside said wall a deformable material, said material may be different from and/or having different characteristics than that of the material of said wall.
[0013] The deformable material inside said wall may be a fluid, or a mixture of fluids, or a foam.
[0014] A container type piston wherein the piston may preferably produced to have a production-size of the container in the stress-free and undeformed state thereof in which the circumferential length of the piston is approximately equivalent to the circumferential length of said chamber at said second longitudinal position, the container optionally being expandable from its production size in a direction transversally with respect to the longitudinal direction of the chamber thereby providing for an expansion of the piston from the production size thereof during the relative movements of the piston from said second longitudinal position to said first longitudinal position.
[0015] In order to expand from and return to said production size of an e.g. inflatable piston, it may be necessary to have an enclosed space in order to cope with the change of volume of the piston, in relation to the inner pressure of said piston. The enclosed space is functioning as the extra volume of the container.
[0016] In the first aspect, the invention relates to a piston chamber combination, wherein the volume of the enclosed space is at least substantially constant.
[0017] The starting point of the design of a device such as e.g. a pump may be the enclosed space having an unvariable volume. Still the piston may have a variable volume, and is than using the enclosed space as extra volume, e.g. in order to comply to demands toward maintaining a certain internal pressure while moving in the elongate chamber, which may be necessary to e.g. maintaining sealability to the wall of the chamber.
[0018] The ultimate solution is just avoiding additional members, which are controlling the variability of the volume of the enclosed space. The enclosed space may be a closed chamber, communicating with the piston, thus having an open end to inside of the piston and for the rest closed, so that the volume of said enclosed space remains constant. Optionally may said volume be adjustable. Specifically for piston-chamber combinations, such as e.g. innovative tyre inflation pumps, where the cross sectional area's of the chamber are differing during the stroke is the size of the operating force of these pumps not anymore representing the size of the pressure in the tyre, and it is necessary to have a reliable and non-expensive pressure reading of the tyre pressure in a gauge, nearby the user during the pump stroke, e.g. nearby the handle on top of the piston rod in case of a floorpump. The piston rod may be hollow and may be used as an enclosed space for the container type piston. Through the piston rod there may be a tube, ranging from the chamber under the piston to a gauge, e.g. positioned on top of the piston rod. Said tube comprising the enclosed measuring space within said tube, in which a parameter in the chamber, e.g. the pressure may be measured.
[0019] The gauge may be a pneumatic gauge (manometer), òr it may be an electric/electronic gauge. A wireloom through the enclosed space of enclosed measuring space may be avoided, when the sensor is positioned near the top of the enclosed measuring space, e.g. in the gauge housing.
[0020] In the second aspect, the invention relates to a piston chamber combination, wherein the piston is inflatable, and wherein the inlet of the enclosed space is comprising a check valve.
[0021] In order to inject the deformable material (a fluid or a mixture of fluids and/or foam) inside the wall of the piston, and, if necessary further pressurizing said piston, the enclosed space may have an inlet. Leakages in the inlet must be avoided, for keeping the volume of the enclosed space constant. This may be done with a check valve. Incidental deflation for e.g. maintenance purposes of the piston may be done manually, by pressing the ball of the check valve to a position inside said check valve.
[0022] In the third aspect, the invention relates to a piston chamber combination, comprising a sensor positioned at the bottom of the piston rod, and a gauge on top of the piston rod, connected through a wireloom through the enclosed space, said wire loom is embedded in a material, which is sealing the inlet and outlet, and which is comprising a stepped transition in the enclosed space at the outlet.
[0023] Said wire loom inlet and outlet should be sealing 100%, in order to keep the volume of the enclosed space unchanged. This may be done by embedding said wire loom in a material, which is sealing the rest hole around the wireloom at the inlet and the outlet spot. In order to avoid that the wireloom and seal are being pressed out by the fluid or foam in the enclosed space, the enclosed space has a stepped transition, wherein the smallest diameter is nearest the top of the piston rod, in which said seal is fitting.
[0024] In a fourth aspect, the invention relates to a piston chamber combination, wherein the combination is comprising an enclosed measuring space with an inlet at the bottom of the piston rod, and a gauge on top of the piston rod, connected by a channel in a tube through the enclosed space, wherein an O-ring is sealing said tube at least at the top of the piston rod.
[0025] In a fifth aspect, the invention relates to a combination which additionally is comprising a measurement system comprising a gauge, and an enclosed measuring space in which a parameter is being measured, wherein said enclosed space may be closed by a sealing between the gauge housing and said gauge.
[0026] Other solutions to close the chamber further from the piston are possible, but not shown.
[0027] And, a combination wherein the gauge may comprising the sensor, and where the sensor is communicating with the enclosed measuring space.
[0028] In the first aspect, the invention relates to a sensor-reader combination, wherein
[0000] the measuring is done in a measuring space, representing said device regarding to the to be measured size of said parameter, said space is positioned nearby said reader.
[0029] Obvious solutions for the transmittal of the information of a value of a parameter between parts of the combination moving relatively to each other is e.g. by an elastic wire of which each end may be connected to each part. In a pump with high pressures, will the life time of such wire being negatively affected by the harsh climate of the inside of the pump, and if not, the solution would be expensive.
[0030] Another obvious solution would be to use contacts which glide over each other during the stroke, where e.g. a contact rail would be connected to one of the moving parts, while a contact (flexible strip, or a springforce operated contact) would slide on said rail, and be connected to the other part. Not a very reliable solution in a harsh climate inside a pump. And, used in a floor pump, this would possibly prohibit the handle to rotate enough for being comfortable to pump with. This solution would be expensive as well, and not very reliable.
[0031] An obvious wireless solution is to measure e.g. the pressure in the hose of a pump, and transmit the information wireless to a receiver on the piston rod, and have a reading on a gauge on top of a handle which is operated by the user. Even this solution seems to be reliable, this solution is expensive, only already by having an electrical source on two different places.
[0032] Better solutions must be provided.
[0033] In this invention is the fact that the space of the tyre to be inflated is in direct contact with the space in the pump under the piston, during overpressure or just before balance of pressure of the pump in relation to the pressure in the tyre. That means that the size of the pressure/temperature in the tyre may be readable by measuring said parameter in the space under the piston of the pump, and in case of a high pressure pump, before the check valve, which is normally positioned between said space under the piston and the hose, which connects the pump to the valve connector, which is mounted on the tyre valve. Said space is called the measuring space. The measuring space is surrounding the bottom part of the piston rod, and thereby it may be possible to communicate by a channel (pneumaticly) or by wires (electrically) between the sensor (a pressurized spring in a manometer, òr a transducer mounted on said piston rod end òr mounted on a printboard and connected by a channel to the measuring space) through said piston rod to the reader on top of the piston rod (manometer òr an electric volt/current meter òr an electronic display, respectively). Said channel is ending at said piston rod end.
[0034] In the second aspect, the invention relates to a sensor-reader combination wherein said measuring space is communicating during a part of the operation with said device.
[0035] In case of current pumps for tyre inflation, measuring of the pressure of the tyre is done in the hose of the pump. This hose is at one end connected to the chamber through a non-return valve, and at the other end connected to a valve connector. The non-return valve limits the size of the dead space of the pump. In current low pressure pumps is no non-return valve present, but no pressure gauge is normally used.
[0036] The pressure in the hose may than be representative for the pressure in the tyre, because the tyre valve closes when there is pressure equivalency between the space in the hose, and the space of the tyre. This happens in current pumps, when the piston has reached its end point after a pump stroke, and is starting to return, thus when the overpressure in the chamber drops. The reason is, that the non-return valve between the cylinder and the hose is closing as well at this point of time.
[0037] The pressure in the space of the chamber between the piston and said non-return valve may than also be representative for the tyre pressure as well, when the piston is about to return for a new stroke. This opens a solution where the pressure may be measured at the end of the piston (rod) which is adjacent the space between the piston and a non-return valve. Thus may a sensor (measuring means) and a reading means be placed on one of the parts, e.g. on the piston (rod) in a pump for tyre inflation. The sensor may be positioned on the piston rod, and best at the end of the piston rod, in order to enable a surface for the guiding means of the piston rod. It may then be possible to have a reading on a gauge which is positioned on top of the handle of the piston rod—thus closest to the user, and readable during operation.
[0038] E.g. in case of pressure reading: this reading may be done by a pneumatic pressure gauge, where the gauge is connected by e.g. a channel within a tube to the measuring space between the piston and the valve connector òr the non-return valve. The same is valid if a temperature is being measured with a e.g. bimetal sensor. The small size of the tube and its length may give rise to dynamic friction, and may contribute to dampen the fluctuations of the pressure due to the strokes the piston is performing.
[0039] The measuring by the sensor may also be done by an electric pressure transducer, which gives through an amplifier a signal to a digital pressure gauge òr an analog pressure gauge (a volt meter or a current meter). The same is valid if a temperature is being electrically monitored.
[0040] In order to make the sensor-reader combination still more profitable, the sensor may be assembled on the printboard, while the sensor is connected to the measuring space through a channel.
[0041] In the third aspect, the invention relates to a sensor-reader combination, wherein:
[0042] the size of the parameter is measured in an enclosed measuring space.
[0043] Direct measuring in the measuring space may give fluctuations of the size of the parameter, as e.g. in a piston floor pump for tyre inflation with regard to the pressure, but also with regard to the temperature. In order to simulate the pressure in the tyre within the pump, a conditioned measuring space is necessary, and this may be done by an enclosed space.
[0044] If the value of the parameter is measured in an enclosed measuring space, it is necessary to get the fluid in, measure it and read it. Thereafter get it out again for the next measurement. E.g. in case a pressure in a tyre is measured in a floor pump, a part of the measuring space may be entered into the enclosed measuring space for enabling the measurement. This may be done by a check valve òr an electrically controlled valve. For getting the contents of the enclosed measuring space out again after the measurement, a new valve (check valve or an electrically controlled valve)—it may also be a channel, which is so tiny that dynamic friction may delay the flow out of the enclosed measuring space so much that this flow does not influence so much the measurement. This delay may be also used for the following purpose. E.g. in case of a pressure measuring in a piston-chamber combination, it may be necessary to maintain the value of the tyre pressure when the piston is returning after a pump stroke, until the value of this parameter in the space adjacent the space between the piston and a non-return valve or valve connector has reached its maximum value of the pump stroke before, by the next pump stroke. That temporary maintaining of this value may be done electronically (e.g. by the use of a condensator), by software controlling an IC, by mechatronics—the position of the piston rod in relation to the pump, controlling an IC, òr just by mechanics alone: e.g. an enclosed measuring space, which may be connected by a valve to the measuring space (between the piston and the valve connector, òr the space between the piston and the non-return valve between the combination and the hose in case of a pump for tyre inflation). The valve may preferably be identical with the valve between the combination and the hose, so that opening and closing happen simultaneously.
[0045] The enclosed measuring space may comprise a channel which is open in a very controlled way, so that the maximum value of the pressure may be temporarily maintained during the return of a piston during a pump stroke, simulating the pressure in the tyre. It may be a tiny channel, which connects the enclosed measuring space with the measuring space. During pumping may a very small part of the volume of the enclosed measuring space flow to the measuring space, and may influence the reading a bit, but only during the return path of the pump stroke, which is not very relevant for the reading. The flow through said tiny channel may be controlled by the dynamic friction of said channel, depending on its length, diameter and surface roughness, but also by a screw which has a tiny hole as well, e.g. in the case where the thread has been locked by a locking fluid .
[0046] When the requested pressure has been reached, will the movement of the piston stop, and will the pressure in the enclosed measuring space become equal with the pressure in the measuring space, which is the pressure of the tyre. Firstly when the hose has been disconnected from the tyre valve, the pressure in the measuring space decreases to atmospheric pressure (even there is a check valve in between), and will the pressure in the enclosed measuring space decrease to atmospheric pressure. It is necessary than to have a valve connector which is open, if no overpressure comes from the pressure source.
[0047] In order to allow the preservation of the pressure (or temperature), the measuring space comprises an outlet valve which may be initiated electrically, and which is closing the measuring space when the pumping is being initiated, and is opening after a certain short period when pumping has been done. This is only an example of a controlling arrangement. It may also be done manually, e.g. by pressing a button for closing the measuring space before the pump session, and opening up again, thereafter, by pressing said button again.
[0048] The best simulation may of course be done by a computer program, which is controlling the inlet and outlet valves, while the last mentioned are valves which may be controlled electrically/electronically. This may be done in much bigger and more costly installations, which may need maintenance, than that of a floor pump for inflation purposes.
[0049] In case of e.g. a container (envelope) piston type (claim 5 ) according to EP 1179140, which uses an enclosed space, the enclosed space may be preferably positioned behind the measuring space, relative to the space adjacent the space between the piston and a non-return valve, if an electric gauge is used.
[0050] In case of a pneumatic gauge (=manometer), the enclosed space may be positioned independently of the measuring space. This may be done by a separate (measuring) channel from the measuring space to the pneumatic pressure gauge.
[0051] A piston-chamber combination comprising an elongate chamber which is bounded by an inner chamber wall and comprising a piston means in said chamber to be sealingly movable relative to said chamber at least between first and second longitudinal positions of said chamber, said chamber having cross-sections of different cross-sectional areas at the first and second longitudinal positions of said chamber and at least substantially continuously differing cross-sectional areas at intermediate longitudinal positions between the first and second longitudinal positions thereof, the cross-sectional area at the first longitudinal position being larger than the cross-sectional area at the second longitudinal position,
[0000] said piston means being designed to adapt itself and said sealing means to said different cross-sectional areas of said chamber during the relative movements of said piston means from the first longitudinal position through said intermediate longitudinal positions to the second longitudinal position of said chamber, wherein the piston comprises an elastically deformable container comprising a deformable material. Said piston means may be comprising an enclosed space communicating with the deformable container (envelope), the enclosed space may have a constant volume. The container(or envelope) may be inflatable. This may be necessary when having a measuring channel or a wire loom inside the enclosed space, if the enclosed space is relatively small, like the situation is in a floor pump for tyre inflation. The circumferential size of this piston type is that of the chamber.
[0052] A piston-chamber combination comprising an elongate chamber which is bounded by an inner chamber wall and comprising a piston in said chamber to be sealingly movable relative to said chamber wall at least between a first longitudinal position and a second longitudinal position of the chamber, said chamber having cross-sections of different cross-sectional areas and different circumferential lengths at the first and second longitudinal positions, and at least substantially continuously different cross-sectional areas and circumferential lengths at intermediate longitudinal positions between the first and second longitudinal positions, the cross-sectional area and circumferential length at said second longitudinal position being smaller than the cross-sectional area and circumferential length at said first longitudinal position, said piston comprising a container which is elastically deformable thereby providing for different cross-sectional areas and circumferential lengths of the piston adapting the same to said different cross-sectional areas and different circumferential lengths of the chamber during the relative movements of the piston between the first and second longitudinal positions through said intermediate longitudinal positions of the chamber, wherein the piston is produced to have a production-size of the container in the stress-free and undeformed state thereof in which the circumferential length of the piston is approximately equivalent to the circumferential length of said chamber at said second longitudinal position, the container being expandable from its production size in a direction transversally with respect to the longitudinal direction of the chamber thereby providing for an expansion of the piston from the production size thereof during the relative movements of the piston from said second longitudinal position to said first longitudinal position. Said piston means may be comprising an enclosed space communicating with the deformable container (envelope), the enclosed space may have a constant volume.
[0053] The circumferential size of this piston type may be that of the chamber on its smallest circumferential size.
[0054] In case of e.g. a piston type according to claim 1 according to EP 1179140 is used, neither an enclosed space 42 ( FIGS. 3A-C ) may be necessary, nor the inflation nipple 43 ( FIGS. 3A-C ). The enclosed space may be used then as channel 52 ( FIGS. 3A-C ) òr as inlet channel for the measuring space. The check valve 43 maybe put in a reversed position.
[0055] The sensor-reader combination may be used in any device where a the sensor is remotely positioned in relation to the reading means, such as pumps, actuators, shock absorbers or motors.
[0056] The above combinations are preferably applicable to the applications.
[0057] Thus, the invention also relates to a pump for pumping a fluid, the pump comprising:
[0058] a combination according to any of the above aspects,
[0059] means for engaging the piston from a position outside the chamber,
[0060] a fluid entrance connected to the chamber and comprising a valve means, and
[0061] a fluid exit connected to the chamber.
[0062] A pump where the engaging means have an outer position where the piston means is at the first longitudinal position of the chamber, and an inner position where the piston means is at the second longitudinal position of the chamber.
[0063] A pump where the engaging means have an outer position where the piston means is at the second longitudinal position of the chamber, and an inner position where the piston means is at the first longitudinal position of the chamber.
[0064] The invention also relates to an actuator comprising:
[0065] a combination according to any of the combination aspects, means for engaging the piston from a position outside the chamber,
[0066] means for introducing fluid into the chamber in order to displace the piston between the first and the second longitudinal positions.
[0067] The actuator may comprise a fluid entrance connected to the chamber and comprising a valve means.
[0068] Also, a fluid exit connected to the chamber and comprising a valve means may be provided.
[0069] Additionally, the actuator may comprise means for biasing the piston toward the first or second longitudinal position.
[0070] And, an actuator where the introducing means may comprise means for introducing pressurised fluid into the chamber.
[0071] An actuator where the introducing means may be adapted to introduce a combustible fluid, such as gasoline or diesel, into the chamber, and wherein the actuator further comprises means for combusting the combustible fluid.
[0072] An actuator where the introducing means may be adapted to introduce an expandable fluid to the chamber, and wherein the actuator further comprises means for expand the expandable fluid.
[0073] An actuator further comprising a crank adapted to translate the translation of the piston means into a rotation of the crank.
[0074] Finally, the invention relates also to a shock absorber comprising:
[0075] a combination according to any of the combination aspects,
[0076] means for engaging the piston from a position outside the chamber, wherein the engaging means have an outer position where the piston is in its first longitudinal position, and an inner position where the piston is in its second longitudinal position.
[0077] The absorber may further comprise a fluid entrance connected to the chamber and comprising a valve means.
[0078] Also, the absorber may comprise a fluid exit connected to the chamber and comprising a valve means.
[0079] A shock absorber wherein the chamber and the piston means form an at least substantially sealed cavity comprising a fluid, the fluid being compressed when the piston means moves from the first to the second longitudinal positions of the chamber.
[0080] A shock absorber may further comprising means for biasing the piston means toward the first longitudinal position of the chamber.
[0081] Piston chamber combination comprising a piston in a chamber with a fluid exit and a sensor-reader combination with a sensor for measuring a parameter wherein the sensor is arranged to measure the parameter in a measuring space before the fluid exit of the chamber.
[0082] Piston chamber combination where the fluid exit is provided with a check valve.
[0083] Piston chamber combination where the sensor is located in an enclosed measuring space in the piston.
[0084] Piston chamber combination comprising a check valve between the enclosed measuring space and the chamber.
[0085] Piston chamber combination where the piston comprises a hollow piston rod enclosing the enclosed measuring space.
[0086] Piston chamber wherein a channel with a very small diameter connects the enclosed measurement space to the chamber.
[0087] Piston-chamber combination comprising a screw for adjusting flow through the channel.
[0088] Piston-chamber combination where the screw has a tapered head matching a correspondingly widened end of the channel and wherein a channel runs through the head from the tapered side to an opposite side of the head.
[0089] Piston-chamber combination wherein the enclosed measuring space comprises an inlet and an outlet valve initiated electrically under the control of a computer.
[0090] Piston-chamber combination wherein the sensor-reader combination comprises pressure sensor, selected from the group of pneumatic or electric pressure gauges, analogue or digital volt or current meters in combination with an electric or electronic sensor, and transducers connected with mechanical conducting devices, such as wires, to an analogue or digital gauge.
[0091] Piston-chamber combination wherein the sensor-reader combination comprises a temperature sensor.
[0092] Piston-chamber combination wherein the piston-chamber combination is a pump comprising means for engaging the piston from a position outside the chamber and a fluid entrance connected to the chamber, the fluid entrance comprising a valve.
[0093] Piston chamber wherein the piston comprises a piston rod with a handle on top of the piston rod, wherein the handle is provided with an electric or pneumatic pressure gauge.
[0094] Method of measuring pressure in a tyre during pumping by using a pump with a piston in a chamber and with a fluid exit connected to a hose and a check valve between the fluid exit and the hose wherein the tyre pressure is measured indirectly by measuring the pressure in the chamber before the check valve, at least during a pump stroke when the piston is pushed into the chamber.
[0095] Method wherein the pressure is measured in an enclosed measuring space in the piston and wherein the enclosed measuring space is connected to the chamber with an opening provided with a check valve which provides an open connection between the enclosed measuring space and the chamber when the piston is moved into the chamber during a pump stroke and which closes off said opening of the enclosed measuring space during a return stroke.
[0096] A sensor-reader combination for measuring the size of a parameter of a device, the device and reader are positioned at a different physical position from each other, the measuring is done in a measuring space representing said device regarding to the to be measured size of said parameter, said space is positioned nearby said reader.
[0097] The measuring space is communicating during a part of the operation with said device.
[0098] The sensor and said reader are part of the same assembly.
[0099] The reading is done by a pneumatic pressure gauge, which is connected to said space.
[0100] The reading of a parameter is done by an analog volt meter or current meter, in combination with an electric or electronic sensor.
[0101] The reading of a parameter is done by a digital volt meter or current meter, in combination with an electric or electronic sensor.
[0102] Said sensor is connected to the measuring space through a channel.
[0103] The parameter is measured inside an enclosed measuring space.
[0104] The enclosed measuring space is comprising a check inlet valve, connecting said enclosed measuring space with said measuring space.
[0105] Said check inlet valve of the enclosed measuring space is identical with the outlet check valve of the measuring space.
[0106] The enclosed measuring space may comprising a check outlet valve, connecting said enclosed measuring space with said measuring space.
[0107] Said enclosed measuring space may comprising a channel connecting said enclosed measuring space with said measuring space.
[0108] The channel may have a very small diameter.
[0109] The channel may comprising a screw.
[0110] The screw may comprising a small channel.
[0111] The channel may have a widened end towards said screw.
[0112] The screw may have a tapered end towards said channel.
[0113] The measuring may be done by a transducer communicating with the measuring space, which is connected with mechanical conducting devices, such as wires, to an analog electrical and/or digital gauge.
[0114] The measuring may be done by connecting the measuring space with the inlet of the pneumatic gauge (manometer) by a measuring channel.
[0115] The measuring may be done by connecting the transducer to the enclosed measuring space, the transducer is connected with mechanical conducting devices, such as wires, to an analog electrical and/or digital gauge.
[0116] The enclosed measuring space may comprise an inlet and an outlet valve which are initiated electrically, and which are opening and closing the measuring space, and are controlled by a computer.
BRIEF DESCRIPTION OF THE DRAWINGS
[0117] In the following, preferred embodiments of the invention will be described with reference to the drawings wherein:
[0118] FIG. 0 shows left the combination of a pneumatic pressure/temperature gauge and a channel within the piston rod, where the measuring point is at the end of the channel, communicating with in the measuring space—the lower part of the drawing has been scaled up 2:1. A scaled up detail is also shown. shows right the combination of a pneumatic pressure/temperature gauge and a wire loom within the piston rod, where the measuring point is at the transducer at the end of the piston rod, the transducer communicating with the measuring space—the lower part of the drawing has been scaled up 2:1. A scaled up detail is also shown.
[0119] FIG. 1A shows the top of the piston rod of a floor pump with an inflatable piston, with an electrical gauge mounted on top of the handle, and the bottom of the piston rod with the transducer in the enclosed measuring space.
[0120] FIG. 1B shows the bottom part of FIG. 1A on a scale 2:1.
[0121] FIG. 2A shows the top of the piston rod of a floor pump with an inflatable piston and a pneumatic gauge mounted on top of the handle, an in-between channel which ends in the enclosed measuring space.
[0122] FIG. 2B shows the bottom part of FIG. 2A on a scale 2:1
[0123] FIG. 3A shows the top of the piston rod of a floor pump with an inflatable piston and a pneumatic gauge mounted on top of the handle, and the bottom of the piston rod mounted in an enclosed measuring space.
[0124] FIG. 3B shows the bottom part of FIG. 3A on a scale 2.5:1.
[0125] FIG. 3C shows the outlet channel of the enclosed measuring space of FIG. 3B on a scale 6:1
[0126] FIG. 3D shows a detail of the outlet channel of FIG. 3C on a scale of 5:1
[0127] FIG. 4 shows the bottom of an advanced floor pump for e.g. tyre inflation.
[0128] FIG. 5A shows a section of a gauge housing, mounted on a handle, where the enclosed space is closed by an O-ring.
[0129] FIG. 5B shows a detail of the O-ring assembly.
[0130] FIG. 6A shows a section of a gauge housing, mounted on the handle, where the enclosed space is closed by a sealing near the gauge.
[0131] FIG. 6B shows a detail of FIG. 6A
DESCRIPTION OF PREFERRED EMBODIMENTS
[0132] FIG. 0 shows left a reading point 100 of the measured value of a pneumatic pressure gauge housing 101 . Within said gauge is a mechanical manometer 102 (not shown). Said gauge housing 101 is mounted on top of a piston rod 103 . The piston rod 103 is hollow with channel 104 , which is mounting a tube with a measuring channel 107 within tube 113 , which makes communication possible between the pneumatic pressure gauge 102 and the entrance 108 of channel 108 at the bottom of the tube 107 . The measuring point 108 in the housing 101 , at the manometer entrance. The measuring room 111 . The handle 2 . The suspension 109 . The spring washer 6 . The bolt 7 . The suspension 110 of the channel 107 in the top of the piston rod 103 . The suspension 112 of the piston. The tube 113 .
[0133] FIG. 0 right shows a reading point 120 of the measured value of an electric pressure/temperature gauge housing 121 . Said housing 121 comprises an analog/digital electric gauge 122 (not shown). Said gauge 122 is mounted on top of a piston rod 123 . The piston rod 123 is hollow with channel 124 , in which a wire loom 125 is mounted. Said wire loom 125 is connected with a transducer 15 , which is mounted on a platform 16 , which makes communication possible between said gauge 121 and the measuring point 128 at the bottom of the piston rod 123 . The measuring space 130 . The handle 2 . The spring washer 6 . The bolt 7 . The suspension 129 of the channel 124 in the top of the piston rod 123 . The transition 22 . The suspension 131 of the piston.
[0134] FIG. 1A shows the top of a piston rod 1 with a handle 2 and an electric (pressure/temperature) gauge 3 . The gauge 3 is mounted on the handle 2 . The piston rod 1 has a upper space 4 . 1 which is serving as an enclosed space 8 for the inflatable piston, of which only the bottom part of its suspension 5 is shown. The spring washer 6 . The top of a bolt 7 is shown with the bottom space 4 . 2 of the enclosed space 8 , which is directly connected to the upper space 4 . 1 . In the top of bolt 10 is a valve body 9 mounted, and fastened by a nut 10 . The core pin 11 is shown in a closed position against the stem 12 in the valve body 9 . This valve 11 is serving to keep the enclosed space 8 on the necessary pressure. On the valve body 9 is the housing 13 of the enclosed measuring space 14 mounted. The (pressure) transducer 15 is shown, mounted on a platform 16 . This platform 16 allows a gentle activation of the transducer 15 , as the opening is between the wall 17 of the enclosed measuring space 14 and the transducer 15 . The valve 18 which connects the measuring space 14 with the measuring space 19 adjacent the outlet of the combination. The top of the hollow piston rod 1 is closed by a filler 20 , which is tightly closing the necessary wire loom 21 from the pressure transducer 15 to the gauge 3 . The rest of the wiring is not shown. The transition 22 prohibits the filler 20 to be burst out of the piston rod. The outlet valve of the enclosed measuring space 14 is not shown.
[0135] FIG. 1B shows the bottom part of FIG. 1A on a scale 2:1.
[0136] FIG. 2A shows the top of a piston rod 31 with a handle 2 and a pneumatic pressure gauge 33 . Said gauge 33 is mounted on the handle 2 . The piston rod 31 has a space 34 . 1 which is serving as an upper part of the enclosed space 32 for an inflatable piston, of which only the bottom part of its suspension 5 is shown. The spring washer 6 . The top of a bold 7 is shown with part 34 . 2 which is serving as the lower part of the enclosed space 32 , which is directly connected to the space 34 . 1 . In the top of bolt 7 is a body 39 mounted, and fastened by a nut 10 . On the body 39 is the housing 13 of the enclosed measuring space 14 mounted. The end 35 of the measuring channel 36 within tube 36 . 2 is shown which is tightly mounted in the top 37 of the piston rod 31 , and connected to the pneumatic pressure gauge. The valve 18 which connects the enclosed measuring space 14 with the measuring space 38 adjacent the outlet of the combination.
[0137] The outlet valve of the measuring space 32 is not shown.
[0138] FIG. 2B shows the bottom part of FIG. 2A on a scale 2:1
[0139] FIG. 3A shows the top of a piston rod 40 with a handle 2 and an electric pressure gauge 41 . The gauge 41 is mounted on the handle 2 . The piston rod 40 has an enclosed space 42 for keeping the piston pressurized. Said space can communicate with the piston (see e.g. WO2000/070227 or WO2002/077457 or WO2004031583). Pressurization to a desired level of the piston is done by an external pressure source (not shown) through an inflation nipple 43 , which has an build in check valve 44 . The exit hole 66 of the check valve 44 . The nipple 43 is positioned at the bottom of the piston rod 40 , and build in the head 45 of the bolt 46 . The enclosed measuring space 47 is build in a separate housing 48 in the head 45 of bolt 46 . Said enclosed measuring space is connected through a check valve 49 with the measuring space 50 . Said check valve 49 is built in a separate housing 51 . The (vertical) channel 52 is connected to the enclosed measuring space 47 within the tube 36 . 2 by means of a (horizontal) channel 53 , and is sealed by a sealing means 54 , e.g. an O-ring, in the enclosed measuring space 47 . The cap 55 , which is a part of the O-ring gland. Either is the transducer 15 mounted on the bottom 56 of the tube 57 , where the channel 52 is filled in with a wire loom 57 to the electric pressure gauge 41 , òr is the channel 52 open, and on top 58 of the channel 52 , within the electric pressure gauge 41 , is the transducer 15 mounted. FIG. 3B shows the bottom part of FIG. 3B on a scale 6:1.
[0140] FIG. 3C shows a part of the enclosed measuring space ( 47 , 43 , 52 ) on a scale of 6:1 in relation to FIG. 3B . The outlet channel 59 in the head 45 of the bolt 46 , with an screw 60 , which sets the flow through the tiny channel 61 in the housing 48 of the enclosed measuring space 47 . The channel 61 has a widened end 62 , which suits the tapered end 63 of the screw 57 . In the screw 60 is a channel 64 that connects the channel 61 with the outlet channel 59 .
[0141] FIG. 3D shows a detail of FIG. 3C on a scale 5:1. The very small space 65 between the widened end 62 and the tapered end 63 . It sets the flow from the channel 53 .
[0142] FIG. 4 shows the bottom part 70 of an advanced floor pump for e.g. tyre inflation. The flexible manchet 71 keeps the cone formed tube 72 in place. The inflatable piston 73 . On the bottom of the piston rod 74 is the embodiment of FIGS. 3A-D mounted, without crew 57 arrangement (may only be necessary for prototypes). The enclosed space 42 . The tube 36 . 2 . The inlet check valve 75 The outlet check valve 76 . The hose 77 . The measuring space 78 , 79 (inside the hose). The valve connector 80 (not shown). The space inside the valve connector 81 is also part of the measuring space (not shown). The central axis 82 of the pump.
[0143] FIG. 5A shows an assembly of a gauge housing—top part 83 and bottom part 84 , assembled with scrues (not shown)—on a handle 85 of a floor pump of FIG. 4 . The piston rod 74 , which is mounted on a nipple 86 , on which the handle 85 has been mounted. This is done by a spring washer 87 and a spacer 88 . A nut 89 which is comprising a washer 90 is keeping the handle 85 in place. The piston rod 74 is comprising the enclosed space 42 , which is permanently separated from space 91 by an O-ring 95 . The O-ring 95 is mounted in the nipple 86 and is tightening the tube 36 . 2 , which is comprising the enclosed measuring space 52 , and thereby has the enclosed space 42 a constant volume. In order to be able to mount the pneumatic pressure gauge 92 on the tube 36 . 2 , the tube is comprising an S-bend 94 , and has on its top a nipple 93 —the nipple 93 is sealed (not shown) to the gauge housing. The pneumatic pressure gauge has been mounted in the top part 83 of the pneumatic pressure gauge housing by e.g. scrues (not shown). The centre axis 82 .
[0144] FIG. 5B shows a detail of the assembly of the O-ring 95 . The gland 96 wherein the O-ring 95 has been mounted, sealing the tube 36 . 2 . The space 91 . The enclosed measuring space 52 . The centre axis 82 .
[0145] FIG. 6A shows an assembly of a gauge housing—top part 133 and bottom part 134 , assembled with scrues (not shown)—on a handle 85 of a floor pump of FIG. 4 . The piston rod 74 , which is mounted on a nipple 136 , on which the handle 85 has been mounted. This is done by a spring washer 87 and a spacer 88 . A nut 89 which is comprising a washer 90 is keeping the handle 85 in place. The nipple 93 —the nipple 93 is sealed (not shown) to the gauge housing. The piston rod 74 is comprising the enclosed space 42 . The sealing 135 is mounted between the electric pressure gauge 132 and the top part 133 of the gauge housing, sealing the enclosed space 42 and thereby has the enclosed space 42 a constant volume. The electric/electronic pressure gauge has been mounted in the top part 83 of the gauge housing by e.g. scrues (not shown). The sensor 137 (not shown) at the top end of the enclosed measuring space 52 , within the top part 133 of the gauge housing, which is communicating with the enclosed measuring space 52 (not shown). The tube 138 comprising the enclosed measuring space 52 . The centre axis 82 .
[0146] FIG. 6B shows a detail of the enclosed space 42 and the enclosed measuring space 52 . The tube 138 . The centre axis 82 . The tube 138 .
[0000]
Piston Chamber Combination reference numbers
1
piston rod
FIG. 1A
2
handle
FIG. 1A/2A/0
3
gauge
FIG. 1A
4.1
upper space (of the
FIG. 1A
enclosed space 8)
4.2
bottom space (of the
FIG. 1A
enclosed space 8)
5
suspension (of the
FIG. 1A/1B/2A/2B
inflatable piston)
6
spring washer
FIG. 1A/1B/2A/2B/0
7
bolt
FIG. 1A/1B/2A/2B/0
8
enclosed space (for
FIG. 1A/1B/2A
the inflatable piston)
9
valve body
FIG. 1A/1B
10
nut
FIG. 1A/1B/2A/2B
11
core pin
FIG. 1A/1B
12
stem
FIG. 1A/1B
13
housing
FIG. 1A/1B/2A/2B
14
enclosed measuring
FIG. 1A/1B/2A/2B
space
15
transducer
FIG. 1A/1B/0R
16
platform
FIG. 1A/1B/0R
17
wall (of the
FIG. 1A/1B/2A/2B
measuring space)
18
valve
FIG. 1A/1B/2A/2B
19
measuring space
FIG. 1A
20
filler
FIG. 1A
21
wiring loom
FIG. 1A
22
transition
FIG. 1A/0R
31
piston rod
FIG. 2A
33
gauge
FIG. 2A
34.1
space (upper part of the
FIG. 2A
enclosed space 32)
34.2
space (lower part of the
FIG. 2A/2B
enclosed space 32)
35
end
FIG. 2A/2B
36.1
measuring channel
FIG. 2A/2B
36.2
tube
FIG. 2A/3B/4/5A/5B
37
top
FIG. 2A
38
measuring space
FIG. 2A
40
piston rod
FIG. 3A/3B
41
electric pressure gauge
FIG. 3A/3B
42
enclosed space
FIG. 3A/3B/4/5A/5B/6A/6B
43
inflation nipple
FIG. 3A/3B
44
check valve
FIG. 3A/3B
45
head
FIG. 3A/3B
46
bolt
FIG. 3A/3B
47
enclosed measuring space
FIG. 3A/3B
48
housing
FIG. 3A/3B
49
check valve
FIG. 3A/3B
50
measuring space
FIG. 3A/3B
51
housing
FIG. 3A/3B
52
channel
FIG. 3A/3B/5B/6B
53
channel
FIG. 3A/3B
54
sealing means
FIG. 3A/3B
55
cap
FIG. 3A/3B
56
bottom
FIG. 3A/3B
57
wire loom
FIG. 3A/3B
58
top
FIG. 3A/3B
59
outlet channel
FIG. 3C
60
screw
FIG. 3C
61
channel
FIG. 3C
62
widened end
FIG. 3C
63
tapered end
FIG. 3C
64
channel
FIG. 3C
65
space
FIG. 3D
66
outlet hole
FIG. 3A/3B
70
bottom part
FIG. 4
71
manchet
FIG. 4
72
tube
FIG. 4
73
piston
FIG. 4
74
piston rod
FIG. 4/5A/6A
75
inlet check valve
FIG. 4
76
outlet check valve
FIG. 4
77
hose
FIG. 4
78
measuring space
FIG. 4
79
measuring space
FIG. 4
80
valve connector
FIG. 4
81
space
FIG. 4
82
central axis
FIG. 4/5A/5B/6A/6B
83
top part (of gauge
FIG. 5A
assembly)
84
bottom part (of gauge
FIG. 5A
assembly)
85
handle
FIG. 5A
86
nipple
FIG. 5A/5B
87
spring washer
FIG. 5A/6A
88
spacer
FIG. 5A/6A
89
nut
FIG. 5A/6A
90
washer
FIG. 5A/6A
91
space
FIG. 5A/5B
92
pneumatic pressure
FIG. 5A
gauge
93
nipple
FIG. 5A/6A
94
S-bend
FIG. 5A
95
O-ring
FIG. 5A/5B
96
gland
FIG. 5B
100
reading point
FIG. 0L
101
housing
FIG. 0L
102
manometer
FIG. 0L
103
piston rod
FIG. 0L
104
channel
FIG. 0L
105
top
FIG. 0L
106
bottom
FIG. 0L
107
measuring channel
FIG. 0L
108
measuring point
FIG. 0L
109
suspension
FIG. 0L
110
suspension
FIG. 0L
111
measuring space
FIG. 0L
112
suspension
FIG. 0L
113
tube
FIG. 0L
120
reading point
FIG. 0R
121
housing
FIG. 0R
122
gauge
FIG. 0R
123
piston rod
FIG. 0R
124
channel
FIG. 0R
125
wire loom
FIG. 0R
126
top
FIG. 0R
127
bottom
FIG. 0R
128
measuring point
FIG. 0R
129
suspension
FIG. 0R
130
measuring space
FIG. 0R
133
top part (of gauge
FIG. 6A
assembly)
134
bottom part (of gauge
FIG. 6A
assembly)
135
seal
FIG. 6A
136
nipple
FIG. 6A/6B
137
sensor
FIG. 6A
138
tube
FIG. 6A/6B
|
A piston chamber combination comprising a container type piston, communicating with an enclosed space, said enclosed space having an at least substantially constant volume.
| 5
|
PRIORITY CLAIM
[0001] This application claims the benefit of U.S. Provisional Application No. 60/330,223 filed Oct. 16, 2001 entitled “Stackable Plastic Containers,” the entire contents of which is hereby expressly incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates generally to plastic containers for holding, organizing and securing optical disks.
[0004] 2. Description of the Related Art
[0005] Stackable containers have long been used in the prior art. Typically, containers with stackable properties use threaded male/female sections. The top female section is constructed with internal threads. This section screws into the male bottom section. The male bottom section is constructed with an additional attached molded female section which is also a container. Several such containers can be combined to form a stack of containers. These types of threaded containers are generally more expensive and much slower to manufacture than “snap-together” containers. Because threaded containers also allow dirt and debris in the threads, threaded containers often have difficulty closing properly. Further, threaded containers are frequently much taller in height due to the minimum amount of threads needed to make the container screw together. Indeed, most threaded containers are at least about 0.375 inches high. Threaded containers also require stiffer plastic and thicker side walls because of the threaded side wall pressures. Soft plastics like polypropylene are typically not suitable for threaded containers because the threads may strip if over-tightened.
[0006] Other containers that use stacking properties are found in the houseware industry. A houseware stackable containers have covers with ribs that match the bottoms of matching containers. The raised rib around the perimeter of a container's lid is larger than the bottom of the container to be stacked on the cover. The bottom nests into the lid. This container relies on gravity and internal weight to stay together. If the containers are dropped, the stack of containers simply falls apart.
[0007] Other containers in the prior art use a “friction fit” lid and bottom. This type of container has a lid which has a raised center section approximately 0.050 inches per side smaller than the outside diameter of the container. This area is raised 0.030 inches to 0.050 inches from the rest of the lid. The bottom of the container which forms the container has a ring a few thousands smaller than the top raised center section. The bottom will fit so that the friction that is created will hold the next container set next to the previous container set. Typically, a container set is made of one top and one bottom. A stack is made up of two or more container sets stacked on each other. This method of stacking containers is expensive because of the extra parts required to manufacture the container.
SUMMARY OF THE INVENTION
[0008] In one aspect, the current invention provides an improved plastic container for holding, organizing and/or securing optical disks, or like contents, that is easy and inexpensive to manufacture and which can be used as a single disk holder or in stackable format, in which an internal cavity is formed by a male/female (top and bottom) container. Preferably, each container is only as thick as the required thickness of the item to be enclosed, such as, for example, an optical disk. The containers may be secured by closing, locking, and/or sealing mechanisms. In a preferred embodiment, the material used for the containers is plastic, preferably polypropylene. The plastic may be tinted or colored with translucent or opaque color additives. In various aspects, the invention has a tab molded onto the side wall to allow easy identification and retrieval of the desired container. The tab may be labeled with a number or a letter which corresponds to a label table on the lid. In several embodiments, the current invention has an opening function which allows the user to pry apart two tabs with both thumbs. In one aspect of the invention, the inside center of the female side has a raised positioning ring which holds and centers the contents in the cavity formed by a male/female junction. By holding the contents in position, this ring prevents the contents from rubbing on the inside of the container
[0009] Various embodiments of the present invention provide stackable plastic containers which can be used for holding, organizing and/or securing optical disks. Optical disks, as used herein, shall mean digital and electronic data storage units, including, but not limited to CDs, DVDs, mini CDs, mini DVDs, floppy discs, computer, audio, video and digital camera discs, and the like. Methods of manufacturing and constructing these containers are also provided. Single non-stackable sealed plastic containers may also be made according to various aspects of the current invention. Some embodiments include ears designed to fit in different notebooks, three-ring binders, or day timers.
[0010] Several embodiments of the current invention are particularly advantageous because they offer light weight non-toxic containers which can be effectively be stacked upon one another and are capable of being latched or closed, thus creating a seal which keeps foreign material from entering the container. Thus, in a preferred embodiment, the current invention is particularly advantageous because it prevents dirt or foreign material from entering the container. A single non-stackable moisture/dirt sealed container can also be made using portions of the same design criteria, i.e. top female, bottom male sections.
[0011] In one aspect of the present invention, an apparatus for stackably storing items, including a first container, a surface included in the first container, the surface substantially planar, the surface having a first side and a second side, the surface having a shape suited to cover at least one item, a first member included in the first container, the first member raised from the first side of the surface, the first member having a first member perimeter, a second member included in the first container, the second member raised from the second side of the surface, the second member having a second member perimeter slightly larger than the first member perimeter, the second member suited to releaseably couple the first container to a first member of a substantially identical second container, wherein the first member forms a substantially complete perimeter around the first side of the surface, and, wherein the second member forms a substantially complete perimeter around the second side of the surface.
[0012] In one aspect of the invention, the first member forms a substantially complete ring around the first side of the surface. In another aspect of the invention, the second member forms a substantially complete ring around the second side of the surface. In another aspect of the invention, the second member includes a bead along the inside perimeter, the bead locking the first member of the second container to the second member of the first container and holding the first container and second container together. In another aspect of the invention, the bead is about 0.020 inches in radius.
[0013] Yet another aspect of the invention includes a tab extending from the surface of the first container, the tab suited to releaseably decouple the first container from the second container. In another aspect of the invention, includes a tang extending from the surface of the first container, the tang suited to prevent the tab of the first container from sliding past a tab of the second container. In another aspect of the invention, the first container is formed from plastic. In another aspect of the invention, the first container is formed from polypropylene. In another aspect of the invention, the first container is formed from clear plastic. In another aspect of the invention, the first container is formed from plastic opaque to visible light. In another aspect of the invention, the first container is formed from plastic opaque to ultraviolet light. In another aspect of the invention, the first container is formed from translucent plastic. In another aspect of the invention, the item stored is at least one of a compact disc or digital versatile disc or other optical disk. In another aspect of the invention, including a third container, the third container including a surface and first member substantially identical to the first container. In another aspect of the invention, a label attached to the second side of the third container. In another aspect of the invention, a tab extending from the surface of the first container, the tab suited to releaseably decouple the first container from the second container. In another aspect of the invention, a tang extending from the surface of the first container, the tang suited to prevent the tab of the first container from sliding past a tab of the second container. In another aspect of the invention, a fourth container, the fourth container including a surface and a second member substantially identical to the first container. In another aspect of the invention, a label attached to the first side of the fourth container. In another aspect of the invention, a tab extending from the surface of the first container, the tab suited to releaseably decouple the first container from the second container. In another aspect of the invention, a tang extending from the surface of the first container, the tang suited to prevent the tab of the first container from sliding past a tab of the second container. In another aspect of the invention, the height of the first member is slightly higher than the height of the item to be held by the container. In another aspect of the invention, the height of the first member is between about 0.010 inches and 0.125 inches. In another aspect of the invention, the surface of the first member is round. In another aspect of the invention, the width of the surface of the first container has an area slightly larger than the item to be held by the container. In another aspect of the invention, the width of the surface of the first container is between about 0.5 inches and 12 inches. In another aspect of the invention, the width of the surface of the first container is about 6 inches. In another aspect of the invention, the surface of the first member is rectangular.
[0014] Another aspect of the present invention includes a positioning ring, the positioning ring raised on the center of the second side of the surface of the first container, the positioning ring formed to hold the contents in the cavity formed by the second member of the first container and the first surface of the second container. In another aspect of the invention, a second positioning ring is included in the center of the second side of the second container. In another aspect of the invention, the positioning ring has a diameter ranging from about 0.5 inches to 0.6 inches. In another aspect of the invention, the positioning ring is raised from the second side of the surface of the first container to a height of about 0.010 inches to 0.300 inches. In another aspect of the invention, the substantially planar surface includes a slight curvature to protect the item from contact with the substantially planar surface. In another aspect of the invention, the substantially planar surface includes a slight curvature to protect the item from contact with the substantially planar surface. In another aspect of the invention, the first member is tapered such that a portion of the first member in contact with the substantially planar surface is thinner than a portion of the first member furthest from the planar surface. In another aspect of the invention, an outer edge of the first member forms an angle with the planar surface that is less than 90 degrees. In another aspect of the invention, the first member is substantially normal to the planar surface. In another aspect of the invention, the second member is substantially normal to the planar surface.
[0015] Another aspect of the present invention includes an apparatus for stackably storing items, comprising a first container, the container including a generally planar surface having a first side and a second side, a first member forming a generally complete perimeter generally normal to and around the first side of the generally planar surface, a second member forming a generally complete perimeter generally normal to and around the second side of the generally planar surface, the second member including a bead, and, a releasable coupling between the first container and a substantially identical second container, the coupling formed by the second member of the first container and the first member of the second container. Several embodiments of the invention further include a positioning ring, the positioning ring raised on the center of the second side of the surface of the first container, the positioning ring formed to hold the contents in the cavity formed by the second member of the first container and the first surface of the second container.
[0016] Another aspect of the invention includes an apparatus for stackably storing items, including a container means, the container means including a substantially planar surface with a first and second side, releaseable coupling means, the releaseable coupling means including a first member attached to the first side of the substantially planar surface and a second member attached to the second side of the substantially planar surface, and, an item fixing means, the item fixing means including a positioning ring to releaseably couple the item to the container. In another aspect of the invention, the first member forms a substantially complete perimeter around the substantially planar surface. In another aspect of the invention, the second member forms a substantially complete perimeter around the substantially planar surface. In another aspect of the invention, the second member includes bead means to seal the releasable coupling between a first container and a second container.
[0017] Yet another aspect of the invention includes an apparatus for storing items, where a first piece and a second piece where said first and second pieces are substantially planar and said first and second pieces each have a first and second surface, the first piece having at least one wall at or near its perimeter extending away from at least one of said surfaces, the second piece having at least one wall at or near its perimeter extending away from at least one of said surfaces, the at least one wall of the first piece and the at least one wall of the second piece are removeably joinable such that said first and second pieces and said walls form a container. In another aspect of the present invention the first and second pieces are attached by a hinge.
[0018] In another aspect of the present invention, the first piece forms a top of the container and the second piece forms a bottom of the container and the top piece includes at least one positioning member for orienting an item to be contained in the container. In another aspect of the present invention the bottom contains at least one positioning member for orienting an item to be contained in the container. In another aspect of the present invention, the bottom contains at least one positioning member for orienting an item to be contained in the container. In another aspect of the present invention, the container is substantially round, said first piece forms a bottom and said second piece forms a top, said bottom piece having a center positioning member and a perimeter positioning member. In another aspect of the present invention, the top piece has a center positioning member. In another aspect of the present invention, the top piece has a perimeter positioning member. In another aspect of the present invention, the top piece has a perimeter positioning member.
[0019] Another aspect of the present invention includes an apparatus for storing items, including a substantially planar and substantially round first piece with a diameter of approximately between about 3.0 inches to about 5.5 inches, a first wall extending laterally from said first piece a distance of approximately between about 0.06 inches to 0.12 inches, a second piece that is substantially planar and substantially round with a diameter of approximately between 3.0 inches to about 5.5 inches, a second wall extending laterally from said second piece a distance of approximately about 0.06 inches to about 0.12 inches, with a positioning ring in the center of each of the first and second piece, where said positioning rings are raised from a surface of each of said pieces approximately between about 0.01 inches to 0.12 inches, said positioning rings having diameters of approximately about 0.20 inch to about 0.62 inches, where said first piece has a stabilizing ring raised from the surface with a diameter approximately between about 2.5 inches and about 5 inches. In another aspect of the present invention the second piece has a stabilizing ring on the surface with a diameter approximately between about 2.5 inches and about 5 inches. In another aspect of the present invention, the container is designed to hold an optical disk and to prevent dust, dirt, moisture, and other debris from reaching said disk.
[0020] In other embodiments, an apparatus is disclosed for individually storing for easy retrieval a plurality of items in respective individual indexed nestable containers which are each substantially sealed against intrusion of foreign material into the container, the containers adapted to form a generally cylindrical stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a substantially planar surface having a first side and a second side, a first substantially circular peripheral enclosure upstanding from the first side, a second substantially circular peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members to abut against the second peripheral enclosure of the mating container member, whereby second substantially circular peripheral enclosures and first substantially circular peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable containers substantially sealed against intrusion of foreign matter, and outwardly extending indexing members on the mating container members adapted to engage the indexing member of an adjacent mating container members to enable indexing of multiple stacked container members.
[0021] Also disclosed is an apparatus for individually storing for easy retrieval a plurality of items in respective individual indexed nestable containers which are each substantially sealed against intrusion of foreign material into the container, the containers adapted to form a stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a substantially planar surface having a first side and a second side, a first substantially circular peripheral enclosure upstanding from the first side, a second substantially circular peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members to abut against the second peripheral enclosure of the mating container member, whereby second substantially circular peripheral enclosures and first substantially circular peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable containers substantially sealed against intrusion of foreign matter, and outwardly extending indexing members on the mating container members adapted to engage the indexing member of an adjacent mating container members to enable indexing of multiple stacked container members.
[0022] Also disclosed is an apparatus for individually storing for easy retrieval a plurality of items in respective individual nestable containers which are each substantially sealed against intrusion of foreign material into the container, the containers adapted to form a stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a substantially planar surface having a first side and a second side, a first substantially circular peripheral enclosure upstanding from the first side, a second substantially circular peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members, whereby second substantially circular peripheral enclosures and first substantially circular peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable containers substantially sealed against intrusion of foreign matter.
[0023] Also disclosed is an apparatus for individually storing for easy retrieval a plurality of items in respective individual nestable containers which are each substantially sealed against intrusion of foreign material into the container, the containers adapted to form a stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a substantially planar surface having a first side and a second side, a first peripheral enclosure upstanding from the first side, a second peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members, whereby second peripheral enclosures and first peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable containers substantially sealed against intrusion of foreign matter.
[0024] Also disclosed is an apparatus for individually storing for easy retrieval a plurality of items in respective individual indexed nestable containers which are each substantially sealed against intrusion of foreign material into the container, the containers adapted to form a stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a surface having a first side and a second side, a first substantially circular peripheral enclosure upstanding from the first side, a second substantially circular peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members, whereby second substantially circular peripheral enclosures and first substantially circular peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable containers substantially sealed against intrusion of foreign matter; outwardly extending indexing members on the mating container members adapted to engage the indexing member of an adjacent mating container members to enable indexing of multiple stacked container members; a positioning member on at least the first or second side to hold in position an optical disk within the formed nestable containers.
[0025] Also disclosed is an apparatus for individually storing for easy retrieval a plurality of items in respective individual indexed nestable containers, the containers adapted to form a stack which resists coming apart unless and until entry of one or more containers is desired, the apparatus having a plurality of mating container members, each of the members having a surface having a first side and a second side, a first substantially circular peripheral enclosure upstanding from the first side, a second substantially circular peripheral enclosure upstanding from the second side, the inner perimeter of the second peripheral enclosure being sufficiently larger than the outer perimeter of the first peripheral enclosure so that the second peripheral enclosure fits over and grips the first peripheral enclosure of another one of the mating container members, whereby second substantially circular peripheral enclosures and first substantially circular peripheral enclosures of adjacent container members are adapted to respectively combine to form a stack of plural nestable, outwardly extending indexing members on the mating container members adapted to engage the indexing member of an adjacent mating container members to enable indexing of multiple stacked container members; a positioning member on at least the first or second side to hold in position an optical disk within the nestable containers, formed by adjacent mating container members.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] [0026]FIG. 1 depicts one embodiment of a cross section of a container stack, including a top lid, two center containers, and a bottom container.
[0027] [0027]FIG. 2 shows one embodiment of the top lid of the container stack, where typically only one top lid is used per stack.
[0028] [0028]FIG. 3 depicts one embodiment of a center container, where the center container forms the container section on top and the lid of the next container on the bottom.
[0029] [0029]FIG. 4 illustrates one embodiment of the bottom container, which forms the base of the stack of containers.
[0030] [0030]FIG. 5 is a top view of a top container.
[0031] [0031]FIG. 6 is a top view of one embodiment of a center container.
[0032] [0032]FIG. 7 depicts one embodiment of the bottom section looking into the container cavity.
[0033] [0033]FIG. 8 illustrates one embodiment of the center container first member, second member, first bead and second bead, which holds items stored therein.
[0034] [0034]FIG. 9 shows one embodiment of a container stack, including a top lid and a bottom container.
[0035] [0035]FIG. 10 shows one embodiment of a container stack, including a labeled top lid, a center container, and a bottom container.
[0036] [0036]FIG. 11 illustrates one embodiment of a container stack where center containers are aligned with their tabs in a spiral fashion.
[0037] [0037]FIG. 12 shows a top view of one embodiment of a center container.
[0038] [0038]FIG. 13 shows a top view of a single disc container with featuring hinged top and bottom pieces.
[0039] [0039]FIG. 14 shows a top view of another embodiment of a container including a hinge and ears.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0040] [0040]FIG. 1 depicts one embodiment of a cross section of a container stack, including a top lid 100 , two center containers 110 , and a bottom container 120 . The center containers 110 each include a generally planar surface 130 , where the planar surface is substantially flat and typically of a size slightly larger than the shape of the items to be held in the container stack. Thus, if the container stack is to hold compact disks (CDs), the planar surface will have a width of at least the diameter of a CD (approximately 4.75 inches) and preferably will be a circular disc with a diameter slightly greater than the CD diameter or a rectangle with sides of the same dimension. The generally planar surface 130 typically has a first side 134 and a second side 132 . The first side 134 is also generally flat, and contains a first member 140 which is generally normal to the first side. Advantageously, the first member 140 typically follows at or near the perimeter of the generally planar surface 130 , and typically has a height slightly greater than the height of the items to be held in the container. Thus, if the container stack is to hold CDs, a height of, for example, about 0.100 inches can be advantageously used. Similarly, the second side 132 is generally flat, and contains a second member 170 which is normal to the second side. The second member 170 typically follows at or near the perimeter of the generally planar surface 130 , but with a diameter or perimeter advantageously slightly greater than the diameter or perimeter of the first member 140 . It is noted that the second member 170 may alternatively have a diameter or perimeter slightly smaller than the first member 140 . Also, the second member 170 and/or first member 140 may include a double wall design where two parts of one or both members fits snugly with the corresponding part(s) of the other member.
[0041] Preferably, in one embodiment, the first member 140 forms a continuous ring near the perimeter of the first side 134 of the planar surface 130 , where the shape of the ring varies based on the shape of the planar surface 130 and items to be stored therein, and the second member 170 similarly forms a continuous ring near the perimeter of the second side 132 of the planar surface 130 . Advantageously, for example, the second member 170 creates a ring slightly larger than the ring created by the first member 140 , such that a first container 110 and a second container 110 can be releasably stacked by coupling of the first member 140 of the first container to the second member 170 of the second container. One skilled in the art will understand that other shapes in addition to rings may be used in accordance with various embodiments of the current invention, and the shape of the first member 140 and second member 170 will vary based on the shape of the planar surface 130 and items to be stored in the container 110 .
[0042] In several of the preferred embodiments, the releasable attachment of multiple containers is further aided by the addition of a first bead 150 placed along the outer edge of the first member 140 . Some embodiments such as those depicted in FIG. 1 include a second bead 180 placed along the outer edge of the second member 170 . In other preferred embodiments, only one bead 180 is found on the second member 170 . Embodiments with no beads are also envisioned. In some embodiments, a bead 150 on the first member 140 may match an indented ridge on the second member. In many embodiments, one of either the first or second member will include a bead 150 with the other member having an orientation in which it is angled with respect to the planar surface 130 , as shown in FIG. 10. FIG. 12 shows another preferred embodiment in which the second member 170 has an angled surface that corresponds to an internally angled first member 140 .
[0043] While it is not necessary, the first bead 150 and second bead 180 preferably run continuously along the surface of the first member 140 and second member 170 respectively. Upon coupling of the first member 140 of a first container to the second member 170 a seal is created against the external environment which advantageously protects the items stored therein from dirt, pollutants, liquids, and the like. In other embodiments, an o-ring may be used to aid in the sealing of the container.
[0044] In a one embodiment of the present invention, a positioning ring 160 is included in the center of the second side 132 of the generally planar surface 130 of the container. The raised positioning ring 160 typically has a diameter ranging from about 0.200 inches to 0.600 inches and a height ranging from about 0.010 inches to 0.300 inches. This positioning ring 160 holds and centers the item stored in the container, such as for example, a CD, in the cavity formed by a junction of the first member 140 of a first container and a second member 170 of a second container. The inside hole of an optical disk, like a CD or DVD, or any similar item to be stored, has an interference fit with an outside drafted, radiused, or tapered diameter of the positioning ring 160 . The contents, including, but not limited to optical disks such as CDs, CD-Rs, CD-RWs, DVDs, Laser Disks, mini CDs, and mini DVDs, can be held away from the first side 134 by the draft angle or taper on the outside diameter of the ring 160 . By holding the contents in position, this ring 160 can help prevent the contents from rubbing on the inside surfaces of the container. While it is not a necessary feature of the disclosed invention, in some embodiments, an item to be stored is in contact with only contact positioning ring 160 . FIG. 12 shows another feature of some embodiments in which a positioning ring 160 is included on both sides of a center container 110 . In some of the embodiments exhibiting this feature an optical disk or other item touches only the top and bottom positioning rings 160 . Some of the embodiments depicted in FIG. 12 prevent movement of an optical disk or other item as it is held in a closed container. Additionally, FIG. 12 shows an stabilizing rib 162 that helps secure the outer edges of an optical disc. Some embodiments include more than one stabilizing rib 162 and some embodiments include stabilizing ribs on the first sides 134 and the second sides 132 .
[0045] In addition to, or instead of, the positioning ring 160 on the first side 134 , a raised positioning ring 160 can be placed on the second side 132 as shown in FIG. 12. Other embodiments have a positioning ring 160 on both sides.
[0046] In another preferred embodiment, the combined height of any combination of positioning rings 160 does not exceed the height of the cavity formed by a junction between two center containers 110 , between a center container 110 and a top lid 100 , and/or between a center container 110 and a bottom container 120 .
[0047] [0047]FIGS. 2 and 3 depicts other embodiments in which the containers include a tab 220 and tang 230 . The tab 220 typically extends from the generally planar surface 130 and aides in prying open a first container and a second container to retrieve the item contained therein. For some embodiments, on one edge of the tab 220 advantageously is included a tang 230 . The tang 230 permits the tab 220 for each center container 110 as well as the top container 100 to easily be aligned to permit simple indexing of the tabs 220 for various items stored in the container(s). Alignment is achieved by rotation of each level of the stacked containers such that the tang 230 of one level contacts the tab 220 of an adjacent level, thereby limiting the rotation of the tang 230 . In several embodiments, this alignment affords a spiral arrangement as shown in FIG. 11 where all or some of the tabs 220 can be seen from an overhead view or an angled view. Advantageously, in one embodiment, depicted in FIG. 4, the bottom lid 120 also includes a bottom tab 190 . The bottom tab 190 in one embodiment is an ordinary tab 220 , but in a preferred embodiment is an extension of the generally planar surface 130 of the bottom lid 120 that extends around the entire perimeter of the bottom lid 120 . In other embodiments, the bottom tab 190 may be a button or a bump or a tang or a similar feature that limits the rotation of a tang on an adjacent center container 110 .
[0048] Another feature of many embodiments includes a tang 230 on the tab 220 that allows for the tabs 220 to be offset rotationally at each level. This creates a spiral column of tabs 220 as shown in FIG. 11. Labels including data or indicia can be included on the tabs 220 and can be quickly and easily referenced with the tabs 220 spiraled. In one embodiment shown in FIG. 4, the bottom male container has a tab 220 that runs around the entire outside diameter except for an area of about 0.200 inches. This gap 240 is where the tang 230 from an adjacent center container 110 is positioned for proper closing. Each tang 230 hangs below the bottom of the center container 110 to which it is attached by about 0.070 inches and stops the tab 220 of the container below from overlapping the tab 220 connected to the tang 230 . This tang/tab combination makes a mechanical stop. In some embodiments, each tang 230 has a gap ranging from about 0.040 inches to 0.050 inches, so that the bottom of the tang 230 does not come into contact with adjacent container.
[0049] In some preferred embodiments of the current invention, tabs 220 and tangs 230 are used for indexing. Each container has a marking on a tab 220 . In some embodiments, the top lid 100 has a raised rib 260 around the outer diameter as seen in FIG. 2. The rib 260 is on the flat surface 130 and ranges from about 0.010 inches to 0.050 inches in height. This allows for a label or other indicia on the top lid 100 and protects such a label from scratches or smears that may occur if the flat surface 130 were allowed to touch other surfaces, such as a tabletop, as would be the case without the rib. The label can include any number of indicia that correspond to the tabs 220 so as to indicate the contents associated with each tab 220 . In some embodiments, a user can change the indicia as the contents are changed. The tangs 230 located on the outside diameter wall can have an attached tab 220 , which also will have a flat surface for some type of indicia. The tab 220 of the invention can be larger if a larger label is needed for more information. For some embodiments, the tab size for the invention is about 2 inches in length, but preferably about 1.2 inches.
[0050] [0050]FIG. 8 illustrates one embodiment of the center container 110 first member 140 , second member 170 , first bead 150 and second bead 180 , which holds items stored therein. In some preferred embodiments, the current invention is especially advantageous because it seals out dirt, moisture and the outside environment. It is foreseen that the size of the first bead 150 and second bead 180 and other aspects of the first member 140 and second member 170 may be adjusted to make the seal between a first container and a second container “tight” in order to prevent inadvertent opening, or “loose” to allow ease of opening.
[0051] In several embodiments, the current invention has an opening function which allows the user to pry apart two tabs 220 with both thumbs. The smallest hands to the largest hands are capable of doing this. In various aspects, this invention allows easy retrieval of the desired container with the use of a tab 220 molded on each center container 110 .
[0052] In several embodiments of the current invention, the container is used for holding, organizing or securing optical discs such as CDs, DVDs, mini CDs, mini DVDs, and floppy discs. One skilled in the art will understand that the containers of the present invention may be used for any object that can fit into the cavity formed by a male/female junction of a first member 140 and a second member 170 .
[0053] [0053]FIG. 2 shows one embodiment of the top lid of the container stack, where typically only one top lid is used per stack. FIG. 5 illustrates one embodiment of the top container section looking down into the inside.
[0054] Returning to FIG. 1, the bottom lid 120 typically includes a generally planar surface 130 , and a bottom surface 210 . The second side 134 of the bottom lid 120 includes a second member 170 , typically including a second bead 180 . The bottom surface 210 typically is left substantially flat for inclusion of secondary features such as labels, advertisements, or attachments. The use of a flat outer surface for the bottom lid 120 and top lid 100 also provide a simple placement position for the container from which the container advantageously will not roll or fall. FIG. 4 illustrates one embodiment of the bottom container, which forms the base of the stack of containers. FIG. 7 depicts one embodiment of the bottom section looking into the container cavity. In this embodiment, a bottom tab 190 extends around most of the perimeter of the bottom container 120 . An optional tab 220 and tang 230 are shown as well, although either form of tab may be used with or with out the other. Advantageously, a gap 240 in the bottom tab may be included to catch the tang 230 from center containers 110 or top containers 100 placed directly above the bottom container 120 .
[0055] In one aspect of the invention, the container is made from clear plastic to allow the user to view the contents in the cavity. In other embodiments, the plastic is tinted or colored with translucent or opaque color additives. In a preferred embodiment, an opaque container which filters potentially damaging UV light is used. Accordingly, the user is able to take the discs into the direct sunlight.
[0056] In some embodiments, the container is square-shaped or rectangular-shaped. In a preferred embodiment, the container is made of plastic that is softer than the polycarbonate plastic used in optical disks, thus preventing or minimizing any damage to the optical disk itself. In some preferred embodiments, surprising new advantages were found using polypropylene. Many plastics have been found to have a degrading effect on optical disks over time. Polypropylene was found to be non-toxic to optical disks.
[0057] [0057]FIG. 10 shows additional features of some embodiments of a container stack, including a top lid 100 , a center container 110 , and a bottom container 120 . Some features of the embodiments represented in FIG. 10 include a container that, when sold as a commercial distribution container, includes two optical disks 250 , or alternatively one optical disk 250 and one set of informational material such as a CD booklet (not shown). Advantageously, a label 260 is added to the top lid 100 and optionally the bottom lid 120 as well. Upon purchase of the commercial distribution container, the consumer can combine the top lid 100 , center container(s) 110 , and/or bottom container 120 with the consumer's other containers purchased in accordance with the present invention, to create a variable size
[0058] Several embodiments of the present invention hold only a single optical disk or other item and may or may not be stackable. Many of these embodiments are depicted in FIG. 13. FIG. 13 shows one such embodiment where the top lid 305 is connected to the bottom lid 307 by a hinge 300 . In other single container embodiments, the top lid 305 and bottom lid 307 are separable. Additional single disk container embodiments include ears 310 that allow the container to be snapped or hooked into a carrying case. For example, one feature of FIG. 13 is the ears 310 designed to be hooked into a two or three-ring binder or a day-timer. The ears 310 depicted in FIG. 13 may also be used in stackable, multi-item containers.
[0059] Another feature of many embodiments is a guard ring 330 as shown in FIGS. 12 and 13. The guard ring 330 extends laterally near or beyond the opening tab 340 and provides protection from accidental opening such as may result from dropping the container or inadvertently brushing the opening tab 340 against another surface.
[0060] The guard ring 330 also serves a function when the containers are sorted by some types of machines such as sorting devices and roller devices. For example, many post offices use rollers in various ways to process, sort, or maneuver mail and some roller devices have trouble climbing over objects that are too thick or too tall. In such situations, the guard ring 330 functions as a ramp and is helpful because it allows the roller to gradually roll over the total thickness or height by first rolling on to the relatively thin guard ring 330 .
[0061] and the guard ring 330 acts as a ramp allowing the roller to first climb the height of the guard ring and then climb over the highest edge of the container.
[0062] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art the various changes in form and details may be made therein without departing from the scope of the invention.
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The present invention relates generally to plastic containers which can be used for holding, organizing and securing optical disks including CDs, DVDs, mini CDs, and mini DVDs. Features of the apparatus serve to prevent dirt, dust, water, and other debris from entering the containers. Additional features include a stackable design that aids in organization and storage of a plurality of optical disks or other items. Some embodiments of the present invention have a hinged top and bottom. Additional features of some embodiments include ears allowing the container to be attached to a travel device such as a notebook or binder.
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BACKGROUND OF THE INVENTION
The invention relates to acoustical panels particularly suited for use in suspended ceilings.
PRIOR ART
Acoustical panels typically used as ceiling tiles or on walls, serve to absorb unwanted noise as well as to enclose a space and/or serve an architectural function.
Most conventional ceiling panels are made from a water-felting process or a water-based cast process. Usually a panel has a homogeneous porous core capable of absorbing sound. Lower cost products of these types are susceptible to sagging over time as a result of moisture absorption and have limited noise absorption capabilities measured as noise reduction coefficient (NRC). Higher grade products are typically more expensive to produce and can be relatively heavy. For the most part, water felted and water cast products exhibit relatively low sound absorption efficiency below 800 Hz. and are especially ineffective below 400 Hz.
SUMMARY OF THE INVENTION
The invention provides an acoustical panel formed of an apertured corrugated layer or layers with highly desirable sound absorbing properties. The panel is arranged to absorb those sound frequencies audible to the human ear and can be readily tuned to absorb sound in the lower frequencies of normal human hearing range. The invention is applicable to corrugated panels made of, for example, cardboard or plastic, either of which can be of a high recycled content.
The invention is based on the realization that corrugated panels perforated in a particular manner behave as pseudo Helmholtz resonating cavities able to produce relatively high NRC values and capable of being tuned to absorb a maximum of sound energy at a relatively low targeted frequency or frequencies.
More specifically, the invention relies on the discovery that the individual flutes of a corrugated panel can be treated like Helmholtz resonating cavities. By adjusting the relative size of the flutes, apertures, and aperture spacings, the frequency of maximum absorption can be determined. This frequency can be selected to target a specific noise or frequency band. Studies have shown corrugated panels can achieve ENRC (estimated noise reduction coefficient) as high as 0.8 with an absorption coefficient of 0.98 at a maximum absorption frequency below 600 Hz., for example. Moreover, these studies have shown a high correlation between classic Helmholtz cavity parameters and the analogous parameters discovered in the apertured corrugated acoustical panels of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isometric view of a first embodiment of an acoustical panel constructed in accordance with the invention;
FIG. 1A is a fragmentary view of the panel of FIG. 1 on an enlarged scale;
FIG. 2 is a fragmentary isometric view of a second embodiment of the invention;
FIG. 3 is a fragmentary isometric view of a third embodiment of the invention;
FIG. 4 is a fragmentary isometric view of a fourth embodiment of the invention;
FIGS. 5 and 6 are graphs of the acoustical absorption properties of examples of panels constructed in accordance with the invention;
FIGS. 7 and 8 are graphs showing the linear correlation between calculated and observed absorption frequency of panels with apertures formed, respectively, by round holes or slits; and
FIG. 9 is a schematic illustration of a suspended ceiling system employing the acoustical panels of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the various embodiments disclosed below, the invention is applied to ceiling panels for use, ordinarily, with suspended ceiling grid. In the industry, such panels have nominal face dimension of 2′×2′ or 2′×4′ or metric equivalents.
FIG. 1 shows an acoustical tile or panel 10 formed of three layers of extruded corrugated plastic sheet. In this construction, each layer 11 has a pair of main walls 12 between which are webs 13 parallel with one another and perpendicular to the main walls 12 . Adjacent pairs of webs 13 and areas of the main walls 12 form flutes or elongated cavities 14 that extend from one edge 16 of a panel to an opposite edge 16 . The main walls 12 of abutting layers 11 are suitably bonded together with an adhesive, by welding or other technique. The layers 11 can be extruded polyethylene copolymer; a suitable source for the layers 11 is Coroplast™, Dallas, Tex. USA. Apertures 17 are drilled, punched, or otherwise formed in a face 18 of the panel 10 formed by an outer wall 12 of one of the layers 11 and all of the other walls 12 of the layers 11 except the layer at a rear face 19 of the panel opposite the face 18 . Thus, in the illustrated arrangement of FIGS. 1 and 1A , each hole on the face 18 overlies a series of coaxial holes or apertures in the inner walls 12 of the sandwiched layers 11 . The panel of FIG. 1 and other panels described below and illustrated in the drawings are inverted from a normal installed orientation when they are used in a suspended ceiling where the apertured face 18 will be facing downwardly towards the interior of a room. In practicing the invention, at least one and ordinarily more than one set of coaxial apertures is formed in each flute 14 .
It has been discovered that an apertured or perforated corrugated panel such as shown in FIG. 1 , and on a larger scale FIG. 1A , forms a series of pseudo Helmholtz resonating cavities. The classical Helmholtz formula for a cavity with a necked opening is:
j H = ν 2 π A V o L
where:
f H is the resonance frequency;
ν is the speed of sound;
A is the cross-sectional area of the neck;
V o is the volume of the cavity; and
L is the length of the neck.
For the embodiment of FIG. 1 and other embodiments including those discussed below, extensive research has demonstrated that certain dimensional parameters of the corrugation flutes and apertures are analogous to the dimensional parameters of the classic Helmholtz formula. These analogous parameters are:
area of aperture A o correlates to A, the neck area;
internal volume V f of a flute between adjacent apertures or holes (essentially a measure of two half flute volumes on each side of an aperture) correlates to V o ;
the distance T from the apertured face to the opposed blind wall, taken as the thickness of the panel, correlates to L.
A maximum absorption frequency of a panel can be determined in accordance with the invention using these correlated parameters in the classic Helmholtz equation.
Sound frequency audible to the human ear and that is of concern, for example, in the NRC rating ranges between 200 Hz and 2,000 Hz. While traditional water-felted or cast ceiling tiles absorb sound at the higher ranges of these frequencies, they are of very limited effectiveness at or below 400 or 500 Hz. Moreover, it is difficult to economically produce a traditional tile with an NRC value greater than 0.7. It has been found that apertured corrugated panels such as disclosed in FIG. 1 , can be readily tuned for maximum absorption at selected frequencies between 200 and 2,000 Hz. Such panels can be especially useful, as compared to conventional tile construction, in targeting noise at 800 Hz. or less. By way of example, ENRC test samples using an impedance tube according to ASTM 384 on three-layer 10 mm Coroplast™ had the following results.
3-Layer Data—10 mm Coroplast™
Number
Hole
Segment
Number
Max Abs
Absorption
of Layers
Diameter
Length
of Holes
Freq (Hz)
Coefficient
ENRC
3
0.075
2.00
16
436
0.694
0.643
3
0.101
2.00
16
526
0.870
0.716
3
0.128
2.00
16
596
0.982
0.809
3
0.157
2.00
16
676
0.999
0.588
3
0.199
2.00
16
792
0.982
0.546
The foregoing table shows the effect of aperture size on the maximum absorption frequency. The smaller the aperture or perforation, the lower the absorption frequency.
Maximum absorption frequency is affected by the spacing between apertures measured in the lengthwise direction of the flutes. The greater the spacing the greater the resonant cavity volume, and consistent with the analogy to Helmholtz's equation, the lower the frequency.
It can be demonstrated that as the panel is made thicker and therefore the effective parameter T analogous to the Helmholtz neck opening length L is increased, the maximum absorption frequency will decrease.
FIG. 2 represents a panel 20 as a second embodiment of the invention utilizing conventional cardboard that includes a corrugated paper sheet. Similar to the panel 10 , the panel 20 comprises several corrugated layers 21 with each layer comprising a flat paper sheet 22 and a curvilinear corrugated paper sheet 23 bonded to the flat sheet at contact lines 24 between flutes 26 . Apertures 27 are drilled, punched or otherwise formed through the corrugated and flat sheets of the layers 21 except the sheet 22 at a panel face 28 opposite a face 29 from which the apertures are formed. The apertures 27 through the several sheets 22 , 23 are of the same size and are coaxial along an axis perpendicular to the faces 28 , 29 .
The analogous parameters of the panel corresponding to the Helmholtz cavity resonant frequency equation are essentially the same as those given above in connection with the Coroplast™ 10. These analogous parameters are:
A o =the area of an aperture;
Vf=the volume of a flute taken as the cross-sectional area of a flute times the distance between apertures;
T=taken as the total thickness of the panel.
It is possible to form apertures through the various layers 21 , except for the last sheet, centered between the flutes 26 so as to utilize the spaces between the flutes as additional resonant cavities.
A third embodiment of an acoustic panel 30 , represented in FIG. 3 , is similar to that of FIG. 1 in that it comprises three extruded double wall corrugated layers 31 . All of the main walls, designated 32 and web walls designated 33 , except for the main wall on a rear face 34 of the panel 30 are cut with vertical slots or slits 36 , extending perpendicularly to the lengthwise direction of flutes 37 of the corrugated layers 31 . The slots 36 create individual apertures 38 for each of the flutes 37 . The analogous parameters of the panel 30 shown in FIG. 3 are as follows:
A o =Aperture area is the slot width times the flute width, i.e. the distance between adjacent flutes;
Vf=the volume of a flute between slots 36 ; or half the flute volume on each side of a slot;
T=the thickness of the panel 30 .
Note that the flute volume relationship holds true for each of the disclosed embodiments. It is contemplated that the flutes could be blocked midway between the apertures extending along a flute such as by crushing or collapsing the walls locally and the same acoustic results would be obtained.
FIG. 4 illustrates an acoustical panel similar to the panel of FIG. 3 . The panel 40 is constructed of corrugated cardboard like the panel of the embodiment of FIG. 2 . Three corrugated cardboard, single wall layers are shown. The corrugations form flutes 42 . Flat walls 43 and corrugated sheets 44 , except for a flat wall on a rear face 45 of the panel 40 are cut through with vertical slots 46 perpendicular to the lengthwise direction of the flutes 42 . Where the slots 46 cross the flutes 42 , apertures 47 are formed.
The analogous parameters of the panel 40 are as follows:
A o =the width of the slot 46 times the distance between flutes;
Vf=the volume of a flute 42 between adjacent slots 46 ;
T=the thickness of a panel 40 .
Spaces 48 intervening the flutes 42 , being of substantially the same volume as the flutes, will absorb sound at substantially the same maximum absorption frequency as that of the flutes.
The panels illustrated in FIGS. 1-4 are exemplary of applications of the invention. In these embodiments, three corrugated layers have been shown, but it will be understood that as few as one and as many of four layers have been found to be practical.
FIGS. 5 and 6 are graphs of the sound absorption characteristics of apertured corrugated acoustic panels constructed in accordance with the invention. It will be seen that the frequency of sound at maximum absorption is about 600 Hz in FIG. 5 and about 900 Hz in FIG. 6 . By adjusting the parameters of a panel, the maximum absorption frequency can be reduced or increased as desired.
As indicated, the flute cavities can be treated as pseudo Helmholtz resonating cavities that produce maximum sound absorption at the resonant frequency. Extensive studies have shown a high linear correlation between a calculated resonant frequency of maximum absorption using the analogous parameters discussed above. Examples of the correlation between calculated and observed frequency are shown in FIGS. 7 and 8 .
If certain parameters are initially determined such as panel thickness, flute cross-sectional area, and distance along the flutes between apertures, two or more samples can be made with a different aperture size. A resonant or maximum absorption frequency can be calculated and be determined by empirical results for the samples. If an ideal actual resonance frequency is not obtained, with these samples, simple extrapolation of these data points can be used to modify the values of the analogous parameters to quickly reach a proper value of a selected variable or variables to obtain a desired maximum absorption frequency. By selecting the proper values of the analogous parameters, essentially any sound frequency between, say 200 and 2,000 Hz. can be established as a maximum absorption frequency. The invention, when practiced as described, is especially useful to produce a panel with a maximum absorption frequency at a value between 200 and 800 Hz. Sound absorption in this audible range is not readily obtained by traditional wet felted or cast ceiling tile.
FIG. 9 schematically illustrates a suspended ceiling of generally conventional construction, including metal runners or tees 49 forming a rectangular grid and acoustic panels 51 of the corrugated construction described above. Different panels 51 tuned to absorb different frequencies of, for example, 250, 500, 1,000 and 2,000 Hz. to thereby obtain a broad sound absorption range. Alternatively, a single panel can have a plurality of distinct areas that each provides different maximum absorption frequency. In either of the latter examples, a ceiling system can be designed to absorb sound through a broad human audible range. The apertured faces of the panels can be covered with an acoustically transparent scrim or veil to visually conceal the apertures. The hollow nature of the various disclosed panel embodiments permits them to exhibit the characteristics of a sandwich panel including a high stiffness in proportion to mass. Relatively high sag resistance is achievable, for example, by treating the paper forming the corrugations with humidity-resistant material.
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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An acoustical panel construction useful as a suspended ceiling tile having a rectangular shape bounded by edges and establishing a face area comprising at least one corrugated layer or layers of a total thickness, the layer or layers having a multitude of parallel flutes extending across an expanse of the rectangular shape substantially from one edge of the panel to an opposite edge, the flutes being formed by walls of the layer or layers and being of known volume, a series of apertures each of known area through the wall or walls of the flutes communicating with the atmosphere at the face, the aperture area, flute cavity volume associated with an aperture, and the total thickness of the corrugated layers associated with an aperture being arranged to produce a maximum absorption frequency between 200 and 2,000 Hz.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to novel piperazine compounds, pharmaceutical compositions containing the same and therapeutic methods of treating cardiac arrhythmias in mammals, particularly humans, including terminating acute episodes of cardiac arrhythmia, restoring normal sinus rhythm, preventing recurrence of cardiac arrhythmia and maintaining normal sinus rhythm.
[0003] 2. Background of the Related Art
[0004] Human Ether-a-go-go Related Gene (hERG) is the pore-forming potassium channel subunit that underlies the cardiac repolarizing current I Kr and consists of six transmembrane segments (S1-S6) and cytoplasmic amino- and carboxyl-termini. HERG has been linked to both congenital and drug-induced long QT syndrome, a serious and potential fatal heart condition.
[0005] Mutations in hERG produce functionally impaired channels and/or trafficking defective channels, both of which reduce I Kr currents. Mutations spanning most of the molecule have been identified in different long QT families. This suggests that hERG plays a critical role in cardiac physiology.
[0006] Most of the drugs associated with long QT syndrome (drug-induced) are hERG blockers. See, e.g., Vandenberg et al., Trends Pharmacol. Sci. 22:240-246 (2001). Since the cardiotoxicity of the non-sedating antihistamine terfenadine (Seldane) was linked to hERG block in 1996 (see Roy et al., Circulation 94:817-823 (1996)), a wide variety of drugs having diverse structures, including antiarrhythmics, antibiotics, antipsychotics as well as antihistamines, have been shown to be potent hERG blockers.
[0007] Accordingly, hERG has become an important target for cardiac safety testing of new therapeutic agents. The US Food & Drug Administration currently recommends that pharmaceutical companies seeking approval for novel therapeutic compounds have them screened for potential hERG blocking.
[0008] Atrial flutter and/or atrial fibrillation (AF) are the most commonly sustained cardiac arrhythmias in clinical practice, and are likely to increase in prevalence with the aging of the population. Currently, AF affects more than 1 million Americans annually, represents over 5% of all admissions for cardiovascular diseases and causes more than 80,000 strokes each year in the United States. While AF is rarely a lethal arrhythmia, it is responsible for substantial morbidity and can lead to complications such as the development of congestive heart failure or thromboembolism. Currently available Class I and Class III anti-arrhythmic drugs reduce the rate of recurrence of AF, but are of limited use because of a variety of potentially adverse effects, including ventricular proarrhythmia. Because current therapy is inadequate and fraught with side effects, there is a clear need to develop new therapeutic approaches.
[0009] Ventricular fibrillation (VF) is the most common cause associated with acute myocardial infarction, ischemic coronary artery disease and congestive heart failure. As with AF, current therapy is inadequate and there is a need to develop new therapeutic approaches.
[0010] Although various anti-arrhythmic agents are now available on the market, those having both satisfactory efficacy and a high margin of safety have not been obtained. For example, anti-arrhythmic agents of Class I, according to the classification scheme of Vaughan-Williams (“Classification of antiarrhythmic drugs,” Cardiac Arrhythmias , edited by: E. Sandoe, E. Flensted-Jensen, K. Olesen; Sweden, Astra, Sodertalje, pp 449-472 (1981)), which cause a selective inhibition of the maximum velocity of the upstroke of the action potential (V max ) are inadequate for preventing ventricular fibrillation because they shorten the wave length of the cardiac action potential, thereby favoring re-entry. In addition, they have problems regarding safety, i.e. they cause a depression of myocardial contractility and have a tendency to induce arrhythmias due to an inhibition of impulse conduction. The CAST (coronary artery suppression trial) study was terminated while in progress because the Class I antagonists had a higher mortality than placebo controls. β-adrenergenic receptor blockers and calcium channel (I Ca ) antagonists, which belong to Class II and Class IV, respectively, have a defect in that their effects are either limited to a certain type of arrhythmia or are contraindicated because of their cardiac depressant properties in certain patients with cardiovascular disease. Their safety, however, is higher than that of the anti-arrhythmic agents of Class I.
[0011] Anti-arrhythmic agents of Class III are drugs that cause a selective prolongation of the action potential duration (APD) without a significant depression of the maximum upstroke velocity (V max ). They therefore lengthen the save length of the cardiac action potential increasing refractories, thereby antagonizing re-entry. Available drugs in this class are limited in number. Examples such as sotalol and amiodarone have been shown to possess interesting Class III properties (Singh B. N., Vaughan Williams E. M., “A third class of anti-arrhythmic action: effects on atrial and ventricular intracellular potentials and other pharmacological actions on cardiac muscle of MJ 1999 and AH 3747 ,” Br. J. Pharmacol 39:675-689 (1970), and Singh B. N., Vaughan Williams E. M., “The effect of amiodarone, a new anti-anginal drug, on cardiac muscle,” Br. J. Pharmacol 39:657-667 (1970)), but these are not selective Class III agents.
[0012] Sotalol also possesses Class II (β-adrenergic blocking) effects which may cause cardiac depression and is contraindicated in certain susceptible patients.
[0013] Amiodarone also is not a selective Class III antiarrhythmic agent because it possesses multiple electrophysiological actions and is severely limited by side effects. (Nademanee, K., “The Amiodarone Odyssey,” J. Am. Coll. Cardiol. 20:1063-1065 (1992)) Drugs of this class are expected to be effective in preventing ventricular fibrillation. Selective Class III agents, by definition, are not considered to cause myocardial depression or an induction of arrhythmias due to inhibition of conduction of the action potential as seen with Class I antiarrhythmic agents.
[0014] Class III agents increase myocardial refractoriness via a prolongation of cardiac action potential duration (APD). Theoretically, prolongation of the cardiac action potential can be achieved by enhancing inward currents (i.e. Na+ or Ca 2 + currents; hereinafter I Na and I ca , respectively) or by reducing outward repolarizing potassium K+ currents. The delayed rectifier (I K ) K+ current is the main outward current involved in the overall repolarization process during the action potential plateau, whereas the transient outward (I to ) and inward rectifier (I KI ) K+ currents are responsible for the rapid initial and terminal phases of repolarization, respectively.
[0015] Cellular electrophysiologic studies have demonstrated that I K consists of two pharmacologically and kinetically distinct K+ current subtypes, I Kr (rapidly activating and deactivating) and I Ks (slowly activating and deactivating). (Sanguinetti and Jurkiewicz, “Two components of cardiac delayed rectifier K+ current. Differential sensitivity to block by Class III anti-arrhythmic agents,” J Gen Physiol 96:195-215 (1990)). I Kr is also the product of the human ether-a-go-go gene (hERG). Expression of hERG cDNA in cell lines leads to production of the hERG current which is almost identical to I Kr (Curran et al., “A molecular basis for cardiac arrhythmia: hERG mutations cause long QT syndrome,” Cell 80(5):795-803 (1995)).
[0016] Class III anti-arrhythmic agents currently in development, including d-sotalol, dofetilide (UK-68,798), almokalant (H234/09), E-4031 and methanesulfonamide-N-[1′-6-cyano-1,2,3,4-tetrahydro-2-naphthalenyl)-3,4-dihydro-4-hydroxyspiro[2H-1-benzopyran-2,4′-piperidin]-6yl], (+)-, monochloride (MK-499) predominantly, if not exclusively, block I Kr . Although, amiodarone is a blocker of I Ks (Balser J. R. Bennett, P. B., Hondeghem, L. M. and Roden, D. M. “Suppression of time-dependent outward current in guinea pig ventricular myocytes: Actions of quinidine and amiodarone,” Circ. Res. 69:519-529 (1991)), it also blocks I Na and I Ca , effects thyroid function, is as a nonspecific adrenergic blocker, acts as an inhibitor of the enzyme phospholipase, and causes pulmonary fibrosis (Nademanee, K. “The Amiodarone Odessey”. J. Am. Coll. Cardiol. 20:1063-1065 (1992)).
[0017] Reentrant excitation (reentry) has been shown to be a prominent mechanism underlying supraventricular arrhythmias in man. Reentrant excitation requires a critical balance between slow conduction velocity and sufficiently brief refractory periods to allow for the initiation and maintenance of multiple reentry circuits to coexist simultaneously and sustain AF. Increasing myocardial refractoriness by prolonging APD, prevents and/or terminates reentrant arrhythmias. Most selective, Class III antiarrhythmic agents currently in development, such as d-sotalol and dofetilide predominantly, if not exclusively, block I Kr , the rapidly activating component of I K found both in atrium and ventricle in man.
[0018] Since these I Kr blockers increase APD and refractoriness both in atria and ventricle without affecting conduction per se, theoretically they represent potential useful agents for the treatment of arrhythmias like AF and VF. These agents have a liability in that they have an enhanced risk of proarrhythmia at slow heart rates. For example, torsade de pointes, a specific type of polymorphic ventricular tachycardia which is commonly associated with excessive prolongation of the electrocardigraphic QT interval, hence termed “acquired long QT syndrome,” has been observed when these compounds are utilized (Roden, D. M. “Current Status of Class III Antiarrhythmic Drug Therapy,” Am J. Cardiol, 72:44B-49B (1993)). The exaggerated effect at slow heart rates has been termed “reverse frequency-dependence” and is in contrast to frequency-independent or frequency-dependent actions. (Hondeghem, L. M., “Development of Class III Antiarrhythmic Agents,” J. Cardiovasc. Cardiol. 20 (Suppl. 2):S17-S22). The pro-arrhythmic tendency led to suspension of the SWORD trial when d-sotalol had a higher mortality than placebo controls.
[0019] The slowly activating component of the delayed rectifier (I Ks ) potentially overcomes some of the limitations of I Kr blockers associated with ventricular arrhythmias. Because of its slow activation kinetics, however, the role of I Ks in atrial repolarization may be limited due to the relatively short APD of the atrium. Consequently, although I Ks blockers may provide distinct advantage in the case of ventricular arrhythmias, their ability to affect supra-ventricular tachyarrhythmias (SVT) is considered to be minimal.
[0020] Another major defect or limitation of most currently available Class III anti-arrhythmic agents is that their effect increases or becomes more manifest at or during bradycardia or slow heart rates, and this contributes to their potential for proarrhythmia. On the other hand, during tachycardia or the conditions for which these agents or drugs are intended and most needed, they lose most of their effect. This loss or diminishment of effect at fast heart rates has been termed “reverse use-dependence” (Hondeghem and Snyders, “Class III antiarrhythmic agents have a lot of potential but a long way to go: Reduced effectiveness and dangers of reverse use dependence,” Circulation, 81:686-690 (1990); Sadanaga et al., “Clinical evaluation of the use-dependent QRS prolongation and the reverse use-dependent QT prolongation of class III anti-arrhythmic agents and their value in predicting efficacy,” Amer. Heart Journal 126:114-121 (1993)), or “reverse rate-dependence” (Bretano, “Rate dependence of class III actions in the heart,” Fundam. Clin. Pharmacol. 7:51-59 (1993); Jurkiewicz and Sanguinetti, “Rate-dependent prolongation of cardiac action potentials by a methanesulfonanilide class III anti-arrhythmic agent: Specific block of rapidly activating delayed rectifier K+ current by dofetilide,” Circ. Res. 72:75-83 (1993)). Thus, an agent that has a use-dependent or rate-dependent profile, opposite that possessed by most current class III anti-arrhythmic agents, should provide not only improved safety but also enhanced efficacy.
[0021] In view of the problems associated with current anti-arrhythmic agents, there remains a need for an effective treatment of cardiac arrhythmias in mammals.
SUMMARY OF THE INVENTION
[0022] Accordingly, it is an object of the present invention to provide compounds and pharmaceutical compositions for preventing or treating cardiac arrhythmia in mammals, particularly humans.
[0023] In accordance with these and other objects, a first embodiment of the present invention comprises novel piperazine compounds having the structure:
[0000]
[0000] where each of R1, R2 and R3 is independently a hydrogen atom or a hydroxyl group, provided that not all of R1, R2 and R3 are the same and further provided that R1 and R2 are not both a hydroxyl group and R2 and R3 and not both a hydroxyl group.
[0024] A second embodiment of the present invention comprises pharmaceutical compositions containing one or more of the novel piperazine compounds shown above in admixture with a pharmaceutically acceptable carrier.
[0025] A third embodiment of the present invention comprises methods for terminating acute episodes of cardiac arrhythmia, such as atrial fibrillation or ventrical fibrillation, in a mammal, such as a human, by administering to that mammal at least one of the novel piperazine compounds shown above in an amount effective to terminate an acute episode of cardiac arrhythmia.
[0026] A fourth embodiment of the present invention is directed to a method for restoring normal sinus rhythm in a mammal, such as a human, exhibiting cardiac arrhythmia by administering at least one of the novel piperazine compounds shown above in an amount effective to restore normal sinus rhythm.
[0027] A fifth embodiment of the present invention is directed to a method for maintaining normal sinus rhythm in a mammal, such as a human, by administering at least one of the novel piperazine compounds shown above in an amount effective to maintain normal sinus rhythm in a mammal that has experienced at least one episode of cardiac arrhythmia.
[0028] A sixth embodiment of the present invention is directed to a method for preventing a recurrence of an episode of cardiac arrhythmia in a mammal, such as a human, by administering to that mammal at least one of the novel piperazine compounds shown above in an amount effective to prevent a recurrence of cardiac arrhythmia.
[0029] Additional advantages, objects and feature of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objects and advantages of the invention may be realized and attained as particularly pointed out in the appended claims.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0030] A first preferred embodiment of the present invention comprises novel piperazine compounds having the structure:
[0000]
[0000] where each of R1, R2 and R3 is independently a hydrogen atom or a hydroxyl group, provided that not all of R1, R2 and R3 are the same and further provided that R1 and R2 are not both a hydroxyl group and R2 and R3 and not both a hydroxyl group. Particularly preferred compounds include those where only one of R1, R2 and R3 is a hydroxyl group. According to a particularly preferred embodiment, R1 is a hydroxyl group and R2 and R3 are each a hydrogen atom.
[0031] Pharmaceutically acceptable salts of the novel piperazine compounds may also be employed in the methods of the present invention. These pharmaceutically acceptable salts of include, but are not limited to, salts of vanoxerine formed from non-toxic inorganic or organic acids. Such pharmaceutically acceptable salts include, but are not limited to, the following: salts derived from inorganic acids, such as hydrochloric, hydrobromic, sulfuric, sulfamic, phosphoric, nitric and the like; salts derived from organic acids, such as acetic, propionic, succinic, glycolic, stearic, lactic, malic, tartaric, citric, ascorbic, pamoic, maleic, hydroxymaleic, phenylacetic, benzoic, salicylic, sulfanilic, 2-acetoxy-benzoic, fumaric, toluenesulfonic, methanesulfonic, ethane disulfonic, oxalic, isethionic, trifluoroacetic and the like; and salts derived from amino acids, such as glutamic add or aspartic acid. See U.S. Pat. No. 6,187,802 and WO 91/01732.
[0032] The novel piperazine compounds of the present invention and the pharmaceutically acceptable salts thereof can be synthesized by conventional chemical methods using starting materials and reagents known and available to those skilled in the art. For example, with respect to pharmaceutically acceptable slats, generally such salts are prepared either by ion exchange chromatography or by reacting the free base with stoichiometric amounts or with an excess of the desired salt-forming inorganic or organic acid in a suitable solvent or various combinations of solvents.
[0033] A second preferred embodiment of the present invention comprises pharmaceutical compositions containing one or more of the novel piperazine compounds shown above in admixture with a pharmaceutically acceptable carrier.
[0034] Such a pharmaceutical composition may be administered by any technique capable of introducing a pharmaceutically active agent to the desired site of action, including, but not limited to, buccal, sublingual, nasal, oral, topical, rectal and parenteral administration. Delivery of the compound may also be through the use of controlled release formulations in subcutaneous implants or transdermal patches.
[0035] For oral administration, a suitable composition containing a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be prepared in the form of tablets, dragees, capsules, syrups and aqueous or oil suspensions. The inert ingredients used in the preparation of these compositions are known in the art. For example, tablets may be prepared by mixing the active compound with an inert diluent, such as lactose or calcium phosphate, in the presence of a disintegrating agent, such as potato starch or microcrystalline cellulose, and a lubricating agent, such as magnesium stearate or talc, and then tableting the mixture by known methods.
[0036] Tablets may also be formulated in a manner known in the art so as to give a sustained release of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof. Such tablets may, if desired, be provided with enteric coatings by known method, for example by the use of cellulose acetate phthalate. Suitable binding or granulating agents are e.g. gelatine, sodium carboxymethylcellulose, methylcellulose, polyvinylpyrrolidone or starch gum. Talc, colloidal silicic acid, stearin as well as calcium and magnesium stearate or the like can be used as anti-adhesive and gliding agents.
[0037] Tablets may also be prepared by wet granulation and subsequent compression. A mixture containing the a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, and at least one diluent, and optionally a part of the disintegrating agent, is granulated together with an aqueous, ethanolic or aqueous-ethanolic solution of the binding agents in an appropriate equipment, then the granulate is dried. Thereafter, other preservative, surface acting, dispersing, disintegrating, gliding and anti-adhesive additives can be mixed to the dried granulate and the mixture can be compressed to tablets or capsules.
[0038] Tablets may also be prepared by the direct compression of the mixture containing the active ingredient together with the needed additives. If desired, the tablets may be transformed to dragees by using protective, flavoring and dyeing agents such as sugar, cellulose derivatives (methyl- or ethylcellulose or sodium carboxymethylcellulose), polyvinylpyrrolidone, calcium phosphate, calcium carbonate, food dyes, aromatizing agents, iron oxide pigments and the like which are commonly used in the pharmaceutical industry.
[0039] For the preparation of capsules or caplets, a mixture of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, and the desired additives may be filled into a capsule, such as a hard or soft gelatin capsule. The contents of a capsule and/or caplet may also be formulated using known methods to give sustained release of the active compound.
[0040] Liquid oral dosage forms of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be an elixir, suspension and/or syrup, where the compound is mixed with a non-toxic suspending agent. Liquid oral dosage forms may also comprise one or more sweetening agent, flavoring agent, preservative and/or mixture thereof.
[0041] For rectal administration, a suitable composition containing a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be prepared in the form of a suppository. In addition to the active ingredient, the suppository may contain a suppository mass commonly used in pharmaceutical practice, such as Theobroma oil, glycerinated gelatin or a high molecular weight polyethylene glycol.
[0042] For parenteral administration, a suitable composition of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be prepared in the form of an injectable solution or suspension. For the preparation of injectable solutions or suspensions, the active ingredient can be dissolved in aqueous or non-aqueous isotonic sterile injection solutions or suspensions, such as glycol ethers, or optionally in the presence of solubilizing agents such as polyoxyethylene sorbitan monolaurate, monooleate or monostearate. These solutions or suspension may be prepared from sterile powders or granules having one or more carriers or diluents mentioned for use in the formulations for oral administration. Parenteral administration may be through intravenous, intradermal, intramuscular or subcutaneous injections.
[0043] A composition containing a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may also be administered nasally, for example by sprays, aerosols, nebulised solutions and/or powders. Metered dose systems known to those in the art may also be used.
[0044] Pharmaceutical compositions of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be administered to the buccal cavity (for example, sublingually) in known pharmaceutical forms for such administration, such as slow dissolving tablets, chewing gums, troches, lozenges, pastilles, gels, pastes, mouthwashes, rinses and/or powders.
[0045] Compositions containing a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, for topical administration may comprise a matrix in which the pharmacologically active compound is dispersed such that it is held in contact with the skin in order to administer the compound transdermally. A suitable transdermal composition may be prepared by mixing a novel piperazine compounds of the present invention, or a pharmaceutically acceptable salt thereof, with a topical vehicle, such as a mineral oil, petrolatum and/or a wax, for example paraffin wax or beeswax, together with a potential transdermal accelerant such as dimethyl sulphoxide or propylene glycol.
[0046] Alternatively, a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may be dispersed in a pharmaceutically acceptable cream or ointment base. The amount of a novel piperazine compounds of the present invention, or a pharmaceutically acceptable salt thereof, contained in a topical formulation should be such that a therapeutically effective amount delivered during the period of time for which the topical formulation is intended to be on the skin.
[0047] A novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, may also be administered by continuous infusion either from an external source, for example by intravenous infusion or from a source of the compound placed within the body. Internal sources include implanted reservoirs containing the a novel piperazine compounds of the present invention, or a pharmaceutically acceptable salt thereof, to be infused which is continuously released for example by osmosis and implants which may be (a) liquid such as a suspension or solution in a pharmaceutically acceptable oil of the compound to be infused for example in the form of a very sparingly water-soluble derivative such as a dodecanoate salt or (b) solid in the form of an implanted support, for example of a synthetic resin or waxy material, for the compound to be infused. The support may be a single body containing all the compound or a series of several bodies each containing part of the compound to be delivered. The amount a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, present in an internal source should be such that a therapeutically effective amount is delivered over a long period of time.
[0048] In addition, an injectable solution of a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, can contain various additives such as preservatives, such as benzyl alcohol, methyl or propyl 4-hydroxybenzoate, benzalkonium chloride, phenylmercury borate and the like; as well as antioxidants, such as ascorbic acid, tocopherol, sodium pyrosulfate and optionally complex forming agents, such as an ethylenediamine tetraacetate salt for binding the metal traces, as well as buffers for adjusting the pH value and optionally a local anaesthetizing agent, e.g. lidocaine. The injectable solution containing a novel piperazine compound of the present invention, or a pharmaceutically acceptable salt thereof, is filtered before filling into the ampule and sterilized after filling.
[0049] A third preferred embodiment of the present invention comprises methods for terminating acute episodes of cardiac arrhythmia, such as atrial fibrillation or ventrical fibrillation, in a mammal, such as a human, by administering to that mammal at least one of the novel piperazine compounds in an amount effective to terminate an acute episode of cardiac arrhythmia.
[0050] A fourth preferred embodiment of the present invention comprises methods for restoring normal sinus rhythm in a mammal, such as a human, exhibiting cardiac arrhythmia by administering at least one of the novel piperazine compounds in an amount effective to restore normal sinus rhythm.
[0051] A fifth preferred embodiment of the present invention comprises methods for maintaining normal sinus rhythm in a mammal, such as a human, by administering at least one of the novel piperazine compounds in an amount effective to maintain normal sinus rhythm in a mammal that has experienced at least one episode of cardiac arrhythmia.
[0052] A sixth preferred embodiment of the present invention comprises methods for preventing a recurrence of an episode of cardiac arrhythmia in a mammal, such as a human, by administering to that mammal at least one of the novel piperazine compounds in an amount effective to prevent a recurrence of cardiac arrhythmia.
[0053] Having now fully described this invention, it will be understood to those of ordinary skill in the art that the methods of the present invention can be carried out with a wide and equivalent range of conditions, formulations, and other parameters without departing from the scope of the invention or any embodiments thereof.
[0054] All patents and publications cited herein are hereby fully incorporated by reference in their entirety. The citation of any publication is for its disclosure prior to the filing date and should not be construed as an admission that such publication is prior art or that the present invention is not entitled to antedate such publication by virtue of prior invention.
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Novel piperazine compounds are disclosed. Also disclosed are pharmaceutical compositions containing these compounds and therapeutic methods of treating cardiac arrhythmias in mammals, particularly humans, including terminating acute episodes of cardiac arrhythmia, restoring normal sinus rhythm, preventing recurrence of cardiac arrhythmia and maintaining normal sinus rhythm using these compounds.
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FIELD OF THE INVENTION
[0001] The present invention relates to foamed plastic, which is used for various uses, and the production method thereof.
BACKGROUND OF THE INVENTION
[0002] So-called foamed plastics such as thermoplastic resin foam materials and thermosetting resin foam materials, which are used as fillers, protective materials, cushioning materials, or the like, for heat-insulated transporting of articles requiring refrigeration, storage boxes, packaging of articles, etc., have been widely used for various uses.
[0003] However, foamed plastics produced by ordinary production method do not have gas permeability and thus scarcely have a sound absorbing property.
[0004] On the other hand, a thermoplastic resin foam material is sometimes used for protecting persons in the inside of a motorcar from impact at the collision of the car by utilizing the excellent cushioning property thereof.
[0005] Also, the present applicant has filed a patent application (Japanese Patent Application No. 61664/1996) about a bulk-increasing material of a motorcar floor using a thermoplastic resin foam material as the core material.
SUMMARY OF THE INVENTION
[0006] Accordingly, an object of the present invention is to provide a foamed plastic imparted with a sound absorbing property and a production method of the foamed plastic.
[0007] The features of the invention are as follows.
[0008] (1) A hole-having foamed plastic comprising a resin foam material, which is formed by heat-foaming, wherein holes each having a sectional area of at least 1 mm 2 are opened at an aperture ratio of at least 3%.
[0009] (2) The hole-having foamed plastic described in above-described feature (1), wherein the foamed plastic has holes penetrating the foam material in the thickness direction thereof.
[0010] (3) The hole-having foamed plastic described in above-described feature (1) or (2), wherein a sheet-form sound absorbing material is laminated on at least one side of the foam material.
[0011] (4) The hole-having foamed plastic described in above-described feature (1), wherein the foamed plastic is the resin foam material, which is formed by heat-forming, having holes having a sectional area of one hole of at least 1 mm 2 and opening at an aperture ratio of from 3% to 25% without penetrating the resin foam material.
[0012] (5) The hole-having foamed plastic described in above-described feature (4), wherein the resin foamed material has holes having a length of from 10% to 150% to the thickness of the foam material being opened without penetrating the material at one side only thereof.
[0013] (6) The hole-having foamed plastic described in above-described feature (4) or (5), wherein a sheet-form sound absorbing material is laminated on the open-hole side of the foam material.
[0014] (7) The hole-having foamed plastic described in above-described feature (4) or (5), wherein a vibration damper is laminated on the non-open-hole side of the foam material.
[0015] (8) The hole-having foamed plastic described in above-described feature (4) or (5), wherein a sheet-form sound absorbing material is laminated on the open-hole side of the foam material and a vibration damper is laminated on the non-hole-open side of the foam material.
[0016] (9) A hole-having foamed plastic having air permeability comprising a resin foam material, which is formed by heat-foaming, wherein the air current resistance value thereof after foaming is from 100 to 3000 N·S/m 3 .
[0017] (10) The hole-having foamed plastic having air permeability described in above-described feature (9), wherein the formed plastic has holes penetrating the foam material in the thickness direction thereof.
[0018] (11) The hole-having foamed plastic having gas permeability described in above-described feature (9) or (10), wherein a sheet-form sound absorbing material is laminated on at least one side of the foamed material.
[0019] (12) A method of producing a hole-having foamed plastic, which comprises injecting a necessary composition into a mold having rod-form projections in the inside of the mold and carrying out heat-foaming.
[0020] (13) A method of producing a hole-having foamed plastic, which comprises making holes in a formed plastic obtained by heat-foaming molding by piercing the foamed plastic with rod-form material(s).
[0021] (14) A method of producing an air-permeable plastic foam, which comprises once heating foamable beads to carry out pre-foaming until volume thereof expands from 2 to 100 times of the original volume, injecting the above-described pre-foamed beads and other necessary composition into a mold, and heat-foaming the mixture.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] [0022]FIG. 1 is a cross-sectional view of an embodiment of the hole-having foamed plastic of the invention,
[0023] [0023]FIG. 2 is a cross-sectional view of an embodiment of the hole-having formed plastic of the invention laminated with a sheet-form sound absorbing material,
[0024] [0024]FIG. 3 is a cross-sectional view of an embodiment of the hole-having formed plastic of the invention laminated with a vibration damper, and
[0025] [0025]FIG. 4 is a cross-sectional view of an embodiment of the hole-having foamed plastic of the invention laminated with a sheet-form sound absorbing material and a vibration damper.
[0026] In the Figures, 1 is a hole-having foamed plastic, 2 is a sheet-form sound absorbing material, and 3 is a vibration damper.
DETAILED DESCRIPTION OF THE INVENTION
[0027] Then, the invention is explained in detail.
[0028] As the plastic used in the invention, various known raw materials such as thermoplastic resins and thermosetting resins can be used, and as the production method, a beads foaming method, an extrusion foaming method, a normal pressure foaming method, a pressure foaming method, etc., are known, and in the invention, foamed plastic obtained by any known methods can be used as the foamed plastic of the invention.
[0029] Examples of the thermoplastic resin used in the invention include polypropylene resins, polystyrene resins, polyethylene resins, vinyl chloride resins, vinyl acetate resins, and ethylene-vinyl acetate copolymer resins. Examples of the thermosetting resin used in the invention include polyurethane resins, urea resins, phenol resins, silicone resins, and epoxy resins.
[0030] In the extrusion foaming method, a granular pellet-form resin becoming the nuclei and a foaming agent such as a low-boiling hydrocarbon, a halogen hydrocarbon, a chemical foaming agent, etc., are quantitatively weighed, the mixture is foamed by an extruding machine, a foam material foamed by the extruding machine is wound round a roll, and cut into a roll-form sheet or a definite size to form a foam material of a form of a board of a definite size, etc.
[0031] The normal pressure method is a method of obtaining a foam material through mixing and extrusion steps, and further through a radiation crosslinking step or a chemical crosslinking step.
[0032] In the pressure foaming method, a method of first forming a foaming crosslinked product by pressure crosslinking and foaming the product at normal pressure is employed.
[0033] In the beads foaming method, the 1st stage of the production method is the stage of producing foamable beads. A production method of foamable beads, which has been widely carried out at present, is a polymerization method and an impregnation method. In the polymerization method, the foamable beads are obtained by suspension polymerizing the monomer of the resin used added with mainly a saturated hydrocarbon-base foaming agent such as butane, pentane, etc., and a catalyst in a polymerization vessel. In the impregnation method, the foamable beads are obtained by pressing pellet-form or spherical resin used into a pressure pot together with a dispersing solution, and then pressing a saturated hydrocarbon-base foaming agent, such as propane, butane, etc., into the pot followed by stirring, whereby the resin is impregnated with the foaming agent in a diffused state.
[0034] Since the foamed plastics obtained by these known methods usually have no gas permeability or have scarcely gas permeability, a sound absorbing faculty is scarcely expected. Accordingly, in the present invention, the foamed plastic having holes of a sectional area of at least 1 mm 2 at an aperture ratio of at last 3% has been developed. It is necessary that the sectional area of one hole is at least 1 mm 2 . When the sectional area of the hole is less than 1 mm 2 , a necessary sound absorbing effect is not obtained. Also, when the aperture ratio is less than 3%, there is a possibility that a sufficient sound absorbing faculty is not obtained.
[0035] Particularly, in the invention, in the case of having non-penetrated holes, it is desirable that the holes have the aperture ratio of from 3 to 25%, and more preferably from 12 to 20%. In this case, it is also necessary that the sectional area of one hole is at least 1 mm 2 . When the sectional area of the hole is less than 1 mm 2 , a necessary sound absorbing effect is not obtained. Also, when the aperture ratio is less than 3%, there is a possibility of not obtaining a sufficient sound absorbing faculty, and when the aperture ratio exceeds 25%, there is a possibility of causing the problems that the strength of the foamed plastic is lowered, whereby the foamed plastics is liable to be cracked.
[0036] In the case of the foamed plastic described in above-described feature (1), the holes formed are not necessarily penetrated ones or may be penetrated ones. When the holes of the above-described conditions are formed in the surface of the foamed plastic, it becomes a so-called Helmholtz type sound absorbing structure to remarkably give a sound absorbing effect. Also, when penetrated holes are formed, it is more preferably to employ a construction of laminating a sheet-form sound absorbing material, and in this case, by the resonance caused in the holes and the laminated sheet-form sound absorbing material, a joint high sound absorbing effect is obtained.
[0037] In the case of the foamed plastic described in above-described feature (4), the holes opened are not penetrated and also, it is preferred that the holes are opened to one side only of the foamed plastic. The open direction of each open hole may be perpendicularly to the surface of the foamed plastic, or may slanted with an angle, or further, the cross section of the inside diameter of each open hole may be changed. By the fact that the open holes are not penetrated, it becomes possible to keep the sound intercepting effect specific to the foamed plastic without lowering the effect simultaneously with generating a sound absorbing effect by the holes.
[0038] For opening surface holes or penetrated holes in the foamed plastic, there are various methods and one of them is a method of carrying out foaming molding in a foaming mold having rod-form projection in the inside of the mold. By controlling the aperture ratio of the holes, that is, the diameter of the projections and by controlling the length of the projections, the holes formed become penetrated holes or surface holes (non-penetrated holes).
[0039] In another method of them, holes are formed in the thickness directions of the foamed plastic by an optional post-working method such as by piercing the foam material obtained after heat-foaming molding with a needle-form material or a rod-form material, holing by a drill having a screw blade, etc. In this case, by heating the needle-form materials or the rod-form materials, narrow holes can be easily formed.
[0040] In the case of the foamed plastic described in above-described feature (4), it is preferred that the foamed plastic has holes opened to one side only with a length of from 10% to 150% to the thickness of the foam material.
[0041] As described above, since it is free that the open direction of each open hole may be perpendicularly to the surface of the foamed plastic, or may slant with an angle, etc., as described above, the non-penetrated holes can be selected in the range of the length of from 10% to 150% of the thickness of the foam material. When the length of the hole is less than 10%, the sound adsorbing performance, etc., are lowered, and on the other hand, when the length exceed 150%, since the holes must be formed at a small angle, the number of the opened holes is reduced, whereby there is a possibility that the holes formed cannot satisfy the aperture ratio defined above, hence a possibility that the foamed plastic has insufficient rigidity and strength to be put to practical use.
[0042] The foamed plastic of the invention has a necessary and sufficient sound absorbing performance even in a simple substance, but by laminating a sheet-form sound absorbing material on one side or both sides thereof, a more excellent sound absorbing effect can be obtained. There is no particular restriction on the sheet-form sound absorbing material, but examples of the sound absorbing material include clothes, nonwoven fabrics, resin felts, thermoplastic felts, and needled felts.
[0043] Even in the case of the foamed plastic described in above-described feature (4), the formed plastic has a necessary and sufficient sound absorbing performance even in a simple substance, but by laminating a sheet-form sound absorbing material on one side of the open holes, a more excellent sound absorbing effect can be obtained. There is no particular restriction on the sheet-form sound absorbing material, but examples of the sound absorbing material include clothes, nonwoven fabrics, resin felts, thermoplastic felts, needled felts and various types of resin foams such as polyurethane. In addition, in case of opening holes by post-working, after laminating the above-described sheet-form sound absorbing material, the non-penetrated holes may be opened from the laminated sheet-form sound absorbing material.
[0044] Also, by laminating various kinds of vibration dampers such as an asphalt-base vibration damper, a rubber sheet-base vibration damper, a thermoplastic resin-base vibration damper, a thermosetting resin-base vibration damper, etc., on the side having no opening of the foamed plastic, simultaneously with a sound absorbing effect, a vibration damper effect can be obtained, and the synergistic sound preventing effect can be expected.
[0045] The foamed plastic having gas permeability comprising a resin foam material formed by heat-foaming, wherein the air current resistance thereof after foaming is from 100 to 3000 N·S/mm 3 described in above-described feature (9), can be obtained in relation to the above-described beads foaming method, which comprises once heating foamable beads to carry out pre-expanding, using the foamable beads expanded to from 2 to 100 times the original volume, injecting the above-described pre-foamed foamable beads and other necessary composition into a mold, and heat-foaming the mixture.
[0046] As the resin constituting the foamable beads, the resins same as those used for the above-described foamed plastic can be used. However, in the resins illustrated above, three kinds of resins such as polypropylene, polystyrene, and polyethylene are preferably used, and in the resins, two kinds of resins such as polypropylene and polyethylene are particularly preferably used.
[0047] In the case of obtaining the foamed plastic having gas permeability, it is necessary, as described above, to use foamable beads as a foaming agent, heating the foamable beads to carry out pre-expanding and to expand the volume to from 2 to 100 times the original volume. This step is indispensable to form gaps in the foamed plastic formed to form a so-called “a millet and rice cake form”. When the volume expansion is less than twice, the formation of gaps is insufficient and a necessary air current resistance is not obtained, and when the volume expansion exceeds 100 times, the rigidity and the strength of the foamed plastic become weak and brittle, and there is a possibility that the foamed plastic obtained cannot be use for practical purposes.
[0048] Then, the foamable beads pre-foamed by the above-described condition are placed in a mold of an optional form, and an in-mold foaming molding is carried out by a known method such as steam superheating foaming, etc., to obtain the foamed plastic. By re-foaming the foamable beads, the volumes of which have been already expanded by the pre-foaming, the beads are imperfectly fused each other and become the state of being point-fused. As the result thereof, different from an ordinary foamed plastic, the foamed plastic formed has air permeability.
[0049] The air permeability in the foamed plastic having air permeability is evaluated by the air current resistance value, and it is necessary that the value of the air permeability is from 100 to 3000 n·S/m 3 .
[0050] This is because the air current resistance value of the range can most effectively absorb the audible sound of a human being. The air current resistance value can be controlled to the above-described range, by controlling the volume expansion by the pre-foaming of the foamable beads, or by controlling the heating temperature and pressure conditions at the foaming. Also, when the air current resistance value of the foamed plastic exceeds 3000 N·S/m 3 , by opening the holes in the thickness direction of the foamed plastic by an optional post-working method such as pin-cushion working, etc., the air current resistance value can be controlled to the above-described range.
[0051] The foamed plastic having air permeability has a necessary and sufficient sound absorbing performance even in a simple substance, but by laminating a sheet-form sound absorbing material on one side or both sides thereof, a more excellent sound absorbing effect can be obtained. There is no particular restriction on the sheet-form sound absorbing material, but examples of the sound absorbing material include clothes, nonwoven fabrics, resin felts, thermoplastic felts, and needled felts.
[0052] As described above in detail, since the hole-having foamed plastic of the invention has as excellent sound absorbing property, the foamed plastic is particularly effectively used for the portions requiring sound absorbing performance simultaneously with shock cushioning and heat-insulating property. For example, by using the formed plastic for insulating material for building, in addition to the heat-insulating property, a sound absorbing performance can be imparted, whereby a pleasant space in room can be obtained, and also by using a cushioning material of collision used as the lower portion of a dash panel of a motorcar, the effect of absorbing noises from the engine room can be added. Also, by using a bulk-increasing material of a motorcar floor, the effect of reducing noises in the car room can be also obtained.
[0053] Then, for more understanding the present invention, examples are described below but, as a matter of course, the invention is not limited to the following examples.
EXAMPLE 1
[0054] Foamable beads were made from a polystyrene monomer, the foamable beads were injected into a mold having disposed in the inside thereof many needle-form materials having a length same as the thickness of the foam formed therein and a sectional area of 5 mm 2 , and by carrying out steam heat-foaming and drying, a polystyrene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. In the polystyrene foam material, many penetrated holes each having a sectional area of 5 mm 2 were formed and the aperture ratio was 10%.
EXAMPLE 2
[0055] Foamable beads were made from a polyethylene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polyethylene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. The foamed polyethylene foam material was pieced by a metal forming jig having many needle-form materials and heated to 200° C. to form penetrated holes each having a sectional area of 5 mm 2 . The aperture ratio was 20%.
EXAMPLE 3
[0056] Foamable beads were made from a polypropylene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polypropylene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. The polypropylene foam material was pieced by a metal forming jig having many needle-form materials and heated to 200° C. to form penetrated holes each having a sectional area of 5 mm 2 . The aperture ratio was 20%. On the form material was laminated a sheet-form sound absorbing material made of a resin felt having a thickness of 20 mm.
Comparative Example 1
[0057] Foamable beads were made from a polystyrene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polystyrene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained.
[0058] Test Method 1:
[0059] About the foamed materials of Examples 1 to 3 and Comparative Example 1, the acoustic absorption coefficients at specific frequencies were measured by the measurement method of acoustic absorption coefficient by the reverberation room method regulated by JIS A 1406.
[0060] Results
[0061] The acoustic absorption coefficients of Examples 1 to 3 and Comparative Example 1 were as follows. (Unit: %)
Frequencies (Hz) 500 1000 2000 4000 Example 1 7.8 22.5 71.2 31.0 Example 2 11.5 30.5 68.0 30.0 Example 3 60.0 84.0 60.0 23.0 Comp. Ex. 1 5.5 15.0 36.0 23.0
[0062] As shown in the above results, in the hole-having foamed materials of Examples 1 to 3, in each case, in the frequency regions of the acoustic range, the improvements of the acoustic absorption coefficient of 2 dB at the minimum to 70 dB at the maximum were observed as compared with the resin foamed material of Comparative Example 1.
EXAMPLE 4
[0063] Foamable beads were made from a polystyrene monomer, the foamable beads were injected into a mold having disposed in the inside thereof many needle-form materials having a length of from 10 to 17 mm and a sectional area of 20 mm 2 , and by carrying out steam heat-foaming and drying, a polystyrene foam material of a rectangular parallelepiped having a thickness of 30 mm was obtained. In the foamed polystyrene form material, many non-penetrated holes each having a sectional area of 20 mm 2 opened to one side were formed and the aperture ratio of the holes at the open side was 12%.
EXAMPLE 5
[0064] Foamable beads were made from a polyethylene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polyethylene foam material of a rectangular parallelepiped having a thickness of 30 mm was obtained. The polyethylene foam material was pieced by a metal forming jig having many needle-form materials and heated to 200° C. to form non-penetrated holes each having a sectional area of 30 mm 2 and opening to one side only. The aperture ratio of the open-hole side was 20%.
EXAMPLE 6
[0065] Foamable beads were made from a polypropylene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polypropylene foam material of a rectangular parallelepiped having a thickness of 30 mm was obtained. The polypropylene foam material was pieced by a metal forming jig having many needle-form materials and heated to 200° C. to form non-penetrated holes each having a sectional area of 20 mm 2 and opening to one side only. The aperture ratio of the open-hole side was 13%. On the side having opening of the formed material was laminated a sheet-form sound absorbing material made of resin felt of a thickness of 20 mm.
EXAMPLE 7
[0066] Foamable beads were made from a polypropylene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polypropylene foam material of a rectangular parallelepiped having a thickness of 30 mm was obtained. In the polypropylene foam material, non-penetrated holes each having a sectional area of 20 mm 2 and opening to one side only were formed by a drill having a spiral blade. The aperture ratio of open-hole side was 13%. On the side having no opening of the formed material was laminated an asphalt-base vibration damper sheet having a thickness of 3 mm.
EXAMPLE 8
[0067] Foamable beads were made from a polypropylene monomer, the foamable beads were injected into a mold in which a rubber sheet having a thickness of 2 mm was previously laminated and by carrying out steam heat-foaming and drying, a polypropylene foam material of a rectangular parallelepiped having a thickness of 30 mm and having laminated thereon a rubber sheet having a thickness of 2 mm was obtained. On the foamed polypropylene foam material was laminated a needled felt having a thickness of 5 mm, and from the surface of the needled felt, non-penetrated holes each having a sectional area of 20 mm 2 opening to one side only were formed by a drill having a spiral blade. The aperture ratio of the open-hole side was 13%.
Comparative Example 2
[0068] Foamable beads were made from a polystyrene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a polystyrene foam material of a rectangular parallelepiped having a thickness of 30 mm was obtained.
Reference Example
[0069] In the same polystyrene form material as in Comparative Example 2, penetrated holes having a sectional area of one hole of 20 mm 2 were formed at an aperture ratio of 20%.
[0070] Test Method 2:
[0071] About each of the foamed materials of Examples 4 to 8, Comparative Example 2 and Reference Example, the absorption coefficients at specific frequencies were measured by “the measurement method of acoustic absorption coefficient by the reverberation room method” regulated by JIS A 1406.
[0072] Test Method 3:
[0073] About each of the foamed materials of Examples 4 to 8, Comparative Example 2 and Reference Example, the sound insulation effect at specific frequencies was measured by “the sound transmission loss measurement method in laboratory” regulated by JIS A 1416.
[0074] Results
[0075] The sound absorbing ratios of Examples 4 to 8, etc., are shown in Table 1 below. The unit is %.
TABLE 1 Frequency (Hz) 500 1000 2000 4000 Example 4 7.5 24.5 73.0 31.0 Example 5 11.5 30.5 68.0 30.0 Example 6 40.0 90.0 85.0 90.0 Example 7 12.0 29.5 70.0 35.0 Example 8 20.0 35.0 76.0 45.0 Ref. Example 55.0 16.0 10.0 8.0 Com. Example 2 6.0 21.0 70.0 30.0
[0076] Also, the sound insulation effects of Examples 4 to 8, etc., are shown in Table 2 below. The unit is dB.
TABLE 2 Frequency (Hz) 500 1000 2000 4000 Example 4 4.8 5.3 9.5 18.0 Example 5 4.5 5.5 9.0 18.0 Example 6 5.2 10.0 21.0 89.0 Example 7 12.0 5.9 10.0 25.0 Example 8 14.0 8.0 16.0 42.0 Ref. Example 5.1 6.0 10.0 19.0 Com. Example 2 3.2 4.1 9.0 17.0
[0077] As shown in the above results, in each of the hole-having foamed materials of Examples 4 to 8, in the frequency regions of the acoustic range, the improvements of the acoustic absorption coefficient of 3% at the minimum to 80% at the maximum were observed as compared with the resin formed material of Comparative Example 2, and also the same or more improvements were observed as compared with the resin foamed material having penetrated hole in the reference example. On the other hand, in each of the hole-having foamed materials of Examples 4 to 8, in the frequency regions of the acoustic range, the improvements of the sound insulating effect of about 20 dB at the maximum were observed as compared with the resin foamed material of Comparative Example 2, and also the same or more sound insulating effects were observed as compared with the resin formed material of the reference example.
EXAMPLE 9
[0078] Foamable beads were prepared from a polypropylene monomer by s suspension method, and the foamable beans were subjected to pre-foaming by heating at 100° C. to obtain foamable beads expanded to 50 times the average volume of the beads. The pre-foamed foamable beads were injected into a mold and by carrying out steam heat-foaming and drying steps, a polypropylene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. The air current resistance value of the foamed polypropylene foam material was 500 N·S/m 3 .
EXAMPLE 10
[0079] Foamable beads were prepared from a polyethylene monomer by s suspension method, and the foamable beans were subjected to pre-foaming by heating at 100° C. to obtain foamable beans expanded to 50 times the average volume of the beads. The pre-foamed foamable beads were injected into a mold and by carrying out steam heat-foaming and drying steps, a polyethylene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. The air current resistance value of the foamed polyethylene foam material was 600 N·S/m 3 .
EXAMPLE 11
[0080] Foamable beads were prepared from a polystyrene monomer by s suspension method, and the foamable beans were subjected to pre-foaming by heating at 100° C. to obtain foamable beans expanded to 50 times the average volume of the beads. The pre-foamed foamable beads were injected into a mold and by carrying out steam heat-foaming and drying steps, a polystyrene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained. The air current resistance value of the foamed polystyrene foam material was 800 N·S/m 3 , but as the result of applying needle working to the thickness direction to form penetrated holes, the air current resistance value became 200 N·S/m 3 .
Comparative Example 1
[0081] Foamable beads were formed from a polystyrene monomer, the foamable beads were injected into a mold and by carrying out steam heat-foaming and drying, a foamed polystyrene foam material of a rectangular parallelepiped having a thickness of 20 mm was obtained.
[0082] Test Method 1:
[0083] About the foamed materials of Examples 9 to 11 and Comparative Example 1, the acoustic absorption coefficients at specific frequencies were measured by “the measurement method of acoustic absorption coefficient by the reverberation room method” regulated by JIS A 1406.
[0084] Results
[0085] The acoustic absorption coefficients of Examples 9 to 11 and Comparative Example 1 were as follows. The unit was %
Frequencies (Hz) 500 1000 2000 4000 Example 9 9.8 24.7 70.2 31.0 Example 10 12.6 33.0 62.0 32.0 Example 11 60.0 84.0 60.0 23.0 Comp. Ex. 1 5.5 15.0 36.0 23.0
[0086] As shown in the above results, in each of the hole-having foamed materials of Examples 9 to 11, in the frequency regions of the acoustic range, the improvements of the acoustic absorption coefficient of 2 dB at the minimum to 70 dB at the maximum were observed as compared with the resin foamed material of Comparative Example 1.
[0087] As described above, the foamed plastic of the invention shows both the shock cushioning property or heat-insulating property and the sound absorbing property which have not be obtained by foamed plastics of related art, and further shows the soundproof performance having both the sound absorbing effect and the sound intercepting effect, which can be said to various kinds of soundproof materials of motorcars as well as for various industrial fields such as, for example, building industries, etc., are expected.
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To provide a foamed plastic provided with holes having a specified area at a specified aperture ratio. The holes are either a through-hole or a non-through-hole and properly provided. The foamed plastic is superior in sound absorbing property and has a strength. In the case of non-through-holes, the foamed plastic can beep a sound absorbing effect as well as a sound intercepting effect, and for example, when used as a cushioning material of collision to be used as the lower portion of a dash panel of a motorear, not only the cushioning of collision but also the absorption of noises from an engine can be achieved. On the other hand, a foamed plastic obtained by pre-foaming foamable beads and again foaming the pre-foamed beads is a foamed plastic having gas permeability, which is different from usual foamed plastics. In this case, when an air current resistance value is set within a specified range, an audible sound of a human being can be most effectively absorbed. Thus, the latter foamed plastic can also be used as a cushioning material of collision and the like similar to the former foamed plastic.
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CROSS REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. patent application Ser. No. 13/112,417 filed on May 20, 2011 and entitled “Windshield Wiper Blade Refill Suited for Removal of Solid Material.” The patent application identified above, application Ser. No. 13/123,417 filed on May 20, 2012 is incorporated here by reference in its entirety to provide continuity of disclosure.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a device for performing the two distinct functions of cleaning solids and wiping water from vehicular windshields. It is generally well known in the field that windshield wipers are effective for removing water, but they are relatively ineffective for removing solids such as solid insect remains and bird droppings without creating extensive and potentially dangerous smears. The smears are caused by the rubber squeegee action of the blades, which tends to smear solids into a thin film by forcing it against the glass surface rather than scooping it or brushing it away. Consequently, the driving practitioner may be forced to halt their vehicle to scrub off solid matter manually or risk further driving with obscured vision through the windshield.
In certain geographic locations and climates, it is common for airborne bugs and insects to collide with, and become compressed against, the windshield of a vehicle. The accumulation of such bugs, insects and other debris on the windshield is greatest when the vehicle is in operation, but significant accumulation can also occur when the vehicle is stationary for a long period. This is particularly true of bird droppings and cars parked in wooded areas for periods of time. Removal of bugs, insects and other debris attached to the windshield is imperative to ensure safe operation of the vehicle as accumulation can significantly impair the driver's vision and line of sight.
The most effective means of removing the accumulated bugs, insects and other debris is to hand wipe the windshield with a towel combined with a solvent or cleaner. However, this form of cleaning is not always possible or feasible during the operation of a moving vehicle. In such instances, the driver must rely on using windshield wipers, which are designed to remove accumulation of water rather than solid debris. Wiper blades are constructed of rubber or a similarly flexible material in order to conform to the sloped surface of the windshield for effective removal of water or other liquids. However, wiper blades are generally ineffective for removing or dislodging these solid materials, particularly those that are stuck, bonded, or otherwise attached to the exterior surface of a windshield and are not easily ushered away by the wiper's sweeping action. There exists a need for a device capable of removing bugs, insects and other debris from the windshield of a car without user intervention. Further, such a device should be easily removable and replaceable, and require no modification to the standard vehicle wiper blades or wiper mounts.
2. Description of the Prior Art
Numerous designs for windshield wipers have been provided in the prior art. Even though these designs may be suitable for the specific individual purposes to which they address, these prior art devices have several known drawbacks. Specifically, such devices do not include or suggest a wiper blade system has removable and replaceable parts that both wipe and clean a windshield surface.
Several prior art patents address the issue of adding a scrubbing sponge portion in parallel with traditional blades. However, these devices have blades that are either fixed in place or restricted from movement. This lack of blade movement can result in damage to a user's windshield when blades drag along its surface. Gilliam, III U.S. Pat. No. 4,649,593 is directed to a combined windshield wiping and cleaning device having a scrubbing member with a reticular surface for removing solid matter along with a wiper member with squeegee for removal of water. These are attached together with a supporting base as a single monolithic extrusion of an elastomeric material. The Gilliam invention fits into the windshield wiper arm in the same way as current blades.
Similarly, Kinder U.S. Pat. No. 5,235,720 is directed to a windshield scrubbing and wiping blade assembly including a scrubbing blade, having a mesh covered scrubbing portion, and at least one wiping blade in parallel, spaced apart in relationship with the scrubbing blade. The mesh and the associated scrubbing portion of the scrubbing blade define side channels for receiving and transporting debris removed by the mesh from the windshield. In the two bladed embodiment of the invention, the scrubbing blade is shorter than the wiping blade and is maintained out of contact with the windshield during the portion of the wiping cycle in which the scrubbing blade trails the wiping blade. Hipke U.S. Pat. No. 5,406,672 is directed to a windshield wiper blade system comprising an elastomeric wiper blade, an elongated base portion, a coupling mechanism for coupling the base portion; a squeegee coupled to the base portion and extended downwards therefrom to contact the surface of a windshield; and a scrubbing blade. The scrubbing blade further comprises a sponge extended along and coupled to the base portion near the squeegee with the sponge having a surface adapted to conform with the surface of a windshield; and webbing disposed about the sponge and defining a scrubbing surface. Thus, when the system swipes back and forth across the surface of the windshield the wiper blade and the scrubbing blade remove both water and bugs.
Additionally, Hsieh U.S. Pat. No. 6,622,337 is directed to a wiper blade for a car comprising a seat part, a moisture absorptive part, and a sweep part. The seat part is an elongated strip made of non-absorptive material. The moisture absorptive part is made of water absorbable material and has a length and a width thereof corresponding to the seat part for joining with the seat part. The sweep part is an elongated strip with a gap and has a size corresponding to the absorptive part for joining with the absorptive part. The moisture absorptive part can keep the sprayed water for next wipe as soon as the sweep part removes the foreign substances on a windshield of the car. Root U.S. Pat. No. 6,748,621 is directed to a vehicle windshield wiper assembly for providing a user with a set of windshield wipers for motor vehicles designed to scrub insects off the glass. The blade member is for providing support to a plurality of cleaning members and a cleaning blade. The cleaning members and the cleaning blade are for facilitating cleaning of debris the windshield of a vehicle. Green, U.S. Pat. No. 6,5327,615 discloses a wiper blade assembly having two wiper blade portions running parallel to a cleaning member disposed therebetween. The cleaning member is comprised of a number of rubber strips having conical ends.
The Gilliam, Kinder, Hipke, Hsieh, Root and Green inventions all describe wiper blade assemblies having fixed blades or blades whose movement is practically impaired due to the structure of the device. These replacement wipers include both one or more standard blade members and one or more sponge members, but they do not allow for the blade position to change during use of the device. As such, they may damage a practitioner's windshield during use because they are incapable of adjusting to accommodate irregularities in the windshield or large debris on the windshield surface. The present invention provides blade portions that have a self-adjusting position within two channels along the device. Thus, there is improved windshield cleaning with a reduced risk of damage to the user's windshield.
Perry U.S. Pat. No. 5,301,384 is directed to a vehicular window cleaning apparatus having a wiper arm, wiper blade and drive means in combination with a scrubber for intensifying the cleaning effort of the wiper blade. The scrubber is detachably connected to the wiper blade. An adjustment means is provided for rotating the wiper blade relative to the wiper arm sequentially positioning the wiper blade and scrubber against an associated windshield. The Perry invention requires the installation of a non-standard articulator control for the sponge portion, requiring a costly deviation from traditional wipers.
Gold U.S. Pat. No. 5,634,841 is directed to an apparatus for removing scratches and/or stains from a vehicle windshield includes a cylindrical sponge having a radial opening which fits snugly over a windshield wiper blade with the windshield wiper arm connected to the blade through the radial opening in the cylindrical sponge. The methods of the invention include moistening the cylindrical sponge and applying a polishing abrasive. Activating the vehicle windshield wiper wipes the abrasive on the windshield with the sponge. Other methods of the invention include impregnating the sponge with a polishing abrasive or moistening the sponge with windshield washer fluid. The device described in Gold is not a windshield wiper in the traditional sense; rather the Gold invention describes a device and means of repairing and improving windshields, and is thus not analogous to the present invention.
Other devices described in the prior art simply add a sponge component to current wiper blades. Squires U.S. Pat. No. 6,505,378 is directed toward a wiper assembly for providing additional scrubbing surface area. The wiper assembly includes a wiper blade designed for coupling to a wiper arm of a vehicle; a scrubbing member, which couples to the wiper blade for removing debris from the windshield; and a plurality of clip members for coupling the scrubbing member to the wiper blade. Similarly, Cabak U.S. Pat. No. 7,707,681 is directed to a windshield wiper clip adapted for connecting a scrubbing blade to a windshield wiper, wherein the clip connects a scrubber to a wiper in order to accommodate bug removal during movement of the wiper about a windshield. The invention also includes an integrated clip and scrubber, as well as wiper-scrubber system. A novel scrubber mount having rounded shoulders is also described. By simply adding a sponge component to current wiper blades, the Squires and Cabak inventions do not describe a complete system of blades and sponges. Further, the Squires and Cabak inventions greatly increase the size of the wiper assembly, risking obscured vision during vehicle operation.
The present invention differs from the prior art in that it offers an easily removable and wiper device with removable wiper blade portions. These wiper blade portions have a range of motion that allows them to adjust to large debris on the windshield surface, reducing the risk of damage to a user's windshield. Additionally, the present invention does not require costly non-standard mounts or modifications to the standard wiper assembly. Further, having two blade members allows for optimal cleaning of debris, such that smears are unlikely whether the wiper is moving up or down on the windshield. The present invention will greatly assist vehicle users in preventing bugs and other debris from remaining lodged upon the windshield. Practitioners will be capable of easily cleaning the windshield during vehicle operation without any significant modification to their wiper blade assemblies. Further, users will find the present invention easy to install and replace when needed.
SUMMARY OF THE INVENTION
In view of the foregoing disadvantages inherent in the known types of wiper blades now present in the prior art, the present invention provides a new wiper blade and sponge device wherein the same can be utilized for providing convenience for the user when removing bugs or other sticky debris from their windshield while operating a motor vehicle.
The present invention is a removable replaceable windshield wiper refill system that utilizes a netted sponge for cleaning debris instantly from the windshield in conjunction with two wiper blade members for water removal. The inner sponge is comprised of a netted mesh, mounted between two blades and inset slightly for optimum efficiency. The present invention allows the practitioner to clean debris anytime and anywhere from the windshield while operating their motor vehicle. The present invention is designed such that a squirt of wiper fluid will wet the sponge, allowing the most dried on and persistent smears to be efficiently cleaned from the windshield. The present invention is composed of one solid unit that can be removed and replaced easily and inexpensively manufactured. Further, the present invention is made in all typical windshield wiper lengths and will fit any of the current windshield wiper mounts.
The present invention will comprise of a base component made of hard plastic, rubber or metal that is shaped for use as a blade refill, capable of attachment to a windshield wiper frame or wiper mount. The present invention further has two wiper blade components made of durable rubber or silicone, positioned to abut with the windshield outer surface. Attached between the two blades is a sponge component made of dense sponge material wrapped in durable nylon mesh netting for grabbing debris. The present invention is distinguished from prior art in that: it will clean, scrub, and remove debris quickly; has the simplicity of only being one assembled device to be easily changed; and is designed to fit any current standard wiper blade rail or wiper blade mount.
The primary object of the present invention is to utilize the mesh netted sponge between two wiper blades to quickly remove debris such as mud, sap or bug remains when crossing the windshield with a minimal number of passes. Minimizing the number of swipes ensures the vehicle operator will not encounter a loss of visibility.
A secondary object of the present invention is to provide a wiper device that will clip or slide onto any type of wiper blade or alternatively, attach to any type of wiper blade arm mount. The present invention has a mesh netted sponge positioned in between double rubber or silicon blade member to better clean debris from the windshield. The netted sponge runs the entire length of the blades and is slightly inset to prevent overlap with the blades during operation.
It is a further object of the invention to provide at least one scrubbing member comprising a net covered sponge member arranged in parallel with to two elongated rubber or silicon wiper members of generally conventional design. Both the wiper function and the scrubbing function are supported by a common base along the entire length of each member, wherein the base is adapted to be held in place and operated by a windshield wiper blade arm mount or wiper blade assembly which may be of conventional design.
Other objects, features and advantages of the present invention will become apparent from the following detailed description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTIONS OF THE DRAWINGS
FIG. 1 is a perspective view of the present invention, with a close-up perspective view of the terminal end of the blades and scrubbing member.
FIG. 2 is a perspective view of the present invention in use, attached to a windshield wiper arm assembly, with a close-up perspective view of the attached ends.
FIG. 3 shows a cross-section view of the wiper device attached to a windshield wiper arm assembly.
FIG. 4 shows a cross-section view of the wiper device attached to a windshield wiper arm assembly and in use for cleaning the surface of an automobile windshield.
DETAILED DESCRIPTION OF THE INVENTION
Reference is made herein to the attached drawings. Like reference numerals are used throughout the drawings to depict like or similar elements of the windshield wiper blade device. For the purposes of presenting a brief and clear description of the present invention, the preferred embodiment will be discussed as used for cleaning and wiping the surface of an automobile windshield. The figures are intended for representative purposes only and should not be considered to be limiting in any respect.
Referring now to FIG. 1 , there is shown a perspective view of the present invention, with a close-up perspective view of the terminal end of the blades 11 and the internal scrubbing member 12 . The present invention 10 consists of a pair of rubber or silicone wiper blade members 11 removably attached on either side of a mesh netting sponge member 12 to a base component 13 . The base component 13 may be made of metal, rubber or any other suitable material, an. A connection bracket 14 is disposed along each end of the base to provide removably securable engagement between the device and a wiper blade mount. The close-up view demonstrates the terminal end of the device 10 , showing the base component 13 with the connection bracket 14 , as well as the mesh net sponge 12 attached in between the wiper blade members 11 .
Referring now to FIG. 2 , there is shown a perspective view of the present invention in use, attached to a standard wiper blade assembly, with a close-up perspective view of the end connection bracket 14 for attachment. The present invention 10 is attached over a traditional wiper blade 17 or to a wiper blade mount 18 using the mount connection bracket 14 on the base component 13 . In a preferred embodiment depressible release buttons 15 are disposed on the connection bracket 14 and must be depressed to release the engagement of the bracket to the wiper blade 17 or wiper blade mount 18 . Thus, the release buttons 15 prevent inadvertent removal of the device while it is in use. FIG. 2 illustrates the device 10 in use on a typical vehicle windshield 16 . The close up demonstrates the terminal end of the device when attached to a standard windshield wiper 17 , and shows the mesh net sponge 12 in between the two blade members 11 , with the connection bracket 14 to secure the device.
Turning now to FIG. 3 , a cross-sectional view of the device is shown, disclosing the structure of the overall device and the engagement of its subparts. Two hollow tunnels 19 run parallel along the length of laterally opposing sides of the base 13 . Each tunnel has two sidewalls an upper wall and a lower wall, which define an empty space therebetween. The upper wall of each tunnel is affixed to the underside of the base. Each lower tunnel wall is separated into two halves with a space between the halves, forming a channel that extends the entire length of the tunnel. Wiper blade members 11 are removably retained within the channels. A wiper blade member comprises a blade 22 and a retaining portion 20 . In a preferred embodiment the wiper blade member also includes a restraining bar 21 that prevents the scrubbing member 12 from interfering with the wiper blade members during operation of the device. A narrow area connecting the retaining portion to the restraining bar is adapted to fit within the channel of a lower tunnel wall. The retaining portion is larger in width than the channel but is adapted to fit loosely within the tunnel. Thus the wiper blade member is removably retained within the tunnel by slidably engaging the narrow portion of the wiper blade member into the lower tunnel wall channel so that the blade member's retaining portion is housed within the tunnel.
The device is removably affixed to an automobile via a connection means 15 that engages with a wiper blade 17 or wiper blade mount 18 . This keeps the windshield-cleaning device in place and in contract with the windshield during use. If a user wants to replace the device, he or she can depress the buttons 14 on either side of the connection bracket to release the engagement. In this way, the device is easily installed and replaced as necessary.
In FIG. 4 the device is shown in use for cleaning the surface of a windshield 16 . As the device is moved across the user's windshield the first of the blades 22 of the wiper blade members 11 pushes debris off the surface, much like a plow. The scrubbing member 12 then moistens and scrubs the surface. A second wiper blade member follows behind the scrubbing member, pushing accumulated moisture and any loosened debris off the windshield surface.
Unlike many conventional wiper blade members, the blade members 11 of the present invention are not fixed to the base of the device, nor are the blade members snuggly retained within the tunnels 19 rendering them practically immobile. The shape of the present wiper blade members allows the retaining portion 20 to shift within the tunnel to adjust to objects on the windshield surface. Immobile wiper blades scrape debris off a windshield but can cause damage to the windshield if the debris has adhered to the windshield surface. The present shifting wiper blade members will push debris off the surface but will adjust to firmly stuck debris, passing over it so that the scrubbing member can loosen the debris for removal by the second scrubbing member. Thus the mobility of the present wiper blade members reduces the potential for damage to the windshield that could result from forcing caked on debris off of the windshield. Further, the shape of the wiper blade members facilitates easy removal and replacement of blade members that become damaged during use. In a fixed blade member device, the entire device must be replaced if any part is damaged. Conversely, the present invention is structurally designed to permit replacement of the wiper blade members without necessitating the replacement of the entire device.
The scrubbing member also has a specialized shape. The wedge shaped tip ensures that as much of the windshield surface as possible is cleaned with each pass of the device. Many devices have round sponges, resulting in a small surface area cleaned on each pass of the sponge. The present invention has a scrubbing member with generally flat surfaces on each side so that when the device passes over a windshield most of the surface area of the applicable side of the scrubbing member tip is in contact with the windshield surface. This maximizes the effectiveness of the scrubbing member and increases the overall cleanliness of the automobile windshield.
In use an individual attaches the device 10 to a standard windshield wiper 17 or wiper mount arm 18 , using the connection bracket 14 . When the vehicle wiper mechanism activates, the device 10 , will swipe across the surface of the windshield 16 . In use, the device will first pass over the bugs or debris with a blade member 11 , then scrub the bugs or debris with the sponge 12 , then again with a second blade member 11 in a single pass. Ideally, practitioners will moisten the mesh net sponge portion 12 of the device 10 with windshield wiper fluid. The mesh net sponge 12 is slightly shorter than the two wiper blade members 11 , thus ensuring that no overlap will occur during usage. When activated the blade will swipe across the windshield 16 , the blade members 11 and sponge 12 will deflect slightly without overlap to conform to the shape of the windshield 16 .
The practical design of the device 10 , allows for easy removal and replacement when one or more portions have worn. Replacement will simply involve depressing the release buttons 15 and disengaging the worn device 10 from the wiper blade 17 or mount 18 , then locking a new device into the connection brackets. The blade members 11 may be made of rubber, silicon or any other appropriate material. The sponge 12 may be covered with a mesh netting of nylon or any other material, such that it is highly durable and capable of scrubbing without scratching the windshield. The sponge 12 will also be slightly shorter than the two blade members 11 , with gaps on either side to prevent overlap during the swiping process and to better clean away bugs and other debris from the windshield.
With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A wiper blade device with a durable mesh sponge member attached between two removable wiper blade members. The combination sponge and wiper blade construction provides a unitary device that combines the two distinct functions of cleaning solids and wiping water from vehicular windshields. The device further provides minimal windshield obstruction given its construction, improving current wiper blade capabilities without degrading visibility or impacting safety of the vehicle. The device may comprise a wiper blade refill attachable to a wiper blade mount, providing the practitioner with an improved windshield wiper blade that is cost effective and one that requires no modification of the vehicle to implement.
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BACKGROUND OF THE INVENTION
The present invention relates to implantable medical electrical leads, and more particularly relates to multi-lumen, multi-conductor leads.
In the context of implantable electrical leads, such as those employed in conjunction with implantable pacemakers, implantable nerve stimulators, and implantable cardioverter/defibrillators, conductors typically have been either tinsel wire or coiled conductors. Recently, however, there has been an increasing level of interest in the use of new conductor types. One of the most promising new conductor types is the wire rope or cable (hereafter cable) conductor, comprising multiple strands, each strand comprising a number of very fine wires. In some cases, the conductors are provided with a thin coating of teflon or other insulating polymer. Examples of such conductors are described in U.S. Pat. No. 5,324,321 issued to Pohndorf et al., in U.S. Pat. No. 5,246,014, issued to Williams et al. and U.S. Pat. No. 4,964,414, issued to Handa et al., all incorporated herein by reference in their entireties.
In working cable type conductors, the inventors have determined that there are some difficulties associated with coupling the conductors to connectors, electrodes, sensors or other components. In particular, such conductors, in the sizes used for implantable electrical leads, are difficult to crimp, and the very fine wires employed tend to melt when welded. Moreover, if insulated, the cables typically must be stripped at their ends, prior to attachment.
SUMMARY OF THE INVENTION
The present invention addresses the problems of coupling cable type conductors to electrodes, connectors, sensors and other components in the context of implantable medical leads. Typically, the invention will take the form of a lead having a body formed of an elongated insulative tube with a lumen containing a conductor, typically coupled at its distal end to an electrode or a sensor and coupled at its proximal end to an electrical connector. The component to which the conductor is connected is provided with an internal lumen into which an end of the conductor and a core are inserted. Either the core or the inner lumen of the component is provided with threading or similar surface texture which engages the conductor. If the threading is on the core, the conductor is placed alongside the core and the core is advanced into the component's lumen, pulling the cable into component's lumen as the core is advanced. Conversely, if the threading is provided on the interior surface of the component's lumen, the cable is placed in the lumen, and the core is advanced into the lumen, with the cable retained in place by the threading. The core is sized so that the conductor is compressed between the core and the component's lumen to provide for electrical and mechanical coupling of the conductor to the component. If the conductor is insulated, the insulation simply shears off as the core is advanced, flowing into the spaces between adjacent threads, eliminating the necessity of stripping the end of the conductor prior to connection.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of an implantable lead of the type in which the present invention may be practiced.
FIG. 2 is a sectional view through the body of the lead of FIG. 1 in the vicinity of the ring electrode.
FIG. 3 is a sectional view of the ring electrode illustrated in FIG. 2.
FIG. 4 is a sectional view of the threaded core illustrated in FIG. 2.
FIG. 5 is a sectional view through the body of the lead of FIG. 1 in the vicinity of its bipolar connector assembly.
FIG. 6 is a cut-away view of the connector ring illustrated in FIG. 5.
FIG. 7 is a sectional view of the threaded core illustrated in FIG. 5.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a plan view of a defibrillation lead of the type in which the present invention may usefully be practiced. The present invention, of course, may also be usefully practiced in the context of other medical electrical leads, such as cardiac pacing leads, nerve and muscle stimulation leads, and so forth.
The lead of FIG. 1 is provided with an elongated insulative lead body 10, preferably fabricated of silicone rubber, polyurethane or other biocompatible elastomer. At the proximal end of the lead, it carries an elongated defibrillation electrode 12, a ring electrode 14 and a tip electrode 16, each coupled to a conductor located within the lead body 10. Tines 18 are employed to maintain electrode 16 in contact with the tissue of the right ventricle, as described in U.S. Pat. No. 3,902,501, issued to Citron. Electrodes 16, 14 and 12 may correspond to conventional, currently available pacing and defibrillation electrodes. The proximal end of the lead carries a connector assembly, beginning with a molded lead bifurcation 20, which splits off two of the conductors within lead body 10 to a bipolar, in-line connector assembly 24, generally corresponding to the IS-1 connector standard for pacing leads. Connector assembly 24 is provided with a first set of sealing rings 28, a connector ring 34, a second sealing rings 32 and connector pin 36. Connector pin 36 is coupled to a conductor which extends through the lead body 10 to tip electrode 16. Connector ring 34 is coupled to a conductor which extends through the lead body 10 to ring electrode 14. Connector assembly 22 carries a set of sealing rings 26 and a connector pin 30, coupled to a conductor extending through lead body 10 to defibrillation electrode 12. The illustrated connector assemblies are conventional elements, and may correspond to any of the numerous known electrical connector assemblies provided on implantable medical leads.
Although not visible in FIG. 1, it should be noted that the elongated conductors passing through lead body 10 may include any of the various known available conductors for use in conjunction with implantable electrical leads, including monofilar or multifilar coiled conductors, cable type conductors, and the like. In the specific context of the lead illustrated in FIG. 1, the conductor coupling connector pin 36 to electrode 16 takes the form of a multifilar coiled conductor to allow passage of a stylet therethrough, while the conductors coupling ring electrode 14 to connector ring 34 and coupling defibrillation electrode 12 to connector pin 30 take the form of cables provided with a coating of PTFE. In the embodiments discussed herein, the cables may be fabricated from silver cored MP35N wire, the cables including seven strands, each strand including seven wires, the cable being coated with an extruded coating of PTFE, and having an overall diameter of 0.017 inches (0.432 millimeters). However, the present invention is believed workable in the context of any stranded conductors appropriate for use in implantable electrical leads.
FIG. 2 is a sectional view through the lead of FIG. 1 in the vicinity of ring electrode 14. In this view it can be seen that the lead body 10 is provided with at least two lumens, one of which carries cable 108. In FIG. 2, lumen 110 is illustrated as empty. However, in an actual lead as illustrated in FIG. 1, lumen 110 would contain a conductor coupling tip electrode 16 to connector pin 36. As described above, this would typically be an insulated, coiled conductor defining a central lumen allowing passage of a stylet therethrough. Cross bore 112 through core 102 allows for backfill of adhesive to bond the lead body 10 to a distal insulative sleeve 104, thereby also providing a mechanical interlock with the assembly of core 102 and ring electrode 14.
Conductor 108 is shown compressed between electrode 14 and threaded core 102, in order to maintain electrical and mechanical contact between conductor 108 and ring electrode 14. The distal end of threaded core 102, located within ring electrode 14, is provided with an outer surface having threads 115 machined therein. For example, threads having a pitch of 125 threads per inch, a depth of 0.002" and a flat of 0.002" on the crest of each thread may be employed. Core 102 may be fabricated of an implantable grade stainless steel or other implantable metal and electrode 14 may be fabricated of platinum/iridium alloy. In the illustrated embodiment, the threaded distal portion of core 102 has an outer diameter of 0.059", with the inner diameter of electrode 14, in its central portion, being 0.063". To assemble the ring electrode 14 to the conductor 108, the conductor 108 is first threaded through ring electrode 14 from its proximal end and placed along the threaded portion of threaded core 102. Threaded core 102 is then driven proximally into ring electrode 14, such that conductor 108 is compressed between the threaded portion of core 102 and the central portion of ring electrode 14 to provide a reliable mechanical and electrical interconnection.
FIG. 3 is a sectional view through ring electrode 14, removed from its surrounding components. In this view it can be seen that the ring electrode is provided with a reduced diameter central portion 120, and proximal and distal end portions having an increased diameter. Located at the proximal end of central portion 120 is a shoulder 118 which serves to limit the insertion depth of core 102.
FIG. 4 illustrates core 102 in more detail. The distal portion 114 of core 102 is provided with threading 115, as described above, which extends to a point adjacent shoulder 116. Shoulder 116, in conjunction with shoulder 118, limits the insertion depth of core 102 into ring electrode 14. Also visible in this view are cross bores 112, which as described above, allow for backfilling of adhesive to couple the lead body 10 to the distal sheath 104 and core 102.
FIG. 5 is sectional view through the bipolar connector assembly 24 of the lead illustrated in FIG. 1. In this view, the proximal end of connector pin 36 is visible in cross-section, and connector ring 34 is visible in cross-section. Connector pin 36 is coupled to coiled conductor 210 by means of a swaging core 200, which compresses conductor coil 210 between the interior lumen of connector pin 36 and the outer surface of swaging core 200, in a conventional fashion. An insulative sleeve 206 surrounds conductor 210, and extends distally, back through the connector assembly into molded sealing ring sleeve 212. The portion of sheath 206 between connector pin 36 and sleeve 212 is omitted in this drawing, for the sake of simplicity.
Surrounding connector pin 36 is a molded sealing ring sleeve 202, which may be fabricated of silicone rubber, which in turn is mounted to a spacer 204 which is typically fabricated of a harder plastic, such as polyurethane. Spacer 204 is molded in situ between connector pin 36 and ring 34, and is maintained in mechanical interconnection with ring 34 by means of internal threading 208, as described in U.S. Pat. No. 4,572,605, issued to Hess, et al., incorporated herein by reference in its entirety. Surrounding the proximal portion of ring 34 is a second molded sealing ring sleeve 212, which may similarly be fabricated of silicone rubber. This much of the connector assembly 22 is conventional, and corresponds to connector assembly on currently available Medtronic pacing and defibrillation leads.
Threaded core 214 can be seen inserted into the lumen at the distal end 216 of connector ring 34, compressing stranded conductor 108 therebetween. Core 214 and connector ring 34 may be fabricated of an implantable grade stainless steel. As described above in conjunction with threaded core 102, threaded core 214 is provided with external threading, which may be, for example, at a pitch of 125 threads per inch, a depth of 0.002", each thread having a 0.002" flat on the crest of each thread. The inner diameter of the ring electrode at its proximal end may be 0.084", with the outer diameter of the threaded portion of threaded core 214 being 0.079" and the inner diameter of the central lumen through the core being 0.063". These dimensions, in conjunction with the conductor described above provide for reliable mechanical and electrical coupling. In the specific case illustrated, the thickness of the core is chosen to allow for a slight, elastic deformation of the core as it is inserted in the lumen of the connector ring. To assemble conductor 108 to connector ring 34, it is placed along the side of threaded core 214, after which threaded core 214 is driven into the lumen at the distal end of ring electrode 34, drawing conductor 108 along, compressing it between the core 214 and the connector 34 and simultaneously shearing off the insulation on the outer surface of conductor 108, so that it makes good electrical contact with connector ring 34. As illustrated, connector ring 34 is an elongated tubular structure provided with multiple cross bores 220. Prior to installation of sealing ring sleeve 212, these cross bores are backfilled with silicone medical adhesive, allowing for interconnection of the internal components of the connector assembly with one another and with sealing ring sleeve 212, as described in the above-cited patent issued to Hess.
FIG. 6 illustrates a cutaway view through connector ring 34, showing the configuration of the lumen 222 at its proximal end in more detail, and also illustrating the cross bores 220 in more detail. In this view it can be seen that the central portion of connector ring 34 is provided with two sets of intersecting cross bores, while the proximal portion is provided with a single cross bore. FIG. 7 illustrates threaded core 214, removed from the assembly illustrated in FIG. 5.
In the above description, specific dimensions, conductor types and so forth are given which the inventors have found to provide workable interconnections in conjunction with the specific embodiments disclosed above. However, it is believed that the method of interconnection provided by the present invention is widely applicable to the various types of stranded conductors proposed for use in implantable medical leads. It must understood that the relative dimensions of the internal lumen of the component to which the conductor is going to be connected, the outer dimensions and thread dimensions of the threaded core, and the dimensions of the stranded conductor will be different for each implementation and will have to be determined empirically. Similarly, while specific thread dimensions are given above, other thread dimensions or other forms of surface texturing may be employed in the context of the present invention. For example, circumferential grooves or other texturing which provides raised edges transverse to the central axis of the core or component lumen, with depressions or grooves of sufficient depth to allow flow of insulation therein may be substituted for threading. Further, while in the specific embodiments described above the texturing is on the exterior surface of the core, it may instead or in addition be provided on the interior surface of the lumen of the component to which the conductor is to be attached. However, it is believed that, given the teaching of the present application, this can readily be accomplished without undue experimentation. Finally, while the above disclosed embodiments deal specifically with interconnection of a stranded conductor to an electrode and to a connector ring on a connector assembly, the basic connection technique is equally applicable to interconnection of a stranded wire to a physiologic sensor or other component of an implantable medical lead. As such, the above disclosure should be considered exemplary, rather than limiting, with regard to the claims which follow:
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A method of interconnecting a core, a stranded conductor such as a wire rope or cable and a component of a medical electrical lead provided with a internal lumen. At least one of the core and the internal lumen of the component is provided with a textured surface, such as threading. The conductor is located alongside said textured surface and the core is advanced into the lumen of said component, such that the textured surface engages the conductor and retains the conductor as the core is advanced into the lumen, and the conductor is compressed between the core and the inner lumen of the component.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This patent application claims priority under 35 U.S.C. §119(e) to U.S. Provisional Patent Application Ser. No. 61/169,563 entitled “RECLAMATION SYSTEM,” having a filing date of Apr. 15, 2009 and is incorporated herein by reference. This patent application Ser. No. 12/761,362 is also related to Utility patent application filed on even date herewith, entitled “SYSTEM AND METHOD FOR RECOVERING MINERALS”.
BACKGROUND
One aspect relates to a system and method of separating or sorting and sizing iron ore and removing gangue. More specifically, in one embodiment the system and method separate and remove the silica components from an iron ore.
Throughout the world, there are quantities of minerals combined with other material. Often, attempts are made to separate materials. For example, ores are treated by mechanical, chemical, or thermal processes, or some combination thereof to liberate marketable minerals from waste minerals (called gangue).
In many mining districts enormous quantities of mineral resources are not utilized because mining and/or mineral processing to recover the marketable constituents is uneconomical. Additional quantities of desired minerals are locked to gangue minerals and are rejected during mining or mineral processing and are sent to stockpiles or tailing basins.
Billions of tons of unmined minerals, mined minerals disposed of in stockpiles and tailing basins, and other waste materials in landfills would be utilized if processing costs for separating gangue from valuable minerals were significantly reduced.
For these and other reasons, there is a need for the present embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawing is included to provide a further understanding of embodiments and is incorporated in and constitutes a part of this specification. The drawing illustrates embodiments and together with the description serve to explain principles of embodiments. Other embodiments and many of the intended advantages of embodiments will be readily appreciated as they become better understood by reference to the following detailed description. The elements of the drawing are not necessarily to scale relative to each other. Like reference numerals designate corresponding similar parts.
FIG. 1 illustrates a length-wise cross-sectional view of an ultrasonic crusher in accordance with one embodiment.
DETAILED DESCRIPTION
In the following Detailed Description, reference is made to the accompanying drawing, which form a part hereof, and in which is shown by way of illustration specific embodiments in which the invention may be practiced. In this regard, directional terminology, such as “top,” “bottom,” “front,” “back,” “leading,” “trailing,” etc., is used with reference to the orientation of the FIGURE(s) being described. Because components of embodiments can be positioned in a number of different orientations, the directional terminology is used for purposes of illustration and is in no way limiting. It is to be understood that other embodiments may be utilized and structural or logical changes may be made without departing from the scope of the present invention. The following detailed description, therefore, is not to be taken in a limiting sense, and the scope of the present invention is defined by the appended claims.
It is to be understood that the features of the various exemplary embodiments described herein may be combined with each other, unless specifically noted otherwise.
FIG. 1 is an ultrasonic crusher 10 in accordance with one embodiment. In one exemplary embodiment, ultrasonic crusher 10 is used to sort and size iron ore and remove gangue. In another example, ultrasonic crusher 10 separates and removes silica components from an iron ore. In one embodiment, ultrasonic crusher 10 includes pump 12 , pipe system 14 , first and second ultrasound sonotrodes 16 and 18 , and first and second supplemental pipes 20 and 22 .
In one embodiment, ultrasonic crusher 10 is used to sort materials so that certain components can be removed. In one example, minerals such as iron ore mixed with gangue are sorted such that the gangue is removed. Iron ore is introduced into ultrasonic crusher 10 as a water-borne slurry through pump 12 . Pump 12 forces the ore and gangue mixture into a first pipe segment 14 A of pipe system 14 toward a first elbow section 26 .
In one embodiment, first pipe segment 14 A is substantially horizontally oriented toward first elbow section 26 . Pipe 14 has a first diameter in first pipe segment 14 A. In one embodiment, the first diameter is configured such that the cross-sectional area in first pipe segment 14 A is approximately 960 mm 2 . The slurry moves through first pipe segment 14 A toward first elbow section 26 in the direction marked with the adjacent arrow in FIG. 1 . In one case, the slurry moves out of first elbow section 26 into second pipe segment 14 B of pipe system 14 . In one example, second pipe segment 14 B is substantially vertically oriented.
In one embodiment, pump 12 forcing the slurry through the combination of first pipe segment 14 A, first elbow section 26 and into second pipe segment 14 B, sets up a first stage elutriator, such that lighter particles are separated from heavier ones using the substantially vertically-directed stream of liquid in second pipe segment 14 B. In one example, separation of particles occurs by allowing particles to settle in a fluid. As such, in one embodiment, the coarser, heavier, and rounder grains settle faster than the finer, lighter, and more angular grains. The fluid is in motion, carrying away the slow-settling grains, while a sediment of fast-settling grains is developed.
In one embodiment, first ultrasound sonotrode 16 is configured adjacent first elbow section 26 . In one embodiment, sonotrode 16 is configured with 1,000 watts and 20 kHz. As the slurry moves upward from first elbow section 26 and first sonotrode 16 , the first stage of elutriation takes place as the slurry enters second pipe segment 14 B. In one embodiment, second pipe segment 14 B has a second diameter. In one embodiment, the second diameter is configured such that the cross-sectional area in second pipe segment 14 B is approximately 1,260 mm 2 , or approximately 1.3 times as large as the cross-section of first pipe segment 14 A. In one case, the cross-sectional area of second pipe segment 14 B is sized to permit the largest and densest particles in the slurry to settle down to first elbow section 26 , which houses first sonotrode 16 . Particles of lesser size and density will continue upward through second pipe segment 14 B in the direction indicated by the adjacent arrow in FIG. 1 .
At first elbow section 26 where first sonotrode 16 is installed, particles that are too large and/or too dense to move upward through second pipe segment 14 B, fall back to first elbow section 26 above first sonotrode 16 . In one embodiment, this settled or sediment material is milled, crushed, and ground by ultrasound energy generated by first sonotrode 16 until the particles are small enough to move upward with the bulk of the slurry.
In one embodiment, first supplemental pipe 20 is used to draw off or to add slurry components to modify slurry properties in pipe system 14 , and to allow sampling of the slurry materials. Ore particles in the slurry that are of the desired density and size can be removed or added, and fluids, or reagents, can also be introduced to the system to adjust the slurry chemistry, density, and rate of particle settling.
In one embodiment, slurry from second pipe segment 14 B moves into third pipe segment 14 C. In one example, third pipe segment 14 C is substantially horizontally oriented toward second elbow section 28 . Pipe 14 has a third diameter in third pipe segment 14 C. In one embodiment, the third diameter is configured such that the cross-sectional area in third pipe segment 14 C is approximately 1,260 mm 2 , or approximately the same as the cross-section of second pipe segment 14 B. The slurry moves through third pipe segment 14 C toward second elbow section 28 in the direction marked with the adjacent arrow in FIG. 1 . In one case, the slurry moves out of second elbow section 28 into fourth pipe segment 14 D of pipe system 14 . In one example, fourth pipe segment 14 D is substantially vertically oriented.
In one embodiment, pump 12 forcing the slurry through the combination of third pipe segment 14 C, second elbow section 28 , and into fourth pipe segment 14 D, sets up a second stage elutriator, which very similarly to the first stage elutriator, allows lighter particles to be separated from heavier ones using the substantially vertically-directed stream of liquid in fourth pipe segment 14 D.
In one embodiment, second ultrasound sonotrode 18 is configured adjacent second elbow section 28 . In one embodiment, second sonotrode 18 is configured with 1,000 watts and 20 kHz. As the slurry moves upward from second elbow section 28 and second sonotrode 18 , the second stage of elutriation takes place as the slurry enters fourth pipe segment 14 D. In one embodiment, fourth pipe segment 14 D has a fourth diameter. In one embodiment, the fourth diameter is configured such that the cross-sectional area in fourth pipe segment 14 D is approximately 1,590 mm 2 , or approximately 1.6 times as large as the cross-section of first pipe segment 14 A. In one case, the cross-sectional area of fourth pipe segment 14 D is sized to permit the largest and densest particles in the slurry to settle down to second elbow section 28 , which houses second sonotrode 18 . Particles of lesser size and density will continue upward through fourth pipe segment 14 D in the direction indicated by the adjacent arrow in FIG. 1 .
As was the case at the first stage elutriator, at second elbow section 28 where second sonotrode 18 is installed, particles that are too large or too dense to move upward through fourth pipe segment 14 D, fall back to second elbow section 28 above second sonotrode 18 . In one embodiment, this settled or sediment material is milled, crushed, and ground by ultrasound energy generated by second sonotrode 18 until the particles are small enough to move upward with the bulk of the slurry.
In one embodiment, second supplemental pipe 22 is used to draw off or to add slurry components to modify slurry properties in pipe system 14 , and to allow sampling of the slurry materials. Ore particles that are of the desired density and size can be removed or added and fluids, or reagents, can also be introduced to the system to adjust the slurry chemistry, density, and rate of particle settling.
One skilled in the art will observe that additional stages of elutriation can be added with combinations of pipe segments and elbow sections, along with adjacent sonotrodes, such that further sorting and separation occurs. Additionally, adjacent supplemental pipes can be used to add and remove material at the stages.
Mechanical characteristics, such as elutriator tube cross-sectional area, shape, and length can be varied as required and along with slurry properties such as flow rate, slurry density, and fluid chemistry controlled in the initial slurry composition and/or via the supplemental pipes, such as 20 and 22 illustrated, act in concert with the ultrasound energy to produce the desired separations of ores and wastes.
In one embodiment, ultrasonic crusher 10 is used to separate particles on the order of −20 to +300 mesh (833 to 50 microns). In one embodiment, larger sizes are sorted when heavy media is introduced, or when extreme hindered settling conditions are produced.
In one embodiment, dilution of the slurry in ultrasonic crusher 10 is 3%-35% solids by weight (finer particles to coarser particles). Sorting is done at as high a fluid density as possible, typically 40%-70% solids by weight.
In one embodiment, ultrasonic crusher 10 is used to crush and/or separate ores such as Oolitic Iron ore, Ferruginous Chert (Silicified hematite/magnetite mix), Banded Iron Formation (Silicified hematite/magnetite mix), Cretaceous Pebbles (Silicified hematite/magnetite mix), Taconite (Magnetite, hematite, and SiO 2 ), Natural Iron Ore (hematite), Dunka Pit type (Fe sulfides, hematite, magnetite), and Gold bearing Quartz (Au, Ag in SiO 2 matrix).
In one embodiment, ultrasonic crusher 10 is used to crush and/or separate minerals such as Bauxite (Al hydroxides), Kaolinite (Al 2 Si 2 O 5 (OH) 4 ), Kyanite (Al 2 SiO 5 ), Andalusite (Al 2 SiO 5 ), Topaz (Al 2 SiO 4 (F,OH) 2 ), Sillimanite (Al 2 SiO 5 ), Corundum (Al 2 O 3 ), Orpiment (As 2 S 3 ), Realgar (AsS), Barite (BaSO 4 ), Witherite (BaCO 3 ), Borax (Na 2 B 4 O 5 (OH) 4 -8H 2 O), Tourmaline (B(Na—Ca—Al—Mg—Fe—Mn) silicate), Beryl (Be 3 Al 2 (Si 6 O 18 )), Calcite (CaCO 3 ), Gypsum (CaSO 4 -2H 2 O), Dolomite (CaMg(CO 3 ) 2 ), Anhydrite (CaSO 4 ), Stilbite (CaAl 2 Si 7 O 18 -7H 2 O), Aragonite (CaCO 3 ), Apatite (Ca 5 (PO 4 ) 3 (F,Cl,OH)), Epidote (Ca 2 (Al, Fe)Al 2 O(SiO 4 )—(Si 2 O 7 )(OH)), Malachite (Cu 2 CO 3 (OH) 2 ), Chrysocolla (Cu 4 H 4 Si 4 O 10 (OH) 8 ), Bornite (Cu 5 FeS 4 ), Chalcopyrite (CuFeS 2 ), Pyrrhotite (Fe 1−x S), Magnetite (Fe 3 O 4 ), Hematite (Fe 2 O 3 ), Arsenopyrite (FeAsS), Siderite (FeCO 3 ), Chromite (FeCr 2 O 4 ), Pyrite (FeS 2 ), Marcasite (FeS 2 ), Ilmenite (FeTiO 3 ), Wolframite ((Fe,Mn)WO 4 ), Goethite (aFeO(OH)), Limonite (Fe—OH nH 2 O), Staurolite (Fe 2 A 19 O 6 (SiO 4 ) 4 —(O,OH) 2 ), Cinnabar (HgS), Muscovite (KAl hydrated silicate), Biotite (KMg hydrated silicate), Talc (Mg hydrate), Chlorite (MgFe hydrate), Serpentine (Mg 3 Si 2 O 5 (OH) 4 ), Magnesite (MgCO 3 ), Spinel (MgAl 2 O 4 ), Manganite (MnO(OH), Pyrolusite (MnO 2 ), Molybdenite (MoS 2 ), Halite (NaCl), Natrolite (Na 2 Al 2 Si 3 O 10 2H 2 O), Galena (PbS), Anglesite (PbSO 4 ), Cerussite (PbCO 3 ), Stibnite (Sb 2 S 3 ), Quartz (SiO 2 ), Opal (SiO 2 -nH 2 O), Cassiterite (SnO 2 ), Celestite (SrSO 4 ), Strontianite (SrCO 3 ), Rutile (TiO 2 ), Sphalerite (ZnS), Hemimorphite (Zn 4 (Si 2 O 7 )(OH) 2 —H 2 O), Smithsonite (ZnCO 3 ), and Zircon (ZrSiO 4 ).
In one embodiment, ultrasonic crusher 10 is used to crush igneous rock such as granite, gabbro, basalt; sedimentary rock such as conglomerate, sandstone, shale, limestone, iron formation; metamorphic rock such as slate, marble, gneiss, quartzite; and various other rocks.
In one embodiment, ultrasonic crusher 10 is configured as a portable system. In one example, each of the components ultrasonic crusher 10 is configured compact enough to be carried on rail cars, such as one or more cars of a train, such that ultrasonic crusher 10 can be rolled over a rail directly to a waste stockpile for processing thereof.
Although specific embodiments have been illustrated and described herein, it will be appreciated by those of ordinary skill in the art that a variety of alternate and/or equivalent implementations may be substituted for the specific embodiments shown and described without departing from the scope of the present invention. This application is intended to cover any adaptations or variations of the specific embodiments discussed herein. Therefore, it is intended that this invention be limited only by the claims and the equivalents thereof.
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One aspect is an ultrasonic crusher including a pipe system having at least one elutriator. A pump is configured to pump a slurry through the pipe system and the at least one elutriator. A first ultrasound sonotrode is configured proximate to the at least one elutriator.
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BACKGROUND
This invention relates to the organization of multiple socket sets and various hand tools. The invention provides multiple tool receiving surfaces upon which to mount hand tools and accessories. The invention preferably rotates to provide easy access to tools and accessories affixed thereto.
It is common for mechanics to have more than thirty different socket and/or tool sets. Organizing these tools is therefore of paramount importance.
Until now there have been socket and tool organizers that organize single sets of tools. Examples are described in U.S. Pat. Nos. 4,337,860; 4,410,095; 4,802,580; 4,927,020; 5,855,284; and 6,047,824, all incorporated herein by reference. Socket organizers typically utilize magnets, spring clips or the like to organize sockets in size order, for example, in a linear fashion. With these prior art organizers, multiple tool sets require multiple organizers.
An example of a prior art tool retainer is the magnetic strip. Long magnetic strips are often secured to workbenches or roll carts commonly found in repair shops. The magnetic strips are typically used to hold sockets and various hand tools such as ratchets, screwdrivers and wrenches and provide the mechanic easy identification and access. Typically multiple sets are stored flat in a toolbox. Various difficulties arise when mechanics try to use multiple sets. Namely, visibility and access can become a problem as multiple sets are stacked and placed on top of one another. Another issue associated with these products is movement of multiple sets, i.e., each set required will have to be obtained individually and brought to the workplace. Organization of multiple sets becomes difficult as different socket sets are moved to different locations as they are used.
Although these prior art tool retainers and organizers are useful and provide a convenient means of organizing and storing tools, there has remained a need for a tool and socket organizer to handle a larger quantity of tools and multiple socket sets.
SUMMARY OF THE INVENTION
The present invention provides a means to store, carry and organize a large number of sockets and tools. The present invention organizes prior art socket and tool retention devices by providing multiple mounting surfaces for multiple tools, tool sets and tool organizers on a single portable organizer. The present invention has multiple tool receiving faces to organize tools by category if desired. For example, ¼″ sockets can be mounted on one face and ⅜″ drive sockets on another face. The present invention is adaptable so that it can be mounted to a roll cart, workbench, shop vise or placed on surfaces such as a shop floor. The present invention facilitates movement of multiple socket sets since multiple sets are contained on a single organizer. The rotatable assembly of the organizer provides easy fingertip access to any socket or tool mounted thereon. The tool receiving faces can accept various tool retention means known in the art such as but not limited to socket clips and rails, spring clips, various magnetic retainer systems and the like. The tool receiving faces allow for customized placement of tools to suit individuals' needs. Additionally, changing the placement or configuration of the tool retention means can alter the appearance of the organizer. The tool retention means can be rearranged on the tool receiving faces to provide custom organization for each user. This allows the user to arrange their most commonly used tools in the most convenient order. The tool organizer places a large number of tools at the user's fingertips for easy access.
The tool organizer keeps tools off of the work surface, leaving more workspace available to the user. In keeping the tools off of the work area, the tools are easier to see and identify, making acquiring tools easier and saving time associated with looking for a hidden tool.
The organizer is preferably rotatably mounted between vertical uprights of a U-shaped frame such as by a rod through the frame and sides of the organizer to provide an axis of rotation for the organizer.
Alternatively the organizer can be fixedly attached to the frame.
The present tool organizer provides several unique advantages over the prior art.
The present invention provides a means to attach and organize multiple socket sets and tools in an easy to obtain format, eliminating the clutter and disorganization commonly encountered with prior art tool organizers.
The present invention further provides multiple mounting options. In one embodiment the tool organizer is adapted to be bolted to a workbench, wall or roll cart.
The present invention still further provides a base for securing to the frame to provide stable placement of the invention on any flat surface such as a shop floor or a workbench.
The present invention still further provides a means for carrying the organizer wherein the frame provides a handle used to carry the organizer and its tools to different workplaces. In a most preferred embodiment the section of frame employed as a handle is knurled.
In another aspect, the present invention further provides a means for holding the rotatable tool retention device in a plurality of stationary positions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of one embodiment of the present invention.
FIG. 1 a is a top plan view of the base plate of one aspect of the present invention.
FIG. 2 is a top view of the frame/handle of the present invention.
FIG. 3 is a front view of the frame/handle of the present invention.
FIG. 4 is a perspective view of a preferred embodiment of the present invention.
FIG. 5 is a perspective view of an alternate embodiment of the present invention.
FIG. 6 is a perspective view of an alternate preferred embodiment of the present invention.
FIG. 7 is a perspective view of a most preferred embodiment of the present invention.
FIG. 8 is a perspective view of a detail of a preferred embodiment of the invention shown in FIG. 4 .
FIG. 9 is a front view of the preferred embodiment of the invention as shown in FIG. 4 .
FIG. 10 is a perspective view of the preferred embodiment of the invention as shown in FIG. 4 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention will be better understood by the following detailed description of the invention and with reference to the drawings.
Now referring to FIG. 1, the organizer 2 comprises frame 10 and tool mounting assembly 30 .
Now referring to FIGS. 1, 2 and 3 , frame 10 typically comprises uprights 12 and 14 and base 16 . Frame 10 can comprise any suitable material such as wood, metal, or fiberglass but is preferably formed of tube steel. Base 16 may further comprise openings 19 formed therein to facilitate mounting the base to a workbench, floor, wall or the like by means of bolting or the like.
Now referring to FIGS. 2 and 3, base 16 preferably further comprises knurling 18 to facilitate carrying. The length of uprights 12 and 14 are preferably approximately equivalent and should be of sufficient length to allow rotation of the tool mounting assembly 30 with an additional five to six inches to allow for socket and tool clearance.
Now referring to FIG. 1, tool mounting assembly 30 comprises an elongated member comprising two ends 90 and 92 connected by at least one longitudinal piece 94 said ends 90 and 92 each further comprising engagement means 98 and 100 for connecting tool mounting assembly 30 to frame 10 such as but not limited to cross members which may be fastened to said frame 10 by any suitable means known to one skilled in the art such as but not limited to by a bolt, screw or the like. Engagement means 98 and 100 may comprise cross members as shown in FIG. 1 and 4 - 7 or may comprise a sheet of material as shown in FIG. 10 . In a preferred embodiment the means for connecting tool mounting assembly 30 to frame 10 are cross members 98 and 100 which further comprise a means for providing an axis of rotation for the tool mounting assembly 30 which is rotatably mounted between the uprights 12 and 14 of frame 10 .
Tool mounting assembly 30 further comprises multiple tool receiving faces 32 , 34 , 36 and 38 for accommodating tools, tool retention means and/or tool organizers. For example, now referring to FIG. 4, the tool receiving faces 32 and 34 (shown in ghost), accommodate a plate 60 to which tool retention means comprising clips 62 such as but not limited to spring clips are mounted. The clips 62 in turn secure other tools such as ratchets, wrenches or screwdrivers. The tool retention means such as clips 62 are attached to the tool receiving faces by any means known in the art such as but not limited to magnetic attachment, nut and bolt attachment, rivets, spring clips and the like. In another example, as best seen in FIG. 4, tool receiving faces 36 and 38 further comprise openings 39 formed therein and accommodate strips 64 comprising retaining clips 66 . Strips 64 are attached to receiving faces 36 and 38 by screws 70 received in opening 39 . Openings 39 may be formed in any of the tool receiving faces 32 , 34 , 36 and 38 . The embodiments shown in FIGS. 1 and 4 are not meant to limit the invention but are merely exemplary. For example, the tool receiving faces shown are 32 , 34 , 36 and 38 which are visible because of the perspective view. Not visible from FIGS. 1 and 4 are further tool receiving faces hidden from view. It is obvious to one skilled in the art that the remaining faces of the four-sided embodiment shown in FIGS. 1 and 4 comprise tool receiving faces.
Now referring to FIGS. 1 and 4 - 7 , tool mounting assembly 30 preferably is rotatable within uprights 12 and 14 . The means for mounting said tool mounting assembly 30 to frame 10 is by any known rotatable mounting means such as but not limited to a rotation pin 120 extending from either end of said tool mounting assembly 30 into openings 80 and 82 formed in said uprights 12 and 14 . As best seen in FIGS. 5-7, pin 120 may extend through tool mounting assembly 30 . Alternatively, pins (not shown) may be mounted on said uprights 12 and 14 and extend into openings formed in the ends of said tool mounting assembly 30 . Such pins may be spring loaded to accommodate removal and installation of said tool mounting assembly 30 onto said frame 10 .
As best seen in FIGS. 5 and 6, in a most preferred embodiment the rotatable attachment in the present invention is effected by a pin 120 rotatably engaged to the frame 10 parallel to the base 16 of the frame 10 . The pin 120 provides a rotation axis for the tool mounting assembly 30 .
In another embodiment, as best seen in FIGS. 8 and 9, the rotation pin 120 preferably comprises a retaining means for impeding side to side movement of the tool mounting assembly 30 on frame 10 . Suitable retaining means are depressions 122 formed on pin 120 outside of said tool mounting assembly 30 , retaining rings, cotter pins and the like as will be obvious to one skilled in the art.
Now referring to FIGS. 4, 8 and 9 , the present invention may further comprise a means for holding the rotatable tool mounting assembly in a static position such as but not limited to anti-rotation pin 150 that is manually releasable for releasing the rotatable tool mounting assembly 30 to freely rotate and engagable such as to opening 99 formed in cross member 98 for locking the tool mounting assembly 30 to impede rotation. As best seen in FIG. 10, it is contemplated that engagement means 98 may have multiple openings 99 formed therein for accommodating anti-rotation pin 150 .
Now referring to FIGS. 1 and 1 a , base plate 40 provides a means to stand said organizer in an upright position if said organizer is not attached to a floor, a bench or a work piece such as but not limited to by bolting, vise grip, C-clamp or the like. Base plate 40 typically comprises a flat plate forming a stable surface, said plate having on one side a retaining means 42 for removably retaining said frame 10 . As best seen in FIGS. 1, 4 , 5 and 6 , the retaining means 42 for removably accepting said frame 10 may comprise any means known in the art such as but not limited to a channel comprising two parallel strips 44 and 46 extending perpendicularly from said plate sufficiently spaced to securably accept base 16 of frame 10 . Base plate 40 may further comprise tube steel. Though not shown, retaining means 42 may comprise latches, clips or other means well known in the art.
Now referring to FIG. 7, in a most preferred embodiment frame 10 and base plate 40 are integral, base plate 40 comprising feet 48 . As shown in FIGS. 1 and 7, knurling 18 may be provided on base 16 to facilitate carrying the tool mounting assembly 30 .
Now referring to FIGS. 5 and 6, tool mounting assembly 30 can comprise several embodiments. Now referring to the embodiment in FIG. 5, the embodiment in tool mounting assembly 30 comprises an elongated member comprising two substantially identical three dimensional substantially geometrically shaped (in FIG. 5, triangles) ends 90 and 92 connected by longitudinal pieces 94 and 96 , said ends having cross members 98 and 100 , respectively, disposed therein and an axis of rotation formed by the rotatable attachment of the tool mounting assembly 30 to the frame 10 disposed in said cross members 98 and 100 .
Now referring to FIG. 6, in another embodiment tool mounting assembly 30 is elongated and comprises pentagonal ends 90 and 92 . As is obvious to one skilled in the art, the tool mounting assembly can have end pieces that are polygonal or circular. Other geometric forms such as hexagons, etc. are contemplated by the present invention, it being obvious to one skilled in the art that the form of the invention is dictated in part by the items to be mounted. The frame 10 is optimally deep enough to allow rotation of the tool mounting assembly 30 with an additional 5-6 inches to allow for socket and tool clearance.
The dimension of the present invention can vary from about 6 inches to about 30 inches in length, about 6 inches to about 30 inches in width and about 6 inches to about 30 inches in height. In a most preferred embodiment, the present invention is 11 inches in length, 9 inches in width and 14.5 inches in height and is fabricated of steel.
While the invention has been described by reference to specific embodiments, this is for illustrative purposes only. Various modifications to the above invention will become apparent to those skilled in the art, all of which are intended to fall within the spirit and scope of the present invention. All patents and publications referred to herein are hereby incorporated by reference.
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A tool organizer and carrying apparatus comprises a rotatable tool mounting assembly having multiple tool receiving surfaces mounted on a frame. The invention preferably comprises a removable base plate to allow for stable placement on a flat surface such as a workbench or shop floor. The frame provides an axis of rotation for the tool mounting assembly to provide a worker fingertip access to tools mounted thereon. Tools such as sockets are retained on multiple tool receiving surfaces with clips, magnets, nuts and bolts and/or other known retention means for easy removal and replacement. The frame is adaptable to mount the organizer on a base or to a workbench, tool chest or the like and further comprises a means for carrying the organizer.
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BACKGROUND OF THE INVENTION
The manufacture of glass-ceramic articles involves three fundamental steps: first, a glass-forming batch, normally containing a nucleating agent, is melted; second, the melt is cooled at a sufficiently rapid rate that a glass body is formed which is essentially free of crystals; and, third, the glass body is exposed to a characteristic heat treatment procedure to cause crystallization in situ to take place.
Customarily, the third or crystallization step is performed in two parts. Thus, the glass body is initially heated to a temperature slightly above the transformation range thereof to cause the development of nuclei in the glass body which provide sites for the subsequent growth of crystals. Thereafter, the nucleated glass body is heated to a higher temperature, commonly above the softening point of the glass, to effect the growth of crystals on the nuclei.
The crystallization in situ mechanism leads to the substantially simultaneous growth of crystals on countless nuclei. Accordingly, a glass-ceramic article conventionally consists of uniformly fine-grained crystals randomly oriented, but homogeneously dispersed, throughout a residual glassy matrix. Normally, a glass-ceramic article is highly crystalline, i.e., at least 50% and frequently in excess of 75% by volume crystalline. This high crystallinity dictates that the physical properties exhibited by a glass-ceramic article are more nearly similar to those of the crystals than to those of the glassy phase. Furthermore, the composition of, and consequently the physical properties of, the residual glassy matrix are far removed from those of the parent or precursor glass since the constituents comprising the crystal phase will have been extracted therefrom. Finally, the crystallization in situ mechanism provides articles which are free from voids and non-porous.
U.S. Pat. No. 2,920,971 initiated glass-ceramic technology and reference is hereby made to that patent for a more detailed discussion of the microstructure, physical properties, and the method for making such articles.
U.S. Pat. No. 3,582,385 describes glass-ceramic bodies exhibiting good dimensional stability up to temperatures of about 800° C. The bodies had compositions consisting essentially, by weight on the oxide basis, of 3.5-5% Li 2 O, 2.5-5% BaO, 15-21% Al 2 O 3 , 65-75% SiO 2 , and 3.5-8% of a nucleating agent composed of 3-8% TiO 2 and 0-3% ZrO 2 , the sum of Li 2 O, BaO, Al 2 O 3 , SiO 2 , TiO 2 , and ZrO 2 constituting at least 98% of the full composition. Beta-spodumene solid solution comprised the primary crystal phase with a minor amount of celsian. Oxides such as MgO, ZnO, and B 2 O 3 were preferably absent from the compositions because their presence led to the formation of secondary crystal phases having varying solid solubility with beta-spodumene. For example, the inclusion of MgO might lead to the growth of such secondary crystal phases as spinel, cordierite, and/or cristobalite either during the crystallization heat treatment or, more significant from a product standpoint, during subsequent prolonged exposures of the body to high temperatures. Cristobalite is a high expansion form of silica which often develops along with cordierite in thermally unstable, magnesia-containing, beta-spodumene solid solution glass-ceramic articles. The density changes that can accompany the growth of such phases will be reflected in overall dimensional instability of the article at elevated temperatures. The combined development of cordierite and cristobalite is particularly undesirable and will result in elongations of several thousand parts per million after relative brief exposures to a temperature of 950° C. Strains of that level far exceed the strain tolerance of the bodies when utilized as fine-bore honeycombs in regenerative heat exchanger applications.
Ser. No. 578,379, filed May 19, 1975 by the present applicant, now U.S. Pat. No. 4,042,403, is also directed to glass-ceramic bodies demonstrating excellent high temperature dimensional stability. The operable compositions consist essentially, by weight on the oxide basis, of about 3-5% Li 2 O, 0.25-2.5% MgO, 15-20% Al 2 O 3 , 68-75% SiO 2 , and 2.5-5% TiO 2 with, optionally, up to 3% ZrO 2 . A vital facet of the composition involves maintaining a molar ratio Li 2 O:MgO of at least 2:1. Beta-spodumene solid solution comprises the principal and, sometimes, sole crystal phase with anatase and/or rutile frequently composing a secondary crystal phase. The Li 2 O:MgO ratio is critical in assuring the absence of the development of cordierite and/or cristobalite as an extraneous crystal phase.
SUMMARY OF THE INVENTION
I have found that glass-ceramic bodies exhibiting average coefficients of thermal expansion (0°-1000° C.) of less than about 20 × 10 -7 /° C. and total elongations after 1000 hours at 950° C. of less than about 750 parts per million (PPM) can be produced wherein beta-spodumene solid solution (s.s.) constitutes the primary crystal phase but which also contain substantial amounts of mullite (3Al 2 O 3 .2SiO 2 ) and/or corundum (Al 2 O 3 ) along with ZrTiO 4 s.s. and, occasionally, ZrO 2 s.s. as secondary crystal phases. The precursor glasses consist essentially, in weight percent on the oxide basis, of 3.7-7.5% Li 2 O, 18.5-33% Al 2 O 3 , 55-75% SiO 2 , and 3.4-5.0% RO 2 , wherein RO 2 consists of 1.5-2.5% TiO 2 and 1-2.7% ZrO 2 in a molar ratio TiO 2 :ZrO 2 between about 3:1-1:1.
Nucleation through a combination of TiO 2 + ZrO 2 is vital to secure the desired minor phase assemblage and fine-grained microstructure. TiO 2 alone is less efficient as a nucleating agent on a molar equivalent basis than the combination of TiO 2 + ZrO 2 . Furthermore, and most importantly, nucleation with TiO 2 alone fosters the development of Al 2 TiO 5 , particularly when As 2 O 3 is present. After extended exposure at elevated temperatures, Al 2 TiO 5 decomposes to rutile (TiO 2 ) and corundum. Such decomposition, which is also augmented by the presence of arsenic (conventionally employed as a fining agent for glass compositions of the present type), can lead to extreme dimensional instability upon prolonged operation of the glass-ceramic at high temperatures. Nucleation with ZrO 2 alone is impractical because of the very limited solubility thereof in the instant glass compositions. Moreover, ZrO 2 alone is a comparatively inefficient nucleating agent up to at least the 3% by weight level. Such amounts would require melting temperatures far in excess of those conventionally utilized with precursor glasses for glass-ceramics.
The inclusion of arsenic not only accelerates the formation of Al 2 TiO 5 when crystallization in situ of the glass is carried out at high temperatures, e.g., 1200°-1300° C., but also accelerates its subsequent decomposition into rutile and corundum when the crystalline article is used in applications involving operating temperatures of about 800°-950° C. This paradox may be rationalized if it is assumed that As +3 ions concentrate in the glassy phase which exists along the grain boundaries or within grain boundary nodes of the initial polycrystalline array of beta-spodumene s.s. crystallites. It is conjectured that As +3 ions soften the glassy phase to allow more rapid diffusion of Al +3 or Ti +4 ions, whichever are the more mobile. Faster diffusion would permit a more rapid approach to equilibrium of the reaction
Al.sub.2 O.sub.3 + TiO.sub.2 ⃡ Al.sub.2 TiO.sub.5
at any given temperature.
Where TiO 2 is utilized alone as the nucleating agent, it is possible to develop mullite as a minor phase rather than Al 2 TiO 5 , but only within very narrow compositional limits. Mullite will be formed as a minor phase in compositions of the type Li 2 O.mAl 2 O 3 .nSiO 2 :XTiO 2 :YAs 2 O 3 wherein m ≧ 1.2, n ≧ 7, X ≦ 3.8 mole percent, and Y ≦ 0.2 mole percent, but preferably zero. TiO 2 at the 3.8 mole percent level is near the lower limit consistent with the formation of a fine-grained beta-spodumene glass-ceramic, but cracking of the article during the crystallization treatment is commonplace. Where TiO 2 is present at about the 4.1 mole percent level, mullite and Al 2 TiO 5 are formed with about equal probability. Either or both may be present, even in the absence of As 2 O 3 , but breakage still remains a problem, however. Fracture of the article is essentially eliminated with TiO 2 contents of at least about 4.4 mole percent, but at such concentrations Al 2 TiO 5 develops to the substantial exclusion of mullite.
The use of a combination of TiO 2 + ZrO 2 for nucleation results in a series of solid solutions depending upon the TiO 2 :ZrO 2 mole ratio:
______________________________________Mole Ratio Solid Solution______________________________________9:1 Rutile only5.7:1 Rutile + ZrTiO.sub.44:1 ZrTiO.sub.4 + Rutile3:1 ZrTiO.sub.4 + Rutile (trace)1.5:1 ZrTiO.sub.4 only1:1 ZrTiO.sub.4 + ZrO.sub.2______________________________________
These experimentally-determined phase assemblages accord with the predictions set out in the TiO 2 :ZrO 2 binary system (Phase Diagrams for Ceramists, Levin, Robbins, and McMurdie, The American Ceramic Society, Inc., 1964, FIGS. 369-370). In this respect, the combination TiO 2 + ZrO 2 in Li 2 O-Al 2 O 3 -SiO 2 glasses appears to function as a subsystem whose ultimate crystallization products are independent of the other constituents of the composition.
The combination of TiO 2 + ZrO 2 permits the use of low total nucleant contents and promotes the growth of mullite instead of Al 2 TIO 5 . Those objectives are achieved by restricting the molar ratio TiO 2 :ZrO 2 to values between about 3:1 and 1:1. In that range efficient nucleation is effected and ZrTiO 4 solid solution is produced which, by competing effectively with Al 2 O 3 for available TiO 2 , inhibits the development of Al 2 TiO 5 . The excess Al 2 O 3 is then free to combine with SiO 2 to form mullite. In compositions containing low SiO 2 levels, Al 2 O 3 is stable with respect to mullite, thereby in agreement with the prediction of the Li 2 O-Al 2 O 3 -SiO 2 ternary phase diagram regarding the stability region for mullite (Phase Diagrams for Ceramists, Levin, Robbins, and McMurdie, The American Ceramic Society, Inc., 1964, FIG. 449). To insure the virtual absence of Al 2 TiO 5 or of any uncombined TiO 2 or ZrO 2 species, a molar ratio TiO 2 :ZrO 2 of about 3:2 is preferred.
Minor amounts (up to 1.5%) of MgO can be substituted on a molar basis for Li 2 O, as described in Ser. No. 578,379, supra. That is, a molar ratio Li 2 O:MgO of at least 2:1 must be maintained. The inclusion of MgO aids in avoiding cracking during the crystallization step and, at the low levels employed and when substituted for Li 2 Oin the proper molar ratio, does not cause the development of cordierite (2MgO. 2Al 2 O 3 .5SiO 2 ) during the crystallization step or after extended exposure of the glass-ceramic to high temperatures.
The inclusion of ZnO also assists in inhibiting cracks during the crystallization but it must be avoided since its presence results in the formation of gahnite (ZnO.Al 2 O 3 ), a reversible phase having a solubility which varies as a function of time and temperature, thereby fostering dimensional instability.
In general, the preferred compositions will consist essentially solely of Li 2 O, Al 2 O 3 , SiO 2 , TiO 2 , and ZrO 2 in the proper proportions to assure excellent long term thermal stability. However, the addition of a minor amount of MgO can be practically useful as a melting aid and a mineralizer. A molar ratio Al 2 O 3 /(Li 2 O + MgO) will be maintained between about 1.2-1.5 to insure the development of the desired mullite and/or corundum phases.
The process of the invention comprehends melting a properly-defined batch for the precursor glass. The melt is simultaneously cooled to a temperature at least within the transformation range (optionally to room temperature) and a glass article of a desired configuration shaped therefrom. The glass article is heated to a temperature between about 1150°-1350° C. to effect the crystallization in situ. Customarily, the crystallization step will be divided into two parts. Thus, the glass article will initially be heated to temperatures between about 750°-950° C. to induce nucleation, after which the temperature will be raised to 1150°-1350° C. This preferred practice results in a glass-ceramic having a more uniformly fine-grained microstructure. [The transformation range has been defined as that temperature at which a molten mass is transformed into an amorphous solid and is conventionally deemed to lie in the vicinity of the annealing point of a glass.]
The glasses of the invention nucleate very rapidly. Therefore, particularly where thin-walled glass tubing is the product configuration, nucleation periods of no more than about 15 minutes can be adequate. However, much longer nucleation times can be employed, e.g., up to 12 hours, with no harm to the final microstructure. As a matter of fact, some crystallization may proceed with such long dwell periods within the nucleation range. Nevertheless, such long nucleation periods are not viewed with favor from a commercial point of view inasmuch as the microstructure of the glass-ceramic is not significantly different from that obtained with a shorter nucleation period. Thus, a nucleation period of about six hours has been deemed to be a practical maximum.
Also, the growth of crystals can be very rapid, especially when undertaken at the upper extreme of the operable crystallization range. For example, a highly crystalline article can be secured after only one hour heat treatment. However, to insure the optimum dimensional stability in the final product, longer exposures will customarily be utilized to accomplish substantially total crystallization. Nonetheless, whereas much longer crystallization periods can be successfully employed, commercial practice has equated an exposure of about 24 hours to be a practical maximum.
In the laboratory examples tabulated below, the molten glass-forming batches were shaped into articles and cooled to ambient or room temperature to permit the inspection of glass quality. That practice is not required and, where speed of production and fuel economics are uppermost, the melts will only be cooled to a temperature at least within, and preferably slightly below, the transformation range to form a glass body. Thereafter, the glass body will be reheated to promote nucleation and crystallization. Finally, whereas the laboratory heat treating schedules reported below contemplated explicit dwell periods at specific temperatures, such practice must be recognized as illustrative only and as a matter of convenience, rather than a limitative. Thus, no hold periods as such are necessary to the operability of the invention. The sole requirement is that the glass article be subjected to temperatures within the 1150°-1350° C. interval.
The dimensional stability of those glass-ceramics having relatively high SiO 2 contents appears to be somewhat improved when crystallization temperatures within the upper extreme of the range are used. However, such high temperatures can have a deleterious effect on compositions of lower SiO 2 content. Thus, a coarse-grained body of poor dimensional stability can result therefrom.
DESCRIPTION OF PREFERRED EMBODIMENTS
Table I records a group of thermally crystallizable glass compositions expressed in weight percent on the oxide basis. The actual batch components can comprise any materials, either the oxides or other compounds, which, when melted together with the other batch ingredients, are converted to the desired oxide compositions in the proper proportions. The molar ratios TiO 2 :ZrO 2 and Li 2 O:MgO are also tabulated. The batch ingredients were compounded, ballmilled together to assist in obtaining a homogeneous melt, and then deposited into clean platinum crucibles. After covering, the crucibles were moved to a furnace operating at 1550° C. and held thereat for 4 hours. The temperature was then raised to 1650° C. to increase the fluidity of the melt and maintained at that temperature for 16 hours to alter the As +3 :As +5 ion ratio for improved fining of the glass. Thereafter, the melts were poured into steel molds to yield slabs about 12 inches × 4 inches × 1/2 inch, and the slabs immediately transferred to an annealer operating at about 500° C.
That low annealing temperature was employed to cool the slabs sufficiently rapidly through the region of crystallization to avoid premature devitrification, especially on the glass face in contact with the pouring surface or the surface of the annealer. However, the cooling through the annealing range is carried out at a rate slow enough to avoid spontaneous breakage in the annealer or when the slab is cut or sawed.
Glass bars about 4 inches × 1 inch × 0.5 inch were cut from the annealed slabs for exposure to the crystallization heat treatment and subsequent physical property measurements.
As 2 O 3 was included to perform its conventional function as a fining agent.
TABLE I__________________________________________________________________________ 1 2 3 4 5 6 7 8 9__________________________________________________________________________SiO.sub.2 56.8 56.6 58.0 60.2 63.3 66.1 65.9 65.8 64.3Al.sub.2 O.sub.3 32.1 32.0 31.1 29.2 26.9 24.9 24.9 24.8 26.7Li.sub.2 O 7.1 6.1 6.8 5.6 5.9 5.5 5.5 5.5 5.3MgO -- 1.3 -- 1.2 -- -- -- -- --TiO.sub.2 1.9 1.9 1.9 1.8 1.8 1.8 1.8 1.5 1.7ZrO.sub.2 1.9 1.9 2.0 1.9 1.9 1.8 1.8 2.3 1.8As.sub.2 O.sub.3 0.2 0.2 0.3 0.2 0.2 -- 0.2 0.3 0.3TiO.sub.2 :ZrO.sub.2 3:2 3:2 3:2 3:2 3:2 3:2 3:2 1:1 3:2Li.sub.2 O:MgO -- 6.5:1 -- 6.5:1 -- -- -- -- -- 10 11 12 13 14 15 16 17 18__________________________________________________________________________SiO.sub.2 65.7 65.5 65.6 68.7 68.5 71.2 61.9 61.7 60.2Al.sub.2 O.sub.3 24.8 24.7 24.7 22.2 22.1 20.1 28.0 27.9 30.0Li.sub.2 O 4.7 4.7 4.4 4.2 4.2 3.8 6.2 6.1 6.0MgO 1.0 1.0 1.5 0.9 0.9 0.8 -- -- --TiO.sub.2 1.8 1.9 1.8 1.8 2.0 1.9 2.0 1.6 1.9ZrO.sub.2 1.8 2.0 1.8 1.9 2.1 2.0 2.0 2.5 2.0As.sub.2 O.sub.3 0.2 0.2 0.3 0.3 0.2 0.2 -- -- --TiO.sub.2 :ZrO.sub.2 3:2 3:2 3:2 3:2 3:2 3:2 3:2 1:1 3:2Li.sub.2 O:MgO 6.5:1 6.5:1 4:1 6.5:1 6.5:1 6.5:1 -- -- -- 19 20 21 22 23 24 25 26__________________________________________________________________________SiO.sub.2 68.4 68.6 69.2 71.8 71.1 73.0 69.1 67.6Al.sub.2 O.sub.3 22.1 22.2 20.9 20.3 20.1 18.6 22.6 21.9Li.sub.2 O 4.9 4.9 4.6 4.5 4.4 4.5 5.0 4.8TiO.sub.2 2.1 1.7 2.5 1.7 2.1 1.9 1.6 2.8ZrO.sub.2 2.1 2.7 2.5 1.7 2.2 2.0 1.6 2.9As.sub.2 O.sub.3 0.4 -- 0.4 -- -- -- 0.1 --TiO.sub.2 :ZrO.sub.2 3:2 1:1 3:2 3:2 3:2 3:2 3:2 3:2Li.sub.2 O:MgO -- -- -- -- -- -- -- --__________________________________________________________________________
Exemplary composition 26, containing over 5.0% by weight TiO 2 + ZrO 2 , showed considerable devitrification and dicing upon cooling from the melt and, therefore, was considered unsuitable for the instant invention.
Table II reports nine different heat treatments conducted in electrically-fired furnaces which were applied to the glass bars cut from the slabs of Table I. As is recited therein, each schedule comprehended heating the bar from room temperature (R.T.) to the nucleation range at 200°-300° C./hour. It will be recognized that slower or more rapid rates are operable where very thick or very thin-walled articles, respectively, are being treated. Moreover, the 200°-300° C./hour rate of temperature rise has been found to be satisfactory with a large number of article geometries in precluding thermal breakage.
Crystallization of the glass body takes place more rapidly as the temperature thereof is increased. Hence, the glass body is commonly raised to a temperature above its softening point to promote crystallization. Nevertheless, a balance must be maintained between the rate of temperature increase at which the glass body approaches and exceeds the softening point thereof, and the rate at which crystals are developing therein. For example, in the first stages of crystallization, the proportion of crystals to glassy matrix is so low that the article will deform quite readily as the softening point of the glass is approached. The use of formers or other means of physical support can be utilized to reduce this effect. The use of a substantial nucleation period enhances the rate of subsequent crystal growth, thereby also acting to reduce thermal deformation of the glass. In summary, the rate at which the temperature is raised will, desirably, balance the rate at which crystal growth takes place within the glass with the necessary degree of fluidity in the residual glass required to inhibit stress buildup and cracking. A heating rate of up to about 200° C./hour from the nucleation temperatures into the crystallization range has produced sound, essentially deformation-free articles in the majority of cases.
The rate at which the crystallized article can be cooled to room temperature from the crystallization range without damage from thermal shock is dependent upon the coefficient of thermal expansion of the article and the thickness dimensions thereof. Since the crystallized articles of the present invention exhibit very low coefficients of thermal expansion, viz., less than 20 × 10 -7 /° C. over the range of 0°-1000° C., thin-walled articles can simply be removed from the furnace into the ambient environment. As a matter of convenience, the crystallized bars were merely left in the furnace at the conclusion of the heat treatment schedule, the electric current to the furnace shut off, and the bars permitted to cool to room temperature at furnace rate, which was estimated to range about 3°-5° C./minute.
TABLE II______________________________________Schedule No. Heat Treatment______________________________________A Heat at 300° C./hour to 750° C. No hold at 750° C. Heat at 25° C./hour to 850° C. No hold at 850° C. Heat at 200° C/hour to 1200° C. Hold at 1200° C. for 12 hoursB Heat at 300° C./hour to 750° C. No hold at 750° C. Heat at 25° C./hour to 950° C. No hold at 950° C. Heat at 200° C./hour to 1225° C. Hold at 1225° C. for 24 hoursC Heat at 300° C./hour to 750° C. No hold at 750° C. Heat at 17° C./hour to 850° C. No hold at 850° C. Heat at 200° C./hour to 1250° C. Hold at 1250° C. for 12 hoursD Heat at 300° C./hour to 750° C. No hold at 750° C. Heat at 25° C./hour to 850° C. No hold at 850° C. Heat at 200° C./hour to 1250° C. Hold at 1250° C. for 12 hoursE Heat at 300° C./hour to 750° C. No hold at 750° C. Heat at 25° C./hour to 850° C. No hold at 850° C. Heat at 200° C./hour to 1300° C. Hold at 1300° C. for 12 hoursF Heat at 200° C./hour to 800° C. Hold at 800° C. for two hours Heat at 67° C./hour to 1000° C. No hold at 1000° C. Heat at 200° C./hour to 1250° C. Hold at 1250° C. for 16 hoursG Heat at 200° C./hour to 750° C. Hold at 750° C. for four hours Heat at 200° C./hour to 1300° C. Hold at 1300° C. for 16 hoursH Heat at 200° C./hour to 850° C. Hold at 850° C. for four hours Heat at 200° C./hour to 1300° C. Hold at 1300° C. for 16 hoursI Heat at 200° C./hour to 850° C. Hold at 850° C. for two hours Heat at 200° C./hour to 1000° C. Hold at 1000° C. for two hours Heat at 200° C./hour to 1300° C. Hold at 1300° C. for 16 hours______________________________________
Table III reports the heat treatment schedules applied to the bar specimens of each member of Table I along with the crystal phases present, as identified through X-ray diffraction analysis, a qualitative appraisal of the grain size of the microstructure, the coefficient of thermal expansion over the range 0°-1000° C. (×10 -7 /° C.), and the change in length (ΔL/L in PPM) after being heated for 500 and 1000 hours at 950° C., and, in the case of Examples 22-24, after 2000 hours at 950° C., as measured by means of a length comparator of the type described by Wilmer Souder and Peter Hidnet, "Measurement of Thermal Expansion of Fused Silica", Scientific Papers of the Bureau of Standards, Vol. 21, Pages 1-23, Sept. 21, 1965. A designation of "poor" in Table III indicates elongations greater than 750 PPM.
The articles appeared to be highly crystalline, i.e. greater than 75% by volume crystalline, with beta-spodumene solid solution (s.s.) constituting at least 75% of the total crystallinity. In table III, the secondary phases are recorded in the order of amount present. In the finegrained samples, substantially all of the crystals were smaller than five microns in diameter with the great majority being less than one micron in diameter. The crystallized articles exhibited a densely-opaque, white appearance.
Whereas the classic formula for beta-spodumene is Li 2 O.Al 2 O 3 .4SiO 2 , the composition of the crystal phase in the glass-ceramic articles of the present invention does not conform exactly to that formula. Instead, it is more in the nature of a solid solution corresponding generally to the formula Li 2 O.Al 2 O 3 .nSiO 2 , where "n " can vary between about 3.5-10, depending upon the silica content of the precursor glass. There is also evidence that magnesium ions can also be incorporated into the crystal structure. However, an X-ray diffraction analysis invariably yields a pattern characteristic of beta-spodumene. Accordingly, that is the sense in which the expression "beta-spodumene solid solution" is employed in Table III.
TABLE III__________________________________________________________________________ Heat Treatment Grain ΔL/L ΔL/LExample No. Schedule Size Crystal Phases Exp. Coef. 500 hrs. 1000 hrs.__________________________________________________________________________1 A Fine Beta-spodumene s.s 15.6 -142 -- Corundum, ZrTiO.sub.4 s.s1 B " " 16.7 -100 -1701 D " " 18.0 -75 --1 E Coarse " 12.9 Poor --2 C Medium " 15.1 -111 -1923 C Fine " 15.2 -161 -2384 C " Beta-spodumene s.s 17.1 -83 -206 Mullite, ZrTiO.sub.4 s.s5 C " " 16.2 -147 -3146 C " " 11.5 -255 -3867 A " " 10.5 -357 --7 E " " 12.1 -52 --8 C " Beta-spodumene s.s 11.0 -413 -558 ZrTiO.sub.4 s.s, Mullite, ZrO.sub.2 s.s. 9 C Medium Beta-spodumene s.s., -- -68 -165 Mullite, ZrTiO.sub.4 s.s.10 A Fine " 11.2 -369 Poor10 D " " 11.9 -217 -35510 E " " 12.4 +115 +3811 D " " -- -345 --12 C " " 12.5 -10 -10313 A " " 9.3 Poor --13 D " " 13.0 -400 --13 E " " 9.8 -244 --14 D " " -- -392 --15 A " " 9.6 Poor -- Heat Treatment Grain L/L L/L ΔL/LExample No. Schedule Size Crystal Phases Exp. Coef. 500 hrs. 1000 hrs. 2000__________________________________________________________________________ hrs.15 D Fine Beta-spodumene s.s., 8.9 Poor -- Mullite, ZrTiO.sub.2 s.s15 E " " 9.5 +51 --16 G " " -- -179 -307 --17 G Very Beta-spodumene s.s -- -185 -292 -- fine Mullite, ZrTiO.sub.4 s.s., ZrO.sub.2 s.s.18 F Fine Beta-spodumene s.s. 16.0 -287 -349 -- Mullite, ZrTiO.sub.4 s.s.19 F " " `8.0 -91 +67 --20 F " Beta-spodumene s.s -- -311 -440 -- Mullite, ZrTiO.sub.4 s.s., ZrO.sub.2 s.s.21 G " Beta-spodumene s.s. -- -227 -348 -- Mullite, ZrTiO.sub.4 s.s.22 F " " -- -338 -442 --22 I " " -- +20 -64 -10823 F Fine Beta-spodumene s.s. -- -367 -467 -- Mullite, ZrTiO.sub.4 s.s.23 H " " 5.5 -92 -190 -30124 I " " -- -27 -106 -20225 G Coarse Poor nucleation -- -- -- --26 -- Devitrified and diced when cooled from the__________________________________________________________________________ melt
An inspection of Table III confirms the observation made above that higher temperature heat treatments tend to improve the thermal dimensional stability of higher silica compositions. This is evidenced in Examples 7, 10, 13, and 15. However, high temperature crystallization treatments may not be beneficial with compositions of low silica content, as is demonstrated by the 1300° C. treatment of Example 1 which yielded a course-grained body of poor stability. Nevertheless, the determination of the optimum crystallization schedule for any particular glass composition is well-within the technical competence of the worker or ordinary skill in the glass-ceramic art. Exemplary compositions 22-24, having Li 2 O, Al 2 O 3 , and SiO 2 in a molar ratio of approximately 1:1.33:8 are particularly noteworthy for yielding products exhibiting low coefficients of thermal expansion and excellent high temperature dimensional stability.
In Examples 16-18, the sum of TiO 2 + ZrO 2 totals approximately 2.6 mole percent. At that level, a molar ratio TiO 2 :ZrO 2 of 4:1 provides such inefficient nucleation that course-grained crystallization results. In view of that factor, a molar ratio TiO 2 :ZrO 2 of about 3:1 has been deemed to constitute a practical maximum.
Example 25, containing less than about 3.5% total of TiO 2 +ZrO 2 , exhibits the result of poor nucleation, leading to the development of a coarse-grained body.
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This invention is directed to the production of glass-ceramic articles having compositions within the Li 2 O-Al 2 O 3 -SiO 2 field nucleated with a combination of TiO 2 + ZrO 2 wherein beta-spodumene solid solution constitutes the primary crystal phase. Mullite and/or corundum along with ZrTiO 4 solid solution and, occasionally, ZrO 2 solid solution are present as secondary crystal phases. Because of their low coefficients of thermal expansion and exceptional long time dimensional stability at temperatures up to 1000° C., the compositions can be useful in applications where extreme changes in temperature are experienced; for example, the construction of honeycomb structures used in regenerative heat exhchangers for turbine engines.
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RELATED APPLICATION
Related subject matter is disclosed in U.S. patent application Ser. No. 09/591,080 filed on Jun. 9, 2000, entitled Method of Determining Time Delay for Round-Trip Transmission of Data and Electronic Apparatus Therefor assigned to the same assignee hereby incorporated by reference.
FIELD OF THE INVENTION
This invention relates, in-general, to data transmission, and more particularly, to methods of determining real-time data latency and apparatuses therefor.
BACKGROUND OF THE INVENTION
A user accessing a computer server across a computer network must transmit data across the computer network from the user's computer to the computer server and must also receive data across the computer network from the computer server to the user's computer. Therefore, the user requires fast data transmission rates across the computer network and requires, in particular, fast round-trip data transmission across the computer network. However, as computer networks continuously grow in size and complexity, the data transmission rates associated with the larger and more complex computer networks may decrease. Accordingly, a need exists for a method of determining real-time data latency and an apparatus therefor.
SUMMARY OF THE INVENTION
In accordance with the principles of the invention, a method of determining real-time data latency can include transmitting a first plurality of data packets, each having a first packet group identification (PGID) and a time stamp, receiving a set of data packets, identifying PGIDs in the set of data packets, identifying time stamps in the set of data packets, using the time stamps to determine time delays for the set of data packets, comparing the time delays of the set of data packets having the first PGID to a first minimum time delay, comparing the time delays of the set of data packets having the first PGID to a first maximum time delay, summing a number of data packets in the set of data packets having the first PGID as a first total count, and summing the time delays of the set of data packets having the first PGID as a first total time delay.
Further, in accordance with the principles of the invention; an electronic apparatus for determining real-time data latency can include a data packet reception portion, a data packet signature verification portion coupled to the data packet reception portion, a data packet validity verification portion coupled to the data packet reception portion, a data packet packet group identification (PGID) identification portion coupled to the data packet reception portion, a statistic array retrieval portion coupled to the data packet signature verification portion, the data packet validity verification portion, and the data packet PGID identification portion, a time delay determination and statistics portion coupled to the statistic array retrieval portion and the data packet reception portion, and a statistic array storage portion coupled to the time delay determination and statistics portion and the data packet PGID identification portion.
BRIEF DESCRIPTION OF THE DRAWING
The invention will be better understood from a reading of the following detailed description, taken in conjunction with the accompanying drawing figures in which:
FIG. 1 illustrates a block diagram of an electronic apparatus for determining real-time data latency in accordance with an embodiment of the invention;
FIG. 2 illustrates a flow chart for a method of determining real-time data latency in accordance with an embodiment of the invention;
FIGS. 3 through 6 illustrate flow charts of detailed portions of the method of FIG. 2 in accordance with an embodiment of the invention; and
FIG. 7 illustrates a graph of the statistics generated by the method of FIG. 2 in accordance with an embodiment of the invention.
For simplicity and clarity of illustration, the same reference numerals in different figures denote the same elements, and descriptions and details of well-known features and techniques are omitted to avoid unnecessarily obscuring the invention.
Furthermore, the terms first, second, third, fourth, and the like in the description and in the claims, if any, are used for distinguishing between similar elements and not necessarily for describing a sequential or chronological order. However, it is understood that the embodiments of the invention described herein are capable of operation in other sequences than described or illustrated herein. It is further understood that the terms so used are interchangeable under appropriate circumstances.
DETAILED DESCRIPTION
FIG. 1 illustrates a block diagram of a portion of an electronic apparatus 100 for determining real-time data latency. Apparatus 100 includes a data packet reception portion 110 , a data packet signature verification portion 120 , a data packet validity verification portion 130 , a data packet Packet Group IDentification (PGID) identification portion 140 , a statistic array retrieval portion 150 , a time delay determination and statistics portion 160 , a statistic array storage portion 170 , and a memory portion 180 . Data packet reception portion 110 is coupled to data packet signature verification portion 120 , data packet validity verification portion 130 , data packet PGID identification portion 140 , and time delay determination and statistics portion 160 . Statistic array retrieval portion 150 is coupled to data packet signature verification portion 120 , data packet validity verification portion 130 , data packet PGID identification portion 140 , time delay determination and statistics portion 160 , and memory portion 180 . Statistic array storage portion 170 is coupled to time delay determination and statistics portion 160 and memory portion 180 . In the preferred embodiment, memory portion 180 is a Dynamic Random Access Memory (DRAM). Also in the preferred embodiment, data packet reception portion 110 , data packet signature verification portion 120 , data packet validity verification portion 130 , data packet PGID identification portion 140 , statistic array retrieval portion 150 , time delay determination and statistics portion 160 , and statistic array storage portion 170 are located within a Field Programmable Gate Array (FPGA), as indicated by a dashed line 190 in FIG. 1 .
A general description of the operation of apparatus 100 is as follows. Data packet reception portion 110 receives incoming data packets from a computer network. Data packet signature verification portion 120 verifies signatures in the received data packets. Data packet validity verification portion 130 verifies a validity of the received data packets. Data packet PGID identification portion 140 identifies PGIDs in the received data packets. Statistic array retrieval portion 150 retrieves statistics stored in memory portion 180 . Time delay determination and statistics portion 160 determines time delays for the received data packets, compares the time delays to the stored statistics, and, if necessary, updates the statistics. Statistic array storage portion 170 stores the updated statistics in memory portion 180 . A more detailed description of the operation of apparatus 100 is described with reference to the subsequent drawing figures.
FIG. 2 illustrates a flow chart for a method 200 of determining real-time data latency. At a step 205 of method 200 , data packets are created by a first electronic apparatus. Each data packet has a time stamp indicating a time when the data packet is transmitted from or out of the first electronic apparatus. Each data packet also includes a signature located at a signature offset within the data packet. The signature offset is the same for all data packets. As an example, the signature can be a unique string of 32 bits indicating that the data packet was transmitted from the first electronic apparatus. Each data packet has a size that is within a predetermined range. In the preferred embodiment for Ethernet networks, the minimum size for any data packet is 64 Bytes, and the maximum size for any data packet is 1518 Bytes. The data packets can have other sizes for non-Ethernet networks.
The data packets are grouped into one or more sets. Each data packet within a particular group or set has a PGID that is unique to that particular group and is different from the PGIDs of other data packets in other groups. The PGID can be a user-defined unique string of 16 bits. As an example, the PGIDs can represent different Internet Protocol (IP) addresses, different IP priorities, different data packet sizes, or different protocol mixes. The PGID within each data packet is located at a PGID offset within the data packet. The PGID offset is the same for all data packets. The PGID offset can be larger than or smaller than the signature offset. Each data packet within a particular group having a particular PGID can have different sizes. As an example, the different sizes may be the result of the data packets having different data patterns.
At a step 210 of method 200 , the first electronic apparatus transmits the data packets out of the first electronic apparatus during a first time period. The data packets are sent to a second electronic apparatus, which receives the data packets. This second electronic apparatus takes portions of the data packets and inserts them into new data packets. As an example, the time stamps of the data packets are inserted into the new data packets. The second electronic apparatus transmits the new data packets back to the first electronic apparatus. Step 210 can be performed continuously during all of the subsequent steps of method 200 .
Next, the first electronic apparatus receives these new data packets during a second time period, which is different from the first time period of step 205 . However, this second time period may overlap the first time period. At a step 215 of method 200 , the first electronic apparatus receives a single one of the new data packets. As an example, data packet reception portion 110 of apparatus 100 in FIG. 1 can perform step. 215 in FIG. 2 .
At a step 220 of method 200 in FIG. 2, the first electronic apparatus verifies or checks the signature in the received data packet of step 215 . Subsequently, at a step 225 of method 200 , the first electronic apparatus verifies or checks the validity of the received data packet of step 215 . The sequence of steps 220 and 225 can be reversed. Details of steps 220 and 225 are provided hereinafter with respect to FIG. 3 and FIG. 4, respectively. As an example, data packet signature verification portion 120 of apparatus 100 in FIG. 1 can perform step 220 in FIG. 2, and data packet validity verification portion 130 of apparatus 100 in FIG. 1 can perform step 225 of FIG. 2 .
At a step 230 in method 200 , the first electronic apparatus identifies a PGID in the received data packet of step 215 . The PGID in the received data packet is located at the same PGID offset as used previously in step 205 . The sequence of steps 220 , 225 , and 230 may be altered or reversed. As an example, data packet PGID identification portion 140 of apparatus 100 in FIG. 1 can perform step 230 in FIG. 2 .
Next, at a step 235 in method 200 , the first electronic apparatus identifies a time stamp in the received data packet of step 215 . Time stamps in the received data packet originates from a time stamp in one of the transmitted data packets of steps 205 and 210 . In other words, the time stamp of the received data packet indicates the time at which the source or original data packet was transmitted from the first electronic apparatus at step 210 . As an example, time delay determination and statistics portion 160 of apparatus 100 in FIG. 1 can perform step 235 in FIG. 2 .
At a step 240 of method 200 , the first electronic apparatus uses the time stamp of the received data packet of step 215 to determine a time delay or latency for the received data packet. In particular, the first electronic apparatus subtracts the time indicated by the time stamp from the time at which the data packet was received by the first electronic apparatus in step 215 . This time delay represents a round-trip time delay for the data packet. As an example, time delay determination and statistics portion 160 of apparatus 100 in FIG. 1 can perform step 240 of FIG. 2 .
At a step 245 of method 200 , the first electronic apparatus updates a set of statistics with the time delay and other statistics from the received data packet. In particular, the first electronic apparatus updates a particular set of statistics for the PGID contained in the received data packet. The details of step 245 are explained hereinafter with respect to FIGS. 5 and 6. As an example, statistic array retrieval portion 150 , time delay determination and statistics portion 160 , and statistic array storage portion 170 of apparatus 100 in FIG. 1 can be used to perform step 245 of FIG. 2 .
Next, steps 215 , 220 , 225 , 230 , 235 , 240 , and 245 can be repeated numerous times. Additional data packets having the same PGID as the first received data packet can be received, and the set of statistics for the same PGID can be successively updated. Other data packets having a PGID different from that of the first received data packet can be received, and another set of statistics for this different PGID can be successively updated. For a particular received data packet, step 215 can be performed while performing steps 220 , 225 , 230 , and 235 and before receiving a subsequent data packet. Also for a particular received data packet, steps 240 and 245 can be performed after terminating step 215 and can be performed before or while receiving the next data packet.
After repeating steps 215 , 220 , 225 , 230 , 235 , 240 , and 245 for a predetermined period of time, a step 250 of method 200 is performed. At step 250 , the first electronic apparatus displays the statistics for the received data packets. Steps 215 , 220 , 225 , 230 , 235 , 240 , and 245 can be repeated or performed continuously while performing step 250 .
As an example of different statistical displays of step 250 in method 200 , FIG. 7 illustrates a graph of instantaneous latency determined by method 200 in FIG. 2 . The graph in FIG. 7 has an X-axis or horizontal axis representing the different PGIDs of the received data packets. The graph also has a Y-axis or vertical axis representing a magnitude of the time delay or latency in the round-trip transmission of the data packets. The graph in FIG. 7 illustrates four different PGIDs, each having a minimum time delay, an average time delay, and a maximum time delay over a specific instance in time.
FIG. 3 illustrates a flow chart of a detailed portion of method 200 in FIG. 2 . In particular, FIG. 3 illustrates additional details of step 220 in FIG. 2 . At a step 321 in FIG. 3, the first electronic apparatus identifies a signature in the received data packet of step 215 in FIG. 2 . The signature in the received data packet is located at a signature offset within the received data packets. This signature offset is the same offset as the signature offset used in step 205 of FIG. 2 . At a step 322 of FIG. 3, the first electronic apparatus compares the signature of the received data packet to the signature of the created and transmitted data packets in steps 205 and 210 of FIG. 2 . At a step 323 of FIG. 3, the first electronic apparatus rejects the received data packet if its signature fails to match the signature of the transmitted data packets. If a received data packet is rejected during step 323 , the rejected data packet is immediately discarded and is not processed any further in method 200 . Accordingly, after rejecting a received data packet during step 323 , method 200 continues by receiving another data packet during step 215 of FIG. 2 .
FIG. 4 illustrates a flow chart of a different detailed portion of method 200 in FIG. 2 . In particular, FIG. 4 illustrates additional details of step 225 of FIG. 2 . At a step 421 of FIG. 4, the first electronic apparatus checks a Cyclic Redundancy Check (CRC) value of the received data packet. To perform step 421 , the first electronic apparatus calculates a CRC value for the received data packet, and identifies a CRC value in the received data packet. Then, the first electronic apparatus compares the calculated CRC value to the CRC value in the received data packet. At a step 422 of FIG. 4, the first electronic apparatus rejects the received data packet if its CRC value is incorrect. An incorrect CRC value indicates an invalid data packet. If a received data packet is rejected during step 422 , the rejected data packet is immediately discarded and is not processed any further in method 200 . Accordingly, after rejecting a received data packet during step 422 , method 200 continues by receiving another data packet during step 215 of FIG. 2 .
If the received data packet is not rejected during step 422 of FIG. 4, step 225 continues by performing a step 423 in FIG. 4 . At step 423 , the first electronic apparatus calculates the size of the received data packet and compares the calculated size to a predetermined range of sizes. At a step 424 , the first electronic apparatus rejects the received data packet if its calculated size is outside of the predetermined range described earlier with respect to step 205 in FIG. 2. A size outside of the predetermined range of sizes indicates an invalid data packet. If a received data packet is rejected during step 424 , the rejected data packet is immediately discarded and is not processed any further in method 200 . Accordingly, after rejecting a received data packet during step 424 , method 200 continues by receiving another data packet during step 215 of FIG. 2 .
FIG. 5 illustrates a flow chart of an additional detailed portion of method 200 in FIG. 2 . In particular, FIG. 5 illustrates additional details of step 245 in FIG. 2 . At a step 541 in FIG. 5, the first electronic apparatus retrieves a set of stored statistics, for the PGID contained in the received data packet of step 215 in FIG. 2 . As an example, the set of stored statistics can be retrieved from memory portion 180 in FIG. 1 . The set of stored statistics can include a minimum time delay, a maximum time delay, a total number of received data packets having the PGID, a total time delay for all of the received data packets having the PGID, and a total number of bytes or byte count for all of the received data packets having the PGID. The set of stored statistics reflects the statistics for only those received data packets having the same PGID.
The PGID of the received data packet is used to perform step 541 . For example, the set of statistics is retrieved from a first array located at a first memory address in a memory portion. The first memory address in the memory portion is identified by the PGID of the received data packet.
Next, at a step 542 in FIG. 5, the first electronic apparatus compares the time delay determined during step 240 of FIG. 2 to time delays in the set of stored statistics retrieved during step 541 . Additional details of step 542 are explained hereinafter with respect to FIG. 6 . Then, at a step 543 in FIG. 5, the first electronic apparatus increases by one the total count or number of received data packets in the set of statistics. At a step 544 , the first electronic apparatus adds the time delay determined during step 240 of FIG. 2 to the total time delay in the set of statistics. At a step 545 of FIG. 5, the first electronic apparatus calculates the number of bytes in the received data packet and adds this number to the total number of bytes or byte count in the set of statistics. The sequence of steps 542 , 543 , 544 , and 545 can be altered or reversed.
Next, at a step 546 , the first electronic apparatus stores the updated set of statistics. The PGID of the received data packet is used to perform step 546 . For example, the set of statistics is stored back into the first array located at the first memory address in the memory portion. The first memory address in the memory portion is identified by the PGID of the received data packet.
The first electronic apparatus uses the updated set of statistics to perform step 250 in FIG. 2 . For example, to display or graph the minimum time delay for a PGID, the first electronic apparatus displays or graphs the minimum time delay stored in the updated set of statistics for the PGID. As an additional example, to display or graph the maximum time delay for a PGID, the first electronic apparatus displays or graphs the maximum time delay stored in the updated set of statistics for the PGID. Furthermore, to display or graph the average time delay for a PGID, the first electronic apparatus divides the first total time delay in the set of statistics by the first total count in the set of statistics.
FIG. 6 illustrates a flow chart of additional details for step 542 of FIG. 5 . At a step 641 in FIG. 6, the first electronic apparatus compares the calculated time delay for the received data packet to a minimum time delay in the retrieved set of statistics of step 541 in FIG. 5 . At a step 642 of FIG. 6, the first electronic apparatus replaces the minimum time delay in the retrieved set of statistics with the-calculated time delay for the received data packet if the calculated time delay is less than the minimum time delay in the retrieved set of statistics. At a step 643 of FIG. 6, the first electronic apparatus compares the time delay of the received data packet to a maximum time delay in the retrieved set of statistics of step 541 in FIG. 5 . At a step 644 of FIG. 6, the first electronic apparatus replaces the maximum time delay in the retrieved set of statistics with the calculated time delay for the received data packet if the calculated time delay is greater than the maximum time delay in the retrieved set of statistics. The calculated time delay is preferably not stored individually in the memory portion unless the calculated time delay is a maximum or minimum time delay for the particular PGID.
Therefore, an improved method of determining real-time data latency and an apparatus therefor is provided to overcome the disadvantages of the prior art. The method enables the detection of an increase or decrease in the time delay for the round-trip transmission of data across a computer network.
Although the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made without departing from the spirit or scope of the invention. For instance, the numerous details set forth herein such as, for example, the specific sequence of steps are provided to facilitate the understanding of the invention and are not provided to limit the scope of the invention. Furthermore, the method described herein is not limited to the round-trip transmission of data between two electronic devices. Instead, the method can be modified and applied to the round-trip or non-round-trip transmission of data between three or more electronic devices. Accordingly, the disclosure of embodiments of the invention is intended to be illustrative of the scope of the invention and is not intended to be limiting. It is intended that the scope of the invention shall be limited only to the extent required by the appended claims.
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A method of and an electronic apparatus for determining real-time data latency are disclosed. The method may include creating a plurality of outgoing data packets having an outgoing time stamp, a group identifier and validation information. The outgoing data packets may be transmitted onto a network. A plurality of incoming data packets may be received over the network. The incoming data packets may be validated. For each of the incoming data packets that is valid, a round-trip time delay for the incoming data packet may be calculated, and statistics for the incoming data packets may be updated based on the round-trip time delay and the group identifier included in the incoming data packet. The method may be implemented on an electronic apparatus.
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BACKGROUND OF THE INVENTION
The present invention concerns a sling strap intended to allow the lifting and handling of objects or loads particularly with the help of appropriate machines such as gantry cranes, hoists etc.
Sling straps are conventionally made up from metal shackles around which the ends of the straps are secured by stitching. Such straps are far from being totally satisfactory, due to relatively long delays in delivery and manufacture connected with the obligatory use in the factory of a sewing machine and, above all, due to the fact that, once sewn, the length of the strap is fixed, and offers no possibility of adjustment; it is therefore always necessary to have in stock a lot of sling straps of different lengths, which also considerably increases their manufacturing cost.
Moreover, the act of sewing leads to a certain amount of deterioration of the strap due to the thread being cut by the switching. This in turn leads to a diminution in the maximum working load.
It is therefore one object of the present invention to overcome these deficiencies by providing a sling strap made up of a flat strap and at least one rigid shackle stirrup fixed to at least one of the ends of the strap, which can be set in place, without stitching, and whose length may be adjusted almost instantly, without requiring any tools. In addition, it is desirable that such sling strap have a resistance to tension at least equal to that of the arrangements used in the prior art.
SUMMARY OF THE INVENTION
According to the invention, the rigid stirrup which is advantageously integrally hot-forged from a high strength alloy steel, comprises means for receiving the end of the strap co-operating with means for positioning and guiding it and with means of clamping the assembly thus formed.
The sling strap is characterised in that the stirrup includes two side members each provided with bores in which is journalled a rotatable assembly made up of two positioning discs connected by a receiving pin which forms an integral part of the strap end receiving means and around which the end of the strap is wound and brought back at 180°. Also, on both sides of the receiving pin and parallel thereto there are two carrying pins defining between them a guide slot into which the end of the strap passes and is aligned at right-angles to the receiving pin. The assembly formed by the rotatable positioning discs and the carrying pins constitute the means of positioning and guiding the strap.
It is clear that the preliminary positioning of the strap, is extremely simple and needs no tools; it is necessary only to make sure that the loose end of the strap is of sufficient length.
The receiving pin has a circular cross-section, and the carrying pins are arranged symmetrically in relation to it, and have for example a cross-section of part-circular shape so as to define between them a rectilinear guide slot. This particular shape must in no way be considered to be limitative and could be different without thereby departing from the scope of the invention; one could for example opt for carrying pins each made up of two identical circular pins.
In order to facilitate the rotation operation of the triple pin, one of the positioning discs or the first positioning disc is preferably fitted with a winding key.
According to another characteristic of the invention, there are clamping means provided which will positively retain the strap in wound up position. Such clamping means includes attached to the rotatable assembly and respectively having holes which may be aligned with corresponding holes on the stirrup, and further includes a locking pin able to be introduced into the holes of the stirrup and of the rotatable assembly when they are aligned in order to clamp the latter against rotation.
The ears are fixed to the positioning discs on the inside of the stirrup, directly against its sides, so as to form an element with optimum rigidity. In order to allow its positioning and fixing, the locking pin is equipped at one end with a studded head and at the other end with a thread which cooperates with a thread provided in some of the holes of the stirrup.
The mounting on the same rotating disc of the three pins forming a triple pin allows an increase in the rigidity of the assembly forming the locking zone, the elimination of the phenomenon of flexure in the pin and increasing the moment of inertia.
According to this configuration, the forces distribute themselves primarily in the triple pin and the balance of the forces pass through the fourth pin, i.e., the locking pin.
The receiving means provides an entry slot for the strap which is essentially parallel to the receiving pin, and the two ends of the strap are returned through the entry slot after winding around the receiving pin.
For reasons of ease of manufacture and consequently reducing the cost price of the equipment, the entry slot is most usually defined by two entry pins arranged parallel to the receiving pin at the end of the stirrup opposite the shackle and hence the lifting zone.
In accordance with the above-mentioned configuration, in order to position the strap on the stirrup, it is first introduced by one of its ends into the entry slot before winding it around the receiving pin and then passing its end through the entry slot again. Then, the triple rotatable pin is turned in such a way that the strap starts to cover one of the carrying pins and then the second. The rotation of the assembly is maintained until the holes of the ears and of the stirrup are opposite each other, which corresponds to a total rotation of about 540 degrees. Thereafter the system is clamped in this position by tightening the locking pin.
This configuration has the advantage that the arrangement is perfectly symmetrical and the direction of rotation of the triple pin is therefore unimportant.
In order to be anchored satisfactorily, it is necessary to ensure that the loose end of the strap overruns the stirrup by at least twenty centimeters.
According to the invention, the locking pin has in fact a dual role; in effect, it ensures the clamping of the device and, at the same time, avoids the rejection of the strap at its upper part by assuring its hold.
In addition, it is essential that, once positioned, the strap should not slip sideways and consequently, its width should correspond exactly to that of the pins around which it is locked.
According to another characteristic of the invention, in order to allow for the adaptation of the stirrup to straps of different thicknesses and different widths (the variable elements of its geometry), the stirrup is provided with a regulating element made up of a tubular element of essentially the same length as the locking pin which it is intended to receive as well as, if necessary, two flaps fixed to the tubular element approximately perpendicular to it and defining between them a gap corresponding to the width of the strap to be fitted.
This tubular element has the advantage that it avoids the rejection of the strap and thus acts as a sort of control or gauge which locates the strap widthwise in the system.
The diameter of the tubular element is a dependent variable of the thickness of the strap: in the particular case of very thin straps, one uses a thick tube to obtain a wedging effect such as to maintain the strap permanently in its working axis and therefore accommodate under-tension or over-tension of the strap.
In the case of straps which are significantly thicker, it is of course necessary to reduce the section of this tubular element correspondingly.
In all cases, the regulatory element presses on the strap and on the triple pin preventing rejection.
It is clear that the strap is thus perfectly maintained laterally by the regulatory element.
The sling strap of the invention has a number of possible applications such as for lifting, bracing, stowing or it can even be used in the field of tension systems (floating strap for anti-pollution barrier, for oceanographic spacial location, for sailing, etc. . .) and therefore is able to be used at sea, on land or in the air. It may also be transformed into a sliding-sling by the addition of a hook with a keeper, or may even be arranged in pairs so as to obtain a double-tension system.
The strap does not undergo any deterioration in any of the fibres during fastening or undoing, while in the conventional prior art devices employing stitching, there is a minimum loss of 20% of the fibres (cutting by sewing/stitching). This new sling-strap consequently is at least 20% more efficient.
To obtain the optimum strength, the stirrup assembly as well as the triple pin, the ears and the locking pin must be made of a high-performance material, such as noble alloy steel.
Another advantage of the sling-strap of the invention, is that because of its symmetry, two active ends of a strap can be used, thus allowing the lifting of more voluminous loads from two gripping points (two-ended sling).
In the case of a symmetrical load, in order to obtain a sling with two active ends, it is sufficient to wind and lock the strap in its usual position, then to pass the two ends above the entry pins and not through the entry slot as in the case of the single-ended sling, in order to allow the obtention of an angle α between the two ends and finally to attach to the lower ends of these latter a strap hook and to fit these two accessories onto the two ends thus formed so that the tensile force may be divided equally between the two ends in relation to the centre of gravity of the load.
In the case of a non-symmetrical load, it is advantageous to adjust the length of the two ends before winding and positioning the locking clip so that the device is thus in effect able to be slid, which allows it to be easily positioned on the axis of gravity. This position having been established, it remains only to wind and lock the strap and to make the final adjustment of its two lower ends.
BRIEF DESCRIPTION OF THE DRAWINGS
The details of the sling-strap of the invention will become more readily apparent from a reading of the description following hereafter and with reference to the accompanying drawings, in which:
FIG. 1 shows a sling-strap according to prior art,
FIG. 2 is a top plan view of the sling-strap of the invention,
FIG. 3 is a plan view, partially in cross-section showing the shackle stirrup,
FIG. 4 is a side view of the sling-strap of the invention,
FIG. 5 is a side view similar to that of FIG. 4, in which the different pins are shown in broken lines,
FIG. 5a is a schematic sectional view showing the position of the rotatable assembly during insertion of the strap
FIG. 5b is a view corresponding to FIG. 5a after turning the rotatable device 360° in the direction of arrow I,
FIGS. 6a to 6b and 6c are perspective views which show the regulatory element,
FIGS. 7 and 8 are side views showing a particular configuration of the sling-strap.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
According to FIG. 1, the prior art sling-straps are made from a flat strap 1 which is fixed by sewing one of its ends 2 around a ring 3 to which one may attach, for example, a hook (not shown).
Such devices of prior art are currently used particularly for lifting, bracing, or stowing and have some inconveniences principally connected on the one hand with the need to use a sewing machine in their manufacture in order to do the stitching, and on the other hand to the impossibility of regulating the length of the strap 1 (variable geometry).
According to FIGS. 2 and 4, the sling-strap of the invention comprises, a rigid stirrup 4 equipped with a shackle 5 around which the end 2 of a strap 1 is wound then clamped in a particular way, which will be described in more detail hereinafter.
The configuration of the shackle 5 which defines the lifting zone of the sling-strap could of course be different without thereby departing from the scope of the invention. Although not shown in the figures, one may employ as the shackle 5 large-eyed swivels, small-eyed swivels, swivel shackles, swivel yokes or even swivel or security (latched) hooks.
According to FIGS. 3 and 5, the sling 4 with a shackle 5 is equipped, on its lower half, with two parallel entry pins 6, 6' defining between them an entry slot 7 through which the end 2 of the strap 1 is introduced into the stirrup as shown by the arrow A.
This entry slot co-operates with an assembly 8 moveable in rotation about an axis x--x' parallel to the entry pins 6, 6'. To allow the positioning of this assembly 8, which is described in more detail hereafter, the stirrup 4 is formed with side members 9, 9' (see FIG. 5) respectively fitted with circular bores 10, 10'.
According to FIGS. 3 and 5, the rotatable assembly 8 is made up of two positioning discs 11, 11' connected on their periphery by an entry pin 12 with a circular cross-section, as well as by two carrying pins 13, 13' which have a cross-section in the shape of segments of a circle and define, between them, a rectilinear guide slot 14 which is situated at right angles to the receiving pin 12 (see FIG. 5A). A winding key 15 allows the assembly 8 to be turned manually about its rotational axis x--x'.
According to FIG. 5a, in order to allow the end 2 of the strap 1 to be introduced into the stirrup, the triple pin rotatable assembly 8 is placed, by moving the key 5, in a position in which the guide slot 14 is situated between the entry slot 7 and the receiving pin 12, then the end 2 of the strap 1 is wound around the pin 12 and brought back at 180° through the slots 14 and 7 so that it emerges again. It is, at this moment, necessary to ensure that the length of the free end corresponding to the end 2 is sufficient to have a good hold.
To achieve the clamping of the strap 1, the rotation of the rotatable assembly 8 with three pins 12, 13, 13' is effected according to the arrow I, the strap then winds around the carrying pins 13, 13'; after rotation through 360° around the axis x--x' from the position shown in FIG. 5a, the strap 1 arrives at the position shown in FIG. 5b in which it is more rigidly held because of the double winding around the three pins 12, 13, 13'; there is thus achieved a "self-locking" of the strap.
According to FIGS. 3 and 5, the positioning discs 11 and 11' of the rotatable assembly 8 have respectively opposite the receiving pin 12, two ears 16, 16' directly adjoining the internal surface of the side members 9, 9' of the stirrup 4.
These ears 16, 16' have holes 17, 17' intended to come into line with the holes 18, 18' in the side members 9, 9' of the stirrup 4 during the rotation of the device 8 in the direction of the arrow I about the axis x--x'.
According to FIGS. 3 and 5, the ears 16, 16' are arranged in such a way that the alignment of the perforations 17, 18, 17', 18' requires a rotation of the rotatable assembly 8 of about 180 degrees from the position shown in FIG. 5b. This angle of rotation--which has the advantage of conferring a perfect symmetry on the device and thus of allowing the user to turn the triple pin 8 either in the direction I or in the opposite direction--could of course be different without thereby departing from the scope of the invention.
According to FIG. 3, the presence of perforations 17, 17', 18, 18' allows the clamping in rotation of the device 8 by means of a locking pin 19 one end of which has a working head 20 while the opposite end has a thread 21 co-operating with a corresponding thread 22 provided on the inside of the hole 18 in the side member 9 of the stirrup 4.
According to FIG. 4, the stirrup 4 has in fact two roles; it serves of course to permit the lifting of loads from the shackle 5; also, the zones marked a of the sides 9, 9' situated on either side of the three-pinned rotatable assembly 8 around which the strap 1 is wound ensure the protection of the latter with regard to abrasion (as opposed to the prior art device shown in FIG. 1 in which the strap is overlaid around the ring 3, which leads to abrasion at the level of this ring when the sling strap lies on the ground).
According to FIGS. 6a, 6b and 6c, a good grip requires that the width W of the strap 1 corresponds approximately to the length of the three pins 12, 13, 13' of the rotatable element 8 (FIGS. 2 and 3) and that this should have a thickness such that it may be perfectly held in the clamping position between the locking pin 19 and the triple pin 12, 13, 13'; a regulatory element 23 allows the sling strap to be adapted to different thicknesses or widths.
According to FIG. 6a, in the case of straps 1 of little thickness, it is necessary to provide around the locking pin 19 a tubular element 24 whose diameter is a variable dependent on the thickness of the strap 1 and whose length corresponds approximately to that of the three pins 12, 13, 13', this element itself thus constitutes the regulatory element 23.
According to FIG. 6b, if the width W' of the strap 1 becomes notably less than the length of the pins 12, 13, 13', one attaches to the tubular element 24 two guide flaps 25 and 25' fixed approximately perpendicular to this element and extending tangentially from its periphery, these flaps defining between them a gap 26 corresponding to the width W' of the strap 1 and extending into the guide slot 14 which separates the two carrying pins 13, 13'.
According to FIGS. 6b and 6c, it is of course necessary to choose a regulatory element 23 whose height h measured between the gap 26 defined by the flaps 25 and 25' and the tubular element 24 (dependent on the diameter of the tubular element 24) increases when the thickness of the strap diminishes; this zone h as well as the periphery of the tubular element 24 defines a zone which may be used for marking and identification.
The addition of the regulatory element 23 allows almost universal utilisation of the strap.
Moreover, and still without departing from the scope of the invention, one could propose appreciable modification to the configuration of the strap 1 and, as shown for example in FIGS. 7 and 8, by pairing together two stirrups 4 1 and 4 2 rigidly fixed together along one edge. One may thus achieve a system of double tension and thereby double load.
The configuration shown in FIG. 7 permits the use of a strap whose free end has no metal tip, which is a very good thing in certain lifting operations where the loads to be handled are delicate; this configuration can be used particularly in spatial and oceanographic fields (shells, fuselages, ice, glass, polished metal, etc. . .). No metal parts thus run the risk of hitting and damaging the load to be lifted.
According to FIG. 8, when it is applied to bracing, this twin configuration allows the passage of one doubled strap and thus doubled tension; moreover, one obtains thus a non-magnetic system given that the strap is most often made from synthetic fibres.
In the particular case of bracing, the locking pin 19 can be held in a known manner by means of a bolt and locking pin.
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A sliding strap for lifting loads wherein a strap is connected to a shackle providing a hook engaging loop and the strap at one end is fed into a rotatable assembly provided with two juxtaposed carrying pins spaced to provide a passage therebetween, and a receiving pin. The carrying pins passage permits the strap to pass therethrough. The receiving pin is aligned with this passage to allow the strap to loop around the receiving pin and pass through the passage. Rotation of the assembly serves to wrap the doubled strap around the three pins. Flanges are provided fixed to the rotatable assembly. A series of holes are provided in the flanges and in the shackle to permit the insertion of a locking pin when a pair of flange holes are aligned with a pair of the shackle holes.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/845,299, filed on Sep. 18, 2006. The disclosure of the above application is incorporated herein by reference.
FIELD
[0002] The present disclosure relates to compressors, and more specifically to noise attenuation mounting structures for compressors.
BACKGROUND
[0003] The statements in this section merely provide background information related to the present disclosure and may not constitute prior art.
[0004] Operation of a compressor may result in noise generation from moving parts associated therewith, such as the motor and compression mechanism. Compressor noise may be transmitted through the air and/or to a structure engaged with the compressor. The structure of the compressor including the shell and mounting portions may contribute to noise generation by transmitting the noise generated by the moving parts and even amplifying the noise.
SUMMARY
[0005] A compressor may include a shell, a compression mechanism, a motor, a base member, and a mounting foot. The compression mechanism may be disposed within the shell and the motor may be drivingly engaged with the compression mechanism. The base member may be coupled to the shell and a mounting foot may be fixed to the base member. The mounting foot may include a mounting aperture extending therethrough and a slot intersecting said aperture that attenuates vibrations within an operating frequency range of the compressor.
[0006] Further areas of applicability will become apparent from the description provided herein. It should be understood that the description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the present disclosure.
DRAWINGS
[0007] The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way.
[0008] FIG. 1 is a sectional view of a compressor according to the present disclosure;
[0009] FIG. 2 is a perspective view of a base member of the compressor of FIG. 1 ;
[0010] FIG. 3 is a alternate base member according to the present disclosure;
[0011] FIG. 4 is a sectional view of the base member of FIG. 3 ;
[0012] FIG. 5 is an alternate base member according to the present disclosure; and
[0013] FIG. 6 is a refrigeration unit according to the present disclosure.
DETAILED DESCRIPTION
[0014] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses.
[0015] The present teachings are suitable for incorporation in many different types of scroll and rotary compressors, including hermetic machines, open drive machines and non-hermetic machines. For exemplary purposes, a compressor 10 is shown as a hermetic scroll refrigerant-compressor of the low-side type, i.e., where the motor and compressor are cooled by suction gas in the hermetic shell, as illustrated in the vertical section shown in FIG. 1 .
[0016] Compressor 10 may include a cylindrical hermetic shell 16 , a compression mechanism 18 , a main bearing housing 20 , a motor assembly 22 , a refrigerant discharge fitting 24 , and a suction gas inlet fitting 26 . The hermetic shell 16 may house the compression mechanism 18 , main bearing housing 20 , and motor assembly 22 . Shell 16 may include an end cap 28 at the upper end thereof, a transversely extending partition 29 , a longitudinally extending intermediate portion 31 , and a lower cover 33 . The portions of shell 16 may be fixed to one another in a variety of ways, such as welding, to seal hermetic shell 16 . The refrigerant discharge fitting 24 may be attached to shell 16 at opening 30 in end cap 28 . The suction gas inlet fitting 26 may be attached to shell 16 at opening 32 . The compression mechanism 18 may be driven by motor assembly 22 and supported by main bearing housing 20 . The main bearing housing 20 may be affixed to shell 16 at a plurality of points in any desirable manner.
[0017] The motor assembly 22 may generally include a motor 34 , a frame 36 and a drive shaft 38 . The motor 34 may include a motor stator 40 and a rotor 42 . The motor stator 40 may be press fit into frame 36 , which may in turn be press fit into shell 16 . Drive shaft 38 may be rotatably driven by stator 40 . Windings 44 may pass through stator 40 . Rotor 42 may be press fit on drive shaft 38 . A motor protector 46 may be provided in close proximity to windings 44 so that motor protector 46 will de-energize motor 34 if windings 44 exceed their normal temperature range.
[0018] Drive shaft 38 may include an eccentric crank pin 48 having a flat 49 thereon and one or more counter-weights 50 at an upper end 52 . Drive shaft 38 may include a first bearing portion 53 rotatably journaled in a first bearing 54 in main bearing housing 20 and a second bearing portion 55 rotatably journaled in a second bearing 56 in frame 36 . Drive shaft 38 may include an oil-pumping concentric bore 58 at a lower end 60 . Concentric bore 58 may communicate with a radially outwardly inclined and relatively smaller diameter bore 62 extending to the upper end 52 of drive shaft 38 . The lower interior portion of shell 16 may be filled with lubricating oil. Concentric bore 58 may provide pump action in conjunction with bore 62 to distribute lubricating fluid to various portions of compressor 10 .
[0019] Compression mechanism 18 may generally include an orbiting scroll 64 and a non-orbiting scroll 66 . Orbiting scroll 64 may include an end plate 68 having a spiral vane or wrap 70 on the upper surface thereof and an annular flat thrust surface 72 on the lower surface. Thrust surface 72 may interface with an annular flat thrust bearing surface 74 on an upper surface of main bearing housing 20 . A cylindrical hub 76 may project downwardly from thrust surface 72 and may include a journal bearing 78 having a drive bushing 80 rotatively disposed therein. Drive bushing 80 may include an inner bore in which crank pin 48 is drivingly disposed. Crank pin flat 49 may drivingly engage a flat surface in a portion of the inner bore of drive bushing 80 to provide a radially compliant driving arrangement.
[0020] Non-orbiting scroll 66 may include an end plate 82 having a spiral wrap 84 on lower surface 86 thereof. Spiral wrap 84 may form a meshing engagement with wrap 70 of orbiting scroll 64 , thereby creating an inlet pocket 88 , intermediate pockets 90 , 92 , 94 , 96 , and outlet pocket 98 . Non-orbiting scroll 66 may have a centrally disposed discharge passageway 100 in communication with outlet pocket 98 and upwardly open recess 102 which may be in fluid communication via an opening 103 in partition 29 with a discharge muffler chamber 104 defined by end cap 28 and partition 29 .
[0021] Non-orbiting scroll 66 may have in the upper surface thereof an annular recess 105 having parallel coaxial side walls in which is sealingly disposed for relative axial movement an annular floating seal 107 which serves to isolate the bottom of recess 105 from the presence of gas under suction and discharge pressure so that it can be placed in fluid communication with a source of intermediate fluid pressure by means of a passageway 109 . A spring 111 may urge floating seal 107 upward to maintain a sealing engagement. Non-orbiting scroll 66 may, therefore, be axially biased against orbiting scroll 64 by the forces created by discharge pressure acting on the central portion of scroll 66 and those created by intermediate fluid pressure acting on the bottom of recess 105 .
[0022] Compressor 10 may use a dual pressure balancing scheme to axially balance non-orbiting scroll 66 with floating seal 107 being used to separate the discharge gas pressure from the suction gas pressure. A solenoid valve 113 may be used to open and close a passageway 115 located within non-orbiting scroll 66 . Passageway 115 extends from the bottom of recess 105 which is at intermediate pressure during operation of compressor 10 to the area of compressor 10 which contains suction gas at suction gas pressure.
[0023] Relative rotation of the scroll members 64 , 66 may be prevented by an Oldham coupling, which may generally include a ring 108 having a first pair of keys 110 (one of which is shown) slidably disposed in diametrically opposed slots 112 (one of which is shown) in non-orbiting scroll 66 and a second pair of keys (not shown) slidably disposed in diametrically opposed slots in orbiting scroll 64 .
[0024] With additional reference to FIG. 2 , lower cover 33 may include an upper portion 200 having a skirt 202 extending from a perimeter thereof. Skirt 202 may extend at an angle relative to upper portion 200 . In the present example, skirt 202 extends at an angle of approximately 90 degrees relative to upper portion 200 . Upper portion 200 may include a central recessed portion 204 surrounded by a vertically extending annular ridge 206 having a flange portion 208 extending radially outwardly therefrom. Flange portion 208 may have a generally planar body extending generally perpendicular to shell intermediate portion 31 . Upper portion 200 may further include a plurality of mounting feet 210 extending radially outwardly from flange portion 208 . Mounting feet 210 may include apertures 212 therethrough for securing lower cover 33 , and therefore compressor 10 , to a base (discussed below).
[0025] Upper portion 200 may include a plurality of slots 214 therethrough. Slots 214 may be disposed symmetrically about upper portion 200 . Slots 214 may extend radially outwardly relative to central recessed portion 204 and may extend to the perimeter of upper portion 200 . More specifically, slots 214 may intersect apertures 212 in mounting feet 210 . A first portion 216 of slot 214 may extend from aperture 212 to the perimeter of upper portion 200 and a second portion 218 of slot 214 may extend from aperture 212 radially inwardly toward central recessed portion 204 .
[0026] Slots 214 may have a width up to the diameter of aperture 212 . Slots 214 may shift lower cover natural frequencies away from undesirable frequencies. For example, slots 214 may reduce 800 Hz ⅓ octave band sound levels. Slots 214 may extend along a majority of mounting feet 210 . More specifically, slots 214 may extend up to the entire distance between an outer perimeter of a mounting foot 210 to intermediate portion 31 of shell 16 .
[0027] An alternate lower cover 333 is shown in FIGS. 3 and 4 . Lower cover 333 may include an upper portion 300 having a skirt 302 extending from a perimeter thereof. Skirt 302 may extend at an angle relative to upper portion 300 and may extend a length (L 1 ) of between 3 and 5 times a material thickness (T) of lower cover 333 . Upper portion 300 may include a central recessed portion 304 surrounded by a vertically extending annular ridge 306 having a first flange portion 308 extending radially outwardly therefrom. Vertically extending annular ridge 306 may have a height (L 2 ) greater than material thickness (T). Flange portion 308 may have a generally sloped body extending at an angle (θ) of between 20 and 60 degrees relative to annular ridge 306 . First flange portion 308 may extend a distance (L 3 ) of between 2 and 6 times material thickness (T) above skirt 302 . A second flange portion 309 may extend from and generally surround first flange portion 308 . Second flange portion 309 may be generally planar and may have a plurality of mounting feet 310 extending radially outwardly therefrom. Mounting feet 310 may include apertures 312 therethrough for securing lower cover 333 to a base (discussed below).
[0028] Lower cover 333 may have a generally square shape with both first and second flange portions 308 , 309 having generally square perimeters. As seen in FIG. 3 , mounting feet 310 may extend from each of the corners of second flange portion 309 . As a result of the features mentioned above, lower cover 333 vibration attenuation may be improved. More specifically, these features may push the natural frequency of lower cover 333 higher, as well as changing the mode shape thereof. For example, the sloped profile of flange portion 308 may stiffen mounting feet 310 and raise the natural frequency of lower cover 333 (ex: from 800 Hz to 1250 Hz). The slot geometry discussed below with respect to FIG. 5 may be used to tune the frequency away from the new frequency (1250 Hz).
[0029] FIG. 5 is an alternate example of a lower cover 433 generally similar to lower cover 333 with the addition of slots 414 . As such, the description of lower cover 333 may generally apply to lower cover 433 , except as otherwise noted. Lower cover 433 may include an upper portion 400 having a skirt 402 extending from a perimeter thereof.
[0030] Skirt 402 may extend at an angle relative to upper portion 400 . Skirt 402 may have a length of between 50 and 90 percent of the length of skirt 302 . Upper portion 400 may include a central recessed portion 404 surrounded by a vertically extending annular ridge 406 having a first flange portion 408 extending radially outwardly therefrom. Flange portion 408 may have a generally sloped body extending at an angle relative to vertically extending annular ridge 406 . Flange portion 408 may have a width of 80 to 110 percent of the width of flange portion 308 .
[0031] The distance between skirts 402 on opposed sides may be greater than the width of flange portion 408 and 90 to 100 percent of the distance between skirts 302 on opposed sides. A second flange portion 409 may extend from and generally surround first flange portion 408 . Second flange portion 409 may be generally planar and may have a plurality of mounting feet 410 extending radially outwardly therefrom. Mounting feet 410 may include apertures 412 therethrough for securing lower cover 433 to a base (discussed below).
[0032] Upper portion 400 may include a plurality of slots 414 therethrough. Slots 414 may be disposed symmetrically about upper portion 400 . Slots 414 may extend radially outwardly relative to central recessed portion 404 and may extend to the perimeter of upper portion 400 . More specifically, slots 414 may intersect apertures 412 in mounting feet 410 . A first portion 416 of slot 414 may extend from aperture 412 to the perimeter of upper portion 400 and a second portion 418 of slot 414 may extend from aperture 412 radially inwardly toward central recessed portion 404 . Second portion 418 may have a length greater than a material thickness of lower cover 433 , similar to material thickness (T) in FIG. 4 , and a width generally less than the diameter of aperture 412 .
[0033] Lower cover 433 may have a generally square shape with both first and second flange portions 408 , 409 having generally square perimeters. Mounting feet 410 may extend from each of the corners of second flange portion 409 . As a result of the features mentioned above, lower cover 433 vibration attenuation may be improved. More specifically, these features may push the natural frequency of lower cover 433 higher, as well as changing the mode shape thereof. For example, the sloped profile of flange portion 408 may stiffen mounting feet 410 and raise the natural frequency of lower cover 433 (ex: from 800 Hz to 1250 Hz). The slot geometry may be used to tune the frequency of lower cover 433 away from the new frequency (1250 Hz). The features of lower covers 33 , 333 , 433 may be used in any combination to achieve a desired noise attenuation.
[0034] As seen in FIG. 6 , compressor 10 may be part of a refrigeration unit 500 . Refrigeration unit 500 may include a housing 502 divided into a condensing unit cabinet 504 , a compressor cabinet 506 , and an electronic cabinet 508 . Condensing unit cabinet 504 may house a condensing unit (not shown) and condenser fans 512 . Compressor cabinet 506 may house one or more compressors 10 , as well as a suction header 514 and a discharge header 516 . Electronic cabinet 508 may enclose a controller 518 in an enclosure accessible from the exterior of housing 502 .
[0035] Compressor 10 may be mounted to a base pan 520 of housing 502 at feet 210 . Sound may be generated from two sources, compressor 10 (air-borne and structure-borne noise) and base pan 520 , or other support structure (structure-borne noise). The pattern of sound generation may be modified by shifting natural frequencies and modifying mode shapes of mounting feet 210 and/or lower cover 33 . This modification may be achieved in a variety of ways. For example, lower cover 33 may be designed in a way such that the natural modes of mounting feet 210 do not match any local or global mode of base pan 520 or any other mounting structures. It is understood that the above description applies equally to lower covers 333 , 433 .
[0036] Base pan 520 may include puck-like protrusions, or grommets, (not shown) for engagement with compressor feet 210 . Mounting feet 210 may be bolted to base pan 520 at the grommets. Double studded grommets may lower natural frequencies, while conventional mounting may increase natural frequencies through increased torque on the bolt when mounting lower cover 33 to base pan 520 or other support structure. The presence of any slots, windows or slits may change the boundary conditions of the cavity beneath lower cover 33 , which in turn may change the noise radiation pattern when compressor 10 is mounted to base pan 520 , or some other mounting structure. While described with respect to lower cover 33 , it is understood that the description of the engagement between lower cover 33 and base pan 520 applies equally to lower covers 333 , 433 .
[0037] By way of example, internal components of compressor 10 may have 800 Hz ⅓ Octave and 1250 Hz ⅓ Octave natural frequencies. These frequencies may be passed through lower cover 33 and amplified. Using the features described above, the natural frequencies of lower cover 33 may be mismatched relative to the natural frequencies of the internal components of compressor 10 to break the chain of energy.
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A compressor may include a shell, a compression mechanism, a motor, a base member, and a mounting foot. The compression mechanism may be disposed within the shell and the motor may be drivingly engaged with the compression mechanism. The base member may be coupled to the shell and a mounting foot may be fixed to the base member. The mounting foot may include a mounting aperture extending therethrough and a slot intersecting said aperture that attenuates vibrations within an operating frequency range of the compressor.
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BACKGROUND OF THE INVENTION
[0001] (1) Field of the Invention
[0002] The invention relates to the fabrication of integrated circuit devices, and more specifically to a method and apparatus to eliminate copper line damage after copper line Chemical Mechanical Polishing.
[0003] (2) Description of the Prior Art
[0004] The use of copper has become increasingly more important for the creation of multilevel interconnections in semiconductor circuits, however copper lines frequently show damage after CMP and clean. This damage of copper lines causes planarization problems of subsequent layers that are deposited over the copper lines because these layers may now be deposited on a surface of poor planarity. Particularly susceptible to damage are isolated copper lines or copper lines that are adjacent to open fields. While the root causes for these damages are at this time not clearly understood, poor copper gap fill together with subsequent problems of etching and planarization are suspected. Where over-polish is required, the problem of damaged copper lines becomes even more severe. The present invention teaches methods for avoiding the observed phenomenon of damaged copper lines.
[0005] Recent applications have successfully used copper as a conducting metal line, most notably in the construct of CMOS 6-layer copper metal devices. Even for these applications however, a wolfram plug was still used for contact points in order to avoid damage to the devices.
[0006] The reliability of a metal interconnect is most commonly described by a lifetime experiment on a set of lines to obtain the medium time to failure. The stress experiment involves stressing the lines at high current densities and at elevated temperatures. The failure criterion is typically an electrical open for non-barrier conductors or a predetermined increase in line resistance for barrier metalization.
[0007] The mean time to failure is dependent on the line geometry where this failure is directly proportional to the line width and the line thickness. Experimentally, it has been shown that the width dependence is a function of the ratio of the grain size d of the film and the width of the conductor w. As the ratio w/d decreases, the mean time to failure will increase due to the bamboo effect.
[0008] Conventional methods proposed for placing copper conductors on silicon based substrates are based on the deposition of a variety of layers where each layer has characteristics of performance or deposition that enhance the use of copper as the major component within conducting lines. This approach has met with only limited success and has as yet not resulted in the large-scale adaptation of copper.
[0009] U.S. Pat. No. 5,187,119 teaches that, in the field of high density interconnect technology, many integrated circuit chips are physically and electrically connected to a single substrate. To achieve a high wiring and packing density, it is necessary to fabricate a multilayer structure on the substrate to connect integrated circuits to one another. Embedded in other dielectric layers are metal conductor lines with vias (holes) providing electrical connections between signal lines or to the metal power and ground planes. Adjacent layers are ordinarily formed so that the primary signal propagation directions are orthogonal to each other. Since the conductor features are typically narrow in width and thick in a vertical direction (in the range of 5 to 10 microns thick) and must be patterned with microlithography, it is important to produce patterned layers that are substantially flat and smooth (i.e., planar) to serve as the base for the next layer.
[0010] Two common techniques used to achieve planarity on a semiconductor surface are a Spin-On-Glass (SOG) etchback process and a Chemical Mechanical Polishing (CMP) process. Although both processes improve planarity on the surface of a semiconductor wafer, CMP has been shown to have a higher level of success in improving global planarity. The assurance of planarity is crucial to the lithography process, as the depth of focus of the lithography process is often inadequate for surfaces, which do not have a consistent height.
[0011] U.S. Pat. No. 5,187,119 further teaches that, if the surface is not flat and smooth, many fabrication problems occur. In a multilayer structure, a flat surface is extremely important to maintain uniform processing parameters from layer to layer. A non-flat surface results in photoresist thickness variations that require pattern or layer dependent processing conditions. The layer dependent processing greatly increases the problem complexity and leads to line width variation and reduced yield. Thus, in fabricating multilayer structures maintaining a flat surface after fabricating each layer allows uniform layer-to-layer processing.
[0012] A further critical consideration for obtaining high yields and suitable performance characteristics of semiconductor devices is that, during the fabrication process, the cleanliness of the silicon wafers is meticulously maintained. It is therefore important to, at all stages of the fabrication process, remove impurities from the surface of the wafer in order to prevent the diffusion of impurities into the semiconductor substrate during subsequent high-temperature processing. Some impurities are donor or acceptor dopants that directly affect device performance characteristics. Other impurities cause surface or bulk defects such as traps, stacking faults or dislocations. Surface contaminants such as organic matter, oil or grease lead to poor film adhesion. The various types of impurities and contaminants must be removed by careful cleaning, such as chemical or ultrasonic cleaning at initiation of silicon processing and in various appropriate steps during processing.
[0013] Chemical Mechanical Polishing is a method of polishing materials, such as semiconductor substrates, to a high degree of planarity and uniformity. The process is used to planarize semiconductor slices prior to the fabrication of semiconductor circuitry thereon, and is also used to remove high elevation features created during the fabrication of the microelectronic circuitry on the substrate. One typical chemical mechanical polishing process uses a large polishing pad that is located on a rotating platen against which a substrate is positioned for polishing, and a positioning member which positions and biases the substrate on the rotating polishing pad. Chemical slurry, which may also include abrasive materials therein, is maintained on the polishing pad to modify the polishing characteristics of the polishing pad in order to enhance the polishing of the substrate.
[0014] A common requirement of all CMP processes is that the substrate be uniformly polished. In the case of polishing an electrical insulating layer, it is desirable to polish the layer uniformly from edge to edge on the substrate. To ensure that a planar surface is obtained, the electrically insulating layer must be uniformly removed. Uniform polishing can be difficult because several machine parameters can interact to create non-uniformity in the polishing process. For example, in the case of CMP, misalignment of the polishing wheel with respect to the polishing platen can create regions of non-uniform polishing across the diameter of the polished surface. Other machine parameters, such as non-homogeneous slurry compositions and variations in the platen pressure, can also create non-uniform polishing conditions.
[0015] U.S. Pat. No. 5,770,095 (Sasaki et al.) teaches Cu CMP methods that include low temperature CMP (temp ranges −2 degrees C. to 100 degrees C.) and various slurries that appear to include inhibitors. See cols. 5 13, examples 1 to 4. FIG. 13 appears to show a chiller for a CMP platen, see col. 12, line 49.
[0016] U.S. Pat. No. 5,607,718 (Sasaki et al.) discloses a Cu CMP method at a low temperature (less than 15 degrees C.), see claims 2, 16, etc.
[0017] U.S. Pat. No. 5,840,629 (Carpio) shows a Cu CMP slurry composition including corrosion inhibitors, see col. 3, lines 21 to 30.
[0018] U.S. Pat. No. 5,300,155 (Sandu et al.) discloses a CMP method where a metal is CMP at different temperatures. This patent has broad claims.
[0019] U.S. Pat. No. 5,780,358 (Zhou et al.) teaches a Cu CMP method, which include anti-oxidation (inhibitors), see col. 8, lines 40 to 49.
SUMMARY OF THE INVENTION
[0020] It is the primary objective of the invention to reduce copper line damage after copper Chemical Mechanical Polishing.
[0021] It is another objective of the present invention to reduce the defect count for copper line polishing using the CMP process.
[0022] It is another objective of the present invention to improve semiconductor wafer throughput as a result of copper line polishing using the CMP process.
[0023] It is another objective of the present invention to improve copper line reliability and the related reliability of the devices contained within the semiconductor wafer.
[0024] It is another objective of the invention to provide a method of copper line polishing that can realize a high semiconductor wafer throughput and that exhibits uniformity and planarity of the surface of the copper line that is to be polished.
[0025] In accordance with the objects of the invention a new method of polishing copper lines is achieved. The object of copper CMP is to remove copper ions in a continuous and uninterrupted manner. Copper ions, if allowed to accumulate, will cause corrosion of the copper lines. This implies that, during the process of CMP, no copper ions accumulation must be allowed. The invention achieves the prevention of the accumulation of copper ions by performing the CMP process at low temperatures and by maintaining this low temperature during the CMP process by adding a slurry that functions as a corrosion inhibitor.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] [0026]FIG. 1 shows a cross section of the polishing plate used for the copper CMP process.
[0027] [0027]FIG. 2 shows a top view of the surface of the polishing platen that is in contact with the copper lines that are being polished.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0028] Referring now specifically to FIG. 1, there is shown a cross section of the polishing platen 10 that is used to polish the copper lines contained within the surface of wafer 12 . Affixed to the polishing table 10 is a polishing pad (not shown) that is in direct physical contact with the wafer 12 that is being polished. The polishing plate 10 rotates around an axis of rotation 14 . A channel 16 is provided through the body of platen 10 , through this channel water is entered as indicated by the direction 18 of the inhibitor. This water exits the platen 10 as indicated by 20 . The water supply is used to control the temperature of the platen 10 and does not exit the platen on the surface of the platen that comes into contact with the copper lines that are being polished. The water serves the function of controlling the temperature of the polishing platen 10 , this temperature is targeted to remain around 22 degrees C. but may, dependent on the intensity of polishing actions, rise to around 28 degrees C.
[0029] The objective of the cooling arrangement is to keep the temperature at the surface of the polishing platen within the range of between 10 and 20 degrees C., best results of preventing the build-up of copper ions on the surface of the polishing platen will be obtained if the temperature on the surface of the polishing platen is kept within the 10 to 20 degrees C. range.
[0030] Equally important to the invention is the use of slurry that inhibits the accumulation of copper ions on the surface of the wafer that is being polishing. Typical slurry used under the invention is slurry with a pH of less than 7.
[0031] The invention can be implemented using one of the various silicon wafer-cleaning systems that are commercially available which clean wafers using mechanical scrubbing. These conventional silicon wafer cleaning machines use a polishing pad affixed to a rotating turntable wherein the polishing pad faces upward as shown in FIG. 1. The turntable is commonly rotated at various controlled speeds, for instance 10 to 100 RPM, in a controlled clockwise or counterclockwise direction. The silicon wafer, generally in the form of a flat, circular disk, is held within a carrier assembly (not shown) with the substrate wafer face to be polished facing downward. The polishing pad and turntable are typically much larger that the silicon wafer. For example, a typical diameter of the pad (not shown) and turntable 10 is 22 inches while the wafer commonly has a diameter of approximately 10 inches. The polishing pad is typically fabricated from a polyurethane and/or polyester base material. Semiconductor polishing pads are commercially available such as models IC1000 or Scuba IV of a woven polyurethane material.
[0032] [0032]FIG. 2 shows another arrangement for routing the cooling water through the polishing platen 22 . Controlling the temperature at the surface of the wafer that is being polished is of key importance to the prevention of the accumulation of copper ions on that surface. This requires that a maximum amount of the heat created during the polishing operation be removed in a direct and efficient manner. This efficiency can be increased by increasing the area of contact between the coolant (water) and the body of the polishing platen. The design shown in FIG. 2 accomplishes this indicated maximization of contact and, in so doing, provides and efficient manner of preventing the temperature at the surface of the substrate that is being polished from exceeding the limit required for optimum results. The design shown in FIG. 2 also provides better temperature uniformity across the surface of the wafer that is being polished since the coolant contacts the body of the polishing platen over a large cross section of the platen. The coolant that is provided to the polishing platen 22 is circulated through the polishing platen 22 via a helix 24 . The helix 24 provides maximum contact between the coolant and the polishing platen 22 thereby allowing maximum impact of the coolant on the temperature and temperature control of the polishing platen 22 . Coolant entry and exit points 26 and 28 are provided. By providing the entry and exit points at unequal distances from the center of the polishing platen 22 , the temperature gradient of the surface of the polishing platen can be further controlled. The coolant can enter the helix at the point of highest temperature of the polishing platen thereby removing thermal energy from the polishing table in the most efficient manner.
[0033] From the invention it is clear that, because the temperature of a wafer is typically higher at the center of the wafer than it is at the edge of the wafer, the cooling system must take this temperature characteristic into account. This means that cooling must be higher in the center of the wafer which in turn means that the heat that is removed from the center of the wafer is higher than the heat that is removed from the edge of the wafer. This objective can be accomplished by increasing the density of the helix that is created in the polishing platen so that the concentration of the coolant is densest in the center of the wafer that is being polished. The density of the helix along the diameter of the polishing platen and the gradient of increasing or decreasing the density of the helix can readily be determined for particular applications and different wafer diameters. It is clear that the heat exchange in the center of the wafer must be high relative to the heat exchange at the edge of the wafer, the density of the openings that are created for the helix inside the polishing platen must therefor accommodate this heat exchange profile by having higher density tubing in the center with gradually decreasing density of tubing towards the edge of the polishing plate.
[0034] It will be apparent to those skilled in the art, that other embodiments, improvements, details and uses can be made consistent with the letter and spirit of the present invention and within the scope of the present invention, which is limited only by the following claims, construed in accordance with the patent law, including the doctrine of equivalents.
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The invention provides a method and an apparatus that prevent the accumulation of copper ions during CMP of copper lines by performing the CMP process at low temperatures and by maintaining this low temperature during the CMP process by adding a slurry that functions as a corrosion inhibitor.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This patent application claims the benefit of U.S. provisional patent application No. 61/392,183 filed Oct. 12, 2010.
BACKGROUND OF THE INVENTION
[0002] The disclosure generally relates to a synthetic process for preparing compounds of formula I including the preparation of chemical intermediates useful in this process.
[0003] CGRP inhibitors are postulated to be useful in pathophysiologic conditions where excessive CGRP receptor activation has occurred. Some of these include neurogenic vasodilation, neurogenic inflammation, migraine, cluster headache and other headaches, thermal injury, circulatory shock, menopausal flushing, and asthma. CGRP antagonists have shown efficacy in human clinical trials, See Davis C D, Xu C. Curr Top Med Chem. 2008 8(16):1468-79; Benemei S, Nicoletti P, Capone J G, Geppetti P. Curr Opin Pharmacol. 2009 9(1):9-14. Epub 2009 Jan. 20; Ho T W, Ferrari M D, Dodick D W, Galet V, Kost J, Fan X, Leibensperger H, Froman S, Assaid C, Lines C, Koppen H, Winner P K. Lancet. 2008 372:2115. Epub 2008 Nov. 25; Ho T W, Mannix L K, Fan X, Assaid C, Furtek C, Jones C J, Lines C R, Rapoport A M; Neurology 2008 70:1304. Epub 2007 Oct. 3.
[0004] CGRP receptor antagonists have been disclosed in PCT publications WO 2004/092166, WO 2004/092168, and WO 2007/120590. The compound (5S,6S,9R)-5-amino-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-yl 4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxylate is an inhibitor of the calcitonin gene-related peptide (CGRP) receptor.
[0000]
[0005] For purposes of large-scale production there is a need for a high-yielding synthesis of compound of formula I and related analogs that is both efficient and cost-effective.
DESCRIPTION OF THE INVENTION
[0006] One aspect of the invention is a process for the preparation of a compound of formula I, or a salt thereof, where Ar 1 is phenyl substituted with 0-3 substituents selected from the group consisting of cyano, halo, alkyl, haloalkyl, alkoxy, haloalkoxy, and alkylSO 2
[0000]
[0000] comprising the reductive amination and alcohol deprotection of a compound of formula IV where R 1 is selected from the group consisting of trialkylsilyl, alkoxy, alkylcarbonyl, benzyl, substituted benzyl, benzoyl, and pivaloyl to a compound of formula II where R 1 is hydrogen, and coupling the compound of formula II, or a salt thereof, with a compound of formula III where R 2 is selected from the group consisting of imidazolyl, pyrrolyl, N-hydroxysuccinimidyl, chloro, phenoxy, substituted phenoxy, phenylthio, and substituted phenylthio.
[0000]
[0007] Another aspect of the invention is a process for the preparation of a compound of formula I, or a salt thereof, where Ar 1 is phenyl substituted with 0-3 substituents selected from the group consisting of cyano, halo, alkyl, haloalkyl, alkoxy, haloalkoxy, and alkylSO 2
[0000]
[0000] comprising coupling a compound of formula II, or a salt thereof, where R 1 is hydrogen, or a salt thereof, with a compound of formula III, or a salt thereof, where R 2 selected from the group consisting of imidazolyl, pyrrolyl, N-hydroxysuccinimidyl, chloro, phenoxy, substituted phenoxy, phenylthio, and substituted phenylthio.
[0000]
[0008] Another aspect of the invention is where the compound of formula II is
[0000]
[0000] or a salt thereof, and the compound of formula III is
[0000]
[0000] or a salt thereof.
[0009] Another aspect of the invention is a process for the preparation of a compound of formula II, or a salt thereof, where Ar 1 is phenyl substituted with 0-3 substituents selected from the group consisting of cyano, halo, alkyl, haloalkyl, alkoxy, haloalkoxy, and alkylSO 2 and R 1 is hydrogen,
[0000]
[0000] comprising the reductive amination and deprotection of a compound of formula IV, or a salt thereof, where Ar 1 is phenyl substituted with 0-3 substituents selected from the group consisting of cyano, halo, alkyl, haloalkyl, alkoxy, haloalkoxy, and alkylSO 2 and R 1 is trialkylsilyl, alkoxy, alkylcarbonyl, benzyl, substituted benzyl, benzoyl, and pivaloyl.
[0010] Another aspect of the invention is a process where Ar 1 is 2,3-difluorophenyl and where R 1 is triisopropylsilyl for the compound of formula IV.
[0011] Another aspect of the invention is a process for the preparation of a compound of formula III, or a salt thereof, where R 2 is imidazolyl
[0000]
[0000] comprising coupling 3-N-piperidin-4-ylpyridine-2,3-diamine, or a salt thereof, or 1-(piperidin-4-yl)-1H-imidazo[4,5-b]pyridin-2(3H)-one, or a salt thereof, with carbonyl diimidazole or triphosgene and imidazole.
[0012] Another aspect of the invention is a compound of formula II, or a salt thereof, where Ar 1 is phenyl substituted with 0-3 substituents selected from the group consisting of cyano, halo, alkyl, haloalkyl, alkoxy, haloalkoxy, and alkylSO 2 and R 1 is hydrogen or trialkylsilyl, alkoxy, alkylcarbonyl, benzyl, substituted benzyl, benzoyl, and pivaloyl. Another aspect of the invention is a compound of formula II where Ar 1 is 2,3-difluorophenyl and R 1 is hydrogen or a salt thereof. Another aspect of the invention is a compound of formula II which is the dihydrochloride salt. Another aspect of the invention is a compound of or formula II where Ar 1 is 2,3-difluorophenyl and R 1 is triisopropylsilyl or a salt thereof. Another aspect of the invention is a compound of formula II which is the dihydrochloride salt.
[0000]
[0013] Another aspect of the invention is a compound of formula III, or a salt thereof, where R 2 is selected from the group consisting of imidazolyl, pyrrolyl, N-hydroxysuccinimidyl, chloro, phenoxy, substituted phenoxy, phenylthio, and substituted phenylthio. Another aspect of the invention is a compound of claim 12 where R 2 is imidazolyl.
[0000]
[0014] Unless specified otherwise, these terms have the following meanings. “Alkyl” means a straight or branched alkyl group composed of 1 to 6 carbons, preferably 1 to 3 carbons. “Alkenyl” means a straight or branched alkyl group composed of 2 to 6 carbons with at least one double bond. “Cycloalkyl” means a monocyclic ring system composed of 3 to 7 carbons. “Hydroxyalkyl,” “alkoxy” and other terms with a substituted alkyl moiety include straight and branched isomers composed of 1 to 6 carbon atoms for the alkyl moiety. “Haloalkyl” and “haloalkoxy” include all halogenated isomers from monohalo substituted alkyl to perhalo substituted alkyl. “Aryl” includes carbocyclic and heterocyclic aromatic ring systems.
[0015] Those skilled in the art understand that there are a variety of alternative reagents and solvents that can be interchanged. The following definitions are meant to serve as non-limiting examples to illustrate a term and are not meant to limit the definition to the examples listed.
[0016] Some suitable protecting groups at R 1 include trialkylsilyl, alkyl ether, benzyl ether, alkyl carbonate, benzyl carbonate, and ester. Trialkylsilyl includes TMS, TES, TIPS, TPS, TBDMS, and TBDPS. Alkyl ethers include methyl, MOM, BOM, PMBM, t-Butoxymethyl, SEM, THP, t-Bu, and allyl. Benzyl ether includes methoxybenzyl, dimethoxybenzyl, trifluoromethylbenzyl, nitrobenzyl, dinitrobenzyl, cyanobenzyl, and halobenzyl, diphenylmethyl and triphenylmethyl. Alkyl carbonate includes methyl, ethyl, isobutyl, vinyl, allyl and nitrophenyl. Substituted benzyl carbonate includes methoxybenzyl, dimethoxybenzyl and nitrobenzyl. Ester includes pivolate, adamantoate, benzoate, phenylbenzoate, and mesitoate.
[0017] Some suitable leaving groups at R 2 include imidazolyl, pyrrolyl, N-hydroxysuccinimidyl, chloro, substituted phenoxy, and substituted phenylthio. Substituted phenoxy includes nitrophenoxy, cyanophenoxy, and trifluoromethylphenoxy. Substituted phenylthio includes nitrophenylthio, cyanophenylthio, and trifluoromethylphenylthio.
[0018] Some suitable reductive amination conditions include using ammonia, hydroxyamine, protected hydroxyamine (for example, methoxyamine, benzyloxyamine, acetoxyamine), benzylamine, and the salts of these aminating reagents (for example, ammonium acetate, ammonium chloride). Benzyl includes methoxybenzyl, dimethoxybenzyl, trifluoromethylbenzyl, nitrobenzyl, dinitrobenzyl, cyanobenzyl, and halobenzyl, diphenylmethyl and triphenylmethyl.
[0019] Some suitable reagents for dehydrating agents in the reductive amination include titanium alkoxides, titanium chloride, mixed titanium alkoxides/chlorides, aluminum chloride, zirconium chloride, tin chloride, boron trifluoride, copper sulfate, magnesium sulfate, and molecular sieves. Titanium alkoxides include isopropoxide, propoxide, ethoxide, methoxide, butoxide, and t-butoxide.
[0020] Some suitable reduction conditions include transition metal catalyzed hydrogenations with for example, palladium, platinum, or iridium catalysts, metal hydrides of aluminum and boron, and zinc with acetic acid. Some catalysts include palladium on alumina, palladium on calcium carbonate, palladium-lead on calcium carbonate, palladium on carbon and Perlman's catalyst.
[0021] Some suitable acids for deprotecting the alcohol include any acid or fluoride containing reagent. For example, hydrogen chloride, hydrogen bromide, sulfuric acid, methanesulfonic acid, p-toluenesulfonic acid, trifluoroacetic acid, hydrogen fluoride, hydrogen fluoride-pyridine, and tetrabutylammonium fluoride.
[0022] Some suitable bases for the coupling include group I and II metal alkoxides (for example, sodium methoxide, potassium t-butoxide and sodium t-butoxide), group I metal disilazides (for example potassium disilazide), group I and II hydrides (for example, sodium hydride), group I amides (for example, lithium diisopropylamide), and group I metal alkydes (for example, butyl lithium).
Synthetic Methods
[0023] The following methods are for illustrative purposes and are not intended to limit the scope of the invention. Those skilled in the art understand that there will be a number of equivalent methods for the preparation of these compounds and that the synthesis is not limited to the methods provided in the following examples. For example, some reagents and solvents may have equivalent alternatives known to those in the art. The variables describing general structural formulas and features in the synthetic schemes are distinct from and should not be confused with the variables in the claims or the rest of the specification. These variables are meant only to illustrate how to make some of the compounds of the invention.
[0024] Abbreviations used in the description generally follow conventions used in the art. Some abbreviations are defined as follows: “1×” for once, “2×” for twice, “3×” for thrice, “° C.” for degrees Celsius, “eq” for equivalent or equivalents, “g” for gram or grams, “mg” for milligram or milligrams, “L” for liter or liters, “mL” for milliliter or milliliters, “μL” for microliter or microliters, “N” for normal, “M” for molar, “mmol” for millimole or millimoles, “min” for minute or minutes, “h” for hour or hours, “rt” for room temperature, “RT” for retention time, “atm” for atmosphere, “psi” for pounds per square inch, “cone.” for concentrate, “sat” or “sat'd “for saturated, “MW” for molecular weight, “mp” for melting point, “ee” for enantiomeric excess, “MS” or “Mass Spec” for mass spectrometry, “ESI” for electrospray ionization mass spectroscopy, “HR” for high resolution, “HRMS” for high resolution mass spectrometry, “LCMS” for liquid chromatography mass spectrometry, “HPLC” for high pressure liquid chromatography, “RP HPLC” for reverse phase HPLC, “TLC” or “tlc” for thin layer chromatography, “NMR” for nuclear magnetic resonance spectroscopy, “ 1 H” for proton, “δ” for delta, “s” for singlet, “d” for doublet, “t” for triplet, “q” for quartet, “m” for multiplet, “br” for broad, “Hz” for hertz, and “α”, “β”, “R”, “S”, “E”, and “Z” are stereochemical designations familiar to one skilled in the art.
[0025] Scheme 1 illustrates a synthesis of formula I compounds.
[0000]
DESCRIPTION OF SPECIFIC EMBODIMENTS
EXAMPLE 1
[0026]
[0027] (6S,9R)-6-(2,3-difluorophenyl)-9-(triisopropylsilyloxy)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-amine. To a 100 mL hastelloy autoclave reactor was charged (6S,9R)-6-(2,3-difluorophenyl)-9-(triisopropylsilyloxy)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-one (5.00 g, 11.22 mmol), 1,4-dioxane (50 mL) and titanium tetra(isopropoxide) (8.33 mL, 28.11 mmol). The reactor was purged three times with nitrogen and three times with ammonia. After the purge cycle was completed, the reactor was pressurized with ammonia to 100 psig. The reaction mixture was heated to 50° C. (jacket temperature) and stirred at a speed to ensure good mixing. The reaction mixture was aged at 100 psig ammonia and 50° C. for 20 h. The mixture was then cooled to 20° C. then 5% Pd/Alumina (1.0 g, 20 wt %) was charged to the autoclave reactor. The reactor was purged three times with nitrogen and three times with hydrogen. After the purged cycle completed, the reactor was pressurized with hydrogen to 100 psig and mixture was heated to 50° C. (jacket temperature) and stirred at a speed to ensure good mixing. The reaction mixture was aged at 100 psig H 2 and 50° C. for 23 h (reactor pressure jumped to ˜200 psig due to soluble ammonia in the mixture). The mixture was then cooled to 20° C. then filtered then transferred to a 100 ml 3-necked flask. To the mixture water (0.55 mL) was added drop wise, which resulted in yellow slurry. The resulting slurry was stirred for 30 min then filtered, then the titanium dioxide cake was washed with 1,4-dioxane (30 mL). The filtrate was collected and the solvent was removed. The resulting oil was dissolved in isopropanol (40 mL). To the solution ˜5N HCl in isopropanol (9.0 ml) was added drop wise resulting in a thick slurry. To the slurry isopropyl acetate (60 ml) was added and heated to 45° C. for 10 min and then cooled to 22° C. over approximately 3 h to afford a white solid (3.0 g, 51.5%). 1 H NMR (500 MHz, CD 3 OD) δ ppm 8.89 (d, J=5.3, 1H), 8.42 (bs, 1H), 8.05 (bs, 1H), 7.35 (dd, J=8.19, 16.71), 7.2 (bs, 2H), 7.22 (m, 1H) 7.15 (m, 1H), 5.7 (dd, J=1.89, J=8.51), 5.4 (m, 1H), 3.5 (m, 1H), 1.9-2.5 (B, 4h) 1.4 (sept, J=15.13,3H), 1.2 (t, J=7.57 18H); 13 C NMR (125 MHz, CD 3 OD) δ 153.5, 151.6, 151.5, 151.3, 149.4, 143.4, 135.03, 129.8, 129.8, 127.8, 126.8, 126.4, 118.6, 72.4, 54.1, 41.4, 34.3, 32.3, 25.4, 18.6, 18.5, 13.7, 13.6, 13.5, 13.3.
EXAMPLE 2
[0028]
[0029] (6S,9R)-5-amino-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-ol. To a 250 ml flask was charged (6S,9R)-6-(2,3-difluorophenyl)-9-(triisopropylsilyloxy)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-amine di HCl salt (15 g, 25.88 mmol) and a solution of isopropanol:water (45 mL:15 mL). The mixture was heated to 82° C. for 6 h then dried via azeotropic distillation at atmospheric pressure using isopropanol until the KF was less than <3%. After fresh isopropanol (25 ml) was added, the mixture was heated to 70° C. and then isopropyl acetate (45 ml) was added that resulting in a white slurry. The slurry cooled to 22° C. for 15 min to afford a white solid (9.33 g, 99%). 1 H NMR (500 MHz CD 3 OD) δ 8.77 (d, J=5.7 Hz, 1H), 8.47 (d, J=7.9 Hz, 1H), 8.11 (dd, J=6.0, 8.2 Hz, 1H), 7.21-7.32 (m, 3H), 5.53 (dd, J=3.8, 9.8 Hz, 1H) 5.33 (d, J=9.8 Hz, 1H), 3.5 (bm, 1H), 2.25-2.40 (m, 2H), 2.15 (bm, 1H), 1.90 (bm, 1H); 13 C NMR (125 MHz, MeOD) δ 159.4, 153.9, 151.9 and 151.8, 149.7, 143.6, 141.8, 135.7, 130.6, 127.7, 126.8, 118.9, 70.0, 54.9, 42.2, 34.5, 33.4.
EXAMPLE 3
[0030]
[0031] (5S,6S,9R)-5-amino-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-yl-4-(2-oxo-2,3-dihydro-1H-imidazo[4,5-b]pyridin-1-yl)piperidine-1-carboxylate. To a round bottom flask was charged (5S,6S,9R)-5-amino-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-ol dihydrochloride (1.00 g, 2.73 mmol) and dichloromethane (15 mL). A solution of sodium carbonate (0.58 g, 5.47 mmol), 20 wt % aqueous sodium chloride (5 mL), and water (10 mL) was added and the biphasic mixture was aged for 30 min. The phases were allowed to separate and the organic stream was retained. The dichloromethane solvent was then switched with azeotropic drying to tetrahydrofuran, with a final volume of (15 mL). At 20° C. was added, 1-(1-(1H-imidazole-1-carbonyl)piperidin-4-yl)-1H-imidazo[4,5-b]pyridin-2(3H)-one (0.95 g, 3.01 mmol), followed by a 20 wt % potassium tert-butoxide solution in THF (4 mL, 6.20 mmol). The thin slurry was aged for 1 h, and then the reaction was quenched with the addition of 20 wt % aqueous sodium chloride (5 mL) and 20 wt % aqueous citric acid (2.5 mL). The layers were allowed to separate and the organic rich layer was retained. The organic layer was washed with 20 wt % aqueous sodium chloride (15 mL). The organic tetrahydrofuran stream was then concentrated in vacuo to afford an oil which was resuspended in dichloromethane (20 mL) and dried with MgSO 4 . The dichloromethane stream was concentrated in vacuo to afford an oil, which was crystallized from ethanol:heptane to afford a white solid (1.14 g, 78.3%). LCMS: [M+H]=535: 1 H NMR (600 MHz, d 6 -DMSO) δ 11.58 (1H, bs), 8.45 (1H, bd), 8.03 (1H, d, J=7.3 Hz), 7.91 (1H, bs), 7.54 (1H, bd), 7.36 (1H, bm), 7.34 (1H, bm), 7.28 (1H, m), 7.21 (1H, m), 7.01 (1H, bs), 6.01 (1H, dd, J=3.2, 9.8 Hz), 4.48 (1H, d, J=9.5 Hz), 4.43 (1H, bm), 4.38 (1H, bm), 4.11 (1H, bm), 3.08 (1H, bm), 2.93 (1H, bm), 2.84 (1H, m), 2.62 (1H, bm), 2.20 (2H, bm), 2.13 (1H, bm), 2.12 (1H, bm), 1.75 (1H, bm), 1.72 (1H, bm), 1.66 (1H, bm); 13 C NMR (125 MHz, d 6 -DMSO) δ 156.6, 154.2, 153.0, 149.8, 148.1, 146.4, 143.5, 139.6, 137.4, 134.0, 132.8, 124.7, 124.5, 123.3, 122.2, 116.3, 115.0, 114.3, 73.7, 52.8, 50.0, 43.8, 43.3, 32.0, 30.3, 28.6; mp 255° C.
EXAMPLE 4
[0032]
[0033] 1-(1-(1H-imidazole-1-carbonyl)piperidin-4-yl)-1H-imidazo[4,5-b]pyridin-2(3H)-one. To a round bottom flask was added, 1,1′-carbonyldiimidazole (8.59 g, 51.4 mmol), diisopropylethylamine (12.6 mL, 72.2 mmol) and tetrahydrofuran (100 mL). This mixture was warmed to 40° C. and aged for 10 min, after which 1-(piperidin-4-yl)-1H-imidazo[4,5-b]pyridin-2(3H)-one dihydrochloride (10 g, 34.3 mmol) was added. The slurry was aged at 40° C. for 3 h, and then upon reaction completion, the solvent was swapped to acetonitrile which afforded an off white solid (9.19 g, 85.9%). LCMS: [M+H]=313; 1 H NMR (400 MHz, d 6 -DMSO) δ 11.58 (1H, s), 8.09 (1H, s), 7.97 (1H, d, J=8.0 Hz), 7.73 (1H, d, J=4.0 Hz), 7.53 (1H, s), 7.05 (1H, s), 7.00 (1H, dd, J=4.0, 8.0 Hz), 4.52, (1H, dd, J=8.0, 12.0 Hz), 4.05 (2H, bd, J=8.0 Hz), 3.31 (2H, m), 2.34 (2H, m), 1.82 (2H, bd, J=12.0 Hz); 13 C NMR (100 MHz, d 6 -DMSO) δ 153.0, 150.4, 143.4, 139.8, 137.2, 128.9, 123.0, 118.7, 116.4, 115.2, 49.3, 45.1, 28.5; mp 226° C.
EXAMPLE 5
[0034]
[0035] 1-(1-(1H-imidazole-1-carbonyl)piperidin-4-yl)-1H-imidazo[4,5-b]pyridin-2(3H)-one. To a 250 ml round bottom flask was added 3-N-piperidin-4-ylpyridine-2,3-diamine dihydrochloride (10 g, 52 mmol) and acetonitrile (100 mL). Triethyl amine (11.44 g, 113 mmol) and 1,1′-Carbonyldiimidazole (18.34 g, 113 mmol) were added at ambient temperature and the mixture was stirred for 2 h. The solvent was evaporated under vacuum to ˜30 ml reaction volume and isopropyl acetate (50 mL) was added into the resulting slurry at 40° C. The slurry was cooled to 10-15° C. and then stirred for 1 h to afford an off white solid (10 g, 85%).
[0036] It will be evident to one skilled in the art that the present disclosure is not limited to the foregoing illustrative examples, and that it can be embodied in other specific forms without departing from the essential attributes thereof. It is therefore desired that the examples be considered in all respects as illustrative and not restrictive, reference being made to the appended claims, rather than to the foregoing examples, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
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The disclosure generally relates to a process for the preparation of compounds of formula I, including synthetic intermediates which are useful in the process.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to strain measurement systems, and more particularly to a strain measurement module and strain measurement system using the strain measurement module, which is used to monitor a structure while collecting the strain information of the structure using a light generator and a fiberoptic sensor.
[0003] 2. Description of the Related Art
[0004] A conventional strain gauge used to diagnose the condition of a structure is disadvantageous in that it does not have durability sufficient to be used for the diagnosis of the structure, a measurement cooper wire must be provided in each of sensors, and it may influence the structure in the case of many measurement points because power must be supplied to measure resistance. For these reasons, various attempts have been made to replace the conventional strain gauge system with the fiberoptic sensor.
[0005] FIG. 1 is a schematic diagram showing the construction of a conventional strain measurement system 100 using a fiberoptic sensor.
[0006] As shown in FIG. 1 , the conventional strain measurement system 100 using the fiberoptic sensor includes a light generator 110 , an optical detection unit 130 , a compensation unit 140 , a fiberoptic sensor unit 150 and a control unit 160 .
[0007] The operation of the conventional strain measurement system 100 shown in FIG. 1 is described below.
[0008] A Light Emitting Diode (LED) driver 112 constituting a part of the light generator 110 supplies power to an LED 114 to generate light having a certain wavelength distribution. The generated light passes through a coupler 120 and proceeds to the fiberoptic sensor unit 150 attached to or embedded in a structure.
[0009] Although a variety of fiberoptic sensors may be used as the fiberoptic sensor unit 150 , FIG. 1 depicts an example in which Fiber Bragg Grating (FBG) sensors are used. Each of the FBG sensors reflects wavelengths of a certain width satisfying the Bragg's condition and passes the remaining wavelengths therethrough.
[0010] The reflected light reflected by the FBG sensor because it satisfies a certain wavelength condition proceeds to the optical detection unit 130 through the coupler 120 . The optical detection unit 130 passes only the reflected light of a certain wavelength therethrough using a Fabry-Perrot (FP) filter 134 and transfers the reflected light to an optical detector, such as a Photo Diode (PD) 136 . The FP filter 134 is provided therein with a lead-zirconate titanate (PZT) element (not shown) to be synchronized with the wavelength of the reflected light. Through the adjustment of the length of the PZT element depending on the extension and contraction of a cavity located in the FP filter 134 , the passage of the reflected light passes through the FP filter 134 is controlled. In order to control the extension and contraction of the PZT element as described above, the FP filter 134 is connected to a PZT driver 132 .
[0011] As described above, the PD 136 measures and outputs the intensity of reflected light. While the output from the PD 136 passes through a differentiator and a comparator, the peak point of the reflected light is detected and intensity is calculated at the peak point. The calculated intensity is input to a Central Processing Unit (CPU) 166 .
[0012] The CPU 166 detects the wavelength of the reflected light from a voltage value that is applied to the PZT driver 132 when the reflected light is detected. From the value of the detected wavelength, the variation of strain generated in the FBG sensor can be calculated.
[0013] To compensate for the non-linearity of a voltage-length relationship that the PZT element of the FP filter 134 has, the compensation unit 140 including an Ethalon filter 144 may be added to the system. The compensation unit 140 is constructed to include an LED 146 , an LED driver 148 , the Ethalon filter 144 and a compensation FBG 142 , and is connected to the coupler 120 . The light output from the LED 146 by the operation of the LED driver 148 is transferred to the coupler 120 through the Ethalon filter 144 and the compensation FBG 142 . The optical detection unit 130 measures the intensity of light in the same manner as in the reception operation of the reflected light, and transfers the measured intensity to the CPU 166 . The CPU 166 utilizes the output value detected in the optical detection unit 130 to compensate for the wavelengths of the reflected light transmitted from the fiberoptic sensor unit 150 .
[0014] In the above-described system, the construction and operation of the FBG 142 , the FP filter 134 and the Ethalon filter 144 are well known to those skilled in the art. Accordingly, detailed descriptions of those are omitted here.
[0015] Since the above-described conventional strain measurement system is provided with the LED having a low output that is used as a light signal, it is not easy to measure a signal. In particular, for architectural structures, the transmission distance of a signal is long, so that it is almost impossible to measure the signal. Furthermore, the conventional strain measurement system using the LED as a light source is disadvantageous in that it must be provided with a plurality of FP filters corresponding to a plurality of FBG sensors in the case where the plurality of FP filters are embedded at a plurality of locations.
[0016] In order to overcome the above-described problems, there was proposed another conventional strain measurement system equipped with a tunable laser generator in which a high output laser and an FP filter were disposed at a source stage. The tunable laser generator of this system uses an Erbium Doped Fiber Amplifier (EDFA) as an amplifying mechanism, which is illustrated in FIG. 2 .
[0017] The operation of the tunable laser generator is described with reference to FIG. 2 below. Weak signal light of about 1550 nm and a laser beam of 1480 nm generated in a pump laser 210 are joined together in a multiplexer 220 , and the joined signal light and laser beam are transferred to a fiberoptic amplifier 250 . The laser beam transferred to the fiberoptic amplifier 250 excites erbium ions Er 3+ to an upper level, while the signal light causes erbium ions to transition to a lower level. In this process, light of 1550 nm is induction-emitted and is joined with the signal light. The intensified signal light excites other erbium ions again so that further intensified light is emitted. The light amplified during circulation through the fiberoptic amplifier 250 passes through an FP filter 230 and is output as a laser signal having a certain wavelength.
[0018] As described above, the tunable laser generator overcomes a limitation in the transmission distance of a signal and simplifies the structure of a reception unit, but has many other problems.
[0019] The tunable laser generator is disadvantageous in that it must be provided with the laser diode and the multiplexer because it must use the laser beam as well as the signal light as input signals, an area that optical fiber occupies is large and, thus, causes the system to be complicated because amplification is performed in the optical fiber, and the temperature control of the laser generator is difficult. Furthermore, since the laser beam has high polarization and coherency compared with general light, an interference phenomenon is serious in an optical detector. Additionally, high manufacturing costs are incurred to apply the laser generator to the strain measurement system.
[0020] The strain measurement system using the tunable laser generator has a high output and can simplify the structure of the optical detector. However, the strain measurement system is problematic in that the structure of a source stage, that is, the laser generator, is complicated, the control of temperature is difficult, the fabrication of a high-precision system is difficult because a laser beam having high polarization and coherency is used as a signal, and the manufacturing costs of the system are high, compared with the strain measurement system using the LED as a light source. As a result, there has been a demand for a strain measurement system that is capable of overcoming the above-described problems.
[0021] Meanwhile, the two conventional strain measurement systems using optical fiber use the FP filter in the optical detector or laser generator. However, the FP filter is problematic in that it is sensitive to the variation of temperature. However, the conventional strain measurement systems do not provide any countermeasure to this problem.
SUMMARY OF THE INVENTION
[0022] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a strain measurement module and strain measurement system, which have simple structures, can be manufactured at low costs, and can perform high-precision measurement.
[0023] Another object of the present invention is to provide a strain measurement system and strain measurement system, which can reduce the variations of characteristic values due to the variation of temperature.
[0024] Still another object of the present invention is to provide a strain measurement module and strain measurement system, which are suitable for the case where a plurality of fiberoptic sensors are disposed at a plurality of locations to measure strain.
[0025] In order to accomplish the above object, the present invention provides a strain measurement system, including a tunable light generator comprising a SLD, and a tunable FP filter cascaded to an output terminal of the SLD to convert light having a wideband spectrum, which is generated in the SLD, into discrete optical signals having central wavelengths at regular intervals; a coupler for receiving and distributing the optical signals output from the tunable light generator; wavelength compensation means for receiving the optical signals from the tunable light generator through the coupler and detecting wavelengths of an optical signal output from the tunable light generator and passed through the FP filter; a fiberoptic sensor unit for receiving the optical signals from the tunable light generator through the coupler and transmitting a response signal corresponding to a variation of strain attributable to load; and an optical detector for detecting the response signal output from the fiberoptic sensor through the coupler.
[0026] In the present invention, the fiberoptic sensor unit may be a FBG sensor unit. In the case where the FBG sensor is used, the present invention may further include a reference FBG sensor between the coupler and the FBG sensor unit to provide a reference value used for wavelength calculation of the FBG sensor unit. In the present invention, the wavelength compensation means may include an Ethalon filter and a second optical detector.
[0027] Additionally, in the present invention, the FP filter may be provided with a thermistor and a thermoelectric element to allow temperature of the FP filter to be controlled. The SLD may be also provided with a thermistor and a thermoelectric element to allow temperature of the SLD to be controlled.
[0028] The present invention can be easily applied to the case where a plurality of optical sensors are disposed at a plurality of locations. In this case, the present invention provides a strain measurement system, including a tunable light generator comprising a SLD, and a tunable FP filter cascaded to an output terminal of the SLD to convert light having a wideband spectrum, which is generated in the SLD, into discrete optical signals having central wavelengths at regular intervals; a first coupler for receiving and distributing the optical signals output from the tunable light generator; a wavelength compensation means for receiving the optical signals from the tunable light generator through the first coupler and detecting wavelengths of an optical signal output from the tunable light generator and passed through the FP filter; a plurality of second couplers for receiving and distributing the optical signal output from the tunable light generator and passed through the first coupler; a plurality of fiberoptic sensor units connected to the plurality of second couplers to receive the optical signals output from the tunable light generator and transmitting response signals corresponding to variations of strain attributable to load; and a plurality of first optical detectors connected to the plurality of second couplers to detect the response signals output from the fiberoptic sensors.
[0029] The strain measurement module and strain measurement system of the present invention have simple structures, can be manufactured at low costs, and can perform high-precision measurement using the tunable light generator.
[0030] The strain measurement system and strain measurement system of the present invention are each provided with a means for controlling the temperature of the FP filter, thus providing temperature stability and high-precision measurement.
[0031] The strain measurement system and strain measurement system of the present invention can be applied to the case where a plurality of fiberoptic sensors are disposed at a plurality of locations to measure strain because a Super Luminescent light emission Diode (SLD) is used as a light source, and enable the structure of a reception stage to be simplified because the FP filter is installed at a light generator side.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] The above and other objects, features and advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
[0033] FIG. 1 is a schematic diagram showing the construction of a conventional strain measurement system using an LED as a light source;
[0034] FIG. 2 is a schematic diagram showing the construction of a conventional tunable laser generator;
[0035] FIG. 3 is a view showing a tunable light generator used in a strain measurement module and strain measurement system in accordance with an embodiment of the present invention;
[0036] FIG. 4 is a schematic diagram showing a strain measurement system using the tunable light generator of FIG. 3 ;
[0037] FIG. 5 is a graph showing optical signal data waveforms obtained in a compensation optical detector and a sensor optical detector after being passed through an Ethalon filter as time elapses; and
[0038] FIG. 6 is a schematic diagram showing a strain measurement system equipped with a plurality of FBG sensor units to detect strain at a plurality of locations in accordance with another embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0039] Reference now should be made to the drawings, in which the same reference numerals are used throughout the different drawings to designate the same or similar components.
[0040] FIG. 3 is a view showing a tunable light generator 100 used in a strain measurement module and a strain measurement system using the strain measurement module in accordance with an embodiment of the present invention.
[0041] As shown in the drawing, the tunable light generator 100 of the present invention employs a SLD 314 as a light source. The SLS 314 is driven by a SLD driver 312 . The SLD 314 generates light having a broadband spectrum, which has a short coherency length and is unpolarized compared with a laser beam. The SLS 314 has an output range of 1 mW, which is greater than that (about 50 μW) of an LED. Accordingly, even in the case where an optical loss may be incurred because a transmission distance is lengthened, the SLD 314 is suitable for a light source.
[0042] The light having a wideband spectrum, which is emitted from the SLD 314 , is directed to a filter means, such as a FP filter 318 . Although not shown, the FP filter 318 is formed of two coated mirror surfaces positioned at the ends of two strands of optical fiber and a cavity positioned between the two coated mirror surfaces, and functions as a resonator that passes light of certain wavelengths, which are defined by the length of the cavity (the interval between the two mirror surfaces), therethrough. As described above, the light that has passed through the FP filter 318 has a peak that has a very small Full Width Half Maximum (FWHM).
[0043] The FP filter 318 is equipped with a means for varying the wavelengths of transmitted light by adjusting the length of the cavity, for example, a PZT element (not shown). The PZT element adjusts the length of the cavity by being extended or contracted depending on the magnitude of voltage supplied from the PZT driver 316 . The PZT driver 316 supplies waveform voltage, that is, saw tooth voltage, which repeatedly increases by a certain magnitude, for example, 0.01 V, within a range of −10 V to +10 V as time elapses, to the PZT element at regular intervals. As a result, the FP filter 318 converts the light having a wideband spectrum, which is generated from the SLD 314 , into a discrete optical signal having central wavelengths that are spaced apart from each other at certain intervals corresponding to the intervals of voltages applied from the PZT element, and continuously outputs the discrete optical signal.
[0044] As described above, the tunable light generator 310 of the present invention is characterized in that it employs the SLD as a light source, and is provided with the FP filter 318 that is cascaded to the output end of the SLD and can vary transmitted wavelengths. However, the present invention is not limited to this construction, and provides an FP filter structure that overcomes the defective in which the FP filter has characteristics sensitive to temperature.
[0045] In more detail, the FP filter 318 has a variation of a transmitted central wavelength of about 1 nm according to a variation of temperature of 1° C. This phenomenon is attributable to the temperature dependency of the PZT element used to control the length of the cavity of the FP filter 318 . The influence of the temperature dependency of the FP filter on the strain measurement system may be described in connection with a Free Spectral Range (FSR). The FSR refers to each of ranges (repeated intervals) in which the transmitted wavelength characteristics of the FP filter are repeatedly exhibited, and actually restricts wavelength ranges in which the FP filter can be used. For example, in the case where a light source having a central wavelength of 1550 nm is used, the FSR is about 50 nm. Accordingly, the variation of the transmitted wavelength (1 nm/° C.) depending on the temperature variation of the central wavelength is great compared with that of the FSR (that is, 50 nm). Accordingly, inconvenience arises in that a correction process is necessary to compensate for the temperature variation.
[0046] The temperature dependency of the FP filter causes another problem. As described above, the light generated in the light source has a wide spectrum approximate to the Gaussian distribution. For example, the output light of the SLD has a FWHM of 45 nm and the Gaussian distribution. When the variation of temperature is applied to the FP filter when such a light source is employed, the transmitted wavelength range transitions. That is, light of a higher-intensity wavelength range does not pass through the FP filter, while light of a lower-intensity wavelength range passes through the FP filter. A decrease in the intensity of an optical signal influences the reception sensitivity of the optical detection unit and, thus, makes the stable and precise measurement of wavelengths difficult.
[0047] For this reason, the FP filter 318 is provided with a temperature measurement sensor, such as a thermistor 316 , and a temperature regulator, such as a thermoelectric element 317 , so as to uniformly control the temperature of the FP filter 318 . The temperature of the FP filter 318 measured by the thermistor 319 is transmitted to a controller, and the controller controls the temperature of the FP filter 318 within a certain range by operating the thermoelectric element 317 . A microprocessor can be used as the controller.
[0048] Additionally, the SLD 314 is provided with a thermistor 315 and a thermoelectric element 313 to further weaken the temperature dependency of the tunable light generator. The operation of the thermistor 315 and the thermoelectric element 313 is the same as that of those of the FP filter.
[0049] FIG. 4 is a schematic diagram showing a strain measurement system using the tunable light generator 310 described in conjunction with FIG. 3 .
[0050] Referring to FIG. 4 , the strain measurement system includes the tunable light generator 310 , a coupler 320 , a sensor optical detector 330 , a wavelength compensation means 340 and a processor 360 .
[0051] As described above, the tunable light generator 310 includes the SLD 314 and the tunable FP filter 318 cascaded to the SLD 314 . The FP filter 318 and the SLD 314 may be each connected to the thermistor 319 or 315 and the thermoelectric element 317 or 313 .
[0052] The optical signal generated from the tunable light generator 310 to have a low FWHM and be discrete at regular intervals proceeds to a reference FBG sensor 325 and a FBG sensor unit 350 through the coupler 320 . Of the optical signal, a response signal reflected because it coincides with the grating interval of the reference FBG sensor 325 and the FBG sensor unit 350 , that is, the reflected light, passes through the coupler 320 and is detected by the sensor optical detector 330 .
[0053] A part of the optical signal generated in the tunable light generator 310 proceeds to the wavelength compensation means 340 through the coupler 320 . The wavelength compensation means 340 compensates for the non-linearity of a voltage-length relationship that the FP filter 318 of the tunable light generator 310 has, and calculates the precise wavelength of the response signal, that is, the reflected light, output from the FBG sensor unit 350 . As shown in FIG. 4 , the wavelength compensation means 340 includes an Ethalon filter 344 and a compensation optical detector 345 . As well known to those skilled in the art, the Ethalon filter 344 has the characteristic of passing therethrough light of corresponding wavelengths at regular wavelength intervals (for example, 100 GHz in terms of frequencies). The light passed through the Ethalon filter 344 is detected by the compensation optical detector 345 . The optical signal detected by the compensation optical detector 345 is used to calculate the wavelengths of the light detected in the sensor optical detector 330 as described later.
[0054] In FIG. 4 , the processor 360 that controls the operation of the tunable light generator 310 , the sensor optical detector 330 and the compensation optical detector 345 is shown. The processor 360 controls the SLD driver 312 , the thermistors 315 and 319 and the thermoelectric elements 313 and 317 , and calculates the intensity and wavelengths of the reflected light output from the FBG sensor unit 350 and detected by the sensor optical detector 330 . The processor 360 may be provided with Analog to Digital (AD) converter or Digital to Analog (DA) converter to control the components 310 , 330 and 340 constituting parts of the strain measurement system of the present invention. Of course, the AD converter or DA converter may be provided in each of the components 310 , 330 and 340 in the form of a separate part.
[0055] As described above, the processor 360 functions to calculate the wavelengths of the reflected light detected by the sensor optical detector 330 using the optical signal measured by the wavelength compensation means 340 . To this end, appropriate software may be installed on the processor 360 .
[0056] The remaining components of the strain measurement system described in conjunction with FIG. 3 except for the FBG sensor unit 350 , that is, the tunable light generator 310 , the coupler 320 , the wavelength compensation means 340 , the sensor optical detector 330 , the reference FBG sensor 325 and the processor 360 , may be provided in the form of a strain measurement module. The reference FBG sensor 325 is preferably provided in the strain measurement module so as to be prevented from being influenced by weight. In this case, the strain measurement module is provided with slots (not shown) to connect with the reference FBG sensor 325 and the FBG sensor unit. Meanwhile, in the case where the processor 360 is not contained in the strain measurement module but is implemented by a Personal Computer (PC), the strain measurement module is provided with an interface to communicate with the PC.
[0057] Since the strain measurement module and strain measurement system of the present invention described in conjunction with FIG. 4 use the light generated from the tunable light generator 310 , interference is considerably reduced, and the reflected light output from the FBG sensor unit 350 can be precisely and stably detected because the temperature of components having high temperature dependency, that is, the FP filter 318 and the SLD 314 , is uniformly maintained, compared with a conventional EDFA system using laser.
[0058] Hereinafter, a process of calculating the wavelengths of reflected light detected by the sensor optical detector 330 using the strain measurement system shown in FIG. 4 , and the particular advantages of the present invention are described. As described above, in the calculation of the reflected light, compensation for the non-linearity of the FP filter must be taken into consideration. This point is described with reference to actual experimental data obtained by calculating the optical signals detected by the sensor optical detector and the compensation optical detector.
[0059] The light of the SLS used in an experiment had an input of 1 mw, a central wavelength of 1550 nm, and an FWHM of 45 nm. The FP filter used in the experiment had an insertion loss of 2.13 dB and an FSR of 50.526 nm. The FWHM of the optical signal output from the FP filter was 56 pm. The FP filter was operated so that voltage was applied to the PZT element of the FP filter while repeatedly increasing by 0.01 V within a range of −10 to +10 V. During the operation of the FP filter, temperature was uniformly maintained. For the FBG sensor, there was employed one having wavelengths of a band of 1550 nm, a self length of 2.0 cam, a line width smaller than 0.2 nm, and a reflectivity of 90%. For the Ethalon filter, there was used a thin film filter that passes therethrough a peak wavelength at every 100 GHz. The insertion loss of the thin film filter was 1 dB, and the loss of the thin film filter was −11.8 dB in a band rejection region.
[0060] FIG. 5 is a graph showing optical signal data obtained in the compensation optical detector 345 and the sensor optical detector 330 after being passed through the Ethalon filter 344 as time elapses. For reference, voltages applied to the FP filter are shown as well. In the graph, the physical properties are normalized values.
[0061] In FIG. 5 , a waveform indicated by reference character S relates to optical signals reflected from the FBG 325 and the FBG sensor unit 350 . In the waveform S, a first peak S 0 represents an optical signal reflected by the reference FBG sensor 325 , and following peaks S 1 to S 3 represent optical signals reflected by component sensors FBG 1 , . . . , and FBGn constituting the FBG sensor unit 350 . A waveform indicated by reference character E represents the output optical signal of the tunable light generator 310 detected after being passed through the Ethalon filter 344 . A curve indicated by reference character F shows driving voltage applied to the FP filter 318 as time elapses.
[0062] As described above, the first peak S 0 of the waveform S indicates the reflected light reflected by the reference FBG sensor 325 , whose wavelength is known. Additionally, since, according to the transmission characteristics of the Ethalon filter 344 , the peaks of the waveform E are formed at regular intervals, the wavelength of the peak E 1 of the waveform E adjacent to the first peak S 0 of the waveform S can be found from the wavelength of the first peak S 0 of the waveform S. If the wavelength of the peak E 1 is found, the wavelengths of all the peaks of the waveform E can be found. In this case, the wavelengths of the second to fourth peaks S 1 to S 3 of the waveform S can be found on the assumption that a proportional relationship exists between each of the peaks S 1 to S 3 and the wavelength of the peak of the waveform E adjacent to the peaks S 1 , S 2 or S 3 .
[0063] The method of the present invention is considerably effective compared with the conventional strain measurement system, in view of the structures of the wavelength compensation means and the optical detector. As described in conjunction with FIG. 1 , in the conventional strain measurement system, the compensation unit 140 is provided with another light source 146 , so that the optical detector 136 must be used to measure not only a reflected light output from the FBG sensor unit 150 but also a light signal output from the compensation unit 140 . As a result, the optical detector 136 must alternately measure the reflected light and the optical signal and, thus, causes delays in measurement. However, since, in the present invention, the waveform compensation unit 340 comprised of the Ethalon filter 344 and the compensation optical detector 345 is employed, reflected light and an optical signal can be measured at the same time.
[0064] FIG. 6 is a schematic diagram showing a strain measurement system equipped with a plurality of FBG sensor units to detect strain at multiple locations in accordance with another embodiment of the present invention.
[0065] In FIG. 6 , the construction and operation of a tunable light generator 310 , a first coupler 320 and a wavelength compensation means 340 are similar to those of FIG. 4 . In the system of FIG. 6 , two FBG sensor units, that is, a FBG sensor unit 1 (FBG 11 , FBG 12 , . . . , and FBG 1 n ) and a FBG sensor unit 2 (FBG 21 , FBG 22 , . . . , and FBG 2 n ), constitute a collection of FBG sensor units 350 ′. Two second couplers 322 and 324 are required to connect the collection of FBG sensor units 350 ′ with the tunable light generator 310 . Additionally, a reference FBG sensor 1 and a reference FBG sensor 2 are included to provide reference wavelengths with respect to reflected light output from the two FBG sensor units. Of course, it is not necessary to provide reference FBG sensors of a number proportional to the number of the FBG senor units, but a single reference FBG sensor may be provided for a plurality of FBG sensor units.
[0066] Although FIG. 6 illustrates the case where the two FBG sensor units are disposed at two different locations, the present invention is not limited to this. It will be apparent to those skilled in the art that the inventive concept of the present invention can be easily applied to the case where three or more FBG sensor units are disposed.
[0067] The strain measurement system described in conjunction with FIG. 6 has particular advantages compared with the conventional strain measurement system. In the conventional strain measurement system, it is impossible to perform measurement through a plurality of FBG sensor units disposed at various locations because the output of a light source is low, and an FP filter must be provided in each of optical detectors even though the plurality of FBG sensor units are disposed. However, as shown in FIG. 6 , when the tunable light generator 310 of the present invention is used, light signals output from a plurality of FBG sensor units can be detected using a signal FP filter.
[0068] The remaining components of the strain measurement system described in conjunction with FIG. 6 except for the collection of FBG sensor units 350 ′ may be provided in the form of a strain measurement module. In this case, appropriate slots (not shown) may be added to connect with the collection of FBG sensor units 350 ′, and an interface may be provided in the strain measurement module to communicate with a PC in the case where the PC functions as the processor.
[0069] As described above, the strain measurement system of the present invention has been described with reference to FIGS. 4 and 6 . Since a method of obtaining actual strain, which an optical sensor experiences, from the wavelength of reflected light obtained through the above-described process can be easily calculate by those skilled in the art based on the properties of optical fiber, a description of the method is omitted here.
[0070] Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
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A strain measurement system includes a tunable light generator, a coupler, a fiberoptic sensor unit, and an optical detector. The tunable light generator includes a Super Luminescent light emission Diode (SLD), and a tunable Fabry-Perrot (FP) filter cascaded to an output terminal of the SLD to convert light having a wideband spectrum into discrete optical signals. The coupler receives and distributes the optical signals and passes them to a wavelength compensation device which detects wavelengths of the optical signals. The fiberoptic sensor unit receives the optical signals from the tunable light generator through the coupler and transmits a response signal corresponding to a variation of strain attributable to load. The optical detector detects the response signal output from the fiberoptic sensor through the coupler.
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This is a division of application Ser. No. 156,852, filed June 25, 1971, now U.S. Pat. No. 3,803,784.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a novel and advantageous development of composite wall elements for walls, ceilings, and floors of every type, for every purpose, and of any suitable material, and in particular also to composite wall elements useful, for instance, for refrigerator houses and refrigerator chambers of means of transportation or the like.
2. Description of the Prior Art
A known wall unit of this kind comprises two sheet metal panels of equal size, sealing strips of resilient material arranged between the margins of said panels, and insulating plates filling the cavity between said panels. When used as components of an external wall, the individual wall units are suspended on wall supports by means of angle brackets. Similar wall units serve as partition walls extending from floor to ceiling for internal rooms. The thermal and acoustic insulation of such wall units is, however, poor.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide novel composite structural elements which are superior in their thermal and acoustic insulation properties to heretofore known insulating structural elements.
Other objects and advantageous features of the present invention will become apparent as the description proceeds.
To enable a person skilled in this art to clearly and completely understand the present invention, the entire structural element according to the present invention together with the insulating element provided therein will be referred to hereinafter and in the claims annexed hereto as "composite wall element", while the actual insulating element will be referred to as "smaller insulating wall element" or "inner wall element" and the outer wall of the composite wall element will be referred to as the "outer wall element".
In principle the composite wall element according to the present invention comprises
A. AN INNER WALL ELEMENT OR SMALLER INSULATING WALL ELEMENT, SAID INNER WALL ELEMENT BEING ARRANGED WITHIN
B. AN OUTER, PRESSURE RESISTANT, PREFERABLY LOAD SUPPORTING, LARGER WALL ELEMENT ENCLOSING THE INNER WALL ELEMENT. Thereby
c. a substantially dry gas and preferably air atmosphere under subatmospheric, atmospheric, or superatmospheric pressure is established and maintained in the inner insulating wall element, for instance, by evacuating the inner wall element or by filling it with a dry gas, preferably dry air.
The smaller insulating wall element consists of a flexible or rigid envelope which seals off the element in air-tight, and preferably vapor-tight, fashion. It is composed, for instance, of plastic material. Within said envelope there are arranged insulating elements, preferably reflective sheets or foils, for instance, aluminum foils or plastic foils which have aluminum vapor-deposited thereon. Between said reflective sheets or foils there are provided preferably pressure-resistant spacers, for instance, reflecting honeycombs of hardened or cured cardboard or plastic.
In place of reflective honeycombs of plastic material having, for instance, a vapor-deposited layer of aluminum, there can also be used flat and/or corrugated plastic boards with reflective coatings, preferably combined in groups.
In place of flexible or rigid envelopes, there can be provided plates or sheets spaced apart from each other and consisting, for instance, of reflectively coated plastic material which are preferably connected with each other at least in air-tight manner on all sides, forming a box-like hollow space.
Around this smaller insulating inner wall element there is cast a pressure resistant outer wall element in such a manner that the inner wall element is surrounded preferably on all sides at least in an air-tight manner. The outer wall element may be composed, for instance, of several individual parts and providing more in particular an inner hollow space which serves to receive the inner insulating wall element.
Thus it is possible to impart to the resultant composite wall element extremely high insulating properties and at the same time any desired load supporting and compressive strength. Both the construction of the inner wall element and that of the outer wall element permit, of course, variations and combinations depending on and corresponding to the individual purposes. Thus, for instance, the outer wall element may only partially surround the inner wall element. The parts of the inner wall element which are not surrounded and lie free can be closed off in air- or vapor-tight fashion, for instance, by means of cover plates of any suitable material. This has the advantage that different types of building materials, depending on the purposes in view, can be combined to form a composite element according to the present invention. That part which is provided or cast around the edge portions of the inner wall element can serve as load-bearing frame. All individual elements, for instance, can be cast in place when casting the inner wall element, or they can be connected in an immediately subsequent operation with the casting material before it has solidified. In this way there is obtained an integral composite element which encloses the inner wall element on all sides.
The inner wall element, and likewise the hollow space of the outer wall element, can be connected by pipes which extend therein and have controllable valves thereon, to gas or, preferably, air drying devices, volume equalization elements, gas or preferably air filter devices, and pressure and suction pumps. In this way it is possible to provide the inside of the wall element with dry gas or preferably air and to maintain this condition therein. In this way precipitation or deposition of water of condensation on the reflective foils is prevented upon a decrease in the temperature. The reflective power of the sheets would be almost entirely eliminated by such precipitation or deposition. For the same reason, it is necessary to seal the inner wall element in as vapor-tight a manner as possible. In order to make the envelopes or covering layers, for instance, the plastic boxes surrounding the inner wall element vapor-tight, a multi-layer construction of the envelope or covering layer or of the box material is provided in accordance with the present invention. If they consist, for instance, of plastic sheets or foils or of plastic panels, they can be bonded, welded, pressed, or otherwise connected flat with each other in multi-layers. Thereby the surfaces to be connected with each other can be metallically coated or can contain metal foils, for instance, aluminum foils, between the surfaces to be connected. Furthermore, the foils or sheets themselves can be made of plastics in which metal powder is admixed.
Finally, the envelopes or covers or the boxes, after completion of the insulating element, can be immersed, for instance, in liquid plastic material to which preferably powdered metal has been added. Metal foils can also be bonded in vapor-tight manner, for instance, overlapped, around the inner wall element. If the inner wall element is then, for instance, cast into an outer wall element, any access of air is prevented. Nevertheless, since, aside from metals and glass, practically all other building materials are pervious to the water vapor of the air in accordance with the water-vapor pressure gradient which is present at the time, the vapor can penetrate into the inner wall element if the envelope or cover of said inner wall element is not sufficiently vapor-tight. It is, therefore, advantageous to provide vapor barriers and the like also in the outer wall element, particularly on its front wall. In particular, the entire hollow space in the outer wall element can be lined in vapor-tight manner.
In order to increase the load-bearing capacity of the connection of the wall surfaces of the outer wall element which extend parallel to each other, connecting anchoring means or armatures passing in an air- and vaportight manner through the inner wall element, can also be cast in place.
For the casting in place of the composite wall element, different construction or, respectively, casting materials for the front and rear sides to be cast and the edge parts of the outer wall element can be used and combined with each other in liquid or pasty state.
The outer wall element can, for instance, be cast in advance on all sides with the exception of the surface directed towards the inner space, a corresponding recess or cavity into which the inner wall element is inserted being provided to receive said inner wall element. The inner wall element can be arranged within or inserted into said recess or cavity in a air- and vapor-tight manner thus occupying the entire distance or space formed by the recess or cavity of the outer wall element. The casting material can be suitably selected and can be formed, for instance, of several materials combined. In particular, it can form an additional vapor-tight covering of the inner wall element. Furthermore, the insulating properties can be increased, for instance, by producing a foamed insulating element, for instance, by foaming to a rigid plastic foam. In the case of such prefabricated outer wall shells, the inner surfaces of the recess or cavity can be shaped, for instance, corrugated. They can be coated in vaportight manner with reflective foils and thus form additional radiation spaces, for instance, of about 10 mm. depth, opposite the inner wall element. Or the inner wall element with its flexible coverings can be caused to snugly or closely contact or engage the corrugations of the inner wall of the hollow space or cavity by means of the superatmospheric pressure of the dry air introduced by a pressure pump via pipelines and pipe lengths, thereby forming corresponding radiation spaces towards the inside of the inner wall element. For this purpose the inner sides of the flexible plastic envelopes or covers are coated, for instance, by vapor deposition with aluminum or they are covered with aluminum foils. In the case of such a close contact of the envelopes or coverings of the inner wall element against the hollow space or cavity of an outer wall shell in which it is inserted, the casting operation can be dispensed with at least towards the profiled or corrugated side of the outer wall element. The free surface of the inner wall element facing inside of the room of the building can nevertheless be cast or produced by foaming after suitably sealing the edges of the inner wall element. In its place there can be placed a covering board, for instance, a plaster board, which may also have a profiled or corrugated, reflecting, vapor-tight surface towards the inner element.
According to the present invention the hollow space or cavity of the outer composite wall element can also be provided or filled with a dry gas, preferably with dry air, said hollow space or cavity being lined, for instance, on all sides with aluminum in a vapor-tight manner and being sealed in a vapor-tight manner after insertion of the inner insulating element that preferably is also covered in a vapor-tight manner. Radiation chambers, for instance, horizontal radiation chambers preferably of a depth of about 10 mm. can be formed by providing spacing strips or bars. Insertion of the inner insulating element into the hollow space or cavity of the outer wall element filled with dry gas or air permits to arrange said inner insulating element in a completely pressureless, for instance, suspended or upright fashion so that heat conduction via the individual parts of the insulting elements contacting each other is reduced.
Of course, the vapor-tight inner wall elements as described hereinafter, can be inserted and preferably be cast in place in corresponding smaller dimension or size, for instance, into hollow bricks.
If vapor-tight sealing is secured by the envelope or covering or by the box of the inner wall element and, in addition thereto, by the outer wall element and its cavity or hollow space for an unlimited period of time, it is sufficient to fill the inner wall element with dry gas or air before sealing it or to effect its sealing in a dry gas or air chamber. As a matter of precaution, a certain quantity of gas or air drying agent, for instance, of calcium chloride, can be inserted in a perforated wrapping in the inner wall element.
BRIEF DESCRIPTION OF THE DRAWINGS
Illustrative embodiments of the invention and its advantages will be described below by way of example in the accompanying schematic drawings in which:
FIG. 1 is a cross-sectional view through a composite wall element consisting of an outer wall element and an inner wall element in place therein;
FIG. 2 is a cross-sectional view through a composite wall element consisting of an outer prefabricated wall shell with a hollow space and a plate or board covering said hollow space, as well as an inner wall element arranged therein;
FIG. 3 is a cross-sectional view through a composite wall element consisting of a peripheral supporting frame with a front plate or facade board and a cover plate or board provided parallel to the front plate, as well as an inner wall element within the hollow space thus formed;
FIG. 4 is a cross-sectional view through a composite wall element with a peripheral supporting frame and inserted cover plates or boards on both sides, the inner side of said boards being corrugated, and an inner wall element being provided between said boards;
FIG. 5 is a cross-sectional view of the same composite wall element as in FIG. 4, but with a flexible inner wall element;
FIG. 6 is a cross-sectional view of part of an inner wall element the inner surfaces of which reflect and are undulated vertically in the drawing, and contained between them a reflecting element with undulations which are horizontal in the drawing;
FIG. 7 shows in perspective cross-sectional and longitudinal sectional view another inner wall element consisting of a box-like outer body and inner insulating elements;
FIG. 8 shows in perspective a hollow block with its right corner cut away;
FIG. 9 is a schematic sectional view through composite wall elements of a building which are arranged in stories one above the other, with filter, drying, and volume equalization devices, and air pump.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows in cross-sectional view the upper part of a composite wall element according to the present invention. This wall element consists of an inner wall element serving as thermally insulating element. It is enclosed on all sides by a covering 10 composed, for instance, of plastic material and is sealed in an at least air-tight and preferably also vapor-tight manner in said covering 10. An outer wall element 15 which, of course, is larger than the smaller inner wall element with its covering 10 is cast around the latter and serves to impart to the resulting composite wall element the required bearing or breaking as well as compressive strength.
The covering 10 is coated at its inner surface with a foil 4 of aluminum or of plastic material having aluminum vapor-deposited on both of its faces in order to ensure vapor-tight sealing. Plates, sheets, or boards 1, 2, and 3 made, for instance, of hardened plastic foam, cardboard, wood, plastic material or the like are inserted all around into the covering 10 so as to impart the desired shape and rigidity to all the inner faces of said covering 10. The inner faces of said plates 1, 2, and 3 are also reflecting towards the inner cavity or chamber of the wall element formed by them due to the reflecting foils 4b provided thereon.
The inner hollow space of the inner smaller wall element is subdivided by the provision of another reflecting foil 4c in the middle of said space. Said foil 4c has perforations 4a which permit exchange and passage of dry air therethrough, if necessary. On both sides of this intermediate reflective foil 4c there are inserted honeycomb-like, preferably pressure resistant supporting and spacer means 5 and 6, for instance, of hardened cardboard or plastic material. Thus radiation and gas or air chambers with their dry gas or air content being at rest are formed. The walls of these honeycomb structures are arranged vertically upon the reflective foils 4b and 4c. They may also be perforated so as to permit replacement and/or renewal of the drying gas or air.
If the thickness of the honeycomb plates 4a is between 5 mm. and 10 mm., gas or air convection due to variations in the temperature cannot take place in the chambers. The honeycomb structures can also be reflective. In place of honeycomb-like structures, there can also be interposed between the separating foil 4c and the reflective foils 4b perforated or otherwise punched out hardened foam plates or the like which serve as chamber-forming supporting and spacer means 5 and 6. If covering 10 is constructed as a pressure resistant box, for instance, of plastic material, it is usually sufficient to stretch or otherwise arrange the reflecting foils or reflecting plates at a distance of about 10 mm. from each other.
A tube or pipe 7, preferably a square tube or pipe or plastic material with perforations 7a at its lower part is provided in the upper part of the inner wall element. U-shaped sieve 8 upon which a hygroscopic agent 9, for instance, calcium chloride is placed, is inserted into said tube 7 as a precautionary measure so as to ensure with certainty dryness of the gas or air enclosed in the hollow space or chambers of the inner wall element.
By the term "dry gas" or "dry air" as used in the specification and in the claims annexed hereto, there is understood a gas or air which has been dried to such an extent that the degree of saturation with relative humidity will never be attained.
The outer supporting wall element 15 cast or otherwise firmly placed around the inner, smaller, insulating wall element comprising structures 1, 2, and 3 and covering 10 can consist of the most suitable structural material adapted to the desired purpose, for instance, of concrete. By casting the outer wall element around the inner wall element and thus completely enclosing the latter, air- and vapor-tight sealing of the inner wall element is additionally secured. Suitable additives can be admixed to the structural material forming the outer wall element for further improving the air- and vapor-tight seal of the inner wall element. As a result of providing such a multiple enclosure and sealing of the inner wall element the dry gas or air present therein remains in the dry state for an unlimited period of time.
It may, however, be desired to connect the inner wall element with an air drying device. For this purpose pipes 16 which are fitted in vapor-tight manner, extend from the outer wall element into the inner wall element and extend, for instance, via replaceable air drying devices 17 through pipes 18 provided with valves 19 out of the outer wall element 15. In this way it is possible subsequently to renew the air in the hollow space of the inner wall element if required.
Furthermore, all inner wall elements can be connected via pipe connections and manifolds with an air pump and circulation of dry air can be effected from time to time. For this purpose it is advisable to provide, for instance, the honeycomb-like and other supporting and spacer means with holes for the circulation of air.
FIG. 1, furthermore, shows two-part connecting and securing anchoring means 11 and 12 which can be joined by screwing said parts 11 and 12 together. These anchoring means are provided with pressure transmitting disks 14. Said disks 14 transmit the pressure from one of the walls 15 to the other wall 15 which is parallel opposed thereto and thus serve for increasing the compression or crushing strength of the composite wall element.
Preferably those places of the inner insulating wall element 10 through which the anchoring means 11 and 12 pass, are provided with corresponding borings or bore holes before inserting the anchoring means. The anchoring means parts 11 and 12 are inserted from both sides through said holes and are fit into one another. Part 12 is provided with screw thread 13 and part 11 with its corresponding internal thread 13a and both parts 11 and 12 are screwed together. The outer wall element is cast around the inner wall element. Disks 14 are arranged so that they vapor-tightly seal the holes in covering or box 10 and, as stated above, serve for pressure transmission by suitable attachment to anchoring means 11 and 12.
Improved pressure resistance is also achieved in a similar manner when using cover plates as described hereinafter in FIGS. 2 to 5 whereby corresponding recesses are provided in said cover plates.
FIGS. 2 to 5 show in cross-sectional view various embodiments of wall elements according to this invention.
FIG. 2 shows a preferred outer wall shell 21 with hollow space 22 which is vapor-tightly sealed on its inner sides, for instance, by aluminum foils 24a and multi-layer plastic foils 24b, thereby avoiding formation of heat bridges. Inner, air-filled or evacuated wall element 23 which is covered all around in vapor-tight manner is placed on spacer ledges 25 into said shell 21. Space 22 is then filled by pouring or foaming with a suitable building material 26. In this way vapor-tight sealing of the inner wall element is assured, the insulating effect with respect to temperature changes and sound transmission is improved, and the loadbearing and compressive strength of the outer wall element 21 is increased. Changes in pressure in the inner wall element caused by variations in temperature, are without effect on the outer wall element.
The outer wall element also includes cover wall 27 directed towards the inside, for instance, a plaster board or concrete slab. Towards the inner wall element it bears a vapor-tight coating 28, as a result of which the hollow space 22 is sealed in a vapor-tight manner all around.
To reduce heat conduction between wall shell 21 and cover wall 27, an insulating strip or band 20 consisting, for instance, of foamed plastic, such as rigid cellular polymers, glass fibers, rubber, or the like, or combinations of such insulating materials, is peripherally interposed in an air- and vapor-tight manner.
FIG. 3 shows a variant of the insulating wall element of FIG. 2. In this case the wall shell 21 of FIG. 2 is made of two parts and consists of a peripheral bearing and supporting frame 21a and a front or facade plate 21b which closes this frame off towards the outside. The cover plate or board 27a arranged towards the inside of the building is inserted into the peripheral frame 21a.
Preferably the vapor-tightly sealed hollow space 22 is filled with dry air, for instance, by introducing therein hygroscopic agents such as calcium chloride. The inner insulating element 23 is arranged either suspended or fixed between spacing ledges, strips, or bars 25 in a pressureless manner. The inner walls of the hollow space 22 as well as the covering 23a of the inner insulating element 23 are coated with reflective layers and the space between the horizontally extending spacing ledges, strips, or bars 25, said space having a depth of about 10 mm., is subdivided into numerous shallow radiation chambers. The ledges, strips, or bars 25 can be omitted and the hollow space 22 can be filled, for instance, with plastic foam plates which are preferably coated on both sides with metal foils and which form an air- and vapor-tight box-like structure after insertion of the insulating element 23 and 23a. To reduce heat conduction between front or face plate 21b and supporting frame 21a a peripherally arranged insulating strip or band 20, as in FIG. 2, is air- and vapor-tightly interposed.
If chamber-forming honeycombs are provided as spacing means in the insulating element 23 (see for instance, FIG. 1, parts 5 and 6), their heat conductivity can be considerably reduced by cutting jagged notches or recesses into the webs or bridges of the honeycombs so that there is only pointwise contact between the chambers. Due to the pressureless embedding of the insulating element 23, 23a into the cavity 22 the contact of all the parts of the wall element which causes heat conduction is reduced to a minimum. Another means of reducing heat conduction consists in applying a slight positive pressure of the dry air in the insulating element 23 which advantageously prevents contact of the parts of the wall element.
FIG. 4 shows another embodiment of the present invention providing a peripheral supporting frame 21a and therewithin cover boards 21c and 27b inserted from both sides. These two cover boards are corrugated on their inner sides and are provided with reflective, vapor-tight coverings 27c and 21d, respectively. In this way radiation spaces 31 are formed radiating towards the inner wall element 23 which also carries a reflective, vapor-tight covering on its outer surfaces 23a. These radiation spaces serve further to increase the effectiveness of the heat-cold insulation. These radiation spaces 31 can be provided with dry air as well as with compressed air or vacuum via pipe lengths 29 which extend on both sides of the element 23 into the radiation spaces 31 and which bear valves 30. Pipelines 32a with valves 33 can be inserted into the inner wall element 23 for ventilating with dry air.
FIG. 5 shows a variant of FIG. 4. The flexible outer coverings 23a of the wall element 23 can be pressed by air pressure via pipe lengths 32a and 32b against the corrugated inner surfaces 27c and 21d of the two cover boards 21c and 27b. Thus by adapting the flexible covering 23a which is reflective on its inner side, to the corrugated shape there are produced within the wall element corresponding radiation spaces 23c. Inner reflective foils 23d are provided in the interior of the inner insulating wall element 23 as indicated in perspective view in FIG. 7 by reflective foils 54.
FIG. 6 shows in cross-sectional view an airtight, vapor-tight inner wall element consisting of two outer insulating boards 41, their inner walls being provided with vertically corrugated surfaces 42 which are covered with reflective foils 43, and of an interposed insulating board 45 provided with horizontally corrugated surfaces 44, which surfaces are also covered on both sides with reflective foils 46. Between the insulating boards 41 and 45 there are clamped vertical reflective foils 47 by which the radiation spaces are subdivided. The hollow space between the boards 41 is sealed hermetically on all sides by frame-like peripheral edge parts 48 and the joints are also closed in air-tight and vapor-tight fashion by the bonding thereon of sealing strips 48a, for instance, of aluminum foils. Hygroscopic agents 50 can be provided as a matter of precaution on screens in recesses 49 in said edge strip 48 after dry air has been introduced into the radiation spaces. In the same way as the inside of the profiled surfaces are lined with vapor-tight and preferably metallic reflective foils, the surface or outer face of the wall element can also be covered on all sides with vaportight foils, for instance, with metal foils 51, which effect hermetical and vapor-tight sealing.
The boards 41 and frame 48 can consist of any suitable material, for instance, rigid plastic foam, corrugated cardboard, plastic material, plaster, glass, and the like. Hardened corrugated cardboard can be provided with a reflective coating, for instance, on all of its parts, i.e. on both sides of the corrugations and on both sides of the flat intermediate surfaces and the outer surfaces.
FIG. 7 shows in perspective view and in transverse and longitudinal section another type of inner wall element consisting of a box-like outer body 52 with vaportight outer covering 51 and inner reflective covering 53; of reflective foils, reflective boards; panels, and the like parts 54 arranged perpendicular thereto at a distance of about 10 mm., as well as of alternately intersecting horizontally and vertically interposed corrugated reflective foils or panels 55 and 56 consisting, for instance, of plastic material with aluminum applied thereto by vapor-deposition.
Said corrugated reflective foils or panels 55 and 56 are preferably of such consistency and strength that the inner wall element is resistant to compression, independently of the strength of the box 52 or of a covering. To achieve such consistency and strength, the reflective foils and/or panels or boards 53, 54, 55, and 56 can be connected in any suitable manner with each other, for instance, by glueing, stapling, or welding, so as to form a single unit, similar to a multi-layer corrugated cardboard. The advantage of this arrangement of high-gloss reflective elements on both sides is to concentrate an extremely high heat-cold insulating capacity onto a very small crosssection. There are particularly suitable for this purpose plastic foils and plastic boards having aluminum vapordeposited thereon which, although highly reflective, does not result in any heat conduction, despite contact, because the thickness of the layer is only about twelve thousandths of a millimeter.
Such foils and/or flat or shaped highly reflective plastic boards or plates can also be arranged individually, for instance, in spacing gaps between two cover walls.
The flat reflective foils or plastic boards can be omitted and, for instance, merely vertically and horizontally intersecting corrugated reflecting means, preferably of plastic material can be arranged and grouped together.
FIG. 8 shows in perspective view a single hollow block 61 open towards the top. The right front corner of this block is illustrated broken away in order to show the hollow space 62. Into this hollow space rectangular inner wall elements 63 can be inserted in the same manner as described in FIGS. 1 to 6. Said inner wall elements are constructed and composed as described hereinabove. They are only of reduced scale. The upper opening of the hollow block can be covered by cover plates or by a lidlike cover 64, for instance, of plastic. Said cover can be developed recessed in order to receive the building material bonding it to the next block.
Pipe lengths 65 for evacuating the hollow space 62 or for filling it with or exchanging dry gas or air can also be provided in the same manner as in the previously described wall elements.
FIG. 9 is a schematic section through composite wall elements 21a according to the present invention, said wall elements forming the walls of a multi-storied building. These wall elements are connected to an air pump P, an air filter device S, a volume equalization device V, an air drying device T, adjustable inlet valves 71 and 71a, and outlet valve 72. Into each wall element there extends a transverse pipe line 32a extending from a common feedline 73 which conducts the air into the lower part of each composite wall element after it has been drawn in by pump P, filtered and dried. In this way the lighter, moist air collected in the upper part of each wall element is forced via upper transverse pipe lines 32b into a air discharge pipe 74 and escapes towards the outside through the adjustable outlet valve 72. Depending on the adjustment of the valves, any desired pressure can be imparted to the dry air in the wall elements. Said pressure can be maintained by the provision of intermediate valve 71a.
If filter and drying devices with an adjustable inlet valve are arranged at the upper end of pipe 74, then the pump remaining at the bottom can draw fresh dry air into the wall elements and force the moist air outwards through an adjustable outlet valve.
Depending on the adjustment of the valves, any desired vacuum can be produced when proceeding in this manner.
If the upper inlet valve is omitted and if the atmospheric air thus has free access through the filter and the drying devices, then the pressure in the hollow space of the wall element is at all times the same as the atmospheric pressure. That the air in the wall element remains continuously dry is assured by providing the drying device. However, when the wall element is in open connection with the atmosphere, the volume equalization device is dispensed with.
On the other hand, if the valves close off the wall elements from the outside atmosphere, the volume equalization device can actuate a contact switch 76 as soon as the movable equilization part V descends in its casing as a result of a reduction in temperature. The actuated contact switch 76 then actuates the pump. In this way the danger of water of condensation forming upon a decrease in temperature or an increase in atmospheric pressure is eliminated. As soon as the required pressure conditions within the wall element have been reestablished, the pump motor, by lifting the movable equalization part V, actuates contact switch 77 which then again stops the motor.
The devices according to the present invention are suitable for achieving acoustic or acoustic and thermal insulation, depending on the selection and combination of the materials used in the construction of the wall elements and their arrangement therein.
All the features and embodiments of the apparatus and method described in the foregoing specification and illustrated in the drawings attached thereto and their combinations are essential for carrying out this invention.
The terms "casting the outer wall element around the inner insulating wall element" or "casting the inner insulating wall element into the outer wall element" or the like describe operations whereby, for instance, the outer wall element is prefabricated by casting, for instance, of concrete, inserting the inner insulating wall element into the hollow space left within said outer wall element, and sealing the hollow space with the inserted inner insulating wall element by pouring the concrete-yielding mixture thereover. It is also possible to insert the inner insulating wall element into a concrete form so that it is suspended therein and is surrounded on all its sides by a free space. The Portland cement-sand or -gravel paste is then poured into the free space of the concrete form. In both procedures there is produced a composite wall element as a combination of pressure-resistant, outer wall element enclosing the inner insulating wall element.
However, as it is evident from FIGS. 2 to 5 and 8, it is not an essential feature of the present invention that the inner insulating wall element is completely enclosed by casting the outer wall element around the same. FIGS. 2 to 5 provide covering plates to seal the hollow space with the inner wall element while in FIG. 8 the inner wall element can be inserted into the hollow space without the outer wall element being cast around the same. Furthermore, as is illustrated in FIGS. 3 and 4 an air or gas space can be provided between the inner insulating wall element and the outer pressureresistant wall element.
It may be pointed out that the distance between two reflecting surfaces in the composite wall element according to the present invention should preferably not exceed about 12 mm. because at a greater distance air or gas convection within said space will take place. It is, however, necessary that the air or gas layer between reflecting foils or plates is substantially at rest, i.e. that it does not move although the temperature on one side of the wall element increases. The most favorable distance at which the air or gas remains stagnant or non-flowing, in spite of a considerable heat or temperature gradient, is a distance of about 5 mm. to about 10 mm.
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The composite wall element of this invention comprises an insulating wall element arranged within or inserted into an outer, pressure resistant, preferably load bearing wall element which completely encloses the former. Within the inner insulating wall element and/or the cavity within the outer wall element a substantially dry gas atmosphere and preferably air atmosphere is established and maintained under sub-atmospheric, atmospheric, or superatmospheric pressure. Such novel composite wall elements are superior in their thermal and/or acoustic insulation properties to heretofore known structural elements.
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FIELD OF THE INVENTION
The present invention describes a process and a device for casing a well drilled ground from a folded preform comprising seal means at both ends. The preform is lowered into the well, then it is inflated by a fluid pumped into the inner space of the preform so that it unfolds and that it takes on a substantially tubular shape prior to hardening in the well. According to the invention, the lower seal means are disconnected and taken up to the surface through the inner channel of the composite casing. Thus, the lower part of the casing is cleared so as to allow operations in the composite casing, for example in order to deepen the borehole.
BACKGROUND OF THE INVENTION
Documents WO 94/25,655 and WO 94/21,887 describe processes for casing wells from a composite preform inflated by means of a sleeve (or die) placed inside the preform. After polymerization of the preform, the sleeve is removed from the cased well by exerting a traction on the end thereof, from the ground surface. Such a system is not suitable for composite casings of great length since it is not possible, in this case, to remove the sleeve. Furthermore, it is not possible to insert a sleeve of great length into a non polymerized preform.
SUMMARY OF THE INVENTION
The present invention thus relates to a method for casing a well from a tubular preform that is radially deformable by inflation between a folded state in which its greatest transverse dimension is smaller than the diameter of the well, and another, unfolded state in which said preform has a substantially cylindrical shape, said preform comprising seal means at both ends, the preform being hardenable in the well so as to constitute said casing. The method comprises the following stages:
means for disconnecting the seal means situated at the lower end of the preform are inserted into the inner space of the preform,
said seal means are taken up to the ground surface after being placed in a receptacle whose transverse dimension is smaller than the inside diameter of the preform once it has hardened.
The receptacle can be fastened to said lower seal means.
The seal means at the upper end of the preform can be disconnected first once the preform has hardened.
The disconnecting means can be lowered into the preform by means of rods.
The disconnecting means can be activated by the rotation of the rods and/or by a pressurized fluid contained in the rods.
The invention relates to a device for casing a well from a tubular preform that is radially deformable by inflation between a folded state in which its greatest transverse dimension is smaller than the diameter of the well, and another, unfolded state in which said preform has a substantially cylindrical shape, said preform comprising seal means at both ends, the preform being hardenable in the well so as to constitute said casing. Said device comprises means for disconnecting said lower seal means, a receptacle in which said seal means are placed after disconnection, a receptacle whose transverse dimension is smaller than the inside diameter of the preform once it has hardened.
In the device, the receptacle can be fastened to the end of said lower seal means, the latter comprising a seat and an orifice.
A measuring assembly can be fastened to the lower seal means with the aid of said seat, said assembly sealing the orifice.
The measuring assembly can be connected to the ground surface by conductors incorporated in the preform.
The disconnecting means can comprise a rod passing through said orifice so as to latch said receptacle, cutting means positioned with respect to the lower seal means with the aid of said seat, said cutting means being activated through at least one of the following actions: rotation, compression on the disconnecting means, pressure of a fluid.
The measuring assembly can comprise detectors suited for locating the lower end of the preform in the well.
The disconnecting means can comprise means for delivering a pressurized fluid.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the present invention will be clear from reading the description hereafter, given by way of non limitative examples, with reference to the accompanying drawings in which:
FIG. 1 shows the principle of setting a preform in a well,
FIGS. 2A and 2B show the upper seal means in two implementation variants,
FIG. 3 shows the lower seal means after or during the hardening of the casing,
FIG. 4A shows the principle of the means for disconnecting the lower seal means,
FIG. 4B shows the function of the receptacle according to the invention,
FIGS. 5A and 5B illustrate an embodiment of the invention,
FIGS. 6A and 6B illustrate another variant of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows the lowering into a well 1 of a supple and hardenable preform 2 set in folded state (a state in which it exhibits a small radial dimension), then radially unfolded by applying an inside pressure. This technique is described in documents FR-A-2,662,207, FR-A-2,668,241, WO 94/25,655 or WO 94/21,887. This preform comprises a composite structure made of resin-impregnated reinforcing fibers. In order to carry out the inflation operation allowing to unfold the preform, the latter is equipped with seal means at both ends, referenced 3 for those situated at the lower end and 4 for those situated at the upper end. The wall of the preform comprises at least one seal coat. The reinforcing fibers of the preform are secured to the two seal means 3 and 4 so as to withstand the stresses generated by the inside pressure. A pipe 5 is connected to the preform so as to allow the setting thereof in the well and to deliver a pressurized fluid into the inner space of the preform. The lower seal means 3 comprise a seat 6 and an orifice 7 in lowered position. A measuring device 8 is preferably positioned in orifice 7, on seat 6. The function of the supporting head 9 of the measuring device is to reversibly connect device 8 to the end of the preform, to allow device 8 to be taken up to the surface by means of a suitable fishing tool, to establish at least one electric connection between the measuring detectors of device 8 with cable 10 by means of conducting wires integrated in the preform at the time of its manufacturing. Thus, during the lowering of the preform in the well to be cased, the detectors of device 8 supply adequate information for controlling the correct setting of the preform in the well. In fact, the preform is supple since the resin is not polymerized, which does not facilitate the lowering thereof into the well. In order to facilitate this setting, load bars can be added to device 8 so as to maintain at best the preform under tension despite frictions on the wall of the well.
The detectors of device 8 can be any types of devices allowing geographic locating, or deepening measurement as a function of the pressure or temperature gradient. Temperature indicators can also be used to control the following polymerization operation.
A receptacle 11 is fastened below means 3. The main function of receptacle 11 is described hereafter. The bottom of receptacle 11 comprises an orifice 12 allowing at least part of device 8 to run through the preform. The function of orifice 12 is also to allow the receptacle to be implemented.
FIGS. 2A and 2B show the position of seal means 4 with respect to the well, in two different variants:
In FIG. 2A, preform 2 covers a well height up to the ground surface, which allows direct access to the upper seal means 4. In this case, after inflation and preferably hardening of the preform, the latter is suspended from wellhead elements 13 resting on the ground. After hardening of the preform, means 4 are cut so as to facilitate operations of suspension from elements 13 and to have access to the inner space 15 of the composite casing in order to carry on operations.
In FIG. 2B, preform 2 is destined to case a well length between the bottom and the lower end of a previous casing 16 already in place. This casing 16 can stem from the same composite casing technology, but it can also be a conventional steel or composite casing. The lower end of casing 16 advantageously ends in a radial widening 17 so that the casinghead 4 fits into this widening as shown in FIG. 2B. Thus, there can be no diameter reduction of the passage between casing 16 and the casing constituted by preform 2. Preform 2, in the folded state, thus before polymerization, is lowered by means of tubes 5 connected to the upper seal means 4. After the polymerization of preform 2, means 4 are detached, either by tearing off by pulling on tubes 5 from the surface, or by cutting means that can be lowered at the end of tubes 5 at the same time as the preform, or after polymerization, which requires an additional manoeuvre with tubes 5. The means for cutting means 4 can be lowered and run through an orifice of means 4, or set in means 4 when they are manufactured.
According to the embodiment of FIG. 2B, conductors 10 are situated in the annulus between tubes 5 and casing 16.
FIG. 3 shows the lower seal means 3 equipped with the receptacle 11 connected to means 3, for example by fastening elements 18 that can be sheared under a determined stress. Conductors 19 connected to the measuring detectors of device 8 are continuously connected to the ground surface with the aid of connection means 20 (between the head of device 8 and the seat of means 3), of conductors 21 included in means 3, of conductors 22 incorporated during the manufacture of the preform, and of cable 10 described above. FIG. 3 shows a tool 23, for example of the "wireline" type, consisting of an operating line 24 (or equivalent) lowered into the casing, a fishing head 25 suited to a supplementary part 26 fastened to the top of device 8. Once device 8 has been taken up, the means for disconnecting lower seal means 3 can be lowered into casing 2 according to the present invention.
FIGS. 4A and 4B show the working principles and the means specific to the disconnection of the lower seal means.
In FIG. 4A, disconnecting means 30 are lowered into the inner space of casing 2 with the aid of operating means 31, for example, rods, tubing, coil tubing, an electro-hydraulic umbilical, an electric cable. Means 30 are positioned precisely with respect to seal means 3 by resting on seat 6 and possibly by means of centralizers 32. A rod 33 forms the extension of means 30 by running through the orifice 7 of means 3 and through the opening 12 of receptacle 11. Fingers 34 latch rod 33 on the receptacle. Cutting means 35 are borne by arms, retracted when means 30 are lowered in order to be installed, expanded when disconnecting means 30 are operated. Bringing into rotation of the part 36 bearing the cutting means causes part 3 to be disconnected from casing 2.
Several variants can be achieved:
the rotation of the cutting means is performed by the rotation of rods 31 from the surface,
means 30 comprise a (hydraulic or electric) motorization for driving part 36 into rotation, the power required to activate the motorization being supplied through means 31 (electric cable, umbilical, . . . ).
In order to work, means 30 comprise means for controlling the spreading of cutting arms 35. These means are not shown in FIGS. 4A and 4B. The disconnecting means 30 according to the invention also comprise translation means for shifting rod 33 (not shown in FIGS. 4A and 4B) after the total cutting of seal means 3. The working principle of these translation means is shown in FIG. 4B.
In FIG. 4B, rod 33 has been run into the body of means 30 so as to raise receptacle 11 around the seal means 3 disconnected from casing 2. Thus, the receptacle acts as a sheath for seal means 3. Since the outside diameter of receptacle 11 is substantially smaller than the inside dimension of casing 2, receptacle 11, disconnecting means 30 can be taken up to the ground surface by operating means 31, whatever they may be.
In FIGS. 4A and 4B, the lower end 17 of casing 2 is widened, which constitutes a non limitative variant.
FIGS. 5A and 5B illustrate a variant of the disconnecting means that are hydraulically activated. Disconnecting means 30 comprise a main body 40 lowered at the end of a pipe 45. A lower extension 44 of body 40 rests and is centred on the seat 6 of the lower seal means 3 of casing 2. Cutting tools 43 are borne by arms 41 articulated at 42 on body 40. A part 46 bearing a piston is linked to each arm by stay bolts 47 having a pin 48 that runs through a slot 49 provided in arm 41, so that a hydraulic pressure in chamber 50 displacing part 46 has the effect of spreading arms 41 radially.
A rod 51 linked to a piston 53 can be hydraulically shifted radially in the liner 54 of body 40. This rod 51 bears, at the end thereof, locking means 52 that fit below receptacle 11 when the rod comes out of the receptacle. Any well-known means can be used, for example dog stop type retractable fingers.
FIG. 5B shows the disconnecting means once the seal means have been cut from the casing and the receptacle in position, ready for means 30 to be taken up.
The disconnecting means work as follows:
Means 30 are lowered into casing 2 by manoeuvring pipe 45, part 46 being locked so that the arms cannot spread during lowering. Locking can be achieved by means of a shear pin or by maintaining a hydraulic pressure in chamber 50' opposite chamber 50. Rod 51 has preferably been run into body 40 so as not to be damaged during lowering.
Once body 40 is blocked by seat 6, a hydraulic pressure in chamber 56 has the effect of moving out rod 51 and of latching its end 52 on receptacle 11.
A hydraulic pressure in chamber 50 has the effect of spreading the cutting arms.
The rotation of tubes 45 actuates cutting tools 43.
Once seal means 3 are disconnected from casing 2 (which can be seen from the surface by applying a given weight onto seat 6, this weight, taken up by rods 45 after cutting, can be observed from the surface), a hydraulic pressure is applied in chamber 55, possibly at the same time in chamber 50', so as to run rod 51 into the body in order to cause receptacle 11 to pass over seal means 3. Arms 41 are kept on body 40 in order to prevent casing 2 from being damaged during pulling.
The assembly is taken up by manoeuvring pipe 45.
The details of the hydraulic lines and of the possible distribution of the hydraulic pressure are not shown here since they are understandable to the engineer. It is clear that the hydraulic action can come from one or more sources, preferably through the pressure of a fluid in pipes 45 or by means of a multiconduit. Hydraulic distribution means can be placed in means 30 in order to deliver the pressurized fluid conveyed through pipe 45 into the various chambers described above. These distribution means can be remote-controlled by any well-known means, or by valves responding to pressure thresholds.
FIGS. 6A and 6B illustrate another variant of the disconnecting means in which the cutting means are spread and pressed against the wall of the lower seal means by the action of an axial force provided by a weight placed on seat 6.
The disconnecting means comprise a body 60 lowered into the casing through a pipe 45. An extension 61 can slide in translation with respect to body 60. Extension 61 comprises, at the ends thereof, a piston 63 on one side and a part 64 co-operating with seat 6 on the other side. The extension also comprises the articulated link 62 of arms 41 bearing the cutting tools 43. A slot 65 is provided in each arm 41 so that the pin 66 linked to body 60 causes arms 41 to spread when body 60 moves towards the dog, extension 61 being stopped by said dog. This relative displacement between parts 60 and 61 is controlled at the surface by means of tubes 45.
As in the variant of FIGS. 5A and 5B, a rod 51 runs through the opening of seat 6 so as to be locked below receptacle 11 by means of dog stops or equivalents. The displacement of rod 51 is performed by means of a piston 53. Application of a hydraulic pressure in chamber 68 has the effect of running rod 51 into body 60 while driving receptacle 11 that covers then seal means 3. Application of a hydraulic pressure in chamber 67 has the effect of shifting body 60 with respect to extension 61 in the direction of closing of the cutting arms. Chambers 67 and 68 preferably communicate hydraulically.
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The present invention relates to a method for casing a well (1) from a tubular preform (2) lowered into a well in folded state. The preform comprises seal means (3, 4) at both ends so that it can be inflated in order to take on a second, unfolded state in which the preform is polymerized.
Means (30) for disconnecting lower seal means (3) in order to take the latter up to the surface in a receptacle (11) are inserted into the casing.
The invention also relates to a casing device comprising disconnecting means (30) and a receptacle (11) for the lower seal means (3).
FIG. 1 to be published.
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This is a division, of application Ser. No. 310,976 filed Feb. 17, 1989 is now pending.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a textile structure for producing structural members such as reinforced spars of composite material, and to a method of producing the same. More particularly, the present invention relates to a textile structure which provides high torsional rigidity to reinforced composite materials such as reinforced spars suitable for use as structural parts for spacecraft, aircraft, automobiles, linear motor cars and the like, and to a method of producing the same. The present application is related to U.S. patent application Ser. No. 07/151,049 filed on Feb. 1, 1988, now U.S. Pat. No. 4,788,101, dated Nov. 29, 1988 wholly incorporated by reference herein.
2. Description of Prior Art
Structural parts such as airplane wings are subjected to high tensile and compressive loads. Fiber-reinforced resin composite materials have begun to be used as raw materials for spars required to have such specific strength. In many cases, spars of fiber-reinforced composite material of this kind have an I-, H-, U-, T-, or L-shaped cross section.
As for textile structures for reinforced composite materials having such cross-sections, Japanese Utility Model Application Laid-Open Specification No. 62-79900 and Japanese Patent Application Laid-Open Specification No. 61-53458 disclose laminated structures of textile filament having a three-dimensional construction of a three-axis orientation type in which textile filaments are laminate along X-, Y- and Z-axes which are orthogonal to each other. Further, Japanese Patent Application Laid-Open Specification No. 62-117842 discloses a base material of I-shaped cross-section in the form of a multilayer fabric opened to assume a three-dimensional configuration.
However, a conventional spar using reinforced members such as described above is constructed such that the laminated structure of textile filament has only a three-dimensional laminated construction of the so-called three-axis orientation type in which the directions of layout of textile filament cross each other. Such a conventional spar exhibits satisfactory strength against tensile, compressive and bending loads acting axially of the textile filaments. However, in the case where the spar has an increased length and when the axial direction of the textile filaments does not coincide with the direction of action of the load, such as when a torsional load is applied, the spar exhibits insufficient strength. As a result, the spar will deform. For example, a fracture or the like may develop due to the inability of a spar to bear the torsional load in a spar used as the main wing or tail assembly of an airplane.
An object of the invention is to provide a textile structure and a method of producing the same which are capable of eliminating the lack of torsional rigidity which has been a problem in spars of fiber-reinforced composite material which use as a reinforcing member a laminated structure of textile filament having a three-dimensional construction of the conventional three-axis orientation type.
SUMMARY OF THE INVENTION
According to the present invention, a textile structure for reinforcing spars of composite material comprises at least two textile planar members, or plates, integrally joined together by textile filaments such that the planes of the members intersect each other, wherein excluding at least one member, the other members are each formed of layers of textile filaments extending along three directions of three axes, i.e., longitudinal, transverse and vertical, of the member, while said at least one member is formed of layers of textile filaments extending obliquely in at least two directions in a brace fashion with respect to the longitudinal and transverse directions, or axes, of the member.
Regarding whether textile filaments should be disposed in said at least one member to extend in all the layout directions of five axes, i.e., in longitudinal, transverse and vertical directions and obliquely in two directions in a brace fashion, or only in some of these directions and as to the proportions of amount of textile filaments extending in the layout directions, selections may be made as desired according to the required specifications, such as strength characteristics, of spars and hence of the textile structures to be produced.
For example, in one form, the at least one member is formed of textile filaments extending in longitudinal, transverse and vertical directions and textile filaments extending obliquely in two directions in a brace fashion. In this case, it is of the five-axis orientation type.
In another form, the at least one member is formed of textile filaments extending in two of the longitudinal, transverse and vertical directions, and textile filaments extending obliquely in a brace fashion in two directions. In this case, it is of the four-axis orientation type.
As yet another form, the at least one member is formed of a textile filament extending in one of the longitudinal, transverse and vertical directions, and textile filaments extending obliquely in a brace fashion in two directions. This is of the three-axis orientation type.
Further, the at least one member may be made in the form of a laminated structure of textile filament of the two-axis orientation type formed solely of textile filaments extending obliquely in a brace fashion in two directions.
A method of producing a textile structure for reinforcing spars of composite material according to the present invention comprises the steps of disposing filament guide members of required length in a vertical direction according to a configuration and design density which are appropriate for the textile structure to be produced, laying out textile filaments among the filament guide members so that they move longitudinally, transversely or orthogonally and zigzag while repeating a combination of these movements, this operation being repeated a required number of times in the vertical direction, extracting the filament guide members, inserting vertical filaments in the extraction-vacated locations to thereby join or integrate a plurality of planar members, or plates, each formed of a laminated structure of textile filament, the method being characterized in that in forming at least one of the members, textile filaments are extended obliquely in at least two directions in a brace fashion with respect to the longitudinal and transverse layout directions of the member.
Functions
At least one of at least two planar members integrally joined together to cross each other is made in the form of a laminated structure of textile filament having a three-dimensional laminated construction including textile filaments which extend obliquely in a brace fashion in two directions and which cross each other; as a result, the strength against torsional loads has been increased. That is, said textile filaments extending obliquely in a brace fashion serve to increase torsional rigidity. Therefore, three of the five layout directions, other than those in which textile filaments extend obliquely in a brace fashion, can be omitted depending upon specifications, thereby contributing to reducing the weight of textile structures and hence the spars.
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
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:
FIGS. 1(A)-1(E) is a perspective view showing cross-sectional shapes of various textile structures according to the present invention;
FIG. 2 is a schematic perspective view showing, by way of example, a textile structure having an I-shaped cross section and illustrating the layout position of filament guide tubes;
FIGS. 3(A) and (B) are plan views showing the layout pattern of a first textile filament;
FIGS. 4(A) and (B) are plan views of another embodiment of the layout pattern of the first textile filament;
FIG. 5 is a plan view of a further embodiment of the layout pattern of the first textile filament;
FIG. 6 is a plan view of another embodiment of the layout pattern of the first textile filament;
FIGS. 7(A)-(H) are plan views of the layout patterns of filament to provide a textile laminated structure of the five-axis orientation type;
FIG. 8 is an explanatory view of a looped filament being inserted into the vacancies left by filament guide tubes and of another filament serving as a bolt filament;
FIG. 9 is an explanatory view showing various dimensions of a textile structure of composite material having an I-shaped cross-section.
DESCRIPTION OF PREFERRED EMBODIMENTS
FIGS. 1(A)-(E) show perspective views illustrating some of the cross-sectional shapes of reinforcing textile structures according to the present invention. A plate 2 (hatched in its cross section)is formed of a laminated structure 2B of textile filament having a three-dimensional laminated construction of a five-axis orientation type. Due to its construction, plate 2 will provide high torsional rigidity against a torsional load acting on a spar, as well as high strength against tensile and compressive loads.
Plates 1 are integrally joined to plate 2 substantially orthogonally thereto, and are each formed of a laminated structure 1A of textile filament having a three-dimensional laminated construction of a conventional three-axis orientation type. Due to the construction of plates 1, they will provide high strength against tensile and compressive loads acting on a spar. Alternatively, plates 1 can be formed of textile filament having a three-dimensional laminated construction of the two-, three-, four- or five-axis orientation type according to the present invention.
FIG. 2 is a schematic perspective view showing a textile structure 3 constructed of plates 1 and plate 2. Plate 2 is constructed of a laminated structure 2B of textile filament having a three-dimensional laminated construction of the five-axis orientation type. The four plates 1 provide high tensile and compressive strength due to their laminated structures 1A1, 1A2, 1A3 and 1A4 of textile filament having a three-dimensional laminated construction of the three-axis orientation type. The plates 1 and plate 2 are joined together to form an I-shaped integral construction. FIG. 2 also shows the orientation of filament guide tubes G1, G2 . . . during construction of the textile structure.
FIGS. 3(A) and (B), 4(A) and (B), 5 and 6 are plan views showing the manner in which a first textile filament Y1 is laminated to form various embodiments of the laminated structure 1A of textile filament. FIGS. 7(A)-(H) are top cross-sectional views illustrating the arrangement of a fourth textile filament Y4 in laminated structure 2B. FIG. 8 is a cross-sectional view showing third (and sixth) textile filaments Y3 (and Y6) serving as bolt filaments passed through loops LA1', LA2' . . . (and LB1', LB2' . . . ) formed at the turns of the second (and fifth) textile filaments Y2 (and Y5). FIG. 9 is an explanatory view showing various dimensions of a textile reinforced structure having an I-shaped cross section.
A method of producing the textile structure 3 having an I-shaped cross section according to an embodiment of the present invention and the resulting construction of the textile structure will now be described with reference to FIGS. 2 through 9. The I-shaped textile structure 3 is defined by a height h, a width w, a length l and a thickness t. The I-shaped textile structure 3 is laid on its side as shown in FIG. 2, and can be considered to be an H-shaped textile structure 3. The H-shaped textile structure 3 is constructed of a plate-like member 2 having a width h, a length l and-a thickness t, placed flat and four plates 1 each having a width t, a length l and a height 1/2 (w-t). The plates 1 are erected on the front and back of plate 2 on widthwise opposite edges thereof and throughout its length.
Prior to forming the I-shaped reinforced textile structure 3, first and second filament guide tubes G1 and G2 having a length of approximately w are suitably erected according to a predetermined pattern. Thereafter, the two first laminated structures 1A1 and 1A2 of textile filament underlying the second plate 2 are built by laminating a first filament Y1. Then, the single second laminated structure 2B of textile filament is built by laminating a fourth textile filament Y4. Subsequently, two first laminated structures 1A3 and 1A4 of textile filament overlying the second plate 2 are built. Then a second textile filament Y2 is passed through the first lower and upper laminated structures 1A1, 1A3 and 1A2, 1A4 and through the portion of the second laminated structure 2B positioned intermediate between said first upper and lower laminated structures. A fifth textile filament Y5 is passed through the portion of the second laminated structure 2B excluding its opposite end portions overlapped by the first laminated structures. A third textile filament Y3 as a bolt filament is passed through a loop formed by the second textile filament Y2, taking up the slack of the second textile filament Y2 and tightening the laminate, each time the second textile filament is pulled up to form a loop on the surface of each of the first laminated structures 1A3, 1A4. Similarly, a sixth textile filament Y6 as a bolt filament is passed through a loop formed by the fifth textile filament Y5, taking up the slack of the fifth textile filament Y5 and tightening the laminate, each time the fifth textile filament is pulled up to form a loop on the surface of the second laminated structure 2B. In the manner as described, reinforcing base material for the intended I-shaped spar 3 is formed.
The invention will now be described in more detail. First, the first textile filament Y1 is laminated in the region where said first filament guide tubes G1 are disposed in the order of layout shown in FIGS. 3(A) and (B). That is, the first textile filament Y1 is disposed in a substantially horizontally disposed zigzag pattern in a first layout plane SA1 defined by the X- and Y-axes, thereby forming a first layout layer LA1 of the first textile filament Y1 shown in solid line in FIG. 3(A). Then the layout arrangement is shifted to a second layout plane SA2 overlying the first layout layer LA1. A second layout layer LA2 of the first textile filament Y1 is formed, as shown by the dotted line in FIG. 3(A). Thereafter, the first textile filament Y1 has its layout layer position shifted to a third layout plane SA3 overlying said second layout layer LA2. The first textile filament Y1 is then positioned along the Y-direction as a Y-axis oriented filament in the third layout layer LA3, shown in dash-double-dot-line in FIG. 3(A).
Thereafter, as shown in FIG. 3(B), the first textile filament Y1 has its layout layers shifted step by step in the order of layout layers LA4, LA5 and LA6. Fourth layout layer LA4 is shown as a solid line, fifth layout layer LA5 is shown as a dotted line, and Y-axis oriented filament in a sixth layout layer LA6 is shown as a dash-double-dot line.
In this embodiment, the first and second layout layers LA1 and LA2 and the fourth and fifth layout layers LA4 and LA5 have been formed by moving the first textile filament Y1 alternately along the X- and Y-axes while changing its direction of layout every two first filament guide tubes G1. The third and sixth layout layers LA3 and LA6 have been formed by laying the first textile filament Y1 in the Y-direction between two rows of filament guide tubes G1. However, the layout pattern of the first textile filament Y1 in the XY-plane is not limited to the example shown in FIGS. 3(A) and (B). For example, it can be selected as desired according to the dynamic characteristics required of the first laminated structures of textile filament (hereinafter referred to as the first laminated structures 1A1, 1A2, 1A3 and 1A4).
An arrangement of layout shown in FIGS. 4(A) and (B) is used in another embodiment. As compared with the embodiment shown in FIGS. 3(A) and (B), the amount of filament in the Y-axis direction is doubled. That is, in FIG. 4(A), the first textile filament Y1 is used to form layout layers LA7 and LA8 in layout planes SA7 and SA8. Subsequently, two separate filaments Y1' in the Y-axis direction are laid and made taut in parallel, in the direction as indicated by arrowheads, and over layout layer LA8. Further, as shown in FIG. 4(B), the first textile filament Y1 is used to form layout layers LA9 and LA10 in layout planes SA9 and SA10 overlaying the arrangement shown in FIG. 4(A). Finally, separate filaments Y1' are made taut, in the direction indicated by arrowheads opposite to that in FIG. 4(A), in parallel. A series of said operations is repeated until the first laminated structure 1A of textile filament is obtained.
Another embodiment of the first textile structure is shown is FIG. 5, wherein the orientation ratio of the number of Y-axis oriented filament to X-axis oriented filament is 3:2. In FIG. 5, three textile filaments a in the Y-axis direction, a plurality of textile filaments b in the X-direction each disposed between adjacent filament guide tubes G1, and a single bolt filament c in the Y-axis direction disposed on a lateral edge are laid in the Y- and X-axis directions in the order (1), (2), (3), (4), (5), (6), (7), and (8). This series of operations is repeated until the desired first laminated structure 1A of textile filament is obtained.
A further embodiment of the first textile structure is shown in FIG. 6, wherein the orientation ratio of Y-axis oriented filament to X-axis oriented filament is 1:1. In FIG. 6, two textile filaments in the Y-axis direction, a plurality of textile filaments a in the X-axis direction each disposed between adjacent filament guide tubes G1, a single bolt filament c in the Y-axis direction disposed on a lateral edge, and a single bolt filament d in the X-axis direction disposed on a lateral edge are laid in the Y- and X-axis directions in the order (1), (2), (3), (4), (5), and (6). This series of operations is repeated until the desired first textile structure 1A is obtained.
The laminating operation with said first textile filament Y1, as shown in FIG. 2, is repeated a required number of times until the two first laminated structures 1A1 and 1A2 of textile filament underlying the second laminated structure 2B of textile filament reach the required height 1/2 (w-t).
Subsequently, a fourth filament Y4 is laminated in the region of layout of second filament guide tubes G2 as shown in FIGS. 7 (A), (B), (C), (D), (E), (F), (G) and (H). More specifically, the fourth textile filament Y4 is disposed substantially horizontally in a zigzag arrangement in the first layout plane SB1 forming the first layout layer LB1 shown as a solid line in FIG. 7 (A). The layout arrangement is then shifted to the second layout plane SB2 overlying said first layout layer LB1 to form the second layout layer LB2 shown as a dotted line in FIG. 7 (A). Thereafter, the fourth textile filament Y4, as shown in FIGS. 7 (B) through (F) has its layout plane shifted step by step in the order (SB3), (SB4), (SB5) . . . (SB15), (SB16), thereby forming a third layout layer LB3, a fourth layout layer LB4, a fifth layout layer LB5, . . . a fifteenth layout layer LB15 and a sixteenth layout layer LB16 with the direction of layout of textile filament changing successively in the order Y-axis, X-axis, V-axis, Y-axis, X-axis, V-axis, W-axis, W-axis.
The laminating operation of the fourth textile filament Y4 is repeated a number of times required for the second laminated structure 2B of textile filament to obtain the predetermined thickness t, as shown in FIG. 2. In addition to the arrangement wherein a single textile filament is caused to travel, as illustrated and described, it is also possible to use separate textile filaments for the individual axes.
In this embodiment, the layout pattern of the second filament guide tubes G2 has been determined so that the V-axis forms a phase angle of 45° with respect to the X-axis and so that the W-axis forms a phase angle of 135° with respect to the Y-axis. However, the phase angle and layout pattern of the fourth textile filament Y4 are not limited to the examples shown in FIG. 7 (A) through (F) and may be selected as desired according to the dynamic characteristics required of the second laminated structure 2B and hence the textile structure 3.
When it is desired to provide a construction for supporting tensile and compressive loads by the plates 1 and torsional stress solely by the plate 2 according to dynamic characteristics, this can be attained either by performing lamination in zigzag patterns alone as shown in FIGS. 7 (C), (F), (G) and (H) while omitting the disposition patterns in which the filament is parallel or orthogonal to the plate axis as shown in FIGS. 7 (A), (B), (D) and (E), or by changing the laminating proportions. A plate 2 resulting from the omission of the parallel and orthogonal patterns is a three-axis orientation type three-dimensional textile structure. This design decreases the amount of reinforcing filament, thus contributing much to weight-saving. Many other modified patterns can be employed without departing from the scope of the invention. In the second laminated structure 2B, a vertical filament to be later described can be omitted, but in that case the self-holdability developed upon completion of lamination is low and hence it is desirable to use a suitable tool resembling a molding tool or other jigs, so as to prevent the structure from losing shape.
The laminating operation of the fourth textile filament Y4 is repeated a number of times required for a desired thickness of the second laminated structure 2B as shown in FIG. 2.
When the thickness of the second laminated structure 2B reaches the predetermined value, the laminating operation on the two first laminated structures 1A3 and 1A4 overlying the same is started. The order of layout of the first filament Y1 in the first textile structures 1A3 and 1A4 is the same as that of the first textile filament Y1 used in the first textile structures 1A1 and 1A2 shown in FIG. 3 (A) or (B) or FIGS. 4 through 6, and hence a further description thereof is omitted.
Subsequently, as shown in FIG. 8, the first filament guide tubes G1 are pulled up one by one toward the upper surface of the first textile structure 1A3. At this time the second textile filament Y2 is bent to form loops LA1', LA2' . . . which are drawn into the filament guide tubes by leading wires or other suitable hooking tools. Each time a loop of the second textile filament is exposed on the upper surfaces of the first laminated structures 1A3 and 1A4 formed of the first textile filament Y1, the third textile filament Y3 serving as a bolt filament is inserted into the loop and the filament Y2 is pulled back, taking up the slack of the second textile filament Y2 and tightening the laminated structure.
Likewise, the second filament guide tubes G2 are pulled up one by one toward the upper surface of the second laminated structure 2B while the fifth textile filament Y5 having loops LB1', LB2' . . . formed at the turns thereof is drawn upwardly through the plurality of layout layers by the lower ends of the second filament guide tubes G2 each provided with a filament catch (not shown). Each time a loop of the fifth textile filament is exposed on the upper surface of the second laminated structure 2B formed of the fourth textile filament Y4, the sixth textile filament Y6 serving as a bolt filament is inserted and the filament Y5 is pulled back, taking up the slack of the fifth textile filament Y5 and tightening the laminated structure. This operation is performed with respect to the filament guide tubes G1 and G2 to respectively integrate the laminated structures 1A1 and 1A3 and the portion of the laminated structure 2B interposed therebetween and the laminated structures 1A2 and 1A4 and the portion of the laminated structure 2B interposed therebetween and finally integrate the single laminated structure 2B.
The laminated structure of textile filament obtained is impregnated with epoxy resin serving as a matrix and then cured, whereby a reinforced textile composite structure 3 of I-shaped cross-section as seen in FIG. 9 is produced.
In one embodiment of the present invention, a textile structure 3 having a long length can be formed and then cut into desired lengths for application.
In the embodiments described above, carbon fiber filaments can be selected for use as the first through sixth textile filaments Y1-Y6, while epoxy resin can be selected for use as the matrix. As for other textile filaments, besides carbon fiber, it is possible to select graphite fiber, glass fiber, aramid fiber, ceramic fiber, alumina fiber, aromatic polyester fiber or mixtures of these and other fibers. Also, various other types of known resins can be substituted for the epoxy resin.
The textile structure for reinforcing spars of composite material according to the present invention comprises at least two planar members, or plates, integrally joined together to cross each other, at least one of said members being formed of a five-axis, four-axis, three-axis or two-axis orientation type three-dimensional laminated structure of textile filament. Thus, a spar using it as a reinforcing base material and impregnated with a matrix which is subsequently cured and serving as a reinforcing base material is capable of exerting high, practically satisfactory rigidity to resist not only tensile and compressive loads but also torsional load. And by selecting the textile filament layout direction and laminating density which agree with the type and direction of load, it is possible to satisfy the requirement for weight-saving intended for spars while retaining the required torsional rigidity. Further, according to the production method of the invention, said textile structures for reinforcing spars can be easily produced.
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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Textile structures for producing structural members such as reinforced spars of composite material and a method for producing the textile structures. In the textile structure at least two textile planar members, or plates, are integrally joined together by textile filaments such that the planes of the members intersect each other, at least one member being formed of layers of textile filaments which extend obliquely in at least two directions in a brace fashion with respect to the longitudinal and transverse directions of the member while the remaining members are each formed of layers of textile filaments extending along the longitudinal, transverse and vertical directions of the member.
The textile structures are made by disposing filament guide members of required length in a vertical direction according to a desired configuration and design density of the structures and laying out textile filaments among said filament guide members so that they move longitudinally, transversely or orthogonally to form a plurality of textile planar members. The members are joined together by extracting the filament guide members and inserting filaments in the spaces vacated by the filament guide members.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a mounting system for mounting a structure whose thickness cannot be tightly controlled, and particularly to a mounting system for mounting an image sensor.
2. Background of the Prior Art
A typical image sensor chip 12 of the type mounted in various types of devices, such as medical instruments, video cameras, and bar code readers is shown in FIG. 6 . The image sensor shown includes a bottom planar member 110 carrying a pixel array 112 . Front and rear lead frames 114 initially extend peripherally from the pixel array and are formed to extend downwardly about front and rear edges respectively, of bottom planar member 110 terminating in pins 32 . Image sensor 12 further includes top planar member 118 which rests against pixel array 112 and lead frame 114 . Top planar member 118 is secured against lead frames 114 and against pixel plane 112 by the force of adhesive material interposed between top and bottom planar members 110 and 118 . Adhesive material is disposed mainly about the periphery of pixel array 112 . In addition, image sensor 12 may include a glass layer 120 . In some popular models of image sensors, top planar member 118 is configured in the form of a frame which retains glass layer 120 . Thus, it is seen that image sensor 12 is of a stacked-up configuration. Like most structures whose design is of a generally stacked up configuration, the thickness, t, of assembly 12 cannot be tightly controlled. In the manufacturing of sensor 12 , the thickness of the various layers will vary from structure to structure. Accordingly, the total thickness, t, will vary from structure to structure. The spacing, s, between top and bottom planar members 110 and 118 of image sensor 12 is particularly difficult to control given that such spacing is a function of the amount of adhesive used, the thickness of pixel array 112 and the thickness of lead frames 114 .
Particularly in applications where such an image sensor must be side mounted (not “plugged into” a PCB), as is the case with most bar code reader applications, then the inability to tightly control image sensor thickness, t, can negatively impact operational characteristics of the device in which the sensor is incorporated in. An explanation of how the inability to tightly control sensor thickness can impact operation of a bar code reader is made with reference to FIGS. 7 and 8 showing a multilayered image sensor incorporated in a bar code reader according to a prior art mounting scheme. In the mounting scheme shown, a multilayered image sensor 12 is disposed into a holding pocket 16 defined by substantially equally tensioned pairs of rear pins 19 and forward pins 18 . The prior art mounting system may further include a spacer 21 for biasing sensor 12 forwardly against forward pins 18 .
A number of operational problems can arise with this mounting scheme. If the thickness of the image sensor which is manufacturable to a thickness in the tolerance range from T min to T max tends toward T min then pins 18 , 19 may not supply sufficient pressure to image sensor 12 to hold sensor 12 in a secure position. Further, it can be seen that the distance, d, from any fixed point in space, P s , to any fixed point P p , on the plane of pixel array 12 will vary depending on the total thickness, t, of sensor 12 which is a thickness having a high degree of variability. This is not preferred since controlling the distance, d, is important to controlling the operation of the reader.
There is a need for an image sensor mounting system for mounting an image sensor in an imaging device which minimizes operational problems resulting from the inability to tightly control an image sensor chip's thickness.
SUMMARY OF THE INVENTION
According to its major aspects and broadly stated the present invention is a mounting system for mounting an image sensor chip in a location in a device apart from a PCB board.
In one embodiment of the invention, a multilayered image sensor is backmounted to a plate, and the plate in turn, is installed in a holding pocket of a device. In that the scheme takes advantage of a high controllability of a mounting plate's thickness, the mounting scheme improves the consistency of holding forces with which several image sensors are secured in like configured imaging devices. In that the scheme provides for back mounting of image sensor on a plate, the mounting system reduces fluctuations in pixel plane to fixed point distances.
The mounting scheme may be enhanced by forming cutout sections in the mounting plate. The cutout sections serve to bench lead frames extending from an image sensor, and thereby serve to minimize sliding or twisting of an image sensor mounted on a mounting plate. In another enhancement, an image sensor mounted on a mounting plate is secured to the plate entirely by a compression force supplied by a flex strip, soldered onto an image sensor's lead frames, impinging on the mounting plate. This arrangement serves to further minimize thickness variations resulting from manufacturing tolerances.
In a variation of the invention, the mounting plate is substituted for by a back plate formed integral with a component frame of a device. The back plate along with the remainder of the frame define an elongated aperture adapted to receive a lead frame of an image sensor. An image sensor may be mounted to a back plate in essentially the same way that an image sensor is mounted to a mounting plate to the end that an image sensor is tightly secured in a device and further to the end that pixel plane to fixed point distance is tightly controlled.
These and other details, advantages and benefits of the present invention will become apparent from the detailed description of the preferred embodiment hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
The preferred embodiment of the invention will now be described, by way of example only, with reference to the accompanying Figures wherein like members bear like reference numerals and wherein:
FIG. 1 is perspective assembly diagram illustrating assembly of a mounting system according to the invention;
FIG. 2 is an enlarged perspective view of a mounting plate shown in FIG. 1;
FIG. 3 is an enlarged perspective view of a component frame shown in FIG. 1;
FIG. 4 a is a perspective partial assembly diagram illustrating assembly of a flex strip onto an image sensor;
FIG. 4 b is a perspective view illustrating an example of a component frame having an integrated back plate for receiving an image sensor;
FIG. 5 a second perspective view of the component frame of FIG. 4 b showing an image sensor installed thereon according to a mounting system of the invention;
FIG. 6 is an exemplary perspective view of an image sensor chip illustrating a multilayered construction thereof;
FIG. 7 is a top view of a prior art optical reader illustrating a prior art image sensor mounting system;
FIG. 8 is a cross sectional side view of the reader shown in FIG. 7 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
An exemplary embodiment of an image sensor mounting system according to the invention is described with reference to the assembly drawing of FIG. 1 . In this embodiment, a plate 10 is provided for back mounting an image sensor 12 . In a simplified form of this mounting scheme, plate 10 is provided by a substantially rigid planar member comprising insulating material, image sensor 12 is mounted to plate 10 by any suitable means such as gluing or taping, and the resulting assembly comprising a plate and sensor 10 and 12 is mounted to an optical reader component frame 14 by inserting plate into a pocket 16 which may be defined, as is shown, by a pair of pins 18 and wall sections 20 . Plate 10 is sized to a length l p such that the edges of plate 10 extend beyond the edges of sensor 12 when sensor is attached to plate 10 to the end that a pocket 16 can hold an image sensor in a secure position by applying lateral holding forces to plate 10 without supplying lateral forces to the top glass, or bottom planar members of image sensor 12 .
Component frame 14 in the example provided is an optical assembly component frame. Optical assembly frames of optical readers are typically comprised of molded plastic and are typically adapted to carry various optical system components of an optical reader. In addition to carrying an image sensor 12 , an optical assembly frame of an optical reader may carry such components as mirrors, lenses and illumination sources, such as LEDs. In most optical readers, an optical assembly component frame 14 is installed on a printed circuit board. e.g. circuit board 15 which, in addition to carrying frame 14 , carries most, if not all, of the electrical components of the optical reader.
The mounting scheme described is advantageous over the prior art because it increases the security with which image sensor 12 is held in pocket 16 and furthermore, increases the precision with which a pixel plane to fixed point distance can be controlled.
While the total thickness, t, of stacked up image sensor 12 cannot be tightly controlled, the thickness T p of plate 10 can be tightly controlled. Accordingly, pockets 16 of several like designed optical assembly frames will apply relatively consistent holding forces to image sensors disposed therein.
The mounting system increases the precision with which pixel plane to fixed point distance, d, is controlled because it reduces the number of manufacturing tolerances which contribute to the distance, d, the distance between any fixed point, P p , on the plane of a pixel array 12 and a fixed point, P s , away from the pixel plane.
In a prior art mounting system described with reference to FIGS. 6, 7 and 8 , the pixel plane to fixed point distance, d, is a function of the total thickness, t, of an image sensor 10 , which is a function of the highly variable top planar member to bottom planar member spacing, s.
Because a pixel plane of an image sensor 10 is disposed flush on a bottom planar member, it is seen that pixel plane to fixed point distance, d, in the mounting system of FIG. 1 is influenced only by the bottom plate thickness t b , and the mounting plate thickness t p , both of which can be tightly controlled.
Additional features can be incorporated in the mounting system thus far described for further improving the operation of the mounting system.
One enhancement to the mounting system thus far generally described is to form in mounting plate 10 first and second cutout sections 26 and 28 . Cutout sections 26 and 28 defined by side walls 30 are sized to a length l c approximately the same length or slightly longer than lead frames 114 so that edges of lead frames 114 are benched on walls 30 when image sensor 10 is mounted on mounting plate 10 . Cutout sections 26 and 28 provide the function of stabilizing the position of an image sensor on mounting plate 10 so as to prevent sliding or twisting of image sensor 12 on plate 10 .
Another enhancement to the mounting system generally described relates to a mounting scheme for mounting an image sensor 12 to mounting plate 10 . It has been mentioned herein that sensor 12 can be secured to plate 10 using any conventional securing means, such as adhesives, glues, double sided tapes, etc. However, such schemes for attachment have the potential drawback in that they add thickness to an assembly including an image sensor and a back plate.
In the image sensor to plate mounting scheme of FIG. 1 the mounting is accomplished without use of any thickness-adding material. As seen in FIG. 1, pins 32 will extend outwardly beyond the back surface 34 of plate 10 when sensor 12 is pressed flush against plate 10 . A flex strip 38 which includes two strips 40 and 42 of pin receptacles for providing electrical connection between sensor leads 12 and certain electrical connectors of reader (normally on PCB), a distance away from sensor 12 may be attached to image sensor 12 such that a first row of pins 32 are received in a first row of receptacles 40 and a second row of pins 32 are received in a second row of receptacles 42 of flex strip 39 . Pins 32 can be soldered onto receptacles 40 and 42 such that the compression force of flex strip 38 impinging on mounting plate 10 to bias plate 10 against sensor 12 is sufficient to hold sensor 12 , securely on plate 10 without additional securing forces supplied by glues, tape, or other adhesive material.
In the mounting system of FIG. 1, plate 10 may further include side wall formations 31 which are received in complementary formations of pocket 16 . In particular, the mounting system can be configured such that bottom surface 31 ′ of formation 30 is received on a complementary surface of pocket 16 . Furthermore, when plate 10 is installed in pocket 16 , at least one screw 33 can be received in at least one hole 29 formed in pocket 16 in such a location that screw head 33 h or associated washer 33 w applies a vertical holding force to a received image sensor 12 . In the particular embodiment shown, a cutaway section defined by walls 35 is provided so that plate 10 does not interfere with the receiving light optics in the particular optical system in the example provided.
A variation on the mounting schemes described thus far is described with reference to FIGS. 4 a through FIG. 5 . In the schemes described thus far, image sensor 12 is mounted to a plate 10 which, in turn, is received in a pocket 16 in an optical assembly frame 14 of a bar code reader.
In the mounting scheme described with reference to FIGS. 4 a , 4 b and 5 , the mounting pocket 16 of optical assembly frame 14 is deleted, and optical assembly frame 14 instead is furnished with a back plate 48 integral with frame 14 which provides essentially the same function as mounting plate 10 . Certain features of an optical system which may be incorporated in a frame of the type shown in FIG. 4 b and FIG. 5 are described in detail in copending applications entitled “Optical Assembly for Barcode Scanner,” Ser. No. 09/111,476 and “Adjustable Illumination System for a Barcode Scanner,” Ser. No. 09/111,583 filed concurrently herewith, incorporated by reference herein, and assigned to the Assignee of the present invention.
In this mounting scheme, image sensor 12 is mounted directly to back plate 48 in essentially the same manner that sensor 12 is mounted to mounting plate 10 in the general scheme described previously.
In mounting sensor 12 to back plate 48 then sensor 12 is pressed against surface 50 of back plate 48 . Frame 14 includes elongated aperture 52 defined by bottom edge of back plate 48 to accommodate bottom pins 32 b of lead frame 114 when sensor 10 is mounted against back plate 48 . Securing material such as glues tapes or other adhesives may be provided to aid in the securing of an image sensor against back plate 48 . In the alternative, image sensor 12 may be secured to back plate 48 as described previously by a compression force supplied by flex strip 38 , which when soldered, works to bias image sensor 12 against plate 48 .
Cutout section 56 and aperture 52 can be sized to have lengths l c approximately equal to the respective lengths of lead frames 114 so that side wall 30 of aperture 52 and of cutaway section 56 operate to bench lead frames 114 and to thereby prevent sliding or twisting of image sensor 12 when image sensor 12 is mounted on back plate 48 . It will be seen that a back plate of the invention can be provided by virtually any substantially planar rigid surface integrated onto a mounted component frame.
While the present invention has been particularly shown and described with reference to the preferred mode as illustrated in the drawing, it will be understood by one skilled in the art that various changes in detail may be effected therein without departing from the spirit and scope of the invention as defined by the claims.
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According to the invention, a multilayered image sensor is backmounted to a plate, and the plate in turn, is installed in a holding pocket of a device. In that the scheme takes advantage of a high controllability of a mounting plate's thickness, the mounting scheme provides for tight control of holding forces with which an image sensor is secured in an imaging device. In that the scheme provides for back mounting of image sensor on a planar surface, the mounting system provides tight control of an imaging assembly's pixel plane to fixed point in space distance.
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BACKGROUND OF THE INVENTION
Certain 6H-7,8-dihydrothiapyrano[3,2-d]pyrimidines are disclosed in Belgian Pat. No. 724745 as intermediates for the preparation of compounds with cardiovascular and coronary dilation activity, however, suggestion is made neither of any hypoglycemic activity nor of weight reducing properties for either the intermediates or the final products. Great Britain No. 2119368 discloses 6H-7,8-dihydrothiapyrano[3,2-d]pyrimidines with a very different substitution pattern on the nucleus when compared with the instant compounds. U.S. Pat. Nos. 3,318,883, 3,272,811, and 3,318,881 disclose dihydrothieno[3,2-d]pyrimidines which differ from the instant compounds in having a 5-membered heteroaromatic sulfur-containing ring rather than a saturated 6-membered ring.
SUMMARY OF THE INVENTION
The instant invention is concerned with novel 6H-7,8-dihydrothiapyrano[3,2-d]pyrimidines which are useful as hypoglycemic and/or weight reducing agents. These compounds are also β-adrenergic blocking agonists and α-adrenergic blocking agents and are also useful as ocular antihypertensives and in the treatment of glaucoma and other eye disorders. Thus, it is an object of this invention to describe such compounds. It is a further object of this invention to describe the hypoglycemic activity of such compounds. A still further object is to describe compositions containing such compounds as the active ingredient thereof. Further objects will become apparent from a reading of the following description.
DESCRIPTION OF THE INVENTION
The 2-substituted-4-substituted 6H-7,8-dihydrothiapyrano[3,2-d]pyrimidines of this invention are novel compounds with significant hypoglycemic activity. The compounds have the following structure: ##STR1## wherein: R 1 is hydrogen, loweralkyl, loweralkenyl of from 2 to 6 carbon atoms, cycloalkyl of from 3 to 6 carbon atoms, phenyl, nitrophenyl, pyridyl, phenylloweralkyl, loweralkoxy, loweralkylthio, loweralkoxyloweralkyl or phenylloweralkoxyloweralkyl;
R is ##STR2## wherein R 2 is hydrogen or lower alkyl; X is --CH(NH 2 ), --(C═NOH)--, --(C═NOAlk)-- where alk is loweralkyl or --(N--R 3 )-- where R 3 is loweralkenyl of from 2 to 6 carbon atoms, loweralkynyl of from 2 to 6 carbon atoms, cycloalkyl of from 3 to 6 carbon atoms, hydroxyloweralkyl, formyl, loweralkoxycarbonyl or phenylloweralkyl; and R 3 can also be loweralkyl provided that R 1 is not simultaneously hydrogen or loweralkyl at the same time; or
R is
hydrogen or loweralkyl and R 1 is morpholino, piperidino, 4-hydroxyiminopiperidino, loweralkoxyiminopiperidino, 4-aminopiperidino, piperazino, N-loweralkylpiperazino or N-hydroxyloweralkylpiperazino.
The loweralkyl group of this invention may contain from 1 to 10 carbon atoms and may be in either a straight or branched configuration. Exemplary of such groups are methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, and the like.
The term "halogen" or "halo" is intended to include those halogens selected from fluorine, chlorine, bromine or iodine.
The preferred compounds of this invention are those wherein R 1 is ethyl, n-propyl, cyclopropyl, vinyl, or 2-hydroxyethyl; X is N--R 3 where R 3 is lower alkenyl or hydroxy lower alkyl. Further preferred embodiments are realized when R 3 is 2-propenyl or 2-hydroxyethyl.
The instant compounds are prepared from the appropriate R 1 -substituted thiapyranopyrimidin-4-one which is treated with phosphorus oxychloride to prepare the analogous 4-chloro compound which, with treatment with the appropriately substituted amine or heterocyclic amine prepares the desired compounds as outlined in the following reaction scheme: ##STR3## wherein R and R 1 are as defined above and Alk is loweralkyl.
In the first step of the above reaction scheme, a 2-carbalkoxy-3-oxotetrahydrothiapyran (I) is reacted with an R 1 -substituted amidine (II). The free base of the amidine is usually employed which is generally generated in situ by treating an amidine salt with a strong base. While any base that is a stronger base than the amidine itself may be used, generally an alkali metal base, such as sodium or potassium alkoxide is preferred. The solvent is generally a solvent compatible with the base and it is thus generally preferred to use an alcohol which corresponds to the alkoxide base used, such as methanol or ethanol. Sodium methoxide in methanol is the preferred solvent system and base. The amidine free base is then combined with compound I to prepare the 2-R 1 -substituted-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine-4-one (III). The reaction is carried out at from 0° C. to the reflux temperature of the reaction mixture and is generally complete in from 30 minutes to 24 hours. It is preferred to carry out the reaction at about room temperature. The product is isolated using techniques known to those skilled in the art with the product generally not being purified but rather used directly in the next step.
The 2-R 1 -substituted-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine-4-one (III) is then reacted with a chlorinating agent such as phosphorus oxychloride, thionyl chloride and the like. While a solvent may be employed it is generally preferred to use the chlorinating agent in excess and to dispense with the use of a solvent. Generally the reaction is heated to at least 50° C. up to the reflux temperature of the reaction mixture for from about 3 hours to 3 days. It is preferred to use phosphorus oxychloride as the chlorinating agent and to heat it at about 100° C. overnight. The chlorinated compound (IV) is isolated using known techniques.
The 2-R 1 -4-R-substituted-7,8-dihydro6H-thiapyrano[3,2-d]pyrimidine compounds (V) are prepared from the 4-chloro compounds (IV) by displacing the chlorine with the appropriate cyclo amine. ##STR4## The reaction may be carried out neat, however, preferably the reaction is carried out in an unreactive alcohol solvent although any solvent which does not react with compound IV or the amine is suitable such as ethers, THF, DMF, benzene, and the like. The reaction is carried out at elevated temperatures of from 80° to 150° C. and is generally complete in from 3 to 24 hours. It is preferred to heat the reaction at from 100°-120° C. in an alcohol solvent with a boiling point in excess of the reaction temperature. Thus, isoamyl alcohol with a boiling point of 132° C. is a preferred solvent.
Generally the amine reactant is used in excess with at least 2 and preferably 3 or more molar equivalents in order to provide a scavenger for the hydrogen chloride liberated during the course of the reaction. Alternatively, where the amine reactant is difficult to obtain or costly, a single molar equivalent may be used along with a tertiary amine such as triethylamine or pyridine to act as the scavenger for the hydrogen chloride. The products are purified using standard techniques, and are preferably isolated as the acid addition or other physiologically acceptable salt such as the hydrochloride, nitrate, sulfate, maleate, citrate, and the like.
Those compounds wherein R is hydrogen or loweralkyl and R 1 is morpholino, piperazino, or N-loweralkylpiperazino are prepared from 2,4-dichloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine, a known compound. (See UK patent application Ser. No. 2119368A) When R is hydrogen, the 4-chloro group is selectively removed by hydrogenation, such as catalytic hydrogenation with a platinum group metal such as platinum, palladium, rhodium, osmium, and the like, preferably supported on an inert carrier, such as carbon. Standard hydrogenation techniques are employed and the reaction is complete in from 1/2 to 8 hours. Hydrogen at from 1 to 4 atmospheres (gauge) is employed and the reaction is carried out in a solvent inert to hydrogenation and the catalyst such as a lower alcohol. Room temperature is preferred, however, elevated temperature of up to 50° C. may be employed. The product is isolated using standard techniques.
When R is loweralkyl, the dichloro compound is treated with an alkylating agent such as loweralkyltriphenyl phosphonium bromide. The reaction is carried out in a dry inert solvent such as dimethoxy ethane under a blanket of an inert gas, such as nitrogen, with a reaction promoter such as n-butyl lithium. The reaction is complete in from 1 to 4 hours at an initial temperature from -50° C. to 0° C. followed by a reaction temperature of from 0° to 50° C., preferably room temperature.
The following reaction scheme outlines the complete process: ##STR5##
The monochloro compound is reacted with morpholine, piperazine, N-loweralkylpiperazine or a piperazine protected with acyl or BOC protecting groups in the same manner as described above for displacing the chlorine for the 4-position group with a heterocyclic base.
Diabetes is a condition characterized by abnormal insulin secretion and a variety of metabolic and vascular manifestations reflected in a tendency toward inappropriately elevated blood glucose levels and which if left poorly treated or untreated can result in accelerated, nonspecific atherosclerosis, neuropathy and thickened capillary lamina causing renal and retinal impairment. Diabetes is characterized as being insulin dependent (Type I) and non-insulin dependent (Type II). Type I diabetes is due to damage and eventual loss of the β-cells of the pancreatic islets of Langerhans with a resulting loss of insulin production. Type II diabetics secrete insulin, however, the insulin is somehow not properly or effectively utilized in the metabolism of blood sugars and glucose accumulates in the blood to above normal levels. This condition is termed insulin resistance.
With the certainty of serious complications resulting from high glucose levels in poorly controlled or uncontrolled diabetics, means to lower blood glucose have been research goals for a considerable period of time. With Type I diabetes glucose control can only be achieved with daily insulin injections. With Type II diabetes glucose control can be effected from a combination of diet and drugs which lower glucose levels. The currently available oral hypoglycemic agents are not completely satisfactory since they may not offer complete blood glucose control or may provide a variety of undesirable side effects or they may elevate insulin concentrations to undesirable and dangerous levels. Thus, the search for improved oral hypoglycemic agents is a continuing one.
As previously indicated, the compounds of this invention are all readily adapted to therapeutic use as oral hypoglycemic agents in view of their ability to lower the blood sugar levels of diabetic subjects to a statistically significant degree. For instance, 2-methyl-4-[4-(2-propenyl)piperazinyl]thiapyrano[3,2-d]pyrimidine, a typical and preferred agent of the present invention, has been found to consistently lower blood sugar levels and improve glucose tolerance in either fasted or fed diabetic (i.e., hyperglycemic) mice to a statistically significant degree when given by the oral route of administration at dose levels ranging from 1 mg/kg to 100 mg/kg, respectively, without showing any toxic side effects. The compounds of the instant invention have an additional advantage in that they produce a hypoglycemic effect only in biological situations of high glucose concentration. The other compounds of this invention also produce similar results. In general, these compounds are ordinarily administered at dosage levels ranging from about 1 mg to about 500 mg per kg of body weight per day, although variations will necessarily occur depending upon the condition and individual response of the subject being treated and the particular type of oral pharmaceutical formulation chosen.
Administration over time to obese, insulin resistant mice, resulted in a significant reduction in body weight.
In connection with the use of the compounds of this invention for the treatment of diabetic subjects, it is to be noted that they may be administered either alone or in combination with pharmaceutically acceptable carriers and that such administration can be carried out in both single and multiple dosages. More particularly, the novel compounds of the invention can be administered in a wide variety of different dosage forms, i.e., they may be combined with various pharmaceutically acceptable inert carriers in the forms of tablets, capsules, lozenges, troches, hard candies, powders, aqueous suspension, elixirs, syrups and the like. Such carriers include diluents or fillers, sterile aqueous media and various non-toxic organic solvents, etc. Moreover, such oral pharmaceutical compositions can be suitably sweetened and/or flavored by means of various agents of the type commonly employed for just such a purpose. In general, the therapeutically-effective compounds of this invention are present in such dosage forms at concentration levels ranging from about 0.5% to about 90% by weight of the total composition, i.e., in amounts which are sufficient to provide the desired unit dosage.
For purposes of oral administration, tablets containing various excipients such as sodium citrate, calcium carbonate and dicalcium phosphate may be employed along with various disintegrants such as starch and preferably potato or tapioca starch, alginic acid and certain complex silicates, together with binding agents such as polyvinylpyrrolidone, gelatin and acacia. Additionally, lubricating agents such as magnesium stearate, sodium lauryl sulfate and talc are often very useful for tabletting purposes. Solid compositions of a similar type may also be employed as fillers in soft and hard-filled gelatin capsules; preferred materials in this connection would also include the high molecular weight polyethylene glycols. When aqueous suspensions and/or elixirs are desired for oral administration, the essential active ingredient therein may be combined with various sweetening or flavoring agents, coloring matter or dyes and, if so desired, emulsifying and/or suspending agents as well, together with such diluents as water, ethanol, propylene glycol, glycerin and various like combinations thereof.
The activity of the compounds of the present invention, as hypoglycemic agents, is determined by their ability to lower blood sugar levels in the fasted or fed genetically hyperglycemic mouse when tested therein for such purposes according to the procedures described by Saperstein et al. as submitted to the journal Diabetes and summarized as follows: Genetically obese mice (ob/ob) were fasted overnight. The compounds were administered orally via a stomach tube and each mouse serially bled from the orbital sinus at various times and the blood samples were analyzed for blood glucose. When the effects of the compounds on blood glucose levels were to be determined, glucose was administered orally at a rate of 2 g per kg. 30 minutes after administration of the test compound. Glucose in the blood was determined by the potassium ferricyanide potassium ferrocyanide oxidation reaction auto analyzer. The latter method measures directly the amount of glucose in the blood at any given time and from this, the maximum percent decrease in blood sugar can be readily calculated and reported as hypoglycemic activity per se. In this way, many of the present compounds are shown to markedly improve glucose tolerance of non-anesthetized hyperglycemic mice when administered to them at dose levels as low as 10 mg/kg orally and to lower fasting blood glucose levels when administered at dose levels as low as 30 mg/kg orally.
The β-adrenergic blocking properties of the novel compounds of this invention indicate that they are useful in the treatment of conditions such as ocular hypertension, hypertension, angina pectoris, or certain arrhythmias which are known to be amenable to treatment with β-adrenergic blocking agents.
For use as β-adrenergic blocking agents, the present compounds can be administered orally, transdermally, or parenterally; i.e., intravenously, interperitoneally, etc. and in any suitable dosage form. The compounds may be offered in a form (a) for oral administration; e.g., as tablets, in combination with other compounding ingredients customarily used such as talc, vegetable oils, polyols, benzyl alcohols, gums, gelatin, starches, and other carriers; as liquids dissolved or dispersed or emulsified in a suitable liquid carrier; in capsules encapsulated in a suitable encapsulating material; or (b) for parenteral administration dissolved or dispersed in a suitable liquid carrier such as solution or as an emulsion, or (c) as an aerosol or patch for transdermal administration. The ratio of active compound to compounding ingredients; i.e., carrier, diluent, etc., will vary as the dosage form requires. Generally, doses of the present compounds of from about 0.01 to about 50 mg/kg and perferably from about 0.1 to about 20 mg/kg of body weight per day may be used. Dosage may be single or multiple depending on the daily total required and the unit dosage.
A further embodiment of this invention is the method of treating elevated intraocular pressure by the topical ocular administration to a patient in need of such treatment of an effective intraocular pressure lowering amount of one of or a mixture of compounds of this invention.
A unit dose comprises about 0.001 to 5.0 mg, preferably about 0.005 to 2.0 mg, and especially about 0.05 to 1.0 mg of active compound per eye. Multiple unit doses are administered as needed to achieve and maintain a normotensive or close to normotensive ocular condition.
A still further embodiment of this invention is the novel ophthalmic formulations comprising one of the previously mentioned compounds as active ingredient. The ophthalmic composition of this invention may be in the form of a solution, suspension, ointment, gel or solid insert and contain about 0.01 to 5% and especially about 0.5 to 2% by weight of medicament. Higher concentrations as, for example about 10% or lower concentrations can be employed.
The pharmaceutical preparation which contains the compound may be conveniently admixed with a non-toxic pharmaceutical organic carrier, or with a non-toxic pharmaceutical inorganic carrier. Typical of pharmaceutically acceptable carriers are, for example, water, mixtures of water and water-miscible solvents such as lower alkanols or aralkanols, vegetable oils, polyalkylene glycols, petroleum based jelly, ethyl cellulose, ethyl oleate, carboxymethylcellulose, polyvinylpyrrolidone, isopropyl myristate and other conventionally employed acceptable carriers. The pharmaceutical preparation may also contain non-toxic auxiliary substances such as emulsifying, preserving, wetting agents, bodying agents and the like, as for example, polyethylene glycols 200, 300, 400 and 600; carbowaxes 1,000, 1,500, 4,000, 6,000 and 10,000; antibacterial components such as quaternary ammonium compounds, phenylmercuric salts known to have cold sterilizing properties and which are non-injurious in use, thimerosal, methyl and propyl paraben, benzyl alcohol, phenyl ethanol; buffering ingredients such as sodium chloride, sodium borate, sodium acetates, gluconate buffers; and other conventional ingredients such as sorbitan monolaurate, triethanolamine, oleate, polyoxyethylene sorbitan monopalmitylate, dioctyl sodium sulfosuccinate, monothioglycerol, thiosorbitol, ethylenediamine tetracetic acid, and the like. Additionally, suitable ophthalmic vehicles can be used as carrier media for the present purpose including conventional phosphate buffer vehicle systems, isotonic boric acid vehicles, isotonic sodium chloride vehicles, isotonic sodium borate vehicles and the like. The pharmaceutical preparation may also be in the form of a solid insert. For example, one may use a solid water soluble polymer as the carrier for the medicament. The polymer used to form the insert may be any water soluble non-toxic polymer, for example, cellulose derivatives such as methylcellulose, sodium carboxymethyl cellulose, (hydroxyloweralkyl cellulose), hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropylmethyl cellulose; acrylates such as polyacrylic acid salts, ethylacrylates, polyacrylamides; natural products such as gelatin, alginates, pectins, tragacanth, karaya, chondrus, agar, acacia; the starch derivatives such as starch acetate, hydroxyethyl starch ethers, hydroxypropyl starch, as well as other synthetic derivatives such as polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl methyl ether, polyethylene oxide, neutralized carbopol and xanthan gum, and mixtures of said polymers.
The instant invention is further described by the following examples which are intended to be merely descriptive and should not be construed as limitative of the invention.
EXAMPLE 1
General Procedure I
An amidine hydrochloride was added to an equivalent amount of 1.5-2N sodium methoxide in methanol. After 5-10 minutes when sodium chloride precipitation was complete the solution of amidine was filtered directly into an equivalent of 2-carbethoxy-3-oxotetrahydrothiapyran (E. A. Fehnel, J. Amer. Chem. Soc. 74, 1569 (1952)) that may or may not be dissolved in a small amount of methanol. In general the concentration of reagents in the final reaction mixture ranges from 1-2 mmoles/ml of methanol. The product usually begins to precipitate after an hour or two. After the reaction mixture was allowed to stand overnight, the product was isolated by filtration. An additional crop of product was sometimes obtained by concentration of the mother liquors. The product is usually sufficiently pure for use in the next step. Should recrystallization be necessary, methanol is the appropriate solvent.
EXAMPLE 2
General Procedure II
A 2-substituted-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one was suspended in phosphorus oxychloride. The concentration of the suspension ranges from 1 g/10 ml to 1 g/5 ml and is preferentially at 1 g/5 ml. The mixture is stirred and heated to reflux (On some occasions, 2 ml of N,N-diethylaniline per gram of pyrimidinone is added). The mixture becomes homogeneous within several hours, but heating is continued for a total of six to eighteen hours. After the mixture has been allowed to cool to room temperature it is poured slowly onto excess ice and water with vigorous agitation and a solvent such as chloroform or methylene chloride is added. It is important to keep the temperature low during hydrolysis and the subsequent neutralization reaction. After the hydrolysis mixture was made alkaline with 10N sodium hydroxide, the product was extracted into chloroform or methylene chloride. The organic extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated to dryness under reduced pressure. It is usually expedient to remove impurities from the product by chromatography on silica gel (E. Merck Kieselgel 60 (70-230 mesh ASTM)). Elution was accomplished with 2% methanol in chloroform or cyclohexane-ethyl acetate (5:1). Concentration of the product-containing fractions to dryness under reduced pressure yields the pure product.
EXAMPLE 3
Procedure III
Amination of the chloroheterocycle of Procedure II was accomplished with N-formylpiperazine, N-t-butyloxycarbonylpiperazine, piperazine, 1-methylpiperazine, or several other appropriate amines.
A. With N-formylpiperazine(piperazine-1-carboxaldehyde)
A solution (1 mmole/3 ml) of chloroheterocycle from Procedure II in benzene was stirred while 4 equivalents of piperazine-1-carboxyaldehyde was added. The mixture was stirred and heated under reflux for about six to eight hours. After the mixture had cooled to room temperature it was filtered, and the benzene phase was concentrated to dryness. The residue was purified by chromatography on silica gel using 2-4% methanol in chloroform for elution. Concentration of product-containing fractions to dryness under reduced pressure yields product that usually will crystallize on standing. Deformylation of the product is carried out according to Procedure IV.
Alternatively, the displacement reaction was run in isoamyl alcohol at 100° C. for 12-18 hours. When the reaction was complete, the mixture was concentrated to dryness under reduced pressure and the residue was partitioned between the components of a chloroform-water system at pH 10-11. The product was purified by chromatography on silica gel using 2% methanol in chloroform for elution.
B. With N-t-butyloxycarbonylpiperazine
A solution (1 mmole/4 ml) of chloroheterocycle from Procedure II in isoamyl alcohol was added dropwise in the course of about one hour to a solution (1 mmole/4 ml) of N-t-butyloxycarbonylpiperazine in isoamyl alcohol at 100°-120° C. The reaction mixture is monitored for disappearance of chloroheterocycle by thin layer chromatography. The reaction is usually complete within several hours. After a reaction time of 4-18 hours the reaction mixture was concentrated to dryness under reduced pressure and the residue was partitioned between chloroform and water after the pH was adjusted to 10-11 with sodium hydroxide. The product is purified by chromatography on silica gel using cyclohexane-ethyl acetate (5:1) for elution. Concentration of product-containing fractions to dryness under reduced pressure yields the compound in sufficient purity for deblocking of the piperazine moiety according to Procedure V.
C. With Piperazine or 1-Methylpiperazine
(i) In Benzene: A solution (1 mmole/3 ml) of chloroheterocycle from Procedure II in benzene was mixed with a four-fold molar excess of piperazine in benzene (1 mmole/ml) and the reaction mixture was heated to reflux. Within an hour piperazine hydrochloride began to precipitate. The reaction was monitored by tlc for disappearance of starting chloroheterocycle. After a period of 4-18 hours, the reaction mixture was filtered and the benzene phase was concentrated to dryness. The residue was taken up in a chloroform-water system in which the pH was adjusted to 10-11 with sodium hydroxide. The chloroform extract was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated by dryness under reduced pressure. The product is usually sufficiently pure for conversion to the mono- or dihydrochloride with a slight excess of 2N hydrochloric acid or anhydrous hydrogen chloride in ethanol. The salt is finally crystallized from ethanol or ethanol-ether mixtures. (ii) In Isoamyl Alcohol: A solution (1 mmole/4 ml) of chloroheterocycle from Procedure II was added dropwise in the course of about one hour to a fourfold molar excess of piperazine or 1-methylpiperazine in isoamyl alcohol (1 mmole/5 ml) at 100°-120° C. The reaction was monitored for disappearance of starting chloroheterocycle by tlc. After a period of 4-18 hours, the reaction mixture was concentrated under reduced pressure, and the residue was partitioned between a chloroform-water system in which the pH was adjusted to 10-11 with sodium hydroxide. Concentration of the chloroform extract to dryness under reduced pressure gave a product that was purified by chromatography on silica gel using 5% methanol in chloroform for elution. Concentration of the product-containing fractions under reduced pressure gave material that was converted to the mono- or dihydrochloride salt with either a slight excess of 2N HCl or anhydrous hydrogen chloride in ethanol. The salt was crystallized from ethanol or ethanol-ether mixtures.
EXAMPLE 4
Procedure IV-Deformylation
The N-formylated product of Procedure III was dissolved in 2N hydrochloric acid at a concentration of about 25 mg/ml and the solution was heated to 90° C. for an hour. The solution was concentrated to dryness under reduced pressure. The residue was taken up in water and the solution was concentrated to dryness under reduced pressure. The dissolution and concentration process was repeated several times. Finally, the salt was crystallized from ethanol.
EXAMPLE 5
Procedure V-De-t-Butyloxycarbonylation
The N-t-butyloxycarbonyl compound of Procedure III was dissolved in trifluoroacetic acid at a concentration of 1 mmole/7 ml. After about one hour the reaction mixture was concentrated to dryness at room temperature. The product in aqueous solution was passed through a column of Dowex-1 ion exchange resin on the hydroxide ion cycle. After the aqueous solution was concentrated to dryness, the residue was converted to the mono- or dihydrochloride salt with a slight excess of 2N HCl; or hydrogen chloride in ethanol. The product was crystallized from ethanol or ethanol-ether.
Alternatively, the residue from evaporation of the trifluoroacetic acid reaction may be partitioned between the phases of a chloroform-water system after the pH was adjusted to 10-11 with sodium hydroxide rather than passing the residue through the ion-exchange column. The residue from the washed and dried chloroform extract is then coverted to the hydrochloride salt in the usual manner.
EXAMPLE 6
2-Cyclopropyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-Cyclopropyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
Cyclopropylcarboxamidine hydrochloride was converted to the title compound according to Procedure I. The crystalline product was obtained in 66% yield and showed an m/e of 208. The 200 MHz pmr spectrum of the product was fully compatible with the assigned structure.
Anal. Calcd for C 10 H 12 N 2 OS (208.28): N, 13.45; C, 57.66; H, 5.81; S, 15.39. Found: N, 13.49; C, 57.80; H, 5.78; S, 15.50.
B. 2-Cyclopropyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step A was converted to the title compound according to Procedure II. For this case the 4-chloro analog crystallized directly from the reaction medium in 95% yield and was washed with ether. The product showed m/e=225 and a 200 MHz pmr spectrum was fully consistent with the proposed structure.
Anal. Calcd for C 10 H 11 N 2 SCl•0.37HCl (240.11): N, 11.67; C, 50.00; H, 4.77; Cl, 20.23; S, 13.36. Found: N, 11.57; C, 49.68; H, 4.76; Cl, 20.78; S, 13.56.
C. 2-Cyclopropyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
The product of step B was reacted with 4 equivalents of piperazine in isoamyl alcohol at 100° C. according to Procedure III. The product was converted to the dihydrochloride with anhydrous hydrogen chloride in ethanol. Crystallization of the product from hot ethanol gave the title compound in 38% yield. The product showed m/e=276 and a 200 MHz pmr spectrum was fully compatible with the designated structure.
Anal. Calcd for C 14 H 22 Cl 2 N 4 S•0.6C 2 H 5 OH (376.96): N, 14.87; C, 48.43; H, 6.85; Cl, 18.81; S, 8.50. Found: N, 14.79; C, 47.96; H, 6.86; Cl, 17.57; S, 8.36.
EXAMPLE 7
2-Benzyl-4-(1-piperazinyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-Benzyl-7,8-dihydro-6H-thiapyrano-[3,2-d]pyrimidin-4-one
Phenylacetamidine hydrochloride was converted to the title compound according to the details of Procedure I. The crystalline product was isolated in 77% yield and showed m/e=258. The 200 MHz pmr spectrum of the product was completely compatible with the assigned structure of the product.
Anal. Calcd for C 14 H 14 N 2 OS (258.33): N. 10.85; C, 65.09; H, 5.46; S, 12.41. Found: N, 10.69; C, 64.88; H, 5.35; S, 12.24.
B. 2-Benzyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step A was converted to the corresponding 4-chloro analog according to Procedure II. The title compound was obtained in 69% yield after purification by chromatography on silica gel using cyclohexane-ethyl acetate (3:1) for elution. The product showed m/e=276 and a 200 MHz pmr spectrum consistent with the projected structure.
Anal. Calcd for C 14 H 13 ClN 2 S (276.77): N, 10.12; C, 60.75; H, 4.73; Cl, 12.81; S, 11.58. Found: N, 10.26; C, 61.26; H, 4.87; Cl, 12.62; S, 11.27.
C. 2-Benzyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
The product of Step B was treated with four equivalents of piperazine in benzene according to Procedure III. The product was converted to the dihydrochloride without purification by chromatography and yielded the title compound in 66% yield after crystallization from ethanol. The product showed m/e=326 and a 200 MHz pmr spectrum full consistent with the assigned structure.
Anal. Calcd for C 18 H 24 Cl 2 N 4 S (399.37): N, 14.03; C, 54.13; H, 6.06; Cl, 17.75; S, 8.03. Found: N, 14.10; C, 53.86; H, 6.25; Cl, 17.56; S, 7.76.
EXAMPLE 8
2-Phenyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-Phenyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
Benzamidine hydrochloride was converted to the title compound in 88% yield using the conditions of Procedure I. The product showed m/e=244 and a 200 MHz pmr spectrum consistent with the assigned structure.
Anal. Calcd for C 13 H 12 N 2 OS (244.30): N, 11.47; C, 63.91; H, 4.95; S, 13.12. Found: N, 11.29; C, 63.69; H, 5.01; S, 13.15.
B. 2-Phenyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step A was reacted with phosphorus oxychloride according to Procedure II. The title compound was obtained in 95% yield and was sufficiently pure so as not to require chromatographic purification. (When this synthesis was run on scales larger than one gram, chromatography on silica gel using cyclohexane-ethyl acetate (3:1) was required and the yield slipped to 52%.) The product showed m/e=262 and a 200 MHz pmr spectrum fully in accord with the designated structure.
Anal. Calcd for C 13 H 11 ClN 2 S (262.76): N, 10.66; C, 59.42; H, 4.22; Cl, 13.50; S, 12.20. Found: N, 10.55; C, 59.29; H, 4.36; Cl, 13.53; S, 11.91.
C. 2-Phenyl-4-(4-formyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step B was reacted with four equivalents of piperazine-1-carboxyaldehyde in isoamyl alcohol at 100° C. according to Procedure III. The title compound was obtained in 38% yield after column chromatography using 2% methanol in chloroform followed by preparative thin layer chromatography on silica using the same eluant. The product showed m/e=340 and a 200 MHz pmr spectrum consistent with the proposed structure.
Anal. Calcd for C 18 H 20 N 4 OS (340.44): N, 16.46; C, 63.50; H, 5.92. Found: N, 16.37; C, 63.34; H, 5.88.
D. 2-Phenyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
The product of Step C was deformylated according to Procedure IV. The title compound was obtained in 77% yield after crystallization from ethanol and showed m/e=312. The 200 MHz pmr spectrum of the product is fully compatible with the designated structure.
Anal. Calcd for C 17 H 22 Cl 2 N 4 S•81H 2 O (399.94): N, 14.01; C, 51.05; H, 6.21; Cl, 17.73; S, 8.02. Found: N, 14.21; C, 50.62; H, 6.09; Cl, 17.53; S, 7.75.
EXAMPLE 9
2-Trichloromethyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-Trichloromethyl--7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
Trichloroacetamidine (K. Dachlauer to I. G. Farbenind, Ger. Pat. No. 671,785, Feb. 14, 1939) is added to a solution (1.5 mmoles/ml) of an equivalent amount of 2-carboethoxy-3-oxotetrahydrothiapyran in ethanol. The mixture was allowed to stand overnight at room temperature. The product was isolated in 7% yield by filtration. (The low yield is apparently a result of the instability of the acetamidine which has a propensity to polymerize.) The product shows m/e=284, 286, 288 and a 200 MHz pmr spectrum consistent with the assigned structure.
Anal. Calcd for C 8 H 7 Cl 3 N 2 OS (285.57): N, 9.81; C, 33.64; H, 2.47; Cl, 37.24; S, 11.23. Found: N, 9.67; C, 34.25; H, 2.75; Cl, 36.21; S, 10.12.
B. 2-Trichloromethyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step A was converted to the 4-chloro analog according to Procedure II. The product was purified by preparative thin layer chromatography on silica gel using cyclohexane-ethyl acetate (5:1) for development. The title compound was obtained in 45% yield. The product showed m/e=302, 304, 306 and a 200 MHz spectrum compatible with the assigned structure.
Anal. Calcd for C8H 6 Cl 4 N 2 S (304.01): N, 9.22; C, 31.60; H, 1.99; S, 10.55; Cl, 46.64. Found: N, 9.23; C, 31.98; H, 2.11; S, 10.77; Cl, 45.36.
C. 2-Trichloromethyl-4-(4-t-butyloxycarbonyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step B was reacted with 4 equivalents of N-t-butyloxycarbonylpiperazine in isoamyl alcohol according to Procedure III. The product was purified by preparative thin layer chromatography on silica gel using cyclohexane-ethyl acetate (5:1) and yielded the title compound in 30-60% yield. The product showed m/e=452 and a 200 MHz pmr spectrum appropriate for the designated structure.
D. 2-Trichloromethyl-4-(1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Monohydrochloride
The product of Step C is converted to the title compound according to Procedure V using the alternative partition step rather than the ion-exchange procedure for generation of the free base form of the title compound. The product was obtained in about 25% yield. The product showed m/e=352, 354, 356 and a 200 MHz pmr spectrum consistent with the proposed structure.
Anal. Calcd for C 12 H 16 Cl 4 N 4 S (390.16): N, 14.36; C, 36.94; H, 4.13. Found: N, 14.13; C, 37.27; H, 4.19.
EXAMPLE 10
2-Trifluoromethyl-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Hydrochloride
A solution of 4.5 g (40 mmoles) of trifluoroacetamidine (W. L. Reilley and H. C. Brown, J. Amer. Chem. Soc. 78, 6032 (1956). R. A. Moss, W. Guo, D. Z. Denney, K. N. Houk, and N, G. Rodan, J. Amer. Chem. Soc. 103, 6164 (1981)) in 15 ml of methanol was added to a solution of 7.6 g (40 mmoles) of ethyl 3-oxotetrahydrothiapyran-2-carboxylate in 15 ml of methanol. After being allowed to stand overnight, the solution was cooled and the wall of the vessel was "scratched" until the product precipitated. In this manner, 1.47 g of 2-trifluoromethyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one was obtained by filtration.
A 0.7 g portion of the above pyrimidinone was converted to the corresponding 4-chloro analog according to procedure II. In this manner, 405 mg of 2-trifluoromethyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine was obtained and used in the next step without further purification.
A solution of 200 mg (785 μmoles) of the above 4-chloro analog in 3 ml of isoamyl alcohol was treated with 315 mg of 1-methylpiperazine according to Procedure III. Purification of the product by preparative thin layer chromatography on silica using 5% methanol in chloroform yielded 198 mg of eluted product that was treated with 75 mg of anhydrous hydrogen chloride in 0.5 ml of ethanol. Crystallization of the product from ethanol yielded 154 mg of the title compound. The 200 MHz pmr spectrum is fully compatible with the projected structure and m/e=318 (calcd 318).
Anal. Calcd for C 13 H 18 ClF 3 N 4 S (354.82): N, 15.79; C, 44.00; H, 5.11; Cl, 9.99; S, 9.04; F, 16.06. Found: N, 15.79; C, 44.29; H, 5.15; Cl, 9.88; S, 8.81; F, 14.74.
EXAMPLE 11
2-Methoxy-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A solution of 570 mg (2 mmoles) of 2-chloro-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (S. Ohno, et al. to Maruko Seiyaki Co., Ltd., U.K. patent application GB 2,117,368 A) in 7 ml of anhydrous dimethylformamide was treated with 540 mg (10 mmoles) of sodium methoxide and the mixture was stirred and heated at 125° C. for 18 hours. The mixture was concentrated to dryness under reduced pressure and the residue was partitioned between 50 ml of CHCl 3 and 50 ml of H 2 O. The chloroform phase was separated and the aqueous phase was extracted with 50 ml of CHCl 3 . The combined chloroform extracts were washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated to dryness under reduced pressure. The 570-mg residue was put on a 100 g (30 cm×5 cm (d)) column of silica gel and the product was eluted with 5% methanol in chloroform. The product which runs only slightly slower than the starting material on silica gel was isolated as "single-spot" pure material. After attempts to crystallize the product as a dimaleate salt failed the product was converted to the dihydrochloride with anhydrous hydrogen chloride in ethanol. The product was crystallized from ethanol-ether giving a 35% yield of title compound showing M+H=281 and a 200 MHz pmr spectrum fully compatible with the assigned structure.
Anal. Calcd for C 13 H 22 Cl 2 N 4 OS•1H 2 O (373.13): N, 15.01; C, 41.84; H, 6.54; Cl, 19.00; S, 8.59. Found: N, 14.91; C, 41.76; H, 6.23; Cl, 18.95; S, 7.73.
EXAMPLE 12
2-(β-Methoxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-(β-Methoxyethyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
3-Methoxypropionamidine hydrochloride (2.77 g, 20 mmoles) in Procedure I yielded 2.6 of the title compound that showed m/e=226 (calcd 226) and a 200 MHz pmr spectrum fully compatible with the assigned structure.
Anal. Calcd for C 10 H 14 N 2 O 2 S (226.29): N, 12.38; C, 53.08; H, 6.24; S, 14.17. Found: N, 12.48; C, 52.91; H, 6.28; S, 13.94.
B. 2-(β-Methoxyethyl)-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
Treatment of 1.2 g of the above pyrimidinone with phosphorus oxychloride according to Procedure II gave after chromatography, 584 mg of product showing m/e=244 (calcd 244) and a 200 MHz pmr spectrum fully in accord with its structure.
C. 2-(β-Methoxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
Treatment of 580 mg of the above 4-chloro intermediate in 9 ml of isoamyl alcohol with 920 mg of 1-methylpiperazine in 15 ml of isoamyl alcohol according to Procedure III yielded 480 mg of product after chromatography. Conversion of this product to the dihydrochloride on treatment with 100 mg of anhydrous hydrogen chloride in ethanol followed by crystallization of the product from ethanol-ether yielded 430 mg of the title compound showing a mass spectrum and a 200 MHz pmr spectrum fully in accord with the projected structure.
Anal. Calcd for C 15 H 26 Cl 2 N 4 OS (381.36): N, 14.69; C, 47.24; H, 6.87; Cl, 18.59; S, 8.41. Found: N, 14.60; C, 46.95; H, 6.99; Cl, 16.89, 16.94; S, 8.11.
EXAMPLE 13
2-(β-Benzyloxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A. 2-(β-Benzyloxyethyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
Treatment of 6.5 g of 3-benzyloxypropionamidine hydrochloride (Prepared in two steps from acrylonitrile, W. P. Untermohlen, Jr., J. Amer. Chem. Soc. 67, 1505 (1945). C. Djerassi and C. R. Scholz, to Ciba Pharm. Prod., U.S. Pat. No. 2,516,108, July 25, 1950.) with 5.7 g of ethyl 3-oxotetrahydrothiapyran-2-carboxylate according to Procedure I yielded 5.26 g of the title compound showing m/e=302 (calcd 302) and a 200 MHz pmr spectrum fully in accord with the projected structure.
Anal. Calcd for C 16 H 18 N 2 O 2 S (302.40): N, 9.27; C, 63.55; H, 6.00; S, 10.60. Found: N, 9.23; C, 63.33; H, 6.04; S, 10.54.
B. 2-(β-Benzyloxyethyl)-4-(2,4,6-triisopropylbenzenesulfonyloxy)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A solution of 3.02 g (10 mmoles) of the above pyrimidinone in 150 ml of methylene chloride was treated with 120 mg (1 mmole) of 4-dimethylaminopyridine 12.1 g (120 mmoles) of triethylamine and 4.54 g (15 mmoles) of 2,4,6-triisopropylbenzenesulfonyl chloride. After one hour the reaction mixture was concentrated to dryness and the residue was taken up in chloroform and plated onto 60 g of silica gel by evaporation under reduced pressure. The resulting adsorbent was added to the top of a 550 g column of silica gel packed in cyclohexane and the column was eluted with a 1:1 mixture of ethyl acetate and cyclohexane. In this manner 6.11 g of title product having a satisfactory 200 MHz pmr spectrum was isolated.
C. 2-(β-Benzyloxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A solution of 2.07 g of the above 4-(2,4,6-triisopropylbenzenesulfonyloxy) analog (3.63 mmoles) and 1.82 g (18.15 mmoles) of 1-methylpiperazine in 35 ml of ethanol was heated at 50° C. overnight. The reaction mixture was concentrated to dryness under reduced pressure and the residue was partitioned between 100 ml of chloroform and 100 ml of water at pH 13. Concentration of the washed and dried chloroform extract to dryness yielded a 1.48 g residue that was purified by chromatography on silica gel using elution with 5% methanol in chloroform. The 200 MHz pmr spectrum of the free base form of the subject compound was fully in accord with the assigned structure.
Anal. Calcd for C 21 H 28 N 4 OS (384.53): N, 14.57; C, 65.59; H, 7.34; S, 8.34. Found: N, 14.70; C, 65.50; H, 7.37; S, 8.42.
A solution of 64 mg of the above free base in 2.5 ml of ethanol was treated with 15 mg of anhydrous hydrogen chloride in 0.1 ml of ethanol. After being concentrated to dryness, the residue was crystallized from 1.2 ml of hot ethanol to yield 38 mg of the subject compound that gave m/e=384 (calcd 384) and a satisfactory 200 MHz pmr spectrum.
Anal. Calcd for C 21 H 30 Cl 2 N 4 OS (457.45): N, 12.25; C, 55.13; H, 6.61. Found: N, 12.07; C, 54.81; H, 6.63.
EXAMPLE 14
2-(β-Hydroxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A solution of 149 mg (390 μmoles) of 2-(2-benzyloxyethyl)-4-(4-methyl-1-piperazinyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine from Example 13 in 3 ml of trifluoroacetic acid was treated with 1.2 ml of 1M boron tris-trifluoroacetate in trifluoroacetic acid at ice bath temperature for one hour. After an additional hour of reaction at room temperature, the reaction mixture was evaporated to dryness. The residue showed some starting material remaining by tlc so that above treatment was repeated. The residue from the second treatment was taken up in a few ml of ethanol and treated with 0.5 ml of 5N NaOH. The mixture was concentrated at room temperature, diluted with water and extracted with chloroform. The chloroform soluble material which amounted to 88 mg was purified by preparative thin layer chromatography on a 500 μ 20×20 cm silica plate using 7.5% methanol in chloroform. A 43 mg fraction (Rf 0.3) was eluted and converted to the hydrochloride after treatment with 75 mg of anhydrous hydrogen chloride in ethanol. The product, isolated as a glass, showed M+H=295 (FAB) and a satisfactory 200 MHz pmr spectrum.
Anal. Calcd for C 14 H 24 Cl 2 N 4 Os (366.73): N, 15.25; C, 45.77; H, 6.59. Found: N, 15.08; C, 45.90; H, 6.65.
EXAMPLE 15
2-Vinyl-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
A solution of 441 mg of 2-(β-hydroxyethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine in 10 ml of anhydrous methylene chloride was treated with 850 mg of methyltriphenoxyphosphonium iodide and the mixture was stirred at room temperature overnight.
The reaction mixture was diluted to a 50 ml volume with methylene chloride and the solution was washed with saturated aqueous sodium bicarbonate, dried over MgSO 4 , filtered and concentrated to dryness. The residue (1.07 g) was purified by chromatography on a 100 g silica gel column that was eluted first with chloroform and then 5% methanol in chloroform. The 310 mg of purified product was taken up in a few ml of ethanol and treated with 150 mg of anhydrous hydrogen chloride in ethanol. Crystallization of the product from 7 ml of hot ethanol yielded 260 mg of the title compound showing a satisfactory mass spectrum and 200 MHz pmr spectrum.
Anal. Calcd for C 14 H 22 Cl 2 N 4 S (349.32): N, 16.04; C, 48.13; H, 6.35; Cl, 20.30; S, 9.18. Found: N, 16.10; C, 47.86; H, 6.24; Cl, 20.52; S, 9.04.
EXAMPLE 16
2-(Carboethoxymethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A. 2-(Carboethoxymethyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one
Treatment of 299 mg of ethyl amidinoacetate hydrochloride (D. J. Collins, J. Chem. Soc. 1337 (1963). Difficulty was experienced in getting reproducibly satisfactory preparations of this intermediate.) with 333 mg of ethyl 3-oxotetrahydrothiapyran-2-carboxylate by a modification of Procedure I in which ethanol was substituted for methanol gave a product which could not be crystallized so the reaction mixture was concentrated to dryness and the residue was triturated with ether. In this manner 314 mg of product was obtained and used directly in the next step. The mass spectrum and 200 MHz pmr spectrum of this product were satisfactory.
B. 2-(Carboethoxymethyl)-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Step A (314 mg) was treated with phosphorus oxychloride according to Procedure II. The 147 mg residue thus obtained was purified by preparative thin layer chromatography on two 20 cm× 20 cm 1000 μ silica gel plates using a 1:1 cyclohexane-ethyl acetate system. In this manner, 52 mg of product showing Rf 0.51 was obtained. The mass spectrum and 200 MHz pmr spectrum were in accord with the projected structure of the title compound.
C. 2-(Carboethoxymethyl)-4-(4-methyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A solution of 113 mg of the product of Step B in 2.5 ml of isoamyl alcohol was treated with four equivalents of 1-methylpiperazine according to Procedure III. The 211 mg of product so obtained was purified by preparative thin layer chromatography on two 20 cm×20 cm 1000 μ silica gel plates using 5% methanol in chloroform. The 111 mg of product of Rf 0.40 showed a mass spectrum of 336 (calcd 336) and a 200 MHz pmr spectrum compatible with the projected structure.
EXAMPLE 17
2-Methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A. 2-Methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidin-4-one (This compound and its synthesis is described by K. Thomae in French Patent 1,593,867, 10 July 1970.)
Acetamidine hydrochloride in Procedure I yielded the title compound in 79% yield. The crystalline product was obtained in two crops, the first melting at 224°-226° C. and the second at 223°-224° C. The 200 MHz pmr spectrum was fully in accord with the structure designated for the product. Similar syntheses gave a product showing:
m/e=182 and Anal. Calcd for C 8 H 10 N 2 OS (182.24): N, 15.38; C, 52.72; H, 5.53; S, 17.59. Found: N, 15.37; C, 52.76; H, 5.52; S, 17.68.
B. 2-Methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (This compound and its synthesis are described by K. Thomae in French Pat. No. 1,593,867, 10 July 1970.)
The product of Step A was converted to the corresponding 4-chloro analog according to Procedure II. The product has been obtained in yields as high as 90% in small scale (e.g. 450 mg) reactions. Such products show m/e=200 and 200 MHz pmr spectra fully consistent with the designated structure.
Anal. Calcd for C 8 H 9 ClN 2 S (200.68): N, 13.96; C, 47.88; H, 4.52; Cl, 17.66; S, 15.98. Found: N, 14.16; C, 48.06; H, 4.48; Cl, 17.76; S, 16.02.
When the scale of the reaction was increased to several grams, it became necessary to purify the product by chromatography on silica gel using cyclohexane-ethyl acetate (1:1) for elution. Yields ranging from 70% to 30% have been realized as the scale of reaction increases. Temperature control at the quenching stage is apparently the critical factor in determining yield.
EXAMPLE 18
2-Methyl-4-(4-formyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2d]pyrimidine
The product of Example 17, Step B, was treated with four equivalents of N-formylpiperazine in benzene at 80° C. according to Procedure III. After the reaction mixture was filtered, the benzene phase was concentrated to dryness and the residue was purified by preparative thin layer chromatography on silica gel using 4% methanol in chloroform for development. The title product obtained in essentially quantitative yield showed m/e=278 and a 200 MHz pmr spectrum consistent with the designated structure of the product.
Anal. Calcd for C 13 H 18 N 4 OS (278.37): N, 20.13; C, 56.09; H, 6.52; S, 11.52. Found: N, 19.83; C, 55.84; H, 6.34; S, 11.25.
EXAMPLE 19
2-Methyl-4-(4-t-butylcarbonyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
The product of Example 17, Step B, is reacted with four equivalents of N-t-butyloxycarbonylpiperazine in isoamyl alcohol at 100° C. as described in Procedure III.
EXAMPLE 20
2-Methyl-4-[4-(2-propenyl)-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
The product of Example 17, Step B was treated with four equivalents of N-allylpiperazine (Prepared from piperazine monohydrate and allyl chloride according to Dahlbom, et al., Acta Chemica Scandanavia 15, 1367-1371 (1961) and references cited therein.) in isoamyl alcohol at 100° C. according to Procedure III. The product was purified by chromatography on silica gel using 5% methanol in chloroform as eluant. The product was converted to the dihydrochloride and crystallized from ethanol-ether. The crystalline product was dissolved in water and filtered through a pad of Super-Cel to remove insolubles and the clear aqueous solution was concentrated to dryness. The residue on crystallization from hot ethanol gave the pure title compound in 16% yield. The product showed M+H=291 (FAB mass spectrum) and gave 200 MHz pmr spectrum fully compatible with the assigned structure.
Anal. Calcd for C 15 H 24 Cl 2 N 4 SO•0.2C 2 H 5 OH•0.5H 2 O (381.56): N, 14.69; C, 48.47; H, 6.92; Cl, 18.58; S, 8.40. Found: N, 14.26; C, 48.27; H, 6.90; Cl, 18.39; S, 8.49.
EXAMPLE 21
2-Methyl-4-(4-cyclopropyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Dihydrochloride
The product of Example 17, Step B, was treated with four equivalents of N-cyclopropylpiperazine (Prepared from N,N-bis(β-chloroethyl)p-toluenesulfonamide and cyclopropylamine as reported by J. Mills and C. W. Ryan to Eli Lilly & Co., U.S. Pat. No. 3,342,816, June 1, 1965.) in isoamyl alcohol at 100° C. according to Procedure III. The product was purified by chromatography on silica gel using 5% methanol in chloroform as eluant and converted to the dihydrochloride. Crystallization of that product gave the title compound in 30% yield. The product gave m/e=290 and showed a 200 MHz pmr spectrum that is fully consistent with the assigned structure.
Anal. Calcd for C 15 H 24 Cl 2 N 4 S (363.34): N, 15.42; C, 49.28; H, 6.66; Cl, 19.51; S, 8.82. Found: N, 15.50; C, 49.50; H, 6.38; Cl, 19.27; S, 8.88.
EXAMPLE 22
2-Methyl-4-(4-benzyl-1-piperazinyl-7,8-dihydro-6H-thiapyrano[3,2-d]-pyrimidine Dihydrochloride
The product of Example 17, Step B, was treated with four equivalents of N-benzylpiperazine, in isoamyl alcohol at 100° C. according to Procedure III. The product was purified by chromatography on silica gel using 2% methanol in chloroform for elution. The product was converted to the dihydrochloride with 2N HCl and the salt was decolorized with Darco charcoal in aqueous solution. The aqueous solution was concentrated to dryness and the residue was treated with hot ethanol and the mixture was centrifuged. The supernatant ethanol solution was concentrated to dryness giving the title compound as a glass, in 70% yield. The product gave a m/e=340 and the 200 MHz pmr spectrum was fully compatible with the structure designated for the compound.
Anal. Calcd for C 19 H 26 Cl 2 N 4 S•0.6C 2 H 5 OH•0.8H 2 O (455.47): N, 12.30; C, 53.26; H, 6.90; Cl, 15.57; S, 7.04. Found: N, 12.18; C, 53.06; H, 6.75; Cl, 15.84; S, 6.56.
EXAMPLE 23
2-Methyl-4-(4-carboethoxy--piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine Hydrochloride
The product of Example 17, Step B, was treated with 4 equivalents of ethyl N-piperazinocarboxylate in isoamyl alcohol at 100° C. according to Procedure III. The product was purified by chromatography on silica gel using 5% methanol in chloroform for elution and the product was converted to the dihydrochloride using anhydrous hydrogen chloride in ethanol. The title compound was isolated in 60% yield after crystallization from hot ethanol. The product showed m/e=322 and gave a 200 MHz pmr spectrum that was completely consistent with the structure projected for the compound.
Anal. Calcd for C 15 H 23 ClN 4 O 2 S (358.88): N, 15.62; C, 50.20; H, 6.46; Cl, 9.88; S, 8.93. Found: N, 15.31; C, 50.12; H, 6.36; Cl, 9.68; S, 8.65.
EXAMPLE 24
2-Chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A mixture of 2,4-dichloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (5.0 g, 22.6 mMol), anhydrous sodium acetate (3.7 g, 45.2 mMol), and 10% palladium on carbon (7.5 g) in absolute ethanol (100 ml) was hydrogenated at 3 atmospheres (gauge) with rocking at room temperature. After 2 hours, additional palladium on carbon (3 g) was added and hydrogenation was continued for 3 hours. The reaction mixture was filtered and concentrated in vacuo. The oil was dissolved in 200 ml of dichloromethane, filtered and concentrated to leave 2-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine as an oil (2.85 g, 15.3 mMol, 68%); nmr (CDCl 3 ) δ: 8.24 (1H, s), 3.02 (2H, t), 2.91 (2H, t), 2.20 (2H, m).
EXAMPLE 25
2-Piperazino-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A mixture of 2-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (187 mg, 1.00 mMol) and piperazine (344 mg, 4.00 mMol) was heated at 100° C. under nitrogen for 1.5 hours. The cooled mixture was worked up with 5% sodium bicarbonate (25 ml) and chloroform (25 ml). The organic layer was concentrated to an oil which was triturated with diethyl ether to give 2-piperazino-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (118 mg, 0.5 mMol, 50%) as white solid, m.p. 125°-6° C.; nmr (CDCl 3 ) δ: 7.98 (1H, s), 3.67 (4H, t), 2.92 (2H, t), 2.86 (4H, t), 2.71 (2H, t), 2.14 (2H, m); mass spectrum (E.I.): 236 (M+).
A mixture of 2-piperazino-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (71 mg, 0.30 mMol) and maleic acid (69 mg, 0.60 mMol) was dissolved in chloroform, concentrated in vacuo and triturated with ether to leave the dimaleate salt, m.p. 180°-2°.
EXAMPLE 26
2-(N-Methylpiperazino)-7,8-dihydro-6H-thiapyrano [3,2-d]pyrimidine
In the manner described in Example 25, 2-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (140 mg, 0.75 mMol) and 1-methylpiperazine (400 mg, 4 mMol) were heated to afford 2-(N-methyl-piperazino)-7,8-dihydro-6H-thiapyrano[3,2d]pyrimidine (129 mg, 0.51 mMol, 68%) as an oil.
A portion of the free base thus obtained was converted into the maleate in methanol and recrystallized from MeOH-ether to give the maleate salt with a m.p. of 191°-192° C. Both mass spectra and nmr were consistent with the desired structure.
EXAMPLE 27
2-Chloro-4-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
To a stirred suspension of methyl triphenylphosphonium bromide (2.2 equiv.) in anhydrous 1,2-dimethoxyethane under dry nitrogen at -30° to -35° C. was added n-butyllithium in hexane (2.2 equiv.); the reaction mixture was stirred for 1 hour, and 2,4-dichloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine (1 equiv.) in anhydrous 1,2-dimethoxyethane was added.
The mixture was allowed to warm slowly (about 1 hour) to room temperature and then stirred at room temperature for 16 hours. Sodium carbonate (1 equiv.) in water was added to the above solution of the heterocyclic ylide; the mixture was refluxed for 3 hours, evaporated under pressure, and then suspended in chloroform and extracted with dilute aqueous hydrochloric acid, the combined aqueous layers were made alkaline with sodium hydroxide and the resulting mixture was extracted with ether. The combined ether extracts were dried and evaporated, and the product was purified by recrystallization.
EXAMPLE 28
2-Piperazino-4-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
In the same manner described in Example 25, 2-piperazino-4-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine was prepared from 2-chloro-4-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine and piperazine.
EXAMPLE 29
4-[4-(2-Hydroxyethyl)piperazino]-2-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine maleate
A mixture of 201 mg (1.0 mMol) of 2-methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine and 520 mg (4.00 mMol) of 2-(2-hydroxyethyl)piperazine was stirred at 105° C. under N 2 for 1 hour. The mixture was treated with 10 ml of 5% NaHCO 3 and was extracted with 20 ml of chloroform. The solution was dried over magnesium sulfate and concentrated to an oil which was chromatographed over 20 cc of basic alumina with 25 ml fractions of chloroform. The solution was removed in vacuo to leave an oil which was treated with 110 mg (0.95 mMol) of maleic acid in a minimum of methanol. The solution was diluted with 25 ml of diethylether to give 230 mg (0.56 mM) of white solid, m.p. 104°-8° C. NMR (free base in CDCl 3 ) δ: 2.21 (2H, 5°), 2.50 (3H, 1°), 2.64 (6H, m), 2.87 (2H, 3°, thiapyrano ring), 2.95 (2H, 3°, thiapyrano ring), 3.45 (4H, 3°), 3.65 (2H, 3°) mass spectrum (EI): m/E 294 (m + ).
Elemental Analysis Calcd for C 14 H 22 N 4 O 5 •C 4 H 4 O 4 : C, 52.67; H, 6.38; N, 13.65; S, 7.81. Found: C, 52.13; H, 6.25; N, 12.74; S, 7.39.
EXAMPLE 30
4-(4-Hydroximinopiperidino)-2-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine maleate
A mixture of 352 mg (1.75 mMol) of 2-methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine, 600 mg (5.25 mMol) of 4-hydroximinopiperidine and 3 ml of isvamyl alcohol was heated at 110° C. for 1 hour under N 2 . The cooled mixture was concentrated in vacuo, treated with 15 ml of 5% sodium bicarbonate solution, and extracted in 2×20 ml of chloroform. The chloroform was dried over magnesium sulfate and concentrated in vacuo to give 220 mg (0.72 mMol) of a white solid, 4-(4-hydroximinopiperidino)-2-methyl-7,8-6H-thiapyrano[3,2-d]pyrimidine)(b). NMR (CDCl 3 ) δ: 2.17 (2H, 5°) 2.41 (1H, 3°), 2.43 (3H, 1°), 2.72 (2H, 3°), 2.81 (2H, 3°, thiapyrano ring), 2.90 (2H, 1°), 2.91 (2H, 3°, thiapyrano ring), 3.48 (2H, 3°), 3.53 (2H, 3°).
MS (EI): m/e 278 (Mf)
Elemental Analysis Calcd for C 13 H 18 N 4 O 5 •H 2 O: C, 52.68; H, 6.80; N, 18.90; S, 10.82. Found: C, 52.74; H, 6.46; N, 19.05; S, 10.21.
A mixture of 41 mg (0.15 mMol) of the free base and 17 mg (0.15 mMol) of maleic acid was dissolved in a small amount of methanol which was removed in vacuo. The residue was triturated with diethyl ether to leave 58 mg of the title compound as a white solid, m.p. 234-7°.
EXAMPLE 31
4-Methoxyiminopiperidine
A mixture of 7.68 g (50.0 mMol) of 4-piperidone monohydrate hydrochloride and 4.17 g (47.9 mMol) of 0-methylhydroxylamine hydrochloride was refluxed in 30 ml of ethanol for 1.5 hours. The mixture was cooled to 35° C. and was diluted with 150 ml of diethyl ether. Cooling gave 5.14 g (31.2 mMol) of 4-methoxyiminopiperidine hydrochloride as fine crystals, m.p. 143° C. (with dec).
A solution of 3.3 g (20.0 mMol) of the hydrochloride was dissolved in 10 ml of H 2 O and was treated with 20 ml of sodium hydroxide (20.0 mMol) to raise the pH to 8.9. The solution was concentrated in vacuo, dried by concentrating from 50 ml of ethanol and the 50 ml of acetonitrile, and extracted with 125 ml of hot benzene which gave 1.27 g (10.0 mM) of white needles on cooling of the title compound, m.p. 115°-18° C. (trace to 132°). NMR (CDCl 3 ) δ: 2.81 (2H, 3°), 2.95 (2H, 3°), 3.27 (2H, 3°), 3.36 (2H, 3°), 3.85 (3H, 3°).
EXAMPLE 32
4-(4-Methoxyiminopiperidino)-2-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine maleate
A mixture of 201 mg (1.0 mMol) of 2-methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine and 500 mg (3.91 mMol) of 4-methoxyiminopiperidine was heated at 110° C. under N 2 for 2 hours. The mixture was treated with 20 ml of 5% sodium bicarbonate and 30 ml of chloroform. The chloroform was concentrated in vacuo and the remaining oil was chromatographed on 30 cc of basic alumia with chloroform (25 ml fractions). Fraction 2 was concentrated in vacuo to give 63 mg (0.22 mMol) of white solid (2), m.p. 125°-6° C. NMR (CDCl 3 ) δ: 2.20 (2H, 5°), 2.46 (2H, 3°), 2.49 (3H, 1°), 2.72 (2H, 3°), 2.88 (2H, 3°), 2.97 (2H, 3°), 3.49 (2H, 3°), 3.56 (2H, 3°), 3.85 (3H, 1°).
A mixture of 46 mg of the free base and 18 mg of maleic acid was dissolved in a minimum of methanol and concentrated in vacuo. The residue was stirred with 50 ml of diethyl ether which gave a white solid on concentration in vacuo to leave the title compound.
EXAMPLE 33
4-(4-Aminopiperidino)-2-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine
A mixture of 201 mg (1.00 mMol) of 2-methyl-4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine, 520 mg (3.00 mMol) of 4-aminopiperidine dihydrochloride, (See Emert et al., Chem. Ber. 48, 691 (1915)) 0.84 ml (6.00 mMol) of triethylamine and 4 ml of isoamyl alcohol was stirred at 130° C. for 2 hours under nitrogen. The cooled mixture was concentrated in vacuo, treated with 20 ml of 5% sodium bicarbonate solution and extracted with 2×20 ml of chloroform. The chloroform was dried over magnesium sulfate and concentrated in vacuo to give an oil which was chromatographed on 30 cc of Brinkman E. Merck kiesel gel 60 (70-230mesh) with 50 ml fractions of 1:1-ethylacetate:hexane. Fractions 3 and 4 were combined and concentrated and the residue was dissolved in 1N hydrochloric acid which was concentrated in vacuo to give 95 mg (0.31 mMol) of 4-piperidino-2-methyl-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine hydrochloride as a solid, m.p. 157°-60° C. NMR (CDCl 3 ) δ: 1.7 (6H, broad 1°), 2.21 (2H, 5°), 2.49 (3H, 1°), 2.86 (2H, 3°), 2.93 (2H, 3°), 3.36 (4H, narrow multiplet).
Mass spectrum (EI): m/e 249 (M + -1).
Calcd for C 13 H 21 ClN 3 S: C, 54.43; H, 7.38; N, 14.65; Cl, 12.35. Found: C, 54.06; H, 6.56; N, 14.15; Cl, 12.11.
EXAMPLE 34
2-(β-Methoxyethyl)-4-(4-ethyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine dihydrochloride
A solution of 2-(β-methoxyethyl)-4-chloro-7,8-dihydro-6H-thiapyrano[3,2d]pyrimidine, the product of Example 12, Step B, in isoamyl alcohol is added dropwise to a hot stirred solution of four equivalents of N-ethylpiperazine in isoamyl alcohol as outlined in Procedure III. The reaction mixture is worked up according to Procedure III yielding the title compound.
EXAMPLE 35
2-(β-Methoxyethyl)-4-(4-n-propyl-1-piperazinyl)-7,8-dihydro-6H-thiapyrano[3,2d]pyrimidine dihydrochloride
A mixture of 6 mmoles of 1-n-propylpiperazine dihydrochloride and 12 mmoles of triethylamine in 10 ml of isoamyl alcohol is heated to 100° C. Next, a solution of 1.5 mmoles of 2-(β-methoxyethyl)4-chloro-7,8-dihydro-6H-thiapyrano[3,2-d]pyrimidine from Example 12, Step B in 10 ml of isoamyl alcohol is added dropwise to the hot stirred solution in the course of about 30 minutes. The reaction is allowed to proceed and is worked up in the manner described in Procedure III to yield the title compound.
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There are disclosed certain 2-substituted-4-substituted 6H-7,8-dihydrothiapyrano[3,2-d]pyrimidines which have oral hypoglycemic activity and with such ability to lower blood sugar are useful in the treatment of type II diabetes and/or obesity with associated insulin resistance. Processes for the preparation of such compounds and compositions containing such compounds as the active ingredient thereof are also disclosed. The compounds are also β-adrenergic blocking agonists or α-adrenergic blocking agents and act as ocular antihypertensives and are useful for the treatment of glaucoma and other eye disorders.
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REFERENCE TO RELATED APPLICATIONS
This application is related to British Patent Application entitled Clock Divider filed on Mar. 24, 1994 as U.K. Serial No. 9405806.2.
BACKGROUND
This invention relates to digital counters, and more particularly, to digital counters used to derive from a system clock one or more subsystem clocks.
Digital counters are a common component of digital systems. A typical digital system includes a system clock, and on each cycle of the system clock the counter will count. The count can be either up (e.g., from 0 to M, where M is an integer) or down (e.g., from M to 0), which ever is most convenient to implement. The counter could be programmable (e.g., M is programmable), or the counter could be hardwired (e.g., M is a single, fixed value, determined by how the counter is constructed). The counter has many applications, including timing (e.g., event timing or delay loop), and dividing down the system clock to a slowing frequency.
In general, the design of a clock is relatively straight forward. Clock design becomes tricky, however, as the desired clock frequency increases. At clock frequencies much above 10 MHZ, careful layout is needed to minimize EMI, clock skew, and other problems. At clock speeds approaching 100 MHz, these problems are even more severe, with connections between the clock and other circuit elements more resembling wave guides than simple wires.
One approach to reducing the required clock rate is to use a multiphase clock. In a multiphase clock, each clock phase operates at the same rate as the other clock phases, but out of phase with the other clock phases. With proper design, successive phases of a multiphase clock can be used to clock successive stages of a sequential logic circuit, thereby creating an effective clock rate of (no. of phases) * (clock frequency). For example, a simple two phase system clock would consist of a "clock" and its inverse, clock. Clock would be 180 degrees out of phase with clock. In a particular system, the effective clock rate of a system could be almost doubled by judicious allocation of clock and clock to clocking various logic elements. For example, a Master-Slave Flip Flop could be clocked by clocking the Master stage with clock, and clocking the Slave stage with clock.
Some digital systems require multiple clocks, operating at different clock rates or frequencies. Often the most practical approach to generating these clocks is to build a single systems clock that runs at a high enough frequency that all other clocks can be obtained by simply dividing (i.e., counting) the systems clock. A simple example is a digital system having three subsystems, one requiring a 2 MHz clock, one a 3 MHz clock, and the third a 4 MHz clock. To minimize the frequency of the systems clock, the choice of systems clock should be the least common multiple of these three subsystems clocks, or 12 MHz. The 2, 3 and 4 MHz subsystem clocks could be provided by dividing the 12 MHz systems clock by divisors of 6, 4 and 3, respectively.
While this least common multiple approach is generally adequate, the required system clock can be prohibitively high. The multiphase system clock can be divided down to produce multiphase slower clocks. In particular, each phase of a multiphase system clock can be divided down to a new clock signal, care being taken to maintain the phase relationships in tact. Alternatively, a single phase of a system clock signal can be divided down to create the new slower clock, and this slower clock then can be used to generate a multiphase clock signal at the slower clock rate.
For multiphase clocks (system or otherwise), the general case is an L-phase clock (L is an integer), with clock phases being spaced symetrically 360/L degrees apart in phase. This approach achieves a maximum possible effective clock of L times the system clock. A popular multiphase clock scheme is the quadrature clock (e.g., four phases, successive phaseses being 90 degrees apart).
Of course, there are practical limits to the number of phases into which a given clock can be split. Moreover, achieving this maximum effective clock rate requires that sequential logic elements are clocked by successive phases of the clock.
The combined multiphase, system clock approach has generally proven adequate. However, the divided subsystem clocks are limited to counting down the subsystem clock, which is 1/(Number of Phases, L) the frequency of the effective system clock. There is therefore a need for a clock divider that makes full use of the multiphase system clock to allow integer divisors of the effective system clock, rather than just integer divisors of the system clock.
More generally, there is a need for a combined clock and counter, with the clock having L phases, and the counter is capable of counting at a frequency scaled by L. There is a further need for the counter to be programmable "on the fly," and to generate an output signal that has a substantially even mark-space ration (i.e., substantially a 50% duty cycle).
SUMMARY OF THE INVENTION
The present invention is directed to a method and system for implementing an L phase clock in conjuction with an apparatus having L counters, where L is an integer, to count at a frequency scalable by L. In accordance with one aspect of the invention, a counter is clocked by a L phase system clock of frequency f, counting an integer number N. The apparatus includes L counters for counting (N-D), where D is a predetermined integer number that allows each counter to settle before N would be counted, each counting being clocked by a predetermined phase of system clock. The apparatus further includes a logic OR gate and L counter controllers, one counter controller associated with each counter, for delaying the output of their associated counter by at least D. The L counters and their associated counter controllers are arranged in series such that the input to each counter is the output of the previous counter in series delayed by the counter controller associated with the previous counter. The outputs of each counter are delayed by their associated counter controller, then are inputs to the OR gate, which ORs the outpours to form the output of the counter.
In accordance with another aspect of the invention, the counter is used to divide the clock by an integer divisor of the effective clock.
In accordance with another aspect of the invention, the counter control includes a master-slave flip flop. The master is connected to the output of the associated counter means and clocked by the clock phase clocking the associated counter means. The slave connected to the input of the OR gate, and to the next counter in series and is clocked by the clock clocking the next counter in series.
In accordance with another aspect of the invention, the clock is a quadrature clock.
Other aspects of the invention will become apparent from the following description with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a digital system that effectively provides a quadrature system clock to each of four subsystems, with the subsystems each containing a clock divider, embodying the apparatus and method of the present invention, for generating subsystem clocks.
FIG. 2 is a timing diagram illustrating the relationship between the quadrature system clock, the effective system clock, and the subsystem clocks.
FIG. 3-1 through 3--3, collectively referred to herein as FIG. 3, are a schematic diagram of a clock divider of FIG. 1, including four counters connected in series/parallel configuration, and a counter controller associated with each counter.
FIG. 4 is a schematic diagram of the logic of a counter controller of FIGS. 3 (1-3).
FIG. 5 is a schematic diagram of the components of a counter of FIG. 3 (1-3) showing how the counter is implemented using fast carry counters.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIGS. 1 and 2, there is shown in FIG. 1 a block diagram of a digital system 10. Digital system 10 includes four subsystems 14, and system clock generator 12 for generating a quadrature system clock 16, shown in FIG. 2, that is provided to subsystems For ease of analysis, shown above clock 16 is effective system clock 17, the theoretical clock rate at which circuit elements in subsystems 14 could be clocked by quadrature clock 16. Provided, that is, these circuit elements could be appropriately clocked. Note that since clock 16 is in quadrature (four phases), effective system clock 17 is four times the frequency (one-fourth the period) of system clock 16.
Subsystems 14 represent typical digital circuit elements that preferably are implemented on the same integrated circuit. Subsystems 14 are not clocked directly by system clock 16. Instead, each subsytem 14 includes a clock divider 18 that receives system clock 16, and uses system clock 16 to generate a subsystem clock 20 that runs at a slower clock rate than system clock 16. The clock divider 18 is an example of a system that uses a counter 22 embodying the present invention.
In accordance with the invention, subsysytem clocks 20 are not limited to being integer divisors of system clock 16 (i.e., integer multiples of the period of clock 16). Rather, subsystem clocks 20 can be integer divisors of effective system clock 17 (i.e., integer multiples of the period of effective system clock 17). For example, referring now to FIG. 2, the period of subsystem clock 20-1 is 4.00 times the period of system clock 16, or 16.0 times the period of effective system clock 17. The period of subsystem clock 20-2 is 4.25 (a noninteger) times the period of system clock 16, but 17 (an integer) times the period of effective system clock 17. The period of subsystem clock 20-3 is 4.50 (a noninteger) the period of system clock 16, but 18 (an integer) times the period of effective systems clock 17. Finally, the period of subsystem clock 20-4 is 4.75 (a noninteger) the period of system clock 16, but 19 (an integer) times the period of effective subsystem clock 17.
The general case for the frequencies of subsystems clocks 20 is given by the following equations: Subsystem clock 20=(Number of Phases,L)(system clock ##EQU1## where NDATA is an integer that specifies the divisor for effective system clock 17.
As a matter of practical design, preferably problems of clock skew are minimized by having clock generator 12 generate only two clocks 16 that are 45 degrees out of phase: The remaining clocks 16 needed by subsystems 14 can be created locally by inverting these two clocks 16. In particular, generator 12 generates i0 clock (in-phase 0) clock 16-1 and q0 clock (quadrature 0) clock 16-2, which can be seen in FIG. 2 to lag i0 clock 16-1 by 45 degrees. Dividers 18 receive respective i0 and q0 clocks 16-1 and 16-2, and invert each to produce additional i1 (in-phase 1) and q1 (quadrature 1) clocks 16-3 and 16-4.
Referring now to FIGS. 1 and 3 (1-3) in FIG. 3 there is shown a simplified block diagram of a clock divider 18. Each clock divider 18 receives as inputs quadrature system clocks 16-1 and 16-2, and produces a subsystem clock 20 that is an integer divisor, NDATA, of the effective system clock rate 17. NDATA is a P-bit binary word, preferably 22 bits in width, which allows NDATA to range from 1 to 2 p =2 22 (4,194,304). In this manner, digital system 10 can be clocked by a relatively fast quadrature systems clock 16, and a divider 18 can divide systems clock 16 to provide useful kHz-range subsystems clocks 20 that are useful for TV and CD player applications.
Each clock divider 18 includes four counters 22 that combine to produce subsytem clock 20. Associated with each counter 22 is a counter controller 24, a system clock buffer 26, and a system clock multiplexer 28. Each clock divider 18 further includes clock divider control logic 30, divisor selector 27, inverter/buffer 32, subtractor 29, N/4 latch 31 and N/8 latch 33.
Divisor selector 27, subtractor 29, N/4 latch 31 and N/8 latch 33 are used to load divisors (derived by subtractor 29 from NDATA) into counters 22, as discussed further below. Clock divider control logic 30 exercises overall control of clock divider 18 (e.g., control over divisor selector 27, multiplexers 28, counter controllers 24, subtractor 29, and latches 31 and 33), and preferably is itself controlled by a microprocessor (not shown). Control logic 30 also clocks latches 31 and 33.
Inverter/buffer 32 receives respective i0 and q0 system clocks 16-1 and 16-2 from clock generator 12, and in turn buffers these clocks, and also inverts these clocks to produce the remaining respective i1 and q1system clocks 16-3 and 16-4. From inverter/buffer 32, quadrature clocks 16 are connected to the multiplexers 28 associated with each counter 22. Under control of control logic 30, each multiplexer 28 switches one of four quadrature clock signals 16, through the associated clock buffer 26, to become the CLOCK IN signal to clock associated counter controller 24 and counter 22. Similarly, each multiplexer 28 also switches the inverse o of the particular clock 16 to become the CLOCK OUT signal, as discussed further herein. Clock buffers 26 not only buffer the particular clock 16 and its inverse, but also condition thses clock signals to prevent any possibility of their overlap.
Counter controllers 24 control their associated counters 22. In particular, controllers 24 control the loading of divisors (from latches 31 or 33) into their counter 22, control the counting of their counter 22, and route the output, CARRY, of their counter 22 to the appropriate locations and with the appropriate delays.
An important aspect of the invention is how counters 22 and their associated controls 24 are connected to produce subsystem clocks 20. Counters 22 are connected in an arrangement that is both serial and parallel at the same time. The parallel aspect is that subsystem clock 20 is formed, in effect, by logically ORing together the CARRY (i.e., output) of each counter 22, using four input OR gate 42. For timing reasons discussed further herein, to reach OR gate 42, each CARRY first passes through associated counter control 24, to become PULSE. When necessary, counter control 24 delays CARRY by two cycles of the quadrature clock 16 that is clocking counter control 24 and its associated counter 22.
Counters 22 are also connected together in series. The CARRY of one counter 22 serves, in effect, to trigger the input of the next counter 22 in series. The loop in the series of counters 22 is closed by having the output of counter 22-4, the last counter 22 in series, in effect triggering the input of counter 22-1, the first counter 22 in series. With proper assignment of the phase (i.e., i0, i1, q0 or q1) of quadrature system clock 16 for each counter 22 and its associated control 24, the subsystem clock 20 can have a period that is an integer multiple of the period of the effective system clock 17 (i.e., a noninteger multiple (to a fourth) of the period of the system clock 16).
In describing the serial aspect of counters 22, the caveat "in effect" is used because the CARRY is not conveyed directly to the next counter 22 in series, but instead is conveyed to the counter control 24 associated with the next counter 22 in series. The control 24 receiving the CARRY latches CARRY, and sends it on to its associated counter 22 only after an appropriate delay to allow the signal to settle into a determinate state. The appropriate delay is at least one clock 16 cycle of the particular clock 16 phase (the indeterminate period of clock 16 depends on the particular design of counters 22, but in any case is at most one period of clock 16).
As previously mentioned, counters 22 are loaded with divisors other than NDATA. NDATA would be inappropriate to load into counters 22, because NDATA is the divisor relative to effective systems clock 20, four times systems clock 16, rather than a real clock. What counters 22 actually count to produce the leading edge of subsystem clocks 20 is a divisor relative to the particular clock 16 that multiplexers 28 have connected to counter 22 and its associated control 24. This divisor is NDATA/4, one-fourth the count of NDATA.
Actually loading NDATA/4 into counters 22, however, would not achieve the desired clock 20. As previously mentioned, counter controls 24 add a delay to the count of their associated counter 22. The actual divisor loaded into counters 22 must take into account the amount of this delay. This delay is two cycles of their respective clock 16 cycles. Consequently, counters 22 are loaded with a count or divisor of NDATA/4-2.
In a preferred embodiment, subsystem clock 20 has substantially equal mark/space ratio (i.e., a 50% duty cycle). Dividers 18 produce a substantially equal mark space ratio by using counters 22 to position the trailing edge of clocks 20. The count or divisor used by counters 22 to produce the trailing edge of clocks 20 is NDATA/8-2. Note that this count also compensates for the delay introduced by control 24, a delay that allows counters 22 to settle to a determinate state before their output signal is used.
To position the trailing edge of clocks 20, control logic 30 loads NDATA/8-2 into a particular counter 22 after that particular counter 22 has generated a CARRY based on NDATA/4-2. The particular counter 22 then counts NDATA/8-2, and the subsequent CARRY is used by the associated counter controller 24 to position the training edge of the particualr clock 20.
The timing considerations mentioned above are vital to the proper operation of dividers 18. Timing problems become more accuse the greater the frequency of system clock 16. For example, a 30 MHz system clock 16 would have a period of 33.33 nS. Adjacent phases of clock 16 would be offset by one-fourth the clock 16 period, or only 8.33 nS. Symmetry of logic design becomes particularly important, since standard logic gates have typical delays of 1-2 nS, which is a significant fraction of the phase difference.
Another important issue is how control logic 30 decides which quadrature clock 16 multiplexers 28 should connect to each counter 22 (and associated counter logic 24). With four counters 22 and their associated control 24, there are many possible combinations, only some of which yield useful results for subsystem clocks 20.
In the case of a four phase system clock 16, all possible subsystem clocks 20 (resulting for NDATA>16) can be described by four combinations or categories of multiplexer 28 connections. These four categories are labeled "EVEN1, EVEN2, ODD1 and ODD2," and are listed in Table 1. For the general case of L counters 22 and L phases of clock 16, the necessary combinations can be derived by constructing an equivalent timing chart to FIG. 2, and observing for each desired divisor what combination of phases of clock 16 should be used.
Referring now to FIGS. 3 (1-3) and Table 1, control logic 30 assigns clock 16 phases by first examining NDATA to determine which of these four categories applies. Table 1 lists these categories and the phase of quadrature clock 16 associated with each category. As discussed further later, these four categories are derived from examining the relationship between the desired subsystem clocks 20 and quadrature system clocks 16. In particular, as shown in Table 1 control logic 30 assigns categories based on the two least significant bits (LSBs) of NDATA.
TABLE 1______________________________________ Quad Quad Quad Quad Clock 16 Clock 16 Clock 16 Clock 16 Phase for Phase for Phase for Phase for2 LSB of Counter Counter Counter CounterNDATA Category 24-1 24-2 24-3 24-4______________________________________00 EVEN1 i0 16-1 i0 16-1 i0 16-1 i0 16-101 ODD1 i0 16-1 q0 16-2 i1 16-3 q1 16-410 EVEN2 i0 16-1 i1 16-3 i0 16-1 i1 16-311 ODD2 i0 16-1 q1 16-4 i1 16-3 q0 16-2______________________________________
The timing considerations for counter conrol 24 to convey a CARRY to the next counter control 24 and associated counter 22 can be better understood with reference to FIGS. 3 (1-3) and 4. In FIG. 4 there is shown a more detailed schematic diagram of a counter control 24. Each control 24 contains the identical circuitry, fabricated essentially the same, in order to provide substantially identical delays and loading.
Control 24 receives three main input signals, LOAD ENB, EVEN1, and CARRY IN. A minor input signal is RESETB, which causes control 24 to reset its associated counter 22. Alternatively, counter 22 could be provided with a reset scheme that operated directly on the registers of counter 22, but this alternative would require more circuitry, and therefore more die space.
CARRY IN is the CARRY from the counter associated with control 24, the signal that control 24 will delay two cycles of the clock 16 clocking control 24. LOAD ENB in essence is the CARRY from the previous counter control 24 in series. EVEN1 is a signal from control logic 30 that identifies the EVEN1 category, a category that requires different handling than the other three 24 in series. EVEN1 is a signal from control logic 30 that identifies the EVEN1 category, a category that requires different handling than the other three categories. This category requires each counter 22 (and its associated control 24) to be clocked by the same phase of clock 16.
Control 24 outputs four main output signals, LOADN8, LOADN4, TOGGLE and PULSE. PULSE is the signal that is connected to four input OR gate 42. Preferably PULSE is the appropriately delayed CARRY signal, conditioned to have a substantially even mark/space ratio (50% duty cycle).
The remaining three output signals are commands to the associated counter 22. LOADN8 commands counter 22 to load NDATA/8 (actually NDATA/8-2, for reasons discussed above). LOADN4 commands counter 22 to load NDATA/4 (actually NDATA/4-2, for reasons discussed above). TOGGLE commands counter 22 to count. Note that these three commands are mutually exclusive. While loading a divisor, a counter 22 cannot be counting. While counting, counter 22 cannot be loading a divisor. While loading NDATA/4, counter 22 cannot be loading NDATA/8.
Referring now to FIGS. 3 (1-3) and 4, control 24 is clocked by two clocks, OUT CLK and IN CLK, received from the associated clock buffer 26. In essence, IN CLK is the system clock 16 associated with the particular counter 22 and control 24 (i.e., the clock 16 that control logic 30 has ordered the associated multiplexer 28 to provide), and OUT CLK is its inverse. Preferably clock buffer 26 also buffers clock 16 and its inverse, and modifies them so that there is no possibility of overlap between these two clocks, since they will be used to clock JK flips flops.
As part of generating its (appropriately delayed) output commands, each counter control 24 includes two JK flip flops (FFs) 70 and 72 connected in series. The input stage of FF 70 is clocked by IN CLK, and receives the output of two input NOR gate 73. One input of NOR gate is CARRY IN. The other input of NOR gate 73 is a reset signal that acts to reset counter 22. The output stage of FF 70 is clocked by OUT CLK, and connects through XOR gate 74 to the input of FF 72, and to the input of NAND gate 76.
Similar to FF 70, the input and output stages of FF 72 are clocked by IN CLK and OUT CLK, respectively. The output of FF 72 is the other input to XOR gate 74. The output of FF 72 also connects to the input of INVERTER 78. The output of inverter 78 is the other input to NAND gate 76, and is also inverted by inverter 84 to become the PULSE output signal. The output of NAND gate 76 is inverted by inverter 80 to become the LOADN8 output signal, and is an input to NAND gate 82. The output of NAND gate 82 passers through Inverter 83 to become TOGGLE.
The series combination of FFs 70 and 72 provide a delay to output signals LOADN/8, PULSE, and TOGGLE of two cycles of the particular clock 16. From a timing viewpoint, recall that the timing of this two cycle delay is vital for PULSE and for TOGGLE, since the two cycle delay compensates for the divisor actually counted by counter 22, NDATA/4-2. For LOADN8, this two cycle delay is acceptable, as will be discussed further herein.
In addition to FFs 70 and 72 and related combinational logic, control 24 includes JK FFs 90 and 92. Like FFs 70 and 72, FFs 90 and 92 are clocked by CLK IN and CLK OUT. FF 90 is used to reset counter 22. FF 92 is used to properly delay the LOAD ENB signal, which becomes LOADN4.
In contrast to the timing of the PULSE and TOGGLE signals, to properly time the LOADN4 signal, control 24 must delay the LOAD ENB signal an amount other than 2 cycles. To understand this, one must understand what the LOADN4 does, and its relationship to the other counter 24 output signals (PULSE and LOADN8).
As previously mentioned, LOADN4 causes counter 22 to load NDATA/4 (actually NDATA/4-2), the divisor that counter 22 will count to determine the leading edge of system clock 22. Obviously this divisor must be loaded into counter 22 before it can be counted. The loading process itself takes one cycle of the particular clock 16 that clocks both counter 22 and its associated control 24. For this reason control 24 must provide delay the LOAD ENB signal only one cycle of the particular clock 16.
Preferably LOADN4 is loaded into each counter 22 each time the counter 22 counts, rather than just on initialization of the counter 22. In this manner, the counting by counters 22 is by algorithm, rather than by dead reckoning, which is less subject to errors induced by alpha particles. Moreover, loading LOADN4 into each counter 22 each time the counter 22 counts enables "on the fly" programming: After a particular counter 22 finishes counting a particular divisor, the next counter 22 in series begins counting the new divisor.
The input to FF 92 is LOAD ENB. The output of FF 92 is essentially LOAD ENB delayed by one cycle of particular clock 16. This output is the input to a logic gate group 96 that has as other inputs EVEN1 and the undelayed LOAD ENB. Gate group 96 is designed such that EVEN1 functions as a control signal to switch either LOAD ENB or the one cycled delayed LOAD ENB (the output of FF 92), through two respective inverters 98 and 100, to become LOADN4.
The output of group 96 is also routed through inverter 98 to the remaining input of NAND gate 82. As previously mentioned, the other input to NAND gate 82 is the output of NAND gate 76. The output of NAND gate 82 is inverted by inverter 83 to become TOGGLE. The net effect is that TOGGLE is low whenever LOADN8 or LOADN4 are high.
Referring now to FIG. 5, there is shown a schematic of how each counter 22 is implemented. Rather than counting down to zero, each counter 22 counts up from the two's complement of the number to be counted, and generates a carry when the count is completed. This approach allows each counter 22 to be implemented as a number of two-bit fast carry counters 40, an implementation that counts two to three times faster than a more traditional ripple counter. Each counter 40 is edge triggered for rapid operation.
Referring now to FIGS. 3(1-3) the divisors NDATA/4-2 and NDATA/8-2 are derived under control of control logic 30. First, the division for both is performed using MUX 27, a two input, one output multiplexer. One input to MUX 27 is simply all but the two LSB of NDATA (i.e., for divide by 4), and the other input is simply all but the three LSB of NDAT (i.e., divide by 8). The output of MUX 27 is the input to subtractor 29, which subtracts two. The output of subtractor 29 is latched to latches 31 and 33, which latch respective NDATA/4-2 and NDATA/8-2.
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The invention discloses a method and an apparatus for implementing an L phase clock in conjuction with L counters, where L is an integer, to count at a frequency scalable by L.
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BACKGROUND OF THE INVENTION
The present invention relates to a profiled member for clamping plate-like elements, especially plates of glass, for display cases, shop counters, exposition furniture, or the like.
DESCRIPTION OF THE PRIOR ART
In contrast to other plate fastening means having clamping strips (German Pat. No. 875,435 Braun dated May 4, 1953), profiled members have the advantage of a more completely effective and easier securing of the plate-like elements. Such profiled members are known as gripping strips for the front plates of shop counters, and are provided with a groove or slot for accommodating the edge of a plate-like element. They have an enlarged slot portion that widens in the direction toward the base of the slot, and serve for mounting a clamping strip having a wedge-shaped cross-section, the wedge point of which faces the introduction opening of the slot. Disposed in the enlarged slot portion, in the region of the base of the slot, is a threaded bore in which is adjustably provided a pressure screw which contacts an abutment surface of the clamping strip that delimits the wedge cross-section. The pressure application direction of the pressure screw that acts upon the clamping strip here extends parallel to the plane of the plate-like element, so that the force exerted by the pressure screw is deflected, with only a small force component being used for clamping the introduced plate-like element. Since during the clamping process the clamping strip moves in the direction toward the opening of the slot, there exists the danger that the plate-like element will be taken along, and will therefore be increasingly pressed out of the slot. There is no assurance that the plate-like element will always be held securely in the slot of the profiled member to the completely desired depth.
An object of the present invention is to provide an economical profiled member of the aforementioned general type whereby the plate-like element can be reliably and particularly securely clamped in the slot via a simple and convenient operation.
SUMMARY OF THE INVENTION
This object is realized by the profiled member of the present invention, which comprises: at least one slot means that extends in the longitudinal direction of the profiled member, with each slot means being defined by a first and a second stationary planar wall, with these walls being disposed at an angle to one another, and with one of these walls being in the form of a guide surface, with said slot means being further defined by a third wall that proceeds from the second wall and, remote from the latter, has a free edge that defines an introduction opening, for a plate-like element, remote from a base portion of the slot means that interconnects the first and second walls, with the third wall and the second wall defining a triangular-shaped, enlarged portion of the slot means, with the third wall being provided with threaded through-holes for accommodating pressure-applying screws; also provided is a profiled clamping strip that can be accommodated in the enlarged slot portion and can be displaced by the pressure-applying screws, with each clamping strip having a fundamentally wedge-like cross-sectional shape which, when the clamping strip is installed in an enlarged slot portion, includes a wedge point region that faces the base portion of the slot, a first wedge surface adjacent to the wedge point that is displaceably supported on the guide surface, a second wedge surface adjacent to the wedge point that extends parallel to the first wall and defines, within the slot means, a parallel-walled slot of changeable width for accommodating and holding in place an edge portion of a plate-like element, with said clamping strips also including an abutment surface that interconnects the first and second wedge surfaces and is acted upon by the pressure-applying screws, with the pressure-application direction of each screw extending parallel to the guide surface; said clamping strip is furthermore provided with integral parts that project from the wedge-like cross-sectional shape and are disposed in the slot means to secure the position of the clamping strip in the enlarged slot portion, with at least a portion of one of the integral parts extending parallel to the guide surface and being accommodated, for effective guidance, in a complementary aperture provided in the third wall and also extending parallel to the guide surface.
Because the pressure application direction of the screw extends parallel to the guide surface of the clamping strip, a particularly high clamping force is exerted upon the plate-like element. This results already when the screw is tightened only slightly, so that there is no danger to fear a deformation of the structural components. The force exerted by the pressure screw is utilized fully for clamping the plate-like element. With this orientation of the pressure application direction, there also results a particularly convenient operation of the pressure screw, because the tool for tightening or loosening the screw then extends at an angle to the plane of the plate-like element, so that the latter does not obstruct the hand that operates the tool. Since the region of the wedge point faces the base of the slot, and the guide surface of the enlarged slot portion that serves for guiding the wedge-shaped clamping strip extends at an angle to the plane of the plate-like element, the clamping strip tries to move as deep into the slot as possible when the screw is tightened, in this way taking the plate-like element along. The more the pressure screw is tightened, the more the plate-like element is pressed against the base of the slot. This assures a reliable clamping of the plate-like element via a high clamping force.
The various functions of the clamping strip can be optimized. Where the pressure is exerted, hard material is used, whereas in the remaining regions, where, for example, only sealing functions are provided, softer and hence also more easily deformable material is used. These features have independent, patentable significance. This can also be used for clamping strips of synthetic material, such as PVC, that can be produced in a particularly economical manner by producing the two zones of the clamping strip by co-extrusion, including a coordinated, side-by-side extrusion of the two zones, with a subsequent combining of the zones in a common tool that has the overall cross-section of the clamping strip.
Securing the clamping strip in the slot has the advantage that the clamping strips, despite the enlarged portion of the slot, cannot fall out or move into a wrong position if no plate-like element is in the slot. Thus, it is possible already during the manufacture of the profiled member to provide the latter with the clamping strip. There is also no danger that the clamping strip will tilt or twist when the slot is empty; the introduced plate-like element will always be clamped by a properly positioned clamping strip. For this purpose there are various measures, which can also be used simultaneously.
A first possibility for securing the position is provided by a flexible flap that projects from the wedge-shaped fundamental cross-section of the clamping strip, with at least a portion of the flap extending transverse to the slot in the installed state of the clamping strip. The features previously described for constructing the clamping strip can be used for a differing material construction where the flap forms the edge zone that comprises soft material, and the wedge-shaped fundamental cross-section forms. If the flap extends in front of the base of the slot, such a flap can also serve as a soft abutment for the introduced plate-like element. Due to a good securing of the position of the clamping strip, a relatively long flap is used which, due to the deformation of the material during clamping, can also be extended; however, due to the recess of provided especially in the region of the base of the slot, disruptive excessive lengths are eliminated. This can be effected by folding the flap. In order to enhance this effect, it is recommended to provide an undercut at the contact area of the flap. It is particularly advantageous to give the flap an angular shape, and to integrate its base part into the wedge-shaped contour region.
A further possibility for securing the position of the clamping strip is provided by a profiled projection which, however, in contrast to the flexible flap, is rigid. In this way, the profiled projection can also carry out guidance functions during movement of the clamping strip if the profiled projection essentially extends in the pressure-application direction of the pressure-applying screws and is provided with planar side surfaces that rest against planar sides of the aperture that accommodates them.
Giving particularly good results is a configuration of the clamping strip in the shape of a right isosceles triangle where the hypotenuse forms the clamping or wedge surface that presses against the plate-like element, the first short side of the triangle that faces the base of the slot forms the slide surface that is guided along the guide surface of the profiled member, and the second short side of the triangle that faces the opening of the slot forms the abutment surface for the pressure-applying screw. The contact area of the flap can be integrated into the triangular region, and the profiled projection can project from the second short side of the triangle and extend parallel to the first short side. The configuration of the profiled projection where the profiled projection, when viewed in the cross-section of the clamping strip, on the one hand comprises a profiled end portion that has parallel side surfaces, and on the other hand comprises a profiled base portion that is wider than the end portion and is seated on the second short side of the triangle is particularly advantageous because this configuration increases the stability of the profiled projection.
The inventive profiled member can additionally be provided with a cover strip that, by extending partly or completely into the slot, can be secured to the profiled member, for example via a snap connection. These cover strips cover the operating locations of the pressure screws in the profiled members, and can advantageously at the same time serve for the support of shelves in a piece of furniture.
In place of a plate-like element, it is also possible to connect strips having a U-shaped cross-section with the profiled member if the legs of such strips are formed in conformity with the contour of the clamping strip. The pressure screws can also be used to secure such a U-profile strip.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings illustrate the present invention via several exemplary embodiments. Shown are:
FIG. 1, an enlarged, cross-sectional view through one inventive profiled member with one plate-like element clamped therein, and with another plate-like element removed from the profiled member,
FIG. 2, a greatly enlarged cross-sectional view of a compression or clamping strip used with the inventive profiled member,
FIGS. 3 and 4, in nearly actual size, are cross-sectional views of two different cover strips, either of which could be used with the inventive profiled member of FIG. 1.
FIG. 5 is a view providing a perspective illustration of one application of the inventive profiled member as a corner support in a piece of furniture, and shows the components illustrated in FIGS. 3 and 4,
FIG. 6 is a view that shows an alternate form for an upper component of the corner support of FIG. 5,
FIG. 7 is an exploded view of an alternate form for a lower component of the corner support of FIG. 5,
FIG. 8 is a cross-sectional view similar to that of FIG. 1 through a profiled member in which a strip having a U-shaped cross-section has been introduced,
FIG. 9 is a front view of the profiled member shown in FIG. 8, with the strip having the U-shaped cross-section being embodied as a slotted strip,
FIG. 10 is a perspective view of the profiled member as it is used pursuant to FIGS. 8 and 9, and more clearly showing the application possibilities for the slotted strip, and
FIGS. 11 to 14 are perspective illustrations or views of pieces of furniture that can be constructed with the inventive profiled members using plate-like elements.
DESCRIPTION OF PREFERRED EMBODIMENTS
In FIG. 1, the bar or profiled member 10 is designed for connecting the corners of two plate-like elements 11, 11'. For this purpose, the profiled member is provided with two longitudinally extending grooves or slots 12, 12', both of which are identical, so that it will be sufficient to describe one slot 12 and its components.
The slot 12 serves to receive an edge portion 13 of the plate-like element 11 to the desired depth, whereby a stationary slot wall 15 that is formed by the profiled member itself rests against the side 14 of the plate-like element. On the opposite side, an enlarged slot portion 16 is located in the profiled member. A compression or clamping strip 20 having the profile 21 shown in FIG. 2 is mounted in the enlarged slot portion. The profile of the clamping strip has the following appearance:
The clamping strip 20 primarily has the fundamentally wedge-shaped profile 22 that is defined by dot-dash lines in FIG. 2, namely the profile of an isosceles right triangle. Projecting from one side of this triangle 22 is the end piece 25 of a profiled flap 47, and projecting from the other side is a profiled projection 23. The clamping strip 20 basically comprises two zones 34, 35 which are made of materials that differ from one another, as indicated by the different cross-hatchings in FIG. 2. The material is plastic, namely PVC or polyvinylchloride, which has different hardnesses. The core zone 34, which determines the actual wedge-profile 22, comprises a relatively hard material, namely PVC having a Shore hardness of 100. The other zone forms an edge zone 35 which is made of softer material, namely PVC having a Shore hardness of 70. Where the two zones 34, 35 contact one another, namely at the contact area 51, they are securely interconnected by being glued or fused together. In this way there results a clamping strip 20 that, although being combined from two different zones 34, 35, is nonetheless one piece. The clamping strip is produced by so-called co-extrusion. The two zones 34, 35 are initially extruded separately of one another, but are immediately joined and pressed together by a common tool, resulting in a secure and permanent connection at the contact area 51.
The flap 47 itself is angled. Beginning at the aforementioned contact area 51 is a base part 24 of the flap, with this base part chiefly extending in the direction of the first short side 27 of the triangle. Connected to this base part, via a bend 65, is the free end piece 25 of the flap 47, with this end piece extending at right angles to the hypotenuse 26 of the triangle. At the connection location 51 of the base part 24, there thus results an undercut 66 between the flap 47 and the core zone 34 that is made of hard material. Critical for the yet to be explained wedge action are the hypotenuse 26 and the aforementioned first short side 27 of the triangle; this hypotenuse and short side determine, as shown in FIG. 2, the region of the wedge point 29, which here is not physically present. This flap 47, as well as the aforementioned profiled projection 23, serve to secure the position of the clamping strip 20 in the groove 12, as can be seen from the following:
In the assembled state of FIG. 1, the flap 47, in the region of the base 18 of the slot, extends transverse to the orientation of the latter, with the end 88 of the flap being supported against the stationary slot wall. As a result, the clamping strip 20 is held in the aforementioned enlarged portion 16 of the slot, even if the plate-like element 11 is not disposed in the slot 12. At the same time, the profiled projection 23 extends into an aperture 17 of the enlarged portion 16 of the slot.
As can be seen from FIGS. 1 and 2, the profiled projection 23 initially extends beyond the other short side 28 of the triangle with a trapezoidal profiled base portion 23' that merges into a profiled end portion 23" having parallel, planar side surfaces 45. In the assembled state of FIG. 1, these side surfaces 45 rest against planar sides 46 of the aforementioned aperture 17. Thus, in addition to holding the clamping strip 20, there additionally results a guidance effect during subsequently-to-be-described movements of the clamping strip 20. A further securing of the position occurs due to the fact that that wedge surface 37 of the clamping strip 20 that is determined by the first short side 27 of the triangle rests against a planar guide surface 30 that extends at an angle to the slot 12. The direction of extension of this guide surface is indicated more clearly in FIG. 1 via the dot-dash auxiliary line 39.
The other short side 28 of the wedge triangle 22 is disposed opposite the wedge point 29 and forms an "abutment surface 38" for the shaft end 41 of a screw 40, which, as can be seen in FIG. 1, can be screwed into a threaded hole 42 in that wall of the profiled member 10 that delimits the enlarged slot portion 16. The control ends 43 of the screws 40 project into the space between the two mounted plate-like elements 11, 11'; in this region, the control ends of the screws are easily accessible by a tool, for example a screwdriver, that can be operated manually. This is true because the line of application 44 of the screw 40 always forms an a 45° angle 49 with the plane 48 (indicated by a dot-dash line) of the two plate-like elements 11, 11'. The line of application 44, which is indicated by a dot-dash line in FIG. 1, is determined by the axis of the screw 40, and should be referred to as the "pressure-application direction 44" of the screw 40. When the screw is screwed in, the shaft end 41 presses against the abutment surface 38, thus moving the clamping strip 20 in the direction of the arrow 31 of FIG. 1. As a result, the one wedge surface 37 of the clamping strip 20 is pushed along the aforementioned guide surface 30 in the enlarged portion 16 of the slot, for which reason this wedge surface can be referred to as "slide surface 37". As can be seen from FIG. 1, the direction 39 in which the guide surface 30 extends, and hence in which the slide surface 37 extends, is disposed parallel to the pressure-application direction 44 of the screw 40. When the pressure screw 40 is tightened, the wedge point 29 of the clamping strip 20 moves deeper against the slot base 18. In so doing, the other wedge surface 36, which is disposed along the hypotenuse 26 of this triangle, acts as a "clamping surface" against the introduced plate-like element 11', and produces the movable slot wall 36 that can be recognized in the slot 12 and comes to rest against the facing side 19 of the plate-like element.
As can be seen in FIG. 1, in the edge portion 13, the plate-like element 11 that is to be introduced is provided on that side 14 thereof that is disposed opposite the aforementioned clamping surface 36 with a soft or yielding strip 50. This strip, for example, can be a plastic strip that can be glued to the plate-like element 11. The latter is then inserted into the slot 12 until the end edge of the plate-like element 11 abuts the transversely extending flap 47 in the slot base 18. This results in a yielding abutment surface for the end of the plate-like element. When the screw 40 is tightened, the clamping strip 20 moves in the direction 31 and takes along the introduced plate-like element, increasingly pressing the latter against the flap 47. When the clamping strip 20 is displaced in the direction 31, the length of the flap 47 is increased, forming a fold 47' that is pressed into a recess 67 disposed in the base 18 of the slot.
Various pieces of furniture, as exemplified in FIGS. 11 to 14, can be produced with the profiled member 10, because the following is common to all of them:
The profiled members 10 form vertical supports in the corner regions between which not only vertical but also horizontal plate-like elements can be disposed. Transversely extending metallic cross-pieces are not required. If glass plates are used, as is the case in FIG. 11, with the exception of the corner supports 10, nothing obstructs the view. FIGS. 5 to 7 show the construction of such a glass display case of FIG. 11. Naturally, modified forms of the illustrated profile members 10 could also be used where, instead of the 90°-position shown in FIG. 1, the two plate-like elements 11, 11' could extend at either an obtuse or acute angle relative to one another. Furthermore, it is also possible to provide more than two or less than two slots 12, 12' in the profiled member 10 for accommodating plate-like elements. However, in each case each plate-like element 11 has its own slot 12, its own clamping strip 20, and its own screws 40. Naturally, in place of the pressure screws 40, other pressure-application means could also be used for the movement 31 of the associated clamping strip 20; for example, a wedge could be used that is introduced behind the abutment surface 38.
The bottom end 52 of a support that is cut off from the profiled member 10 is provided with a bottom cap 53, which is shown in FIG. 7. The bottom cap is provided with corner pins 54 which in the assembled state engage the ends of channels 55 as shown in the alternative profiled members 10 of FIGS. 4 and 5. As shown in FIG. 7, the bottom cap 53 has a plurality of holes. Guided through the outer hole is a connecting screw 56 that extends into a circular recess 57 of a hollow space 58 of the profiled member 10. (see FIG. 1) The threaded shaft 61 of a base 60, the height of which can be adjusted, extends through a central hole 59; as shown in FIGS. 5 and 7, the base can have different base plates 62, 62'. To adjust the height of the base 60, the threaded shaft 61 can be screwed into a threaded central bore 79 of the profiled member 10.
In the embodiment of FIG. 11, a bottom plate 63 is placed directly upon the free corner region 64 of the bottom cap 53 shown in FIG. 5. So that the bottom plate 63 cannot lift off, a cover strip 70 is supported thereon; the profile of this cover strip is shown in FIG. 3, and is indicated by dot-dash lines in FIG. 1. The cover strip 70 covers the inner side 33 of the profiled member 10, so that the control ends 43 of the pressure screws 40 are no longer visible. The cover strip 70 has an angular profile, and completes the square or rectangular cross-sectional shape of the profiled member 10. A hollow space 69 results wherein electrical lines or the like can be placed. The cover strip 70 can be mounted via a snap connection, for which purpose edge portions 71 are provided that extend into corresponding recess portions of the slot, so that in the adjacent region, the slot opening 32 remains free for the introduction of a plate-like element 11, as shown in FIG. 1. The cover strip 70 can be made of flexible material, such as aluminum or plastic. The cover strip 70 has a selected length 75, and has the further function of serving, with its upper end, as a support for a further bottom plate 68, as shown in FIG. 11. In conformity with FIG. 5, the plate 68 has cut-off corner regions which, although they cover the aforementioned hollow space 69, end prior to the inner side 33 of the continuous profiled member 10.
The glass display case 80 of FIG. 11 is finally provided with a top plate 76 that is supported in the same manner as the aforementioned bottom plate 68 via a further partial piece of a cover strip 70. To hold this top plate in place, the top cap 77 or 77' shown in FIGS. 5 and 6 can be used, with the one cap 77 being provided with a downwardly directed edge, whereas the other cap 77' is flat. If the cap 77 is used, the top plate 76 can rest upon the upper end 78 of the profiled member 10, whereas if the flat cap 77' is used, the top plate 76 has a cut-away corner portion as was the case with the aforementioned bottom plate 68. Securing of the top caps 77, 77' is effected via screws 81 that extend through holes 82 or 82' and can be screwed tightly into the already aforementioned central bore 79 of the profiled member 10. The head of the screw 81 can be masked or disguised with a cover 83.
As clearly shown in FIG. 5, it is also possible to mount plate supports 72 on the cover strips 70; the ends 73 of the plate supports extend into holes 74 of the cover strips 70. In this way, non-illustrated intermediate plates can also be arranged in the display case 80 of FIG. 11. In contrast, the length 75 of the individual cover strip members 70 determines the distance between the preliminarily standardized bottom and top plates 63, 68 and 76.
To the extent that support legs 85 are to be provided, as with the table 84 of FIG. 14, alternative cover strips 70' are used, the function and construction of which can be seen from FIGS. 4 and 5. In contrast to the previously described cover strips 70, these alternative cover strips are provided with wider edge portions 86, which close off the slot openings 32 in the manner of a stopper. Here also the profiled member 10 can be mounted via a snap connection, for which purpose projections 87, 89 are provided on the edge portions 86; these projections cooperate with the aforementioned channel 55 and aperture 17 in the profiled member 10. Since with the cover strip 70' no plates have to be secured, the clamping strips 20 can be omitted, as shown in FIG. 4. In the angle region of the cover strip 70', a recessed portion 90 can be provided for receiving a fastening screw if, for example, in the table 84 of FIG. 14, a plate 68 is to be placed upon the lower part of the support leg 85.
Starting from a profiled member 10 that is continuous over the entire length 93 of a piece of furniture, by suitable dimensioning and selection of the two cover strips 70 and 70' it, is possible to obtain sections which have the function of a support leg or of a connection support for plates, as can be seen in conjunction with the cabinet or case 92 of FIG. 12. After the bases 60, there follows first a short support leg 85 that is produced by a correspondingly short cover strip 70'. Placed thereon is a bottom plate that is not shown in detail. Following this is a first section of a connection support 95 for the securing of wood panels 94. Therefore, in this section the other cover strip 70 of FIG. 3 is used, which has an appropriate length 75. In this section 95, clamping strips 20 are naturally provided which are held in their height position in the support leg section 95 by the cover strips 70 disposed therebelow, because with the cover strips 70' the projections 89 extend into the region of the enlarged slot portion 16 and therefore in turn support the clamping strip 20 disposed thereabove in the section 95. Via appropriate lengths 75 or 91 of the two cover strips 70, 70', there thereupon follow in the cabinet first three support leg sections 85', 85", and 85'", between which are located the cover strips 70' respectively position plates 68', 68". There finally again follows a section of a connection support 95' for securing wood strips 94'.
The embodiment of FIG. 13 shows a chest 96, the lower portion of which initially has a connection support 95" for wall panels that cannot be seen. In the front region is disposed a door 97 having hinges 98 that are held firmly in place by the clamping action of the clamping strip disposed at that location in the slot of the associated profiled member 10. This is basically also what occurs with the glass door 97' of the glass cabinet 80 of FIG. 11. In this support section 95" again appropriately long cover strips 70 of the type illustrated in FIG. 3 are used. There the follows a section 85' in the form of a support leg, so that here the cover strips 70' of FIG. 4 are used. Disposed therebetween is again a plate 68, with the chest 96 being closed off at the top by a top plate 76. The aforementioned table 84 of FIG. 14 also has a similar construction, although in this case only the cover strips 70' of FIG. 4 are utilized in the two support leg sections 85, 85'.
FIGS. 8 to 10 show a further variant of a cover strip 70", the edge portions of which have a construction similar to that of the cover strip 70, so that it permits securing of plate-like elements 11. However, this cover strip 70" is provided with an undercut longitudinal groove 99 for receiving intermediate plate supports 100, which comprise a hammer-head-like securing part 101 having a threaded shaft 103 upon which can be screwed a threaded sleeve 104. By screwing the threaded sleeve 104, the groove wall 102 is clamped between the hammer head of the securing part 101 on the one hand, and the end face of the threaded sleeve 104 on the other hand. The intermediate plate support 100 is thus secured at a certain height, and can serve for the support of an intermediate plate 105.
A strip 106 having a U-shaped cross-section is introduced into the other slot 12' in FIGS. 8 to 10, where it is held in place by the pressure screw 40. One leg 109 of this strip is essentially planar and rests against the stationary slot wall 15 of the profiled member 10. In contrast, the other U-leg 110 is bent in conformity with a partial contour of the pressure strip 20. Thus here also there results an abutment surface against which the pressure screw 40 can engage. The leg end 111 can be supported in the recess 67 in the slot base 18. In the present embodiment, the U-side or crown 107 of the strip 106 is provided with slots 108 into which can be introduced the hook ends of known support arms 113. As shown in FIG. 10, these support arms 113 can hold a shelf plate 112. With such strips 70" and 106, the possible variations for the furniture of FIGS. 11 to 14 are increased even further.
The present invention is, of course, in no way restricted to the specific disclosure of the specification and drawings, but also encompasses any modifications within the scope of the appended claims.
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A profiled member for clamping plate-like elements, including a slot that accommodates the edge of a plate-like element. A clamping strip having a wedge-shaped cross-section is disposed in this slot, and the clamping strip is pressed against the plate-like element via pressure screws. The clamping strip is disposed in an enlarged slot portion that is provided with a guide surface for guiding the wedge-shaped clamping strip. So that the clamping action is particularly reliable, secure, and easy to operate, it is proposed that the direction of abutment or impact of the pressure agent that acts upon the clamping strip extend essentially parallel to the guide surface, and that the wedge point of the wedge-shaped clamping strip face the base of the slot. In the enlarged slot portion, the guide surface is disposed at a greater and greater distance from the plate-like element as one proceeds in the direction toward the opening of the slot.
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CROSS REFERENCE TO RELATED APPLICATION(S)
This Application is a continuing application of application Ser. No. 10/464,994, entitled “APPARATUS AND METHOD FOR RACKMOUNTING A CHASSIS,” filed Jun. 18, 2003, which is a continuing application of patent application Ser. No. 10/073,478, entitled “APPARATUS AND METHOD FOR RACKMOUNTING A CHASSIS,” filed Feb. 11, 2002, now U.S. Pat. No. 6,644,481.
FIELD OF THE INVENTION
This invention relates in general to mounting devices, and in specific to an apparatus and method for rackmounting a chassis.
BACKGROUND OF THE INVENTION
Large-scale computer systems typically include a plurality of towers or racks of computer equipment. Each rack comprises several pieces of equipment or chassis. Each chassis may comprise a board that includes processors, memory, and/or power supplies. Other chassis might include telecommunications equipment, writing equipment, networking equipment, I/O equipment, and/or user interface equipment.
Ideally, the equipment should be removably mounted into the rack. This would allow the equipment to be easily serviced and/or installed. One way that the equipment can be removably attached to the rack is to use sliding rails that are attached to the workstation. The equipment or the chassis equipment may then be attached to the sliding rails. Thus, the chassis is supported by the sliding rails and can be moved into and out of the rack by the sliding rails, which slidably extend from the rack. The sliding rails may incorporate ball bearings to more readily facilitate the sliding action. Another way that the chassis can be slidably mounted into the rack is to use a shelf. The shelf is mounted inside the rack, and rails are provided on the shelf to guide the chassis in the shelf.
Both of these designs allow the chassis to be mounted in only one orientation. Thus, the chassis mounted so that the front of the chassis faces out of the rack; the chassis cannot be mounted so that the rear is facing out of the front of the rack, unless substantial modifications are made to the mounting system. Also, such modifications utilize parts that are not common for the left and right sides and increases the cost of the mounting kit. Note that the sliding rail design may use identical parts to comprise the rails for the left and right sides, but the assembly of these parts to form the sliding rails is different such that the sliding rails are different for the left side and the right side.
BRIEF SUMMARY OF THE INVENTION
A system for mounting a device into a rack comprising a mounting shelf that is attached to the rack, a first bracket that is attached to a first side of the device, and a second bracket that is attached to a second side of the device, wherein the second side is located opposite to the first side, wherein the first bracket and the second bracket are substantially similar, and wherein the device, with the first bracket and the second bracket attached thereto, is slideably positioned into the mounting shelf and attached to the mounting shelf via the first bracket and the second bracket.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 depicts mounting a chassis in a front facing orientation consistent with the teachings of the invention.
FIG. 2 depicts an embodiment of the inventive arrangement of the slide brackets and mounting shelf.
FIG. 3 depicts a slide bracket of FIGS. 1 and 2 .
FIG. 4 depicts an embodiment of the invention mounting a chassis in a rear-facing orientation.
FIG. 5 depicts an alternative embodiment of the slide bracket shown in FIG. 3 .
FIG. 6 depicts an alternative embodiment of the inventive arrangement using the slide bracket of FIG. 5 .
DETAILED DESCRIPTION OF THE INVENTION
The invention preferably comprises a folded sheet metal slide bracket assembly and a folded sheet metal mounting shelf. Two slide brackets are preferably used with one slide bracket supporting the left side of the chassis and the other supporting the right side of the chassis. The rack mount shelf is preferably connected to the rack through the use of screws and mounting holes. The slide bracket is preferably attached to the chassis by screws through holes and provides alignment and final positioning of the chassis within the rack.
The slide bracket of the invention can be mounted on either side of the chassis. This allows the chassis to be mounted with either the front or rear of the chassis facing out of the front of the rack. This flexibility is desirable as some users require access to the front of the chassis, for example, to load/unload storage media, while other users prefer access to the rear of the chassis, for example, to allow connection/disconnection of cables.
After attachment of the slide brackets to the chassis, the chassis with the slide brackets is mounted onto the mounting shelf. Each slide bracket preferably includes a flange, which together are used to position the chassis on the mounting shelf. The mounting shelf preferably comprises flanges such that when the chassis is properly located on the mounting shelf, the flanges of the slide brackets align with the flanges of the mounting shelf. Fasteners or other forms of connectors can then be used to attach the slide bracket to the mounting shelf. Thus, the invention allows either front-or-rear-orientation equipment mounting and minimizes the costs of mounting by using common parts regardless of orientation.
FIG. 1 depicts an arrangement of the inventive rack mount 100 for mounting chassis 103 into rack 101 . The inventive mount 100 includes mounting shelf 102 which supports chassis or device or equipment 103 . Preferably attached to chassis 103 are two slide brackets 104 , with one bracket being mounted on one side, e.g., left, and the other bracket being mounted on the other side, e.g., right. Note that the inventive rack mount 100 preferably does not include rack 101 or chassis 103 .
Each slide bracket 104 preferably includes a flange 105 that is located on the front distal end of the slide bracket 104 . Flange 105 is used to position the chassis within the rack. As shown in FIG. 1 , chassis 103 is being installed into (or removed from) the rack 101 . Flange 105 will stop the insertion of the chassis 103 when flange 105 encounters either rack 101 or mounting shelf 102 . Slide bracket 104 may then be attached to either rack 101 or mounting shelf 102 via connectors such as fasteners, screws, nuts and bolts, pins, adhesives, welds, hooks and slots, keyholes and keyhole standoffs, or any combination thereof.
Mounting shelf 102 is preferably attached to rack 101 by one or more connectors 204 ( FIG. 2 ) which could comprise one or more pins, screws, nuts and bolts, adhesives, welds, fasteners, hooks and slots, keyholes and keyhole standoffs, or any combination thereof.
Note that mounting shelf 102 may be sized so as to receive chassis 103 and be able to be attached to rack 101 . Mounting shelf 102 may include adjustable supports or brackets (not shown) so as to attach to rack 101 . This means that the rack 101 does not have to be sized to exactly fit chassis 103 . Thus, rack 101 may be significantly larger than chassis 103 . As shown in FIG. 1 , the chassis is mounted into rack 101 so that the front 106 of chassis 103 is accessible at front of rack 101 .
FIG. 2 depicts a view similar to that of FIG. 1 except that chassis 103 is not present for easier viewing of the components of the invention. The invention also preferably includes two handles 201 , one of which is mounted on each flange 105 . Handles 201 allow for chassis 103 to be more easily installed into and/or removed from the rack 101 .
FIG. 2 also depicts a preferred embodiment wherein shelf 102 includes two flanges 202 , each of which is located so as to contact a respective flange 105 of slide brackets 104 when the chassis 103 is properly located in rack 101 . Flange 105 and flange 202 preferably have co-located holes 203 which enables a connector to securely connect the slide brackets 104 , and hence, chassis 103 , to mounting shelf 102 .
FIG. 3 depicts an elevational view of one of the flanges 104 . Each flange 104 would preferably have a chassis mounting system that would allow the chassis 103 to be mounted in either a front orientation or a rear orientation.
In the embodiment shown in FIG. 3 , mounting system 300 preferably comprises hole sets 301 and 302 . Each hole set is specifically configured and placed on flange 104 to enable flange 104 to be attached to a side of chassis 103 . For example, hole set 301 may enable the left side of the chassis to be attached to flange 104 , while hole set 302 enables the right side of chassis 103 to be attached to flange 104 . Thus, flange 104 could be attached to either side of chassis 103 . Note that the mounting system 300 could comprise one or more pins, screws, nuts and bolts, adhesives, welds, fasteners, hooks and slots, keyholes and keyhole standoffs, or any combination thereof.
Note that the flange shown in FIG. 3 is oriented to attach to the left slide of chassis 103 . The flange would be inverted to be attached to the right side of chassis 103 .
Note that the holes 203 and hole sets 301 , 302 are shown by way of example only. There could be more holes, fewer holes, holes located in different positions, different-sized holes, or whatever is needed to accommodate attachment of the flange 104 to the mounting shelf 102 or attachment with chassis 103 , respectively. Further note that the connectors 204 are shown by way of example only, as there could be more connectors, fewer connectors, connectors located in different positions, different-sized connectors, or whatever is needed to accommodate attachment of the shelf 102 to rack 101 .
FIG. 4 depicts an arrangement of the chassis 103 in the rack 101 such that the rear 401 of chassis 103 is located at the front of rack 101 .
FIG. 5 depicts an alternative embodiment 500 of the slide bracket that can be used in arrangements of FIGS. 1 , 2 and 4 in place of the slide bracket 104 shown in FIG. 3 . Slide bracket 500 includes at least one additional flange, e.g. 501 and/or 502 . The additional flange(s) 501 , 502 increase(s) the strength of the slide bracket 500 . Also, slide bracket 500 may be of sufficient height so that flange 501 interfaces with flange 503 of mounting shelf 102 , and thereby provide easier mounting of the chassis into the rack. Note that bracket 104 may also be of sufficient height so that its upper portion also interfaces with flange 503 .
FIG. 6 depicts an alternative embodiment 600 using the slide bracket 500 of FIG. 5 . Note that in the embodiments shown in FIGS. 1 , 2 , and 4 , the slide bracket does not contact the upper flange 503 of the mounting shelf 102 , and the upper portion of chassis 103 may contact the upper flange 503 . Thus, the height of the chassis 103 is limited by the height of the mounting shelf 102 . In the alternative embodiment 600 , the flange 601 of mounting shelf 102 does not contact chassis 103 . The flange 601 preferably contacts the upper flange 501 of each slide bracket 500 . This would prevent vertical movement of the chassis, but would allow the chassis to be of any height.
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A system and method for mounting a device into a rack comprises a mounting shelf that is attached to the rack, a first bracket that is attached to a first side of the device, and a second bracket that is attached to a second side of the device, wherein the second side is located opposite to the first side, wherein the first bracket and the second bracket are substantially similar, and wherein the device, with the first bracket and the second bracket attached thereto, is slideably positioned into the mounting shelf and attached to the mounting shelf via the first bracket and the second bracket.
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BACKGROUND OF THE INVENTION
This invention relates to thermally-transferable ink compositions, and processes for transferring a dry layer of a thermally-transferable ink composition from a carrier to a receptor. The present invention is particularly useful in manufacturing sign faces by transferring indicia from a carrier to a receptor in a completely dry process.
Past techniques for manufacturing sign faces have not proven entirely satisfactory. For example, these techniques have involved masking or outlining the surface of the sign face so as to provide a desired outline, followed by painting (e.g., by brushing or spraying) to obtain the desired colored design. Such techniques are time consuming, messy, and require that steps be taken to provide adequate ventilation for the hazardous solvents employed with the paints or inks. Moreover, steps must be taken to insure that the solvents used in the inks do not destroy the surface to which they are applied. Furthermore, such prior art techniques frequently require that various inks be mixed. This of course means that a color match must be made before the mixed ink can be utilized.
Processes for thermally transferring indicia from a carrier (e.g., release liner) to a receptor (e.g., a fabric such as cotton) and composition useful therewith are also known. See for example U.S. Pat. Nos. 3,361,281; 3,519,463; 3,684,545; 3,928,710; and 4,037,008. These processes and compositions generally require the use of high heat and pressure to effect transfer. Typically temperatures of 120° C. or more are required.
The use of the foregoing processes has not proven entirely satisfactory. For example, the temperatures employed require the use of large quantities of energy and limit the number of materials that can be utilized as receptors as the heat generated may degrade certain polymeric receptors. Still further, these prior art processes have not been found to provide strongly adhered images on uneven or textured and three dimensional substrates. Consequently, it is clear that a need exists for compositions, and processes for transferring thermally-transferable inks that overcome these disadvantages.
SUMMARY OF THE INVENTION
Provided herein are a novel process and composition that provides unique results. The process comprises a dry technique for transferring a thermally-transferable ink composition from a carrier to a receptor. This process eliminates the need to employ adhesives to bond the ink to the receptor. It also eliminates the need to go through the time consuming and potentially hazardous techniques described above. Furthermore, it eliminates the need for the sign fabricator to employ volatile solvents in sign preparation. Still further, the process provides the sign fabricator with almost unlimited versatility in the design of the artwork to be utilized on the sign face. Consequently, the fabricator can employ a wide variety of colors and decorative designs on the sign face.
The process of the invention comprises the steps of
(a) providing a carrier bearing a thermally-transferable ink composition;
(b) applying said ink to a receptor surface;
(c) adjusting said receptor surface so that it is free from wrinkles;
(d) evacuating substantially all of the air from the interface between said ink and said receptor surface;
(e) heating said ink and said receptor surface to a temperature, and for a time, sufficient to soften said ink and intimately bond it to said receptor, said heating occurring after substantially all of said air has been evacuated from said interface.
The novel composition provided herein is particularly preferred for use with the above-described process. It comprises a thermally-transferable ink composition having a 20% elongation temperature of less than 85° C. and an elongation at break of at least about 15%. The ink is made up of
(a) from about 50 to 95% by weight of a thermoplastic polymer selected from the group consisting of polyvinyl chloride and copolymers thereof;
(b) from about 50 to 5% by weight of a flexibilizer for said thermoplastic polymer that is compatible with said thermoplastic polymer; and
(c) up to about 40% by weight of a colorant.
Sign faces made by utilizing the novel process and composition described herein offer several advantages. For example, the ink compositions conform virtually exactly to the surface of the receptor. Thus, the ink can be applied to textured substrates and be totally adhered thereto.
Still further the inks of the invention can be utilized to fill-in openings left for indicium in a previously applied layer. The ink conforms exactly to the surface and completely fills in the opening and becomes totally adhered to the receptor. This is particularly useful in providing indicia of one color on a differently colored background.
The conformability of the inks of the invention is of particular significance in the preparation of large are flexible sign faces. These sign faces typically require that two or more sheets of the receptor be joined or seamed together. Each juncture or seam is thicker than an individual sheet of the receptor so that a mound or ridge is formed. The inks of the invention conform and adhere to both the seam and the balance of the receptor tenaciously.
This excellent adhesion and conformability is surprising, particularly with respect to the most preferred aspects of the invention, since low transfer temperatures are employed during the process. Furthermore, ink transferred in accordance with the present invention exhibit excellent flexural characteristics. Thus, when a completed pliant sign face is flexed, the ink does not crack or peel off. Moreover, when completed rigid sign faces expand and contract due to temperature changes, the ink does not crack or peel off.
Still further, the ink compositions of the invention exhibit excellent weatherability. For example, they do not show any significant fading or darkening when exposed to outdoor conditions. Moreover, they do not chip, peel, crack, etc. under these conditions.
The adhesion of the transferred ink to the receptor is demonstrated by the tape adhesion test described in ASTM D 3359-74, method B with the modification that the receptor is 0.5 mm thick.
In the tape adhesion test, a lattice cut is made so as to provide intersecting cut lines through the ink layer and into the receptor. Pressure sensitive tape is applied over the lattice and then stripped away. The ink compositions of the invention exhibit a classification number of at least 4, and preferably 5. A classification number of 4 means that virtually none of the transferred ink is removed while a classification number of 5 means that none of the transferred ink is removed.
DETAILED DESCRIPTION OF THE INVENTION
In the process of the present invention, a thermally-transferable ink is transferred from a carrier to a receptor at a temperature sufficient to soften the ink and intimately bond it to the receptor. While any temperature sufficient to achieve this result may be utilized, the temperature is preferably in the range of 75° C.-110° C., and most preferably in the range of 85° C.-95° C.
The essential steps of the process of the invention are set forth above. Thus, a carrier bearing a dry layer of thermally-transferable ink (hereinafter referred to as the "transfer sheet") is placed on a desired receptor so that the ink contacts the receptor surface. Carriers and techniques for applying the ink thereto will be described hereinafter.
While it is not necessary to the process, it is frequently desirable to provide an image of the desired art work on the receptor prior to placing the transfer sheet on the receptor. A variety of techniques may be employed to do this. In one useful technique a reduced-size black and white photocopy of the sign face to be prepared is made. The photocopy is then utilized to make a projection transparency, which is then projected onto the desired receptor surface. The size of projected image can be readily adjusted so as to obtain the desired size of sign by techniques known to the art.
The transfer sheet may be fastened to the receptor by a variety of techniques. However, simply taping the transfer sheet is sufficient. If, it is desired to provide a differently colored background, that is a color that is different than the color of the receptor, a transfer sheet of one color may be fastened to the portion of the receptor surface desired to be differently colored followed by removing (e.g., by cutting out) the image areas from the transfer sheet. A second transfer sheet, having the color desired for the art work may then be fastened over the cut-out areas of the first transfer sheet.
Once the appropriately colored transfer sheets have been fastened to the receptor, the resulting intermediate structure is placed in a device, such as a vacuum frame, and adjusted so as to provide a wrinkle free surface. If necessary, this may be accomplished by placing the intermediate structure under tension.
A particuarly advantageous technique for providing a wrinkle-free surface is to turn on the vacuum pump of the vacuum frame with the intermediate on the vacuum bed thereof and with the top thereof up. If the intermediate does not cover the entire vacuum bed, sheets of substantially non-porous material may be placed over the uncovered portions. Wrinkles in the intermediate may then be squeezed out or otherwise removed. The non-porous sheets may then be removed (leaving the wrinkle-free intermediate) and the top lowered.
Typically the intermediate is placed in the vacuum frame so that the receptor contacts the vacuum bed and the transfer sheeting contacts the top when the top is closed. The exact vacuum frame utilized in the process of the invention is not critical to the invention as a variety of commercially available vacuum frames are useful.
Preferably the vacuum bed of the frame has a smooth surface free from ridges, lumps, etc., especially where the perforated vacuum bed meets the outer supports of the vacuum frame. Additionally, the vacuum bed is preferably covered with a porous material such as muslin.
The top of the vacuum frame contains an air bladder and, above the bladder, a lamp bank. The top is preferably hinged on one end and has locks on the other end. The hinges and locks are located so that a wide sheet of receptor can pass therebetween. A porous fabric, such as muslin, is preferably fastened to the surface of the bladder that contacts the transfer sheet. The lamp bank preferably comprises a plurality of lamps that, preferably, emit radiation in the infra red range. A temperature controller is also preferably included so as to regulate the heat input into the vacuum frame.
Once the wrinkles have been removed from the intermediate, the vacuum frame is closed and a vacuum created therein to evacuate substantially all of the air from the interface between the ink and the receptor and provide intimate contact between the receptor and the ink. It has been found that this may be accomplished by reducing the pressure in the frame to between about 0.1 to 0.25 atmosphere for from 2 to 5 minutes. Preferably the pressure is reduced to at least about 0.2 atmosphere.
The receptor surface and the ink are then heated to the predetermined transfer temperature. Heating may be accomplished by a variety of techniques, although it has been found that a bank of 300 watt incandescent light bulbs that emit radiation in the infrared range is satisfactory. The intermediate, particularly receptor surface and ink, is heated to a temperature sufficient to soften the ink and intimately bond it to the receptor. The exact temperature is dependent upon the nature of the ink and the receptor employed. The temperature must, however, be below that at which the ink and receptor degrade.
During heating, the ink and receptor surface fuse together and form an intimate bond. Preferably heating is carried on only for a time sufficient to accomplish this result. It has been found that, with the compositions of the invention, heating need only be at a temperature between about 75° to 110° C. for from 2 to 10 minutes.
Evacuating substantially all of the air from the interface between the receptor surface and the ink causes a pressure differential between the interface and the exterior of the intermediate structure. The lack of air at the interface in combination with the pressure differential makes it possible to achieve the tenacious and intimate bonding of the ink to the receptor at low temperatures. Preferably the pressure differential is at least about 0.75 atmosphere.
The vacuum is then released and the receptor and ink are cooled. This may be done by passive means or by active means, for example by blowing air over the intermediate. Once the intermediate has cooled to a temperature (e.g., a temperature of 65° C. or less ) sufficient to harden the ink and cause the adhesion of the ink to the receptor to be greater than the adhesion of the ink to the carrier, the carrier is stripped from the receptor. The resultant receptor then bears indicia that are firmly anchored thereto and that conform exactly to the surface thereof.
In the event that the receptor is too large to fit entirely within the vacuum frame at one time, the above described process may be repeated in a step-wise manner until the entire sign face has been completed. During a step-wise process it is preferred that indicia (e.g., letters, numbers, etc.) to be transferred be located entirely within the frame during heating.
A wide variety of receptors may be utilized in the process of the invention. They may be polymeric or non-polymeric, flexible or rigid, and thick or thin. Moreover, the surface of the receptor may be smooth or irregular.
Receptors useful wth the present invention include a variety of polymeric films including polyvinylchloride (e.g., Panaflex® film from National Advertising Company and Scotchal® film from 3M Company), acrylic films (e.g., Plexiglas® from Rohm and Haas), cellulose acetate butyrate film, and urethane films. Other resin films may also be employed a receptor materials. The receptor materials may be used as such or they may have their surface modified by, for example, priming, corona treatment, solvent wiping, etc.
The novel compositions described herein comprise a defined thermoplastic resin, a flexibilizer for said resin, and, optionally, a colorant, an ultraviolet light absorber, a heat stabilizer, a surfactant, a flow aid, etc. They have a 20% elongation temperature of no more than about 85° C. and preferably one in the range of 70° C. to 85° C. Additionally, they have an elongation at break of at least 15%.
The 20% elongation temperature is determined in the same manner as the ring and ball softening point described in ASTM E-2842-T except that the film thickness is 25 microns, the ball weight is 1.5 g, the ring width is 14 cm, and heating is done in air and commences at 60° C. and is raised at a uniform rate of 1.7° C. per minute. The 20% elongation temperature is that temperature at which a film of the resin has elongated 120% of its original dimension.
Elongation at break is measured according to ASTM D412-75, Method A, section 12.2. Test samples are 1.25 cm wide with a spacing of 1.25 cm. Pulling speed is 10 cm per minute. The measurement of elongation at break is set forth at section 5.2 of the test method.
The ink compositions may be readily prepared by, for example, dissolving the thermoplastic resin and flexibilizer together in a suitable screen-printing solvent, such as isophorone or cyclohexanone, followed by addition of the colorant and other ingredients. The colorant may be added directly if a dye is used. If a pigment is used, it is first preferably dispersed in a solvent, resin, or plasticizer that is compatible with the solvent used to dissolve the thermoplastic resin. Known processing techniques may be employed in preparing the compositions.
The thermoplastic resins useful in the novel compositions comprise from about 50% to 95% by dry weight of the composition, and preferably from about 65% to 95% by dry weight. They are selected from polyvinyl chloride and copolymers thereof. Specific examples include, for example, polyvinyl chloride, polyvinyl chloride-polyvinyl acetate copolymers (e.g., Bakelite® VYHH available from Union Carbide Company).
The flexibilizer employed in the novel compositions comprises from about 50 to 5% by dry weight of the composition, and preferably from about 20 to 5%. It flexibilizes the composition and is compatible with the vinyl polymer or copolymer. Moreover, it imparts conformability and elasticity to the ink composition, and improves its film strength by improving the elongation characteristics of films of the ink.
Representative classes of useful flexibilizers are selected from the group consisting of synthetic resins that are free from vinyl chloride units and that have a 20% elongation temperature of less than about 85° C., and plasticizers for polyvinyl chloride.
Specific examples of useful vinyl chloride-free resins include ethyl, methyl, and butyl methacrylate homopolymers, and copolymers of said homopolymers with methyl, ethyl, and butyl acrylate. Such resins are available from Rohm and Haas as the Acryloid® series and from DuPont as the Lucite® series.
Other useful vinyl-chloride-free resins are urethane polymers such as polyester-functional aromatic urethanes (e.g., the Estane® series from B. F. Goodrich), and polyester and polyether-functional aliphatic urethanes (e.g., respectively QI-12 and PE-192 from Quin).
Other useful thermoplastic resins include linear polyester resins (e.g., Vitel® PE-222 from Goodyear), acrylonitrile-butadiene-styrene resins (e.g., Cycolac® WA 2021 from Borg-Warner), polycaprolactam polymers (e.g., PCL-700 Union Carbide, sucrose acetate isobutyrate, available as SAIB from Eastman Chemical, ethylene vinyl acetate resin, ethyl methacrylate, and butyl methacrylate resin. Combinations of vinyl chloride-free thermoplastic resins may be utilized if desired.
Specific examples of classes of plasticizers useful in the compositions of the invention are alcohol phthalates (e.g., Santicizer® 711, a mixture of alcohol phthalates containing from 7 to 11 carbons in the phthalate chain from Monsanto); polymeric polyesters (e.g., Santicizer® 429, available from Monsanto); aromatic phthalates (e.g., Santicizer® 160, butyl benzyl phthalate from Monsanto) and mixed lower alkyl benzyl phthalates (Santicizer® 261 from Monsanto); epoxidized vegetable oils (e.g., epoxidized linseed oil, epoxidized soybean oil, epoxidized safflower oil); and phosphoric acid derivatives (e.g., Santicizer® 141, 2-ethylhexyl-diphenyl phosphate from Monsanto), and tricresyl phosphate from Monsanto.
Blends of flexibilizers e.g., combinations of one or more resins with one or more plasticizers, may be employed if desired.
Colorants useful in the compositions of the invention comprise up to about 40% by dry weight of the composition. Preferably they comprise from about 1% to 30%. Quantities of from about 1% to 15% are useful in providing light and pastel shades while quantities of from about 15% to 30% are useful in providing dark colors. The colorants may be selected from dyes or pigments, although pigments are preferred.
______________________________________Molybdate Orange Primrose YellowQuinacridone Red Phthalocyanine BlueCarbon Black Phthalocyanine GreenRutile Titanium Dioxide Carbazole VioletChrome Yellow Irgasine YellowLead Chromate Yellow Quinacridone Pink______________________________________
The pigments may be provided in dry bulk form, or as a dispersion in a solvent, liquid or solid resin, plasticizer, or combinations thereof.
A variety of other ingredients may be utilized in the compositions of the invention. Thus, for example, ultraviolet light absorbers, heat stabilizers, surfactants to aid application of the composition to a carrier, and solvents may be employed. Examples of materials useful for these purposes are known as will be understood as a result of this disclosure.
As discussed above, the compositions useful in the present invention are prepared by dissolving the ingredients together in an appropriate solvent. The solution is then filtered and coated onto a suitable carrier. Coating is preferably carried out by screen printing. Other coating techniques, such as reverse roll, knife, and rotogravure, may be utilized if desired. The solvent is removed from the coated layer by, for example, impinging the coating with air at about 80° C.
The thickness of the dry layer of thermally-transferable ink is not critical to the invention. However, it has been found that good results, in terms of transferred indicia quality, may be obtained if the layer has a thickness in the range of 5 to 50 microns. Preferably the thickness is in the range of 8 to 25 microns. Most preferably the thickness is about 25 microns.
The carrier utilized in the transfer sheet may be any material that is dimensionally stable and exhibits high release characteristics. Thus, the carrier must release from the thermally-transferable ink once it has been adhered to a receptor. The carrier usually is coated or impregnated with a suitable release material so as to facilitate this release. The carrier preferably is flexible and exhibits good hand, that is, it may be cut easily by die cutting or hand cutting techniques.
Sheeting materials that have suitable release characteristics are known. They include Warren O-Duplex, available from S. D. Warren Paper Co.; Trans-Eze® 2000 and 3000, and Kimdura, all available from Kimberly-Clark; polyethylene sheeting, and polypropylene sheeting. Silicone or other treated paper may also be employed.
The thermally-transferable ink may occur on the carrier in a variety of ways, including, for example, as a continuous layer of the ink or as one or more discrete indicium. The former type of transfer sheet may be used to provide large background areas or individually prepared indicium on sign faces. The latter type of transfer sheet may be used in applying pre-prepared indicium to a receptor.
In the process of transferring thermally-transferable ink, especially to form sign faces, described herein it is preferable, though not necessary, to apply a clear (i.e., colorless and transparent) layer over the indicium-bearing surface. The clear layer is most preferably thin (i.e., approximately 25 microns) and clear layer acts as a barrier to the loss of flexibilizer (especially plasticizer). Additionally, it reduces the ability of nutrients to come to the surface thereby reducing the growth of fungus. Still further, it serves as a moisture barrier. Furthermore, it can contain other additives such as ultraviolet light absorbers, antioxidants, fungistats, and so forth.
The clear coat may be applied by the same techniques used to transfer the ink from the carrier to the receptor. Like the ink, the clear coat is preferably provided on a material that exhibits high release characteristics. Common processing techniques can be utilized to apply the clear coat to a release material.
A useful clear coat comprises at least 95% by weight of acrylic polymers such as polymethyl methacrylate, and copolymers of methyl methacrylate with ethyl and butyl methacrylate. The remaining 5% by weight is made up of other additives such as those mentioned above. Examples of these materials include the 3900 and 4000 series of Scotchcal® resins available from 3M Company.
Known thermoplastic compositions may also be employed to provide the thermally-transferable ink in the process of the present invention. However, these materials must be combined with a flexibilizer if they are to have a combination of a 20% elongation temperature less than about 85° C. and an elongation at break of at least 15%. Examples of such commercially available formulations include the 600 Series inks from General Formulations (a division of General Research Incorporated), the G.V. series inks from Naz Dar, the 9600 series inks from Colonial Inks, the "Lov" series from Advance Screen Printing Co., and the 8000 series vinyls from Tibbetts & Westerfield.
The present invention is further described in the following examples wherein all percentages are by weight unless otherwise indicated.
EXAMPLE 1
Thermally transferable ink formulations were prepared from the following ingredients using the quantities indicated.
______________________________________ %______________________________________Polyvinyl Chloride-Polyvinyl Acetate Copolymer 18(Bakelite ® VYHH from Union Carbide,86% vinyl chloride and 14% vinyl acetate)Polymethyl Methacrylate-Ethyl Methacrylate 4Copolymer (Acryloid ® B82 from Rohm and Haas)Aliphatic Urethane (QI 12 from K. J. Quin)* 4Butyl Benzyl Phthalate (Santicizer ® 160 7from Monsanto)Mixed Alkyl Benzyl Phthalate (Santicizer ® 261 7from Monsanto)Quinacridone Red 102,2-dihydroxy-4,4-dimethoxy benzophenone 0.1Ba & Cd Stearate 0.25Epoxidized Linseed Oil 0.5Isophorone 25.1Butyl Cellosolve 7.75Mixed aromatic solvents (SC solvent 150 from 5.1Central Solvents and Chemicals)Diacetone Alcohol 7.1Cyclohexanone 4.1______________________________________ *Provided in solution, solvent evaporated and dry urethane added.
The ink solution was prepared by mixing all ingredients together unitl they had dissolved and the pigment had dispersed. The pigment was provided in a dispersion in cyclohexanone before addition.
The solution was then applied to the release surface of a carrier of Trans-Eze® 2000 and dried at 60° C. to remove the solvent. The thickness of the dried layer was 25 microns. The ink composition had a 20% elongation temperature of 82° C. and an elongation at break of 110%.
The resulting dry transfer sheet was applied to the surface of a polyvinyl chloride sheet that was reinforced with thermoplastic fibers so that the thermally-transferable ink contacted the polyvinyl chloride sheet. The surface of the polyvinyl chloride sheet was three-dimensional. The resulting intermediate structure was placed in a vacuum frame and adjusted to remove all wrinkles. The frame was then closed and the pressure therein reduced to 0.2 atmosphere after which the temperature therein was raised to 88° C. This pressure and temperature were maintained for 2 minutes. The pressure was then increased to atmospheric pressure and the temperature in the vacuum frame was lowered to 50° C. The carrier was then stripped from the receptor. The ink transferred completely from the carrier to the receptor. The carrier left no residue on the indicia. When the tape adhesion test was performed on the transferred ink, a classification number of 5 was obtained (i.e., no ink was removed from the receptor).
EXAMPLES 2-5
Thermally-transferable ink formulations were prepared and coated onto Trans-Eze® 2000 carrier as described in Example 1 from the following formulations. All quantities are in %.
______________________________________ 2 3 4 5______________________________________Bakelite ® VYHH 18 18 25 25Acryloid ® B82 4 4 -- --Sucrose Acetate Isobutyrate 4 4 -- --Santicizer ® 711 (mixture of 7 7 -- 6.25alcohol phthalates fromMonsanto)Santicizer ® 261 (Aromatic 7 7 -- --Phthalate Plasticizer fromMonsanto)Phthalocyanine Blue 8 -- -- --Rutile Titanium Dioxide 0.5 -- -- --Carbazole Violet 1.5 -- -- --Quinacridone Red -- 8 -- --Molybdate Orange -- 2 -- --2,2-dihydroxy-4,4-dimethoxy- 0.4 0.4 -- --benzophenoneBa & Cd Stearate 0.5 0.5 -- --Epoxidized Soy Bean Oil 1 1 -- --Dimethoxy Silicone (SF-96 0.1 0.1 -- --from General Electric)Isophorone 30 30 -- --Butyl Cellosolve 8 8 -- --Mixed aromatic solvents (SC 10 10 -- --solvent from CentralSolvents and Chemicals)Cyclohexanone -- -- 75 68.75______________________________________
The ink compositions had respective 20% elongation temperatures of 71° C., 71° C., 85° C., and 84° C. and elongations at break of 130%, 130%, 0%, and 95%.
The ink compositions of the resulting transfer sheets were transferred to a Panaflex® receptor as described in Example 1 at various temperatures. The pressure was 0.2 atmosphere. It was found that a temperature of only 82° C. was sufficient to transfer the ink composition of Example 2. A classification number of 5 was obtained in the tape adhesion test. The ink compositions of Examples 3-5 demonstrated the same classification number when transferred at a temperature of about 88° C.
When the composition of Example 4 was transferred as described above to a seam, it was found that the tape adhesion classification number was less than 4 for that portion of the ink on the seam. This demonstrates that while many ink compositions may be transferred according to the process of the invention, those of the invention provide superior results.
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A process and composition are provided that provide for thermal transfer of ink compositions and eliminate the need to prepare articles such as sign faces, particularly flexible sign faces, by painting with ink compositions that contain solvents. The present process and composition permit thermal transfer from a carrier to a receptor at low temperatures with the use of vacuum pressure. The transferred ink adheres tenaciously to the receptor and is flexible.
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BACKGROUND
[0001] The present invention relates generally to the field of computers, and more particularly to filesystem checker failure.
[0002] Most filesystems have a filesystem checker, such as a “file system consistency check” fsck) which is used to ensure that the metadata of the filesystem is consistent. Such a filesystem checker is typically used after a system crash to ensure the filesystem is consistent before being mounted. The filesystem checker may also be used whenever a filesystem has been corrupted to attempt to fix any metadata inconsistencies and recover any lost files caused by corruption.
SUMMARY
[0003] According to one embodiment, a method for repairing a corrupted filesystem, whereby the corrupted filesystem includes a plurality of corrupted metadata structures is provided. The method may include determining a plurality of missing metadata structures associated with the corrupted filesystem, whereby the missing metadata structures have been overwritten by a corruption. The method may also include determining a plurality of current addresses corresponding to a plurality of valid metadata structures in a hierarchical metadata structure of the corrupted filesystem based on the determined plurality of missing metadata structures, whereby at least one metadata structure within the plurality of metadata structures serves as a node pointing to a plurality of other metadata structures. The method may further include locating the plurality of missing metadata structures and a plurality of addresses associated with the missing metadata structures based on the determined plurality of current addresses corresponding to a plurality of valid metadata structures. The method may also include rebuilding the plurality of missing metadata structures based on the located plurality of addresses associated with the missing metadata structures, whereby the rebuilding comprises assigning the located plurality of address to the plurality of missing metadata structures and redirecting the plurality of missing metadata structures to point to a correct plurality of other metadata structures.
[0004] According to another embodiment, a computer system for repairing a corrupted filesystem, whereby the corrupted filesystem includes a plurality of corrupted metadata structures is provided. The computer system may include one or more processors, one or more computer-readable memories, one or more computer-readable tangible storage devices, and program instructions stored on at least one of the one or more storage devices for execution by at least one of the one or more processors via at least one of the one or more memories, whereby the computer system is capable of performing a method. The method may include determining a plurality of missing metadata structures associated with the corrupted filesystem, whereby the missing metadata structures have been overwritten by a corruption. The method may also include determining a plurality of current addresses corresponding to a plurality of valid metadata structures in a hierarchical metadata structure of the corrupted filesystem based on the determined plurality of missing metadata structures, whereby at least one metadata structure within the plurality of metadata structures serves as a node pointing to a plurality of other metadata structures. The method may further include locating the plurality of missing metadata structures and a plurality of addresses associated with the missing metadata structures based on the determined plurality of current addresses corresponding to a plurality of valid metadata structures. The method may also include rebuilding the plurality of missing metadata structures based on the located plurality of addresses associated with the missing metadata structures, whereby the rebuilding comprises assigning the located plurality of address to the plurality of missing metadata structures and redirecting the plurality of missing metadata structures to point to a correct plurality of other metadata structures.
[0005] According to yet another embodiment, a computer program product for repairing a corrupted filesystem, whereby the corrupted filesystem includes a plurality of corrupted metadata structures is provided. The computer program product may include one or more computer-readable storage devices and program instructions stored on at least one of the one or me tangible storage devices, the program instructions executable by a processor. The computer program product may include program instructions to determine a plurality of missing metadata structures associated with the corrupted filesystem, whereby the missing metadata structures have been overwritten by a corruption. The computer program product may also include program instructions to determine a plurality of current addresses corresponding to a plurality of valid metadata structures in a hierarchical metadata structure of the corrupted filesystem based on the determined plurality of missing metadata structures, whereby at least one metadata structure within the plurality of metadata structures serves as a node pointing to a plurality of other metadata structures. The computer program product may further include program instructions to locate the plurality of missing metadata structures and a plurality of addresses associated with the missing metadata structures based on the determined plurality of current addresses corresponding to a plurality of valid metadata structures. The computer program product may also include program instructions to rebuild the plurality of missing metadata structures based on the located plurality of addresses associated with the missing metadata structures, whereby the rebuilding comprises assigning the located plurality of address to the plurality of missing metadata structures and redirecting the plurality of missing metadata structures to point to a correct plurality of other metadata structures.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0006] These and other objects, features and advantages of the present invention will become apparent from the following detailed description of illustrative embodiments thereof, which is to be read in connection with the accompanying drawings. The various features of the drawings are not to scale as the illustrations are for clarity in facilitating one skilled in the art in understanding the invention in conjunction with the detailed description. In the drawings:
[0007] FIG. 1 illustrates a networked computer environment according to one embodiment;
[0008] FIG. 2 is an exemplary illustration of tools included in the set of fs_Tools associated with the Analyzing and Correcting Filesystem Checker Failure Program according to at least one embodiment;
[0009] FIG. 3 , is an operational flowchart illustrating the steps carried out by a program for analyzing and correcting corruption which has led to Filesystem Checker Failure according to at least one embodiment;
[0010] FIG. 4 , is an exemplary illustration of metadata setup on disk with addresses according to at least one embodiment;
[0011] FIG. 5 is an exemplary illustration of how structures point to each other according to at least one embodiment;
[0012] FIG. 6A-6D are exemplary illustrations of applying the method steps described in FIG. 3 according to at least one embodiment;
[0013] FIG. 7 is a block diagram of internal and external components of computers and servers depicted in FIG. 1 according to at least one embodiment;
[0014] FIG. 8 is a block diagram of an illustrative cloud computing environment including the computer system depicted in FIG. 1 , in accordance with an embodiment of the present disclosure; and
[0015] FIG. 9 is a block diagram of functional layers of the illustrative cloud computing environment of FIG. 8 , in accordance with an embodiment of the present disclosure.
DETAILED DESCRIPTION
[0016] Detailed embodiments of the claimed structures and methods are disclosed herein; however, it can be understood that the disclosed embodiments are merely illustrative of the claimed structures and methods that may be embodied in various forms. This invention may, however, be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein. Rather, these exemplary embodiments are provided so that this disclosure will be thorough and complete and will fully convey the scope of this invention to those skilled in the art. In the description, details of well-known features and techniques may be omitted to avoid unnecessarily obscuring the presented embodiments.
[0017] Embodiments of the present invention relate generally to the field of computers, and more particularly to filesystem checker failure. The following described exemplary embodiments provide a system, method and program product to, among other things, analyze and correct a corruption which has caused a filesystem checker failure so that the filesystem checker will run without error. Therefore, the present embodiment has the capacity to improve the technical field of filesystem checker failure by analyzing and correcting a corruption which has led to filesystem checker failure. More specifically, fsck failures may be analyzed to determine why fsck is failing and to fix fsck if possible by analyzing the state of the metadata on the filesystem and determining if any changes to the metadata can be made so that the fsck tool can run successfully.
[0018] Furthermore, the present embodiment may be used for other executables in addition to fsck. As such, any executable which depends on obtaining addresses to on disk structures to cause the data on the structure to be accessed could have the same technique described herein if it is not able to be executed because of corruption. For example:
[0000] 1) One example is fsdb. Fsdb is a “filesystem debugger”. It may not work until certain address are remade. However, once fsdb is able to work again, it can be used to complete changing other addresses more easily to get fsck to work faster.
2) Another example could be storage pools. Storage pools of disks are used by pool managers to create virtual disks to be exported to clients in a virtual environment. These pools depend on a “pool_start” program to make the disk pools accessible to pool managers. Disk corruption could cause “pool_start” to not be able to work. Creating a pool_discover program to discover needed pool structure addresses to be replaced in corrupted pool structures by “pool update” executables could be done in a similar manner as described herein with respect to the present embodiment.
[0019] Therefore, as illustrated in the previous examples, fsck is not the only executable that can benefit from the technique described with respect to the present embodiment.
[0020] As previously described, most filesystems have a filesystem, such as fsck checker to ensure that the metadata of the filesystem is consistent. The filesystem checker is typically used after a system crash to ensure the filesystem is consistent before being mounted. The filesystem checker may also be used whenever a filesystem has been corrupted to attempt to fix any metadata inconsistencies and recover any lost files caused by corruption. However, if fsck is not able to complete, then the operating system will not allow the filesystem to be mounted and used. As such, the customer is required to restore the filesystem data from backup which may be in a consistent state so it can be used and mounted. However, restoring from backup is often a very expensive and time consuming process that should be avoided if possible. As such, it may be advantageous, among other things to provide tools and a method for dealing with fsck failures to analyze why fsck is failing and to fix fsck if possible. As such, the tools may be able to analyze the state of the metadata on the filesystem and determine if any changes to the metadata can be made so that the fsck tool can run successfully. Additionally, the process may be defined that will either explain to customer why fsck cannot be made to work because corruption is to severe or to make changes to metadata and allow fsck to work to completion so that the filesystem can be mounted and re-used.
[0021] According to at least one implementation, the present embodiment may provide tools and a process utilizing the tools to eliminate the problem of fsck failure due to corruption. As such, the combination of the tools working together with the provided technique may provide an explanation that may be given to the customer which explains the reason for the problem. Additionally, the technique may demonstrate how to overcome corruption problems by using, for example, tool such as a J2_discover tool to discover addresses which need to be used to correct corrupted metadata structures. Therefore, if the J2_discover tool is able to determine the addresses of the missing data, then other tools are available to update the corrupted structures with proper addresses. According to the present embodiment, such an implementation may be performed independent of fsck since it is not usable due to the fact that fsck is unable to find the missing addresses that fsck needs to access metadata.
[0022] The present invention may be a system, a method, and/or a computer program product. The computer program product may include a computer readable storage medium (or media) having computer readable program instructions thereon for causing a processor to carry out aspects of the present invention.
[0023] The computer readable storage medium can be a tangible device that can retain and store instructions for use by an instruction execution device. The computer readable storage medium may be, for example, but is not limited to, an electronic storage device, a magnetic storage device, an optical storage device, an electromagnetic storage device, a semiconductor storage device, or any suitable combination of the foregoing. A non-exhaustive list of more specific examples of the computer readable storage medium includes the following: a portable computer diskette, a hard disk, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or Flash memory), a static random access memory (SRAM), a portable compact disc read-only memory (CD-ROM), a digital versatile disk (DVD), a memory stick, a floppy disk, a mechanically encoded device such as punch-cards or raised structures in a groove having instructions recorded thereon, and any suitable combination of the foregoing. A computer readable storage medium, as used herein, is not to be construed as being transitory signals per se, such as radio waves or other freely propagating electromagnetic waves, electromagnetic waves propagating through a waveguide or other transmission media (e.g., light pulses passing through a fiber-optic cable), or electrical signals transmitted through a wire.
[0024] Computer readable program instructions described herein can be downloaded to respective computing/processing devices from a computer readable storage medium or to an external computer or external storage device via a network, for example, the Internet, a local area network, a wide area network and/or a wireless network. The network may comprise copper transmission cables, optical transmission fibers, wireless transmission, routers, firewalls, switches, gateway computers and/or edge servers. A network adapter card or network interface in each computing/processing device receives computer readable program instructions from the network and forwards the computer readable program instructions for storage in a computer readable storage medium within the respective computing/processing device.
[0025] Computer readable program instructions for carrying out operations of the present invention may be assembler instructions, instruction-set-architecture (ISA) instructions, machine instructions, machine dependent instructions, microcode, firmware instructions, state-setting data, or either source code or object code written in any combination of one or more programming languages, including an object oriented programming language such as Smalltalk, C++ or the like, and conventional procedural programming languages, such as the “C” programming language or similar programming languages. The computer readable program instructions may execute entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the latter scenario, the remote computer may be connected to the user's computer through any type of network, including a local area network (LAN) or a wide area network (WAN), or the connection may be made to an external computer (for example, through the Internet using an Internet Service Provider). In some embodiments, electronic circuitry including, for example, programmable logic circuitry, field-programmable gate arrays (FPGA), or programmable logic arrays (PLA) may execute the computer readable program instructions by utilizing state information of the computer readable program instructions to personalize the electronic circuitry, in order to perform aspects of the present invention.
[0026] Aspects of the present invention are described herein with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the invention. It will be understood that each block of the flowchart illustrations and/or block diagrams, and combinations of blocks in the flowchart illustrations and/or block diagrams, can be implemented by computer readable program instructions.
[0027] These computer readable program instructions may be provided to a processor of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions/acts specified in the flowchart and/or block diagram block or blocks. These computer readable program instructions may also be stored in a computer readable storage medium that can direct a computer, a programmable data processing apparatus, and/or other devices to function in a particular manner, such that the computer readable storage medium having instructions stored therein comprises an article of manufacture including instructions which implement aspects of the function/act specified in the flowchart and/or block diagram block or blocks.
[0028] The computer readable program instructions may also be loaded onto a computer, other programmable data processing apparatus, or other device to cause a series of operational steps to be performed on the computer, other programmable apparatus or other device to produce a computer implemented process, such that the instructions which execute on the computer, other programmable apparatus, or other device implement the functions/acts specified in the flowchart and/or block diagram block or blocks.
[0029] The flowchart and block diagrams in the Figures illustrate the architecture, functionality, and operation of possible implementations of systems, methods, and computer program products according to various embodiments of the present invention. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of instructions, which comprises one or more executable instructions for implementing the specified logical function(s). In some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems that perform the specified functions or acts or carry out combinations of special purpose hardware and computer instructions.
[0030] The following described exemplary embodiments provide a system, method and program product to analyze and correct a corruption which has caused a filesystem checker failure so that the filesystem checker will run without error.
[0031] According to at least one implementation, the present embodiment may create three tools to resolve the problem of fsck failure due to corruption, such as the Tool fs_discover; the tool fs_formatter; and update tools (e.g., update_superblock). For example, the tool j2_discover may re-discover metadata objects and outputs their addresses. Additionally, the present embodiment may combine tools to further analyze fsck failure problem and ensure everything possible has been done to overcome fsck failures. The idea of rediscovering addresses of key metadata structures and re-building metadata objects to overcome fsck failure may assist when dealing with fsck failures in the future. As such, after the proper updates have been made from the update_tools, the fsck can be run. The filesystem can then be mounted and further analyzed to see if it can be used without having to do a total restore from backup.
[0032] Furthermore, an advantage of the present embodiment may be that the customer has been given complete analysis of the filesystem state and knows that everything has been done to possibly recover. As such, customer satisfaction may be improved. Also, the present embodiment may provide a method in some cases to actually fix the problem with fsck failing and therefore, allow fsck to complete so work on the filesystem can continue.
[0033] The present embodiment may create algorithms for each metadata type which take advantage of internal relationships in metadata structures so that each algorithm can announce if it has discovered a metadata page of the type mentioned. As such, a case statement is used to process each page of the volume and announce its metadata type and offset or announce it is a non-metadata page. The executable can run with threads to improve performance. The following is an example of what a typical output may look like:
[0000]
LV
PAGE
METADATA
ADDITIONAL
OFFSET
COUNT
TYPE
DATA
0x0
0x8
NONMETA
0x8
0x1
SUPER
0x9
0x1
IMAP_CTL
0xa
0x1
IAG
0
0xb
0x1
AIT1
0xc
0x3
NONMETA
0xf
0x1
SUPER
0x10
0x1
BLK_H
0x11
0x2
NONMETA
0x13
0x1
BLK_CTL
. . .
. . .
[0034] The above LV OFFSET data provide addresses (sometime called pointers) which is the information fsck needs to work. These pointers are normally kept in key metadata-structures. If these structures have been overwritten (not discovered by fs_discover), then they need to be re-made through using the fs_discover, formatter, and update_<meta-data> tools.
[0035] According to at least one implementation of the present embodiment, four steps may be implemented as follows: determine from fs_discover output if there are any metadata structures missing (e.g., over written by corruption); determine what type of structures the corrupted structure points to; using fs_discover output, determine if these structures and their addresses can be located; and if missing addresses can be determined, then remake the corrupted structure with addresses that it should be using so that it once again points to structures allowing fsck to run.
[0036] Referring to FIG. 1 , an exemplary networked computer environment 100 in accordance with one embodiment is depicted. The networked computer environment 100 may include a computer 102 with a processor 104 and a data storage device 106 that is enabled to run a software program 108 and an Analyzing and Correcting Filesystem Checker Failure Program 116 A. The networked computer environment 100 may also include a server 114 that is enabled to run an Analyzing and Correcting Filesystem Checker Failure Program 116 B that interacts with a set of fs_Tools 112 and a communication network 110 . The set of fs_Tools 112 may be used to determine addresses of the missing data (fs_discover), view discovered data (fs_formatter), and update corrupted structures with the proper addresses (Update Tools).
[0037] The networked computer environment 100 may include a plurality of computers 102 and servers 114 , only one of which is shown. The communication network may include various types of communication networks, such as a wide area network (WAN), local area network (LAN), a telecommunication network, a wireless network, a public switched network and/or a satellite network. It should be appreciated that FIG. 1 provides only an illustration of one implementation and does not imply any limitations with regard to the environments in which different embodiments may be implemented. Many modifications to the depicted environments may be made based on design and implementation requirements.
[0038] The client computer 102 may communicate with the Analyzing and Correcting Filesystem Checker Failure Program 116 B running on server computer 114 via the communications network 110 . The communications network 110 may include connections, such as wire, wireless communication links, or fiber optic cables. As will be discussed with reference to FIG. 7 , server computer 114 may include internal components 800 a and external components 900 a , respectively, and client computer 102 may include internal components 800 b and external components 900 b , respectively. Client computer 102 may be, for example, a mobile device, a telephone, a personal digital assistant, a netbook, a laptop computer, a tablet computer, a desktop computer, or any type of computing devices capable of running a program, accessing a network, and accessing a set of fs_Tools 112 .
[0039] As previously described, the client computer 102 , may access the set of fs_Tools 112 or the Analyzing and Correcting Filesystem Checker Failure Program 116 B, running on server computer 114 via the communications network 110 . For example, a user using a client computer 102 may be given a complete analysis of the filesystem state. As previously described, the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B may assist the user in re-discovering metadata objects and outputting their addresses. Furthermore, the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B may actually fix the discovered problem with fsck failing and allow fsck to complete so work on a filesystem may continue. The Analyzing and Correcting Filesystem Checker Failure method is explained in more detail below with respect to FIG. 3 .
[0040] Referring now to FIG. 2 , an exemplary illustration 200 of the tools included with the set of fs_Tools 112 and associated with the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B ( FIG. 1 ) in accordance with one embodiment is depicted. The Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B ( FIG. 1 ) may interact with a set of created fs_Tools 112 . According to at least one implementation, the present embodiment may create three tools to resolve the problem of fsck failure due to corruption as follows:
[0041] 1) The creation of a tool called fs_discover 202 which is not dependent on fsck and has the ability to discover where metadata resides on the volume that the filesystem resides on. It is able to discover all metadata that still resides on the volume and outputs its page offset and type as it is discovered.
[0042] 2) The creation of a tool called fs_formatter 204 . Fs_formatter may be able to use a symbol file that contains the definitions of metadata objects and use it to output the contents of a metadata structure (such as a superblock) given as input:
[0043] a) the type definition (example superblock)
[0044] b) the volume name
[0045] c) page offset on the volume where data resides (this page offset is obtained from output of fs_discover)
[0046] This output can be redirected to a file and used to analyze what changes may be needed in structure to help make meta-data consistent.
[0047] 3) Creation of update tools 206 (e.g., update_superblock) which will take formatter output that has been changed to make metadata more available to fsck and update these changes given as input:
[0048] a) the text file where changes have been made
[0049] b) the volume needed to be updated
[0050] c) the page offset where update needs to occur.
[0051] Referring now to FIG. 3 , an operational flowchart 300 illustrating the steps carried out by a program for analyzing and correcting corruption which has led to Filesystem Checker Failure is depicted. As previously described, the present embodiment may provide the capability for a user to utilize the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B ( FIG. 1 ) in conjunction with the set of fs_Tools 112 ( FIG. 1 ) to re-discover metadata objects and outputting their addresses. Furthermore, the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B ( FIG. 1 ) and the set of fs_Tools 112 ( FIG. 1 ) may be utilized to actually fix the discovered problem with fsck failing and allow fsck to complete so work on a filesystem may continue. Each step of the method depicted in FIG. 3 is explained further with respect to FIGS. 6A-6D .
[0052] At 302 , the method will determine by the output of the tool fs_discover 202 ( FIG. 2 ), whether there are any metadata structures missing (i.e., over written by corruption). As previously described, fs_discover 202 ( FIG. 2 ) is not dependent on fsck and has the ability to discover where metadata resides on the volume that the filesystem resides on. Therefore, fs_discover 202 ( FIG. 2 ) is able to discover all metadata that still resides on the volume and outputs its page offset and type as it is discovered.
[0053] Next at 304 , the type of structures that the corrupted structure points to is determined. Then at 306 , using fs_discover output 202 ( FIG. 2 ), the method will determine if these structures and their addresses can be located.
[0054] Next at 308 , it is determined whether missing addresses can be determined. If at 308 it is determined that missing addresses cannot be determined then the method will end. However, if at 308 it is determined that missing addresses can be determined, then at 310 the method will remake the corrupted structure with addresses that it should be using. As such, the addresses will once again point to structures allowing fsck to run, thereby recovering groups of files.
[0055] According to at least one implementation, the method may remake the corrupted structure by obtaining additional data. As such, the additional data can be determined through computation of values currently in the block discovered. When there is no direct pointer to the previous block, the value in the data indicates which parent block must point to it. For example, with respect to a group of inodes, their inode numbers will be within a certain range. If the range is, for example, between 0 and 4095 then this page must have a pointer to it in IAG 0. However, if the group of inodes have a range 0 through 31, then the address of the first page of these inodes will be in the first extent of the JAG 0 structure that points to groups of inodes. If the group of inodes have a range from 32 to 63 then the address of the first page of these inodes will be in the next array element of the array of extents kept in the IAG 0. Therefore, by looking at the values of the inode numbers, the method may determine the IAG block (e.g., 0, 1, 2, 3 etc.) and the array element in the extent array that points to it. Each IAG has 128 element array of extents pointing to 32 groups of inodes for a total of 4096. Since the block has been “discovered” (i.e., has passed requirements to be the type of block the method is looking for) it should then have the data to determine what parent it belongs to. In the same manner, regarding an IAG structure that has an index field with value 0, 1, 2, etc., the method may look at this index field and determine which index of the inode of inode (IOI) extents will point to it.
[0056] According to the present embodiment, j2_discover's main function is to discover the addresses where these blocks reside. The method may use the contents of the child's blocks (as described above) to determine at what place in the parent block the discovered addresses should be placed. Furthermore, the design of J2 is such that algorithms exist which allow you to know where to put the discovered addresses in the parent block. One advantage of the present embodiment is that rather than fixing everything that is corrupt, the method puts the pointers in place that fsck needs in order to work. Then fsck run and fix what needs to be fixed.
[0057] If the groups of inodes are at the bottom of the hierarchy, the present embodiment may remake all of the parent objects and therefore, enable fsck to work. However, if some of the groups of inodes are corrupt or lost, then fsck will not be able to fix everything and some null pointers may be in some of the IAG arrays and fsck will work with what is given to it. The present embodiment allows the environment is in such a state so that fsck can run properly.
[0058] Additionally, the present embodiment may not only be implemented with respect to J2, but the same strategy may be employed to other filesystems and their fsck's since similar relationships may exist in other designs. Every fsck depends on a design of pointers. As such, if the design can be recreated, then fsck may work in every type of filesystem. Additionally, the fs_discover Tool 202 ( FIG. 2 ) (e.g., j2_discover) may allow the method to evaluate in great detail whether there is enough pointers to pursue fixing filesystem. As such, the present embodiment allows for a complete analysis that may be given to a corrupt filesystem.
[0059] Additionally, as previously described, the present embodiment may be used for other executables in addition to fsck. Therefore, any executable which depends on obtaining addresses to on disk structures to cause the data on the structure to be accessed could have the same technique described herein if it is not able to be executed because of corruption.
[0060] It may be appreciated that FIG. 3 provides only an illustration of one implementation and does not imply any limitations with regard to how different embodiments may be implemented. Many modifications to the depicted environments may be made based on design and implementation requirements. For example, fs_discover may be used to create both a sparse and a non-sparse metacapture file that may be used in problem diagnosis. A metacapture file is all the metadata of a filesystem put into one file. As such, the present embodiment may alleviate fsck having to work in order to create a metacapture file. Therefore, both a sparse and non-sparse metacapture file may be created without the use of fsck.
[0061] Referring now to FIG. 4 , an exemplary illustration of metadata set up on disk with addresses 400 in accordance with one embodiment is depicted. An inode is a data structure used to represent a filesystem object, which can be a file or a directory. Each inode stores the attributes and disk block location(s) of the filesystem object's data. An Inode of Inodes (IOI) 402 contains the addresses of Inode Allocation Groups (IAG) 406 a , 406 b . An IAG 406 a , 406 b contains the addresses 408 a - 408 g of Groups of Inodes (GOI) 404 a - 404 d . A Group of Inodes GOI 404 a - 404 d contains metadata structures which describe files.
[0062] Referring now to FIG. 5 , an exemplary illustration of how structures point to each other 500 in accordance with one embodiment is depicted. As such, the mode of modes (IOI) 502 points to mode Allocation Groups (IAGS) 504 , 506 . The mode Allocation Groups (IAGS) 504 , 506 point to the Groups of modes (GOI) 508 - 514 .
[0063] Referring now to FIGS. 6A-6D , examples of applying the method steps described in FIG. 3 in accordance with one embodiment are depicted. For example purposes only, FIGS. 6A-6D may depict J2 filesystem, however the present embodiment may be applied to other filesystems and their fsck's. In FIG. 6A , the mode of modes IOI 502 gets overwritten. As such, the ability to find modes is lost and therefore, a filesystem checker, such as a “file system consistency check” fsck fails. As previously described with respect to FIG. 3 at 302 , it is determined from an fs_discover output tool 202 ( FIG. 2 ) (e.g., j2_discover) if there are any metadata structures missing or overwritten by corruption. Regarding FIG. 6A , it may be discovered from the fs_discover output 202 ( FIG. 2 ) that the IOI structure 502 is missing. Therefore, at step 304 ( FIG. 3 ) the method will determine what type of structures the corrupted structure points to. Regarding FIG. 6A , the IOI structure 502 points to IAG structures 504 and 506 .
[0064] Next, at step 306 ( FIG. 3 ), using fs_discover output 202 ( FIG. 2 ), the method will determine if these structures and their addresses can be located. Therefore, regarding FIG. 6A , the method will look for IAG structures 504 and 506 in fs_discover output 202 ( FIG. 2 ). For example:
[0000]
−>j2_discover /dev/fslv01
LV
PAGE
METADATA
ADDITIONAL
OFFSET
COUNT
TYPE
DATA
0x0
0x8
NONMETA
0x8
0x1
SUPER
. . .
0x14
0xf
BLK_DMAP
0x16
0x1
IAG
0
0x23
0x1
NONMETA
0x24
0x1
BLK_DMAP
. . .
. . .
. . .
. . .
0x50
0x1
IAG
1
[0065] Next, at step 308 ( FIG. 3 ), the method will check whether any missing addresses can be determined and if so, then at step 310 ( FIG. 3 ) the method will remake the corrupted IOI structure 502 ( FIG. 6B ) with addresses that it should be using so that once again IOI structure 502 ( FIG. 6B ) points to structures 504 , 506 allowing fsck to run. Regarding FIG. 6B , addresses (0x16) 516 and (0x50) 518 will be put into their appropriate places in a replica of corrupted IOI structure 502 allowing fsck to work.
[0066] Regarding FIG. 6C , it may be discovered from the fs_discover output 202 ( FIG. 2 ) that an IAG 506 is corrupted. For example, at 302 ( FIG. 1 ) the method may determine from an fs_discover output tool 202 ( FIG. 2 ), such as J2_discover output, if there are any metadata structures 504 , 506 missing or overwritten by corruption. With respect to FIG. 6C , it can be determined from the j2_discover output that the IAG structure IAG1 506 is missing,
[0067] Next at step 304 ( FIG. 3 ), the method will determine what type of structures the corrupted structure 506 points to. Therefore, regarding FIG. 6C , the corrupted IAG structure IAG 1 506 points to GOI structures 510 and 514 . Then at step 306 ( FIG. 3 ) using j2_discover output, the method will determine if these structures and their addresses can be located. Therefore, regarding FIG. 6C , the method will look for GOI structures 510 and 514 in j2_discover output.
[0068] Next, at step 308 ( FIG. 3 ), the method will check whether any missing addresses can be determined and if so, then at step 310 ( FIG. 3 ) the method will remake the corrupted IAG structure 506 ( FIG. 6D ) with addresses that it should be using so that once again it points to structures 510 , 514 allowing fsck to run. Regarding FIG. 6D , addresses (0x3c) 602 and (0x5a) 604 will be put into their appropriate places in a replica of corrupted IAG structure 506 allowing fsck to work.
[0069] FIG. 7 is a block diagram 7000 of internal and external components of computers depicted in FIG. 1 in accordance with an illustrative embodiment of the present invention. It should be appreciated that FIG. 7 provides only an illustration of one implementation and does not imply any limitations with regard to the environments in which different embodiments may be implemented. Many modifications to the depicted environments may be made based on design and implementation requirements.
[0070] Data processing system 800 , 900 is representative of any electronic device capable of executing machine-readable program instructions. Data processing system 800 , 900 may be representative of a smart phone, a computer system, PDA, or other electronic devices. Examples of computing systems, environments, and/or configurations that may represented by data processing system 800 , 900 include, but are not limited to, personal computer systems, server computer systems, thin clients, thick clients, hand-held or laptop devices, multiprocessor systems, microprocessor-based systems, network PCs, minicomputer systems, and distributed cloud computing environments that include any of the above systems or devices.
[0071] User client computer 102 ( FIG. 1 ) and network server 114 ( FIG. 1 ) may include respective sets of internal components 800 a,b and external components 900 a,b illustrated in FIG. 7 . Each of the sets of internal components 800 include one or more processors 820 , one or more computer-readable RAMs 822 and one or more computer-readable ROMs 824 on one or more buses 826 , and one or more operating systems 828 and one or more computer-readable tangible storage devices 830 . The one or more operating systems 828 and the Software Program 108 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 A in client computer 102 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 B ( FIG. 1 ) in network server 114 ( FIG. 1 ) are stored on one or more of the respective computer-readable tangible storage devices 830 for execution by one or more of the respective processors 820 via one or more of the respective RAMs 822 (which typically include cache memory). In the embodiment illustrated in FIG. 7 , each of the computer-readable tangible storage devices 830 is a magnetic disk storage device of an internal hard drive. Alternatively, each of the computer-readable tangible storage devices 830 is a semiconductor storage device such as ROM 824 , EPROM, flash memory or any other computer-readable tangible storage device that can store a computer program and digital information.
[0072] Each set of internal components 800 a,b also includes a R/W drive or interface 832 to read from and write to one or more portable computer-readable tangible storage devices 936 such as a CD-ROM, DVD, memory stick, magnetic tape, magnetic disk, optical disk or semiconductor storage device. A software program, such as the Software Program 108 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 A, 116 B ( FIG. 1 ) can be stored on one or more of the respective portable computer-readable tangible storage devices 936 , read via the respective R/W drive or interface 832 and loaded into the respective hard drive 830 .
[0073] Each set of internal components 800 a,b also includes network adapters or interfaces 836 such as a TCP/IP adapter cards, wireless Wi-Fi interface cards, or 3G or 4G wireless interface cards or other wired or wireless communication links. The Software Program 108 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 A ( FIG. 1 ) in client computer 102 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 B ( FIG. 1 ) in network server 114 ( FIG. 1 ) can be downloaded to client computer 102 ( FIG. 1 ) and network server 114 ( FIG. 1 ) from an external computer via a network (for example, the Internet, a local area network or other, wide area network) and respective network adapters or interfaces 836 . From the network adapters or interfaces 836 , the Software Program 108 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 A ( FIG. 1 ) in client computer 102 ( FIG. 1 ) and the Analyzing and Correcting Filesystem Checker Failure Program 116 B ( FIG. 1 ) in network server 114 ( FIG. 1 ) are loaded into the respective hard drive 830 . The network may comprise copper wires, optical fibers, wireless transmission, routers, firewalls, switches, gateway computers and/or edge servers.
[0074] Each of the sets of external components 900 a,b can include a computer display monitor 920 , a keyboard 930 , and a computer mouse 934 . External components 900 a,b can also include touch screens, virtual keyboards, touch pads, pointing devices, and other human interface devices. Each of the sets of internal components 800 a,b also includes device drivers 840 to interface to computer display monitor 920 , keyboard 930 , and computer mouse 934 . The device drivers 840 , R/W drive or interface 832 and network adapter or interface 836 comprise hardware and software (stored in storage device 830 and/or ROM 824 ).
[0075] It is understood in advance that although this disclosure includes a detailed description on cloud computing, implementation of the teachings recited herein are not limited to a cloud computing environment. Rather, embodiments of the present invention are capable of being implemented in conjunction with any other type of computing environment now known or later developed.
[0076] Cloud computing is a model of service delivery for enabling convenient, on-demand network access to a shared pool of configurable computing resources (e.g. networks, network bandwidth, servers, processing, memory, storage, applications, virtual machines, and services) that can be rapidly provisioned and released with minimal management effort or interaction with a provider of the service. This cloud model may include at least five characteristics, at least three service models, and at least four deployment models.
[0077] Characteristics are as follows:
[0078] On-demand self-service: a cloud consumer can unilaterally provision computing capabilities, such as server time and network storage, as needed automatically without requiring human interaction with the service's provider.
[0079] Broad network access: capabilities are available over a network and accessed through standard mechanisms that promote use by heterogeneous thin or thick client platforms (e.g., mobile phones, laptops, and PDAs).
[0080] Resource pooling: the provider's computing resources are pooled to serve multiple consumers using a multi-tenant model, with different physical and virtual resources dynamically assigned and reassigned according to demand. There is a sense of location independence in that the consumer generally has no control or knowledge over the exact location of the provided resources but may be able to specify location at a higher level of abstraction (e.g., country, state, or datacenter).
[0081] Rapid elasticity: capabilities can be rapidly and elastically provisioned, in some cases automatically, to quickly scale out and rapidly released to quickly scale in. To the consumer, the capabilities available for provisioning often appear to be unlimited and can be purchased in any quantity at any time.
[0082] Measured service: cloud systems automatically control and optimize resource use by leveraging a metering capability at some level of abstraction appropriate to the type of service (e.g., storage, processing, bandwidth, and active user accounts). Resource usage can be monitored, controlled, and reported providing transparency for both the provider and consumer of the utilized service.
[0083] Service Models are as follows:
[0084] Software as a Service (SaaS): the capability provided to the consumer is to use the provider's applications running on a cloud infrastructure. The applications are accessible from various client devices through a thin client interface such as a web browser (e.g., web-based e-mail). The consumer does not manage or control the underlying cloud infrastructure including network, servers, operating systems, storage, or even individual application capabilities, with the possible exception of limited user-specific application configuration settings.
[0085] Platform as a Service (PaaS): the capability provided to the consumer is to deploy onto the cloud infrastructure consumer-created or acquired applications created using programming languages and tools supported by the provider. The consumer does not manage or control the underlying cloud infrastructure including networks, servers, operating systems, or storage, but has control over the deployed applications and possibly application hosting environment configurations.
[0086] Infrastructure as a Service (IaaS): the capability provided to the consumer is to provision processing, storage, networks, and other fundamental computing resources where the consumer is able to deploy and run arbitrary software, which can include operating systems and applications. The consumer does not manage or control the underlying cloud infrastructure but has control over operating systems, storage, deployed applications, and possibly limited control of select networking components (e.g., host firewalls).
[0087] Deployment Models are as follows:
[0088] Private cloud: the cloud infrastructure is operated solely for an organization. It may be managed by the organization or a third party and may exist on-premises or off-premises.
[0089] Community cloud: the cloud infrastructure is shared by several organizations and supports a specific community that has shared concerns (e.g., mission, security requirements, policy, and compliance considerations). It may be managed by the organizations or a third party and may exist on-premises or off-premises.
[0090] Public cloud: the cloud infrastructure is made available to the general public or a large industry group and is owned by an organization selling cloud services.
[0091] Hybrid cloud: the cloud infrastructure is a composition of two or more clouds (private, community, or public) that remain unique entities but are bound together by standardized or proprietary technology that enables data and application portability (e.g., cloud bursting for load-balancing between clouds).
[0092] A cloud computing environment is service oriented with a focus on statelessness, low coupling, modularity, and semantic interoperability. At the heart of cloud computing is an infrastructure comprising a network of interconnected nodes.
[0093] Referring now to FIG. 8 , illustrative cloud computing environment 700 is depicted. As shown, cloud computing environment 700 comprises one or more cloud computing nodes 100 with which local computing devices used by cloud consumers, such as, for example, personal digital assistant (PDA) or cellular telephone 700 A, desktop computer 700 B, laptop computer 700 C, and/or automobile computer system 700 N may communicate. Nodes 100 may communicate with one another. They may be grouped (not shown) physically or virtually, in one or more networks, such as Private, Community, Public, or Hybrid clouds as described hereinabove, or a combination thereof. This allows cloud computing environment 700 to offer infrastructure, platforms and/or software as services for which a cloud consumer does not need to maintain resources on a local computing device. It is understood that the types of computing devices 700 A-N shown in FIG. 8 are intended to be illustrative only and that computing nodes 100 and cloud computing environment 700 can communicate with any type of computerized device over any type of network and/or network addressable connection (e.g., using a web browser).
[0094] Referring now to FIG. 9 , a set of functional abstraction layers 9000 provided by cloud computing environment 700 ( FIG. 8 ) is shown. It should be understood in advance that the components, layers, and functions shown in FIG. 9 are intended to be illustrative only and embodiments of the invention are not limited thereto. As depicted, the following layers and corresponding functions are provided:
[0095] Hardware and software layer 9010 includes hardware and software components. Examples of hardware components include: mainframes; RISC (Reduced Instruction Set Computer) architecture based servers; storage devices; networks and networking components. In some embodiments, software components include network application server software.
[0096] Virtualization layer 9012 provides an abstraction layer from which the following examples of virtual entities may be provided: virtual servers; virtual storage; virtual networks, including virtual private networks; virtual applications and operating systems; and virtual clients.
[0097] In one example, management layer 9014 may provide the functions described below. Resource provisioning provides dynamic procurement of computing resources and other resources that are utilized to perform tasks within the cloud computing environment. Metering and Pricing provide cost tracking as resources are utilized within the cloud computing environment, and billing or invoicing for consumption of these resources. In one example, these resources may comprise application software licenses. Security provides identity verification for cloud consumers and tasks, as well as protection for data and other resources. User portal provides access to the cloud computing environment for consumers and system administrators. Service level management provides cloud computing resource allocation and management such that required service levels are met. Service Level Agreement (SLA) planning and fulfillment provide pre-arrangement for, and procurement of, cloud computing resources for which a future requirement is anticipated in accordance with an SLA. An Analyzing and Correcting Filesystem Checker Failure Program may provide a process and a set of tools for analyzing and correcting corruption which has led to filesystem checker failure so that the checker will run without error.
[0098] Workloads layer 9016 provides examples of functionality for which the cloud computing environment may be utilized. Examples of workloads and functions which may be provided from this layer include: mapping and navigation; software development and lifecycle management; virtual classroom education delivery; data analytics processing; and transaction processing.
[0099] The descriptions of the various embodiments of the present invention have been presented for purposes of illustration, but are not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope of the described embodiments. The terminology used herein was chosen to best explain the principles of the embodiments, the practical application or technical improvement over technologies found in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
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A method for repairing a corrupted filesystem, whereby the corrupted filesystem includes a plurality of corrupted metadata structures is provided. The method may include determining a plurality of missing metadata structures associated with the corrupted filesystem. The method may also include determining a plurality of current addresses corresponding to a plurality of valid metadata structures in a hierarchical metadata structure of the corrupted filesystem. The method may further include locating the plurality of missing metadata structures and a plurality of addresses associated with the missing metadata. The method may also include rebuilding the plurality of missing metadata structures based on the located plurality of addresses associated with the missing metadata structures, whereby the rebuilding comprises assigning the located plurality of address to the plurality of missing metadata structures and redirecting the plurality of missing metadata structures to point to a correct plurality of other metadata structures.
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This is a division, of application Ser. No. 497,962, filed on May 25, 1983, now U.S. Pat. No. 4,464,380.
BACKGROUND OF THE INVENTION
This invention relates to new imidazolidinedione derivatives of interest to those in the field of medicinal chemistry and chemotherapy. More particularly, it is concerned with a novel series of spiro-oxindole imidazolidinedione compounds for the control of certain chronic complications arising from diabetes mellitus (e.g., diabetic cataracts, retinopathy and neuropathy).
Past attempts to obtain new and better oral antidiabetic agents have, for the most part, involved an endeavor to lower blood sugar levels. However, little is known about the effect of organic compounds in preventing or arresting certain chronic complications of diabetes, such as diabetic cataracts, neuropathy and retinopathy, etc. Nevertheless, K. Sestanj et. al. in U.S. Pat. No. 3,821,383 do disclose that certain aldose reductase inhibitors like 1,3-dioxo-1H-benz[d,e]isoquinoline-2(3H)-acetic acid and some closely-related derivatives thereof are useful for these purposes even though they are not known to be hypoglycemic. These compounds function by inhibiting the activity of the enzyme aldose reductase, which is primarily responsible for catalyzing the reduction of aldoses (like glucose and galactose) to the corresponding polyols (such as sorbitol and galactitol) in the human body. In this way, unwanted accumulations of galactitol in the lens of galactosemic subjects and of sorbitol in the lens, retina, peripheral nervous system and kidney of diabetic subjects are prevented or reduced. As a result, these compounds control certain chronic diabetic complications, including those of an ocular nature, since it is already known in the art that the presence of polyols in the lens of the eye leads to cataract formation and concomitant loss of lens clarity.
SUMMARY OF THE INVENTION
The present invention relates to novel spiro-oxindole imidazolidinedione compounds useful in therapy as aldose reductase inhibitors for the control of certain chronic complications arising in a diabetic subject. More specifically, the novel compounds of this invention are selected from the group consisting of spiro-hydantoin derivatives of the formulae: ##STR1## and the pharmaceutically acceptable salts thereof, wherein X and Y are each hydrogen, fluorine, chlorine, bromine, nitro or amino; Z is hydrogen or amino, with the proviso that Z is always other than amino when at least one of X and Y is other than hydrogen; R is a member selected from the group consisting of hydrogen, aryl and aralkyl having up to three carbon atoms in the alkyl moiety wherein each of said aryl moieties is chosen from the group consisting of pyridyl and ring-substituted pyridyl, with each ring substituent being chosen from the group consisting of fluorine, chlorine, bromine and alkyl having from one to four carbon atoms, with the proviso that said R is always other than hydrogen when each of X, Y and Z is other than amino; ═A--B═D-- of formula II represents ═N--CH═CH--, ═CH--CH═N-- or ═CH--N═CH--; R' is a member selected from the group consisting of hydrogen, alkyl having from one to four carbon atoms, aryl and aralkyl having up to three carbon atoms in the alkyl moiety wherein each of said aryl moieties is chosen from the group consisting of pyridyl, thienyl, phenyl and mono and di-substituted phenyl, with each ring substituent being chosen from the group consisting of fluorine, chlorine, bromine, alkyl and alkoxy each having up to four carbon atoms and trifluoromethyl; and R" is hydrogen, hydroxy, fluorine, chlorine, alkyl or alkoxy each having up to four carbon atoms or trifluoromethyl. These novel compounds are aldose reductose inhibitors and therefore, possess the ability to reduce or inhibit sorbitol accumulation in the lens and peripheral nerves of diabetic subjects.
One group of compounds of interest of the present invention is that of formula I wherein X is fluorine, Y and Z are each hydrogen and R is pyridylalkyl having up to three carbon atoms in the alkyl moiety. Another group of compounds of interest of the present invention is that of formula I wherein X and Y are each chlorine, Z is hydrogen and R is pyridylalkyl having up to three carbon atoms in the alkyl moiety.
A further group of compounds of interest of the present invention is that of formula II wherein ═A-- B═D-- is ═CH--N═CH-- and R" is hydrogen or alkyl having up to four carbon atoms (e.g., methyl). Preferably, R' is hydrogen, alkyl having from one to four carbon atoms (e.g., isopropyl), mono-substituted phenylalkyl having up to three carbon atoms in the alkyl moiety (e.g., p-fluorobenzyl or p-chlorobenzyl), di-substituted phenylalkyl having up to three carbon atoms in the alkyl moiety (e.g., 3,4-dichlorobenzyl) or mono-substituted phenyl (e.g., p-fluorophenyl).
Of special interest in this connection are such typical and preferred member compounds of the invention as 6'-amino-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 5'-chloro-7'-amino-spiro[imidazolidine-4,3'-indoline]-2,2', 5-trione, 1'-(3-pyridylmethyl)-5,'-fluoro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 1'-(3-pyridylmethyl)-5,7'-dichloro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione and spiro-[imidazoline-4,3'-(6-azaindoline)]-2,2',5-trione, respectively. These particular compounds are highly potent as regards their aldose reductose inhibitory activity.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with the process employed for preparing the novel compounds of this invention (viz., those of structural formulae I-II), an appropriately substituted carbonyl ring compound of structural formulae III or IV as respectively set forth below: ##STR2## wherein X,Y,Z,R,R' and R" are each as previously defined (with proviso), is condensed with an alkali metal cyanide (e.g. sodium cyanide or potassium cyanide) and ammonium carbonate to form the desired spiro-oxindole imidazolidinedione final product of the structural formulae previously indicated. This particular reaction is normally carried out in the presence of a reaction-inert polar organic solvent medium in which both the reactants and reagents are mutually miscible. Preferred organic solvents for use in this connection include cyclic ethers such as dioxane and tetrahydrofuran, lower alkylene glycols like ethylene glycol and trimethylene glycol, water-miscible lower alkanols such as methanol, ethanol and isopropanol, as well as N,N-di(lower alkyl) lower alkanoamides like N,N-dimethyl-formamide, N,N-diethylformamide and N,N-dimethylacetamide, etc. In general, the reaction is conducted at a temperature that is in the range of from about 50° C. up to about 150° C. for a period of about two hours to about four days. Although the amount of reactant and reagents employed in the reaction can vary to some extent, it is preferable to employ at least a slight molar excess of the alkali metal cyanide reagent with respect to the carbonyl ring compound starting material in order to effect maximum yield. In this way, for example, 1-(3-pyridylmethyl)-5 -fluoroindoline-2,3-dione is converted to 1'-(3-pyridylmethyl)-5'-fluoro- spiro[imidazolidine-4,3'-indoline]-2,2',5-trione and 1-(3-pyridylmethyl)-5,7-dichloroindoline-2,3-dione is converted to 1'-(3-pyridylmethyl)-5', 7'-dichloro- spiro[imidazolidine-4,3'-indoline]-2,2',5-trione.
Compounds of the invention of formula I where X and Y are each hydrogen and Z is amino are best prepared by the alkylation of sodio-ethyl hydantoin-5-carboxylate with 2,4-dinitrochlorobenzene, followed by reductive cyclization in a conventional manner. This last step is usually accomplished by using iron powder in the presence of an acid such as hydrochloric acid or glacial acetic acid, generally in the presence of an aqueous alkanol medium at ambient to slightly elevated temperatures (e.g., ca. 20°-100° C.). C ompounds of the invention of formula II wherein R' is hydrogen and R" is as previously defined are also best prepared in this manner by merely substituting the appropriate halonitro-disubstituted pyridine compound in place of 2,4-dinitrochlorobenzene in the first step of the reaction. In this way, the use of 3-nitro-4-chloropyridine ultimately leads to spiro-[imidazolidine-4,3'-(6-azaindoline)]-2,2',5-trione as the desired final product. Moreover, compounds of the invention of formula I where X and Y are both halogen (as previously defined) and Z is hydrogen may alternatively (and preferably) be prepared from the corresponding unsubstituted compounds wherein at least one of X and Y is hydrogen by means of direct halogenation techniques well known to those skilled in the field of synthetic organic chemistry. Additionally, these same manohalo starting materials (e.g., where X is halogen and Y and Z are both hydrogen) can be converted to the corresponding compounds where Y is nitro and amino, etc., by conventional procedure well-known to those skilled in the art (e.g., nitration and subsequent reduction, etc.). In the latter connection, the reduction step is preferably accomplished by using catalytic hydrogenation, e.g., by using a platinum, palladium or nickel catalyst and gaseous hydrogen, or by using sodium amalgam and the like. Lastly, compounds of the invention of formula II wherein R' is other than hydrogen can alternatively (and preferably) be prepared from the corresponding compounds where R' is hydrogen by the use of standard techniques well-known to those skilled in the art. For instance, the use of an appropriate reagent of the formula R"' X", where R"' is other than hydrogen or aryl and X" is a leaving group such as an aryl or alkylsulfonyloxy radical, in the presence of a base such as sodium hydride or sodium hydroxide ultimately leads to the formulation of compounds of formula II where R' is alkyl or aralkyl as previously defined.
The ketone starting materials (i.e., carbonyl ring compounds of structural formulae III-IV) required for preparing the desired final products of structural formulae I-II in the overall process of this invention are, for the most part, known compounds and are either readily available commercially, like isatin (2,3-indolinedione), 5-fluoroisatin, 5-chloroisatin and 5,7-dichloroisatin, etc., or else they can easily be synthesized by those skilled in the art starting from common chemical reagents and using conventional methods of organic synthesis. For instance, the 1-aralkyl-5-haloisatins are easily obtained by alkylating 5-fluoro or 5-chloroisatin with the appropriate aralkyl halide of choice (e.g., 3-chloromethylpyridine) in the presence of a base such as sodium hydride or potassium carbonate, while the corresponding 1-aryl-5-haloisatins are best synthesized by treatment of the appropriate diarylamine compound with oxalyl chloride, followed by ring-closure with aluminum chloride in the usual manner. In either case, the ultimate starting materials are both readily derived from readily available compounds.
Inasmuch as the spiro-oxindole imidazolinedione compounds of this invention all possess one asymmetric center, they may exist in separated d- and 1-optically active forms, as well as in racemic or d1-mixtures. The present invention includes all these forms. For instance, an optically active isomer may be obtained by simply resolving the racemic mixture via the use of standard techniques well-known to those skilled in the art, e.g., by fractional crystallization of a spiro-oxindole imidazolidinedione salt derived from an optically active acid or base. Alternatively, the optically active isomers may be prepared by using the appropriate enantiomers as starting materials in the foregoing series of reactions.
The pharmaceutically acceptable acid addition salts of the spiro-oxindole imidazolidinedione base compounds of this invention are prepared by simply treating the aforementioned organic bases with various mineral and organic acids which form non-toxic acid addition salts having pharmacologically acceptable anions, such as the hydrochloride, hydrobromide, hydroiodide, sulfate or bisulfate, phosphate or acid phosphate, acetate, lactate, maleate, fumarate, citrate or acid citrate, tartrate or bitartrate, succinate, gluconate, saccharate, methanesulfonate, ethanesulfonate, benzenesulfonate and p-toluenesulfonate salts. For instance, the salt-formation step may be carried out by using a substantially equimolar amount of the appropriate acid in an aqueous solvent medium or in a suitable organic solvent such as methanol or ethanol. Upon careful evaporation of the solvent, the solid salt is readily obtained.
The chemical bases which are used as reagents to prepare the pharmaceutically acceptable base salts of this invention are those which form non-toxic base salts with the herein described acidic spiro-oxindole imidazolidinedione compounds. These particular non-toxic base salts include those derived from such pharmacologically acceptable cations as sodium, potassium, calcium and magnesium, etc. These salts can easily be prepared by simply treating the aforementioned spiro-oxindole imidazolidinedione acidic compounds with an aqueous solution of the desired pharmacologically acceptable cation, and then evaporating the resulting solution to dryness while preferably being placed under reduced pressure. Alternatively, they may also be prepared by mixing lower alkanolic solutions of the acidic compounds and the desired alkali metal alkoxide together, and then evaporating the resulting solution to dryness in the same manner as before. In either case, stoichiometric quantitites of reagents are preferably employed in order to ensure completeness of reaction and maximum production of yields of the desired final product.
As previously indicated, the spiro-oxindole imidazolidinedione compounds of this invention are readily adapted to therapeutic use as aldose reductase inhibitors for the control of chronic diabetic complications, in view of their ability to reduce lens sorbitol levels in diabetic subjects to a statistically significant degree. For instance, 1'-(3-pyridylmethyl)-5',7'-dichloro-sprio-[imidazolidine-4,3'-indoline]-2,2',5-trione, a typical and preferred agent of the present invention, has been found to inhibit the formation of sorbitol levels in diabetic rats to a significantly high degree when given by the oral route of administration at dose levels ranging from 0.5 mg./kg. to 20 mg./kg. Furthermore, the herein described compounds of this invention can be administered by either the oral or parenteral routes of administration. In general, these compounds are ordinarily administered in dosages ranging from about 0.10 mg. to about 10 mg. per kg. of body weight per day, although variations will necessarily occur depending upon the weight and condition of the subject being treated and the particular route of administration chosen.
In connection with the use of the spiro-oxindole imidazolidinedione compounds of this invention for the treatment of diabetic subjects, it is to be noted that these compounds may be administered either alone or in combination with pharmaceutically acceptable carriers by either of the routes previously indicated, and that such administration can be carried out in either single or multiple dosages. More particularly, the compounds of this invention can be administered in a wide variety of different dosage forms, i.e., they may be combined with various pharmaceutically-acceptable inert carriers in the form of tablets, capsules, lozenges, troches, hard candies, powders, sprays, aqueous suspensions, injectable solutions, elixirs, syrups, and the like. Such carriers include solid diluents or fillers, sterile aqueous media and various non-toxic organic solvents. In general, the compounds of the invention will be present in such dosage forms at concentration levels ranging from about 0.5% to about 90% by weight of the total composition to provide the desired unit dosage.
For purposes of oral administration, tablets containing various excipients such as sodium citrate, calcium carbonate and calcium phosphate may be employed along with various disintegrants such as starch and preferably potato or tapioca starch, alginic acid and certain complex silicates, together with binding agents such as polyvinylpyrrolidone, gelatin and acacia. Additionally, lubricating agents such as magnesium stearate, sodium lauryl sulfate and talc are often very useful for tabletting purposes. Solid compositions of a similar type may also be employed as fillers in soft and hard-filled gelatin capsules; preferred materials in this connection would also include the high molecular weight polyethylene glycols. When aqueous suspensions and/or elixirs are desired for oral administration, the essential active ingredient therein may be combined with various sweetening or flavoring agents, coloring matter or dyes, and if so desired, emulsifying and/or suspending agents as well, together with such diluents as water, ethanol, propylene glycol, glycerin and various like combinations thereof.
For purposes of parenteral administration, solutions of these spiro-oxindole imidazolidinediones in sesame or peanut oil or in aqueous propylene glycol or N,N-dimethylformamide may be employed, as well as sterile aqueous solutions of the corresponding water-soluble, non-toxic mineral and organic acid addition salts or alkali or alkaline-earth metal salts previously enumerated. Such aqueous solutions should be suitably buffered if necessary and the liquid diluent first rendered isotonic with sufficient saline or glucose. These particular aqueous solutions are especially suitable for intravenous, intramuscular, subcutaneous and intraperitoneal injection purposes. In this connection, the sterile aqueous media employed are all readily obtainable by standard techniques well-known to those skilled in the art. Additionally, it is also possible to administer the aforesaid spiro-oxindole oxazolidinedione compounds topically via an appropriate ophthalmic solution applied dropwise to the eye.
The activity of the compounds of the present invention, as agents for the control of chronic diabetic complications, is determined by their ability to successfully pass one or more of the following standard biological or pharmacological tests, viz., (1) measuring their ability to inhibit the enzyme activity of isolated aldose reductase; (2) measuring their ability to reduce or inhibit sorbitol accumulation in the sciatic nerve of acutely streptozotocinized (i.e., diabetic) rats; (3) measuring their ability to reverse already-elevated sorbitol levels in the sciatic nerve and lens of chronic streptozotocin-induced diabetic rats; (4) measuring their ability to prevent or inhibit galactitol formation in the lens of acutely galactosemic rats, and (5) measuring their ability to delay cataract formation and reduce the severity of lens opacities in chronic galactosemic rats.
PREPARATION A
A solution consisting of 3.0 g. (0.014 mole) of ethyl ureidomalonate dissolved in 43 ml. of absolute ethanol was heated under reflux in a nitrogen atmosphere, while a 0.017 molar solution of sodium ethanolate (sodium in ethanol) while slowly added thereto over a period of 2.5 hours. Upon completion of this step, the resulting reaction mixture was cooled to room temperature (˜20° C.) and the desired product collected by means of suction filtration and subsequently washed with two-20 ml. portions of absolute ethanol and one-20 ml. portion of absolute ether. In this manner, there was ultimately obtained pure sodio-ethyl hydantoin-5-carboxylate.
When the reaction was repeated using 10 g. of starting material (ethyl ureidomalonate) and 1.06 g. of sodium in 60 ml. of absolute ethanol, the yield of pure final product amounted to 7.53 g. (85%).
PREPARATION B
A mixture consisting of 20 g. (0.14 mole) of 3-nitro-4-hydroxypyridine, 33.3 g. of phosphorus pentachloride and 2 ml. of phosphorus oxychloride was heated in an oil both at 130° C. for a period of three hours. Upon completion of this step, the excess phosphorus oxychloride was removed from the spent reaction mixture by means of fractional distillation and the residual material was subsequently taken up in methylene chloride. The latter solution was then washed with saturated aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and filtered. Evaporation of the solvent from the resulting filtrate then gave the desired product, viz., 3-nitro-4-chloropyridine.
When the procedure was repeated using 2.8 g. (0.02 mole) of starting material (3-nitro-4-hydroxypyridine), the yield of pure final product amounted to 2.35 g. (74%).
PREPARATION C
A solution consisting of 20.2 g.(0.182 mole) of p-fluoroaniline and 22.1 g. (0.182 mole) of p-fluorobenzaldehyde dissolved in 100 ml. of ethanol was refluxed for a period of five minutes. Upon completion of this step, the spent reaction mixture was cooled to room temperature (˜20° C.) and the desired product subsequently collected by means of suction filtration. A second crop of product was thereafter obtained by concentrating the resulting filtrate in vacuo. The total yield of pure 3-[(p-fluorophenyl)methylidene]pyridine amounted to 33 g. (84%).
To 11.0 g. of the above intermediate in 50 ml. of methanol, there were added 1.92 g. of sodium borohydride at room temperature. Upon completion of this step, the resulting reaction mixture was diluted with water, extracted with diethyl ether and the ethereal extracts subsequently dried over anhydrous magnesium sulfate and filtered. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was ultimately obtained a crude residual product which thereafter crystallized from n-hexane to afford pure 3-[(p-fluorophenyl)aminomethyl]pyridine. The yield of pure product amounted to 8.6 g. (77%).
EXAMPLE 1
A solution consisting of 500 mg. (0.230 mole) of spiro-[imidazolidine-4,3'-indoline]-2,2', 5-trione [H. Otamasu et al., Chem. Pharm. Bull. (Tokyo), Vol. 23, No. 7, p.1431 (1975)] dissolved in 10 ml. of dioxane and 2 ml. of water was treated with chlorine gas by bubbling the gas through the mixture at room temperature (˜20° C.) until saturation of same was complete with respect to said gas (this required a period of approximately two minutes). The course of the reaction was followed by means of thin layer chromatography (using acetone/hexane as the eluant) in order to ensure that no dichlorination occurred. Upon completion of this step, the reaction mixture was diluted with sodium sulfite solution and extracted with ethyl acetate to ultimately afford pure 5'-chloro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione. The yield of pure product amounted to 150 mg. (26%).
A well-stirred mixture consisting of 300 mg. of 5'-chloro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 48 ml. of glacial acetic acid and 16 ml. of fuming nitric acid was heated at 90° C. for a period of one-half hour. Upon completion of this step, the cooled reaction mixture was poured into water, partially neutralized with sodium bicarbonate solution and the resulting product subsequently collected by means of suction filtration. In this manner, there was ultimately obtained 2.05 mg. (58%) of pure 5'-chloro-7'-nitro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, m.p.>270° C.
A solution consisting of 80 mg. of 5'-chloro-7'-nitro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione dissolved in 5 ml. of ethanol containing 0.5 ml. of concentrated hydrochloric acid was treated with 10 mg. of 10% palladium on carbon catalyst and stirred in a hydrogen atmosphere at room temperature for a period of one hour. The resulting reaction mixture was then filtered thru filter-cel to remove the catalyst, which was thereafter washed with ethanol, and the combined washings and filtrate were subsequently concentrated in vacuo to afford a crude residual product. Recrystallization of the latter material from chloroform then gave pure 5'-chloro-7'-amino-spiro-[imidazolidine-4,3'-indolidine]-2,2',5-trione as the hydrochloride salt. The yield of pure material amounted to 56 mg. (68%). The pure product was characterized by means of high resolution mass spectroscopy (m/e, 266.0125; theory, 266.0177) and nuclear magnetic resonance data.
EXAMPLE 2
A mixture consisting of 1.0 g. of a 50% dispersion of sodium hydride in mineral oil that had been covered with 50 ml. of dimethylformamide was treated with 2.16 g. of 5,7-dichloroindoline-2,3-dione (5,7-dichloroisatin) by adding the latter material slowly thereto in small portions. This was then followed by the addition of 1.64 g. of 3-pyridylmethylchloride and the resulting reaction mixture was heated at 90° C. for a period of one hour. Upon completion of this step, the spent reaction mixture was diluted with water, acidified and then extracted with ethyl acetate, followed by basification of the organic layer with aqueous sodium bicarbonate solution. The latter aqueous solution was then extracted with ethyl acetate, and the resulting organic layer saved and subsequently concentrated in vacuo to afford a crude residual product. Recrystallization of the latter material from diethyl ether/ethyl acetate then gave 1.7 g. (55%) of pure 1-(3-pyridylmethyl)-5,7-dichloroindoline-2,3-dione.
A mixture of consisting of 1.53 g. of 1-(3-pyridylmethyl)-5,7-dichloroindoline-2,3-dione, 390 mg. of potassium cyanide and 1.86 g. of powdered ammonium carbonate in 40 ml. of 50% aqueous methanol was heated in an oil bath at 80° C. for a period of one-half hour. At the end of this time, the spent reaction mixture was cooled in an ice bath, quenched (i.e., acidified) with concentrated hydrochloric acid and diluted with additional water. After extracting the resulting aqueous solution with ethyl acetate, there were obtained several organic extracts that were later combined and subsequently dried over anhydrous magnesium sulfate to give a clear solution. Upon removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was ultimately obtained a residual material that was later chromatographed over 30 g. of silica gel using ethyl acetate as the eluant. The appropriate fractions were then combined and subsequently concentrated in vacuo to afford a pure solid residual material. Recrystallization of the latter material from ethanol/hexane then gave 750 mg. of pure 1'-(3-pyridymethyl)-5',7'-dichloro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, m.p. 274° C.(decomp.). The pure product was further characterized by means of mass spectroscopy and nuclear magnetic resonance data.
EXAMPLE 3
To a stirred solution consisting of 1.1 ml. of oxalyl chloride in 40 ml. of methylene chloride at 0° C., there was added in a dropwise fashion a clear solution consisting of 3-[(p-fluorophenyl)aminomethyl]pyridine (the product of Preparation C) dissolved in 30 ml. of methylene chloride. After stirring at room temperature (˜20° C.) for five minutes, 2.7 g. of anhydrous aluminum chloride was added to the mixture in one full portion with the aid of vigorous agitation. The resulting reaction mixture was then refluxed for a period of 15 minutes. At the end of this time, the spent mixture was poured into ice water in order to decompose the aluminum chloride, neutralized with sodium bicarbonate and extracted with ethyl acetate. After drying the organic extract over anhydrous magnesium sulfate, the solvent was removed in vacuo and the residue crystallized from ethyl acetate to afford 1.25 g. (50%) of pure 1-(3-pyridylmethyl)-5-fluoroindoline-2,3-dione.
A mixture consisting of 1.024 g. of 1-(3-pyridylmethyl)-5-fluoroindoline-2,3-dione, 390 mg. of potassium cyanide and 1.86 g. of powdered ammonium carbonate in 40 ml. of 50% aqueous methanol was heated in an oil both at 80° C. for a period of 20 minutes. At the end of this time, the spent reaction mixture was cooled in an ice bath, acidified with glacial acetic acid and diluted with additional water. After extracting the resulting aqueous solution with ethyl acetate, there were obtained several organic extracts that were later combined and suesequently dried over anhydrous magnesium sulfate to give a clear solution. Upon removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was ultimately obtained a residual material that was later crystallized from ethyl acetate to afford 700 mg. (43%) of pure 1'-(3-pyridylmethyl)-5'-fluorospiro-[imidazolidine-4,3'-indoline]-2,2',5-trione. Recrystallization from methanol in the presence of activated carbon then gave an analytically pure sample, m.p. 202° C.(decomp.). The pure product was further characterized by means of mass spectroscopy and nuclear magnetic resonance data.
EXAMPLE 4
A solution consisting of 2.0256 g. (0.01 mole) of 2,4-dinitrochlorobenzene and 2.384 g. (0.014 mole) of sodio-ethyl hydantoin-5-carboxylate (the product of Preparation A) dissolved in 10 ml. of dimethylformamide was allowed to stand at room temperature (˜20° C.) for a period of ca. 0.5-1.0 hour. Upon completion of this step, the spent reaction mixture was diluted with 50 ml. of water and extracted with two-25 ml. portions of ethyl acetate. The separated organic extracts were then combined and subsequently dried over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was ultimately obtained pure ethyl 5-(2,4-dinitrophenyl)hydantoin-5-carboxylate as the desired product.
A solution consisting of 0.3142 g. (0.001 mole) the above intermediate dissolved in 50 ml. of 50% aqueous ethanol was then brought to a rapid reflux, followed by the addition of 0.3351 g. (0.006 mole) of iron powder and 1 drop of concentrated hydrochloric acid to the stirred mixture. The resulting reaction mixture was then stirred mechanically for a period of ca. 0.5-1.0 hour. Upon completion of this step, the spent reaction mixture was neutralized with saturated aqueous sodium bicarbonate solution and the solvents were thereafter evaporated from the neutralized solution. In this manner, there was ultimately obtained pure 6'-amino-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione (m.p.>275° C.).
When the reaction was repeated using 2.63 g. of pure ethyl 5-(2,4-dinitrophenyl)hydantoin-5-carboxylate as starting material and with the aid of mechanical stirring for a period of three hours, the yield of the desired final product amounted to 1.5 g. (77%). The pure product was further characterized by means of mass spectroscopy and nuclear magnetic resonance data.
EXAMPLE 5
A solution consisting of 639.2 mg. (0.00403 mole) of 3-nitro-4-chloropyridine (the product of Preparation B) and 1.0288 g. (0.0053 mole) of sodio-ethyl hydantoin-5-carboxylate (the product of Preparation A) dissolved in 10 ml. of dimethylformamide was allowed to stand at room temperature (˜20° C.) overnight for a period of approximately 16 hours with the aid of mechanical stirring. Upon completion of this step, the solvent was evaporated from the mixture and the crude residual material was thereafter dried under a high vacuum and eventually crystallized from methylene chloride to afford 525 mg. of pure ethyl 5-(3-nitro-4-pyridyl)hydantoin-5-carboxylate, m.p. 203.5°-204.5° C.
When the reaction was repeated using 2.35 g. of 3-nitro-4-chloropyridine as starting material and 3.74 g. of sodio-ethyl hydantoin-5-carboxylate as the alkylating agent, the yield of pure product obtained amounted to 3.83 g. (88.3%).
A mixture consisting of 158.5 mg. (0.00054 mole) of ethyl 5-(3-nitro-4-pyridyl)hydantoin-5-carboxylate, 335.1 mg. of iron powder and 5 ml. of glacial acetic acid was heated to 100° C. and then cooled to ca. 65° C. The reaction was complete in approximately 10-15 minutes. Upon completion of this step, the spent reaction mixture was filtered thru filter-cel in order to remove the unwanted solids and the resulting filtrate was subsequently evaporated under reduced pressure to finally afford pure spiro-[imidazolidine-4,3'-(6-azaindoline)]-2,2',5-trione as the desired final product. The yield of pure material melting at 265° C. (decomp.) amounted to 80 mg. (68%). The pure product was further characterized by means of mass spectroscopy and nuclear magnetic resonance data.
EXAMPLE 6
The following spiro-oxindole imidazolidinedione final products of Examples 1-5, respectively, were tested at a concentration level of 10 -6 M for their ability to reduce or inhibit aldose reductase enzyme activity via the procedure of S. Hayman et al., as described in the Journal of Biological Chemistry, Vol. 240, p. 877 (1965) and as modified by K. Sestanj et al. in U.S. Pat. No. 3,821,383. In every case, the substrate employed was partially purified aldose reductase enzyme obtained from calf lens. The results obtained with each compound are expressed below in terms of their percent inhibition of enzyme activity (%) with respect to the particular concentration level chosen (10 -6 M):
______________________________________ % InhibitionCompound at 10.sup.-6 M______________________________________Product of Example 1 72Product of Example 2 81Product of Example 3 71Product of Example 4 27Product of Example 5 49______________________________________
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A series of novel spiro-oxindole imidazolidinedione derivatives have been prepared, including their pharmaceutically acceptable salts. These compounds are useful in therapy as aldose reductose inhibitors for the control of certain chronic diabetic complications. Preferred compounds include 6'-amino-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 5'-chloro-7'-aminospiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 1'-(3-pyridylmethyl)-5'-fluoro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione, 1'-(3-pyridylmethyl)-5',7'-dichloro-spiro-[imidazolidine-4,3'-indoline]-2,2',5-trione and spiro-[imidazolidine-4,3'-(6-azaindoline)]-2,2',5-trione. Methods for preparing these compounds from known starting materials are provided.
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FIELD OF THE INVENTION
The present invention relates generally to a picture hanging device, and more specifically relates to a device for accurately and precisely positioning a picture, mirror, or the like on a retention member or retention members engaged to a wall or like surface.
BACKGROUND OF THE INVENTION
The art of hanging a picture, mirror, or the like can be a tedious process. A retention member or retention members must be placed on a wall at a desired height and then the picture, mirror, or the like must be correctly positioned on the retention member. Many pictures and mirrors either contain a hanging wire or hanging hook on the rear of the picture or mirror for positioning the picture or mirror on the retention member. The act of positioning the hanging wire or hanging hook correctly on the retention member can be challenging. Additionally, the act of straightening the picture or mirror while it is engaged to the retention member can be equally challenging.
There is a need for a device that easily allows a user to position the hanging wire or hanging hook of a mirror or picture on a retention member positioned on a wall. There is also a need for a device that easily allows a user to accurately align the picture or mirror on the retention member.
BRIEF SUMMARY OF THE INVENTION
According to an embodiment of the invention, the present invention is a picture hanging device for mounting a picture to a retention member engaged to a wall. The picture hanging device includes a tube having a top portion and a bottom portion, a bottom portion of the tube that is designed to receive a retention member mounted to a wall, and the top portion of the tube extends into the air for correctly aligning the picture on the retention member. The hanging mechanism is engaged to the picture and is positioned around the tube and is slid down the tube for engagement to the retention member and the tube is positioned within the center of the picture for correctly aligning the picture on the retention member.
According to another embodiment of the present invention, the tube is generally cylindrical.
According to yet another embodiment of the present invention, the top portion of the tube is crimped, closed-in, or flattened.
According to yet another embodiment of the present invention, the tube is composed of plastic.
According to yet another embodiment of the present invention, the retention member has an upper portion that is bent in upon itself and has a bore extending therethrough.
According to yet another embodiment of the present invention, a method for hanging a picture that includes providing a retention member, a nail, a picture having a hanging mechanism, and a tube having a top portion and a bottom portion. The retention member is placed on the wall and the retention member is attached to the wall using the nail. The tube is engaged to the bottom portion of the retention member, the hanging mechanism of the picture is placed over the tube, and the hanging mechanism is slid down the tube until the hanging mechanism is engaged to the retention member.
According to yet another embodiment of the present invention, a kit of parts for hanging a picture that includes at least one retention member, at least one nail and at least one tube for engaging the retention member.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is illustrated and described herein with reference to the various drawings, in which like reference numbers denote like method steps and/or system components, respectively, and in which:
FIG. 1 is a perspective view of the picture hanging device;
FIG. 2 is another perspective view of the picture hanging device;
FIG. 3 is a perspective view of the picture hanging device mounted to a wall and a picture about to be installed on the picture hanging device;
FIG. 4 is a perspective view of a picture inserted on the picture hanging device;
FIG. 5 is a side view of a picture inserted on the picture hanging device;
FIG. 6 is a perspective view of the tube being removed from the retention member of the picture hanging device; and
FIG. 7 is a top view of the tube of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now specifically to the drawings, a picture hanging device is illustrated in FIGS. 1 and 2 and is shown generally at reference numeral 10 . The device 10 includes a retention member 12 , a nail 14 , and a tube 16 . The tube 16 is a generally cylindrical tube that has a top portion 18 and a bottom portion 20 . The retention member 12 has an upper portion and a lower portion. The lower portion of the retention member 12 is angled upward to receive a hanging mechanism of a picture 24 . The upper portion of the retention member 12 is designed to receive the nail 14 and the lower portion of the retention member 12 is designed to receive the bottom portion 20 of the tube 16 .
The retention member 12 is designed to be engaged to a wall 22 or other like structure. Preferably, the retention member 12 is a standard picture bracket that is one, solid piece. The upper portion of the retention member 12 is bent in upon itself and has a bore extending therethrough. The bore is designed to receive the nail 14 for engaging the retention member 12 to the wall 22 .
In addition to receiving the hanging mechanism of a picture 24 , the lower portion of the retention member 12 also receives the bottom portion 20 of the tube 16 . When the tube 16 is positioned on the lower portion of the retention member 12 , the tube 16 extends upward at an angle. The tube 16 is designed to receive the hanging mechanism of a picture 24 for engaging the hanging mechanism to the lower portion of the retention member 12 .
Although the tube 16 is preferably generally cylindrical, it may be any shape as required by the user. It also should be noted that the tube 16 may have any length, width, or diameter that is desired by the user. However, it is preferred that the length of the tube 16 is a length that would extend above the top of a picture 24 , when the hanging mechanism of the picture 24 is engaged to the lower portion of the retention member 12 . Preferably, the tube 16 extends above the top of the picture 24 a length of about 1 inch or more. However, a person of ordinary skill in the art will recognize that the tube 16 can extend any distance above the top of the picture 24 as desired by the user.
The term hanging mechanism of the picture 24 is generally a term meaning the mechanism or device located on the picture 24 for suspending the picture 24 from the retention member 12 . Generally, the hanging mechanism consists of a hook, a wire, a string, a nylon string, or the like that is positioned on the back of the picture 24 . It should also be noted that picture may be interchanged with a minor, or other like structure that a user may desire to hang from the wall 22 or other support structure.
As illustrated in FIG. 7 , the top portion 18 of the tube 16 is closed-in on itself and has a center point 26 . In other words, the top portion 18 is flattened or crimped and both sides are engaged to one another. The tube 16 has a constant inner and outer circumference. However, one of ordinary in the art will recognize that the inner and outer circumference of the tube 16 may have differing or varying inner and outer circumferences based upon the desires of the user. It will be noted that the top portion 18 may have any shape that is desired by the user.
During use, the retention member 12 is engaged to the wall 22 with the nail 14 , as illustrated in FIGS. 3 , 4 , and 5 . The bottom portion 20 of the tube 16 is engaged to the lower portion of the retention member 12 . Preferably, the tube 16 is hollow and the lower portion of the retention member 12 is inserted into the bottom portion 20 of the tube 16 and is retained therein by friction fit. The top portion 18 of the tube 16 is closed-in or crimped and the closed-in or crimped side is positioned parallel to the wall 22 .
The hanging mechanism of the picture 24 is positioned over or around the tube 16 , as illustrated in FIGS. 4 and 5 . In other words, the tube 16 is positioned between the hanging mechanism and the picture 24 with the hanging mechanism positioned around the tube 16 when the hanging mechanism is a wire or the like. If the hanging mechanism is a hook or the like, the tube 16 is positioned within the hook with the hook around the tube 16 . The hanging mechanism and picture 24 is slid down the tube, until the hanging mechanism is engaged to the lower portion of the retention member 12 . A user will be able to determine whether the tube 16 is positioned between the hanging mechanism and the picture (or within the hanging mechanism should the hanging mechanism be a hook or the like) by moving the picture 24 towards and away from the wall 22 because the tube 16 will move in conjunction with the picture 24 . When the hanging mechanism is engaged to the retention member 12 , the tube 16 extends above the picture 24 , as shown in FIG. 4 .
Once the hanging mechanism is engaged to the retention member 12 , the user may utilize a measuring tape to determine the center portion of the picture 24 . This center portion may be marked utilizing a pencil, tape, or another marking device or mechanism that can be removed easily from the picture 24 without leaving a mark. The picture 24 can be moved to the left or right to ensure the center of the picture 24 is aligned with the tube 16 . The tube 16 may also include an indicator or mark 26 that indicates the center of the tube 16 for enabling the user to position the center of the picture 24 with the center of the tube 16 . Further, the user may apply a level to ensure the picture is hanging level. Afterwards, the tube 16 is disengaged from the retention member 12 by pulling the tube 16 upwards, as illustrated in FIG. 6 .
The retention member 12 may also be a self-adhering plastic bracket, such as the Command™ line of brackets or hooks from the 3M Corporation. The retention member 12 may also be a cloth bracket, a nail, or the like. The retention member 12 may be anything that is engaged to a wall that receives a picture or mirror and holds the picture or mirror on the wall. The retention member 12 may be a standard picture hanging bracket that one of ordinary skill in the art would understand and purchase. In another embodiment, the retention member 12 is a metal picture bracket as illustrated in FIGS. 1 and 2 .
A kit of goods is disclosed herein. The kit may include a retention member 12 , a nail 14 , and a tube 16 for accurately and efficiently hanging a picture 24 . The kit may be situated in a bag, box or other suitable packaging for retaining the items in the kit. The kit may also include a hanger, a bore or the like for hanging the kit on a display shelf. Additionally, the kit may include a hanging mechanism, such as a wire, hook, eye hook, string, nylon string, a nail, at least two nails, a plurality of nails, or the like that would be utilized to hang a picture 24 , mirror or the like. The kit may also include more than one retention member 12 , more than one nail 14 , and more than one tube 16 . The kit may also include varying sizes of retention members 12 , nails 14 , and tubes 16 . The kit may also include a set of instructions for using the picture hanging device 10 .
It will be known by one of ordinary skill in the art to have a tube 16 of multiple sizes and dimensions, depending upon the uses by the user. The tube 16 may be composed of plastic, but could also be composed of a material other than plastic, such as nylon, rubber, paper product, plastic composites or the like, that has similar rigidity and/or flexibility, is light weight, and has similar durability as plastic.
Although the present invention has been illustrated and described herein with reference to preferred embodiments and specific examples thereof, it will be readily apparent to those of ordinary skill in the art that other embodiments and examples may perform similar functions and/or achieve like results. All such equivalent embodiments and examples are within the spirit and scope of the present invention and are intended to be covered by the following claims.
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The present invention provides methods and systems for a picture hanging device for mounting a picture to a retention member engaged to a wall that includes a tube having a top portion and a bottom portion, the bottom portion of the tube is designed to receive a retention member mounted to a wall, the top portion of the tube extends into the air for correctly aligning the picture on the retention member, whereby a hanging mechanism engaged to the picture is positioned about the tube and is slide down the tube for engagement to the retention member and the tube is positioned within the center of the picture for correctly aligning the picture on the retention member.
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